environmental quality validation of analytical chemistry
DESCRIPTION
An Engineering Manual Published by Army Corps of EngieersTRANSCRIPT
CEMP
MemorandumNo.
200-1-1
Department of the ArmyU.S. Army Corps of Engineers
Washington, DC 20314-1000
EM 200-1-1
1 Jul 94
Environmental Quality
VALIDATION OF ANALYTICAL CHEMISTRY
Distribution Restriction StatementApproved for public release; distribution is unlimited.
CEMP-RTCECW-E
DEPARTMENT OF THE ARMYU.S. Army Corps of EngineersWashington, DC 20314-1000
EM 200-1-1
ManualNo. 200-1-1
1 July 1994
Environmental QualityVALIDATION OF ANALYTICAL CHEMISTRY LABORATORIES
Table of Contents
Subject Paragraph Page
CHAPTER 1.
1 - 1 1 - 11 - 2 1 - 11 - 3 1 - 11 - 4 1 - 11 - 5 1 - 21 - 6 1 - 81 - 7 1 - 8
CHAPTER 2.
2 - 1 2 - 12 - 1 2 - 12 - 3 2 - 52 - 4 2 - 1 52 - 5 2 - 2 3
Section II. 2 - 6 2 - 2 62 - 7 2 - 2 72 - 8 2 - 2 8
Section III.
INTRODUCTION
Purpose-------------------------Applicability-------------------References----------------------Overview-----------------------Responsibilities---------------Expenses and, Funding------------Effective Date and Amendments----
PROCEDURES FOR COMMERCIAL LABORATORIES
Validation ProceduresInitiation Procedures-----------Implementation Procedures-------Implementation Procedure Steps--Approval Procedures-------------Inspection/Evaluation Report----
Revalidation, Termination, and AppealRevalidation-------------------Termination--------------------Appeal------------------------
Information ManagementRecord Files--------------------Database------------------------
2 - 9 2 - 3 12-10 2-31
CHAPTER 3. PROCEDURES FOR USACE DIVISION LABORATORIES
USACE Division Laboratories-----Contract QA Laboratories--------
3 - 1 3 - 13 - 2 3 - 2
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Page
APPENDIX A
APPENDIX B
Appendices
REFERENCE A-1
INTRODUCTION TO THE U.S. ARMY CORPSOF ENGINEERS VALIDATION PROGRAM FORCOMMERCIAL ANALYTICAL CHEMISTRYLABORATORIES
B-1
APPENDIX C C-1
APPENDIX D D-1
APPENDIX E E-1
APPENDIX F F-1
APPENDIX G G-1
APPENDIX H H-1
APPENDIX I
APPENDIX J
APPENDIX K
APPENDIX L
INFORMATION FOR COMMERCIAL ANALYTICALCHEMISTRY LABORATORIES UNDERGOINGVALIDATION BY THE U.S. ARMY CORPS OFENGINEERS
GUIDELINES FOR ANALYZING AND REPORTINGPERFORMANCE EVALUATION SAMPLES FROMTHE U.S. ARMY CORPS OF ENGINEERS
PRELIMINARY QUESTIONNAIRE FOR THE U.S.ARMY CORPS OF ENGINEERS VALIDATIONPROGRAM FOR ANALYTICAL CHEMISTRYLABORATORIES
ANALYTICAL PARAMETERS, METHODS, AND FEESCHEDULE FOR PERFORMANCE EVALUATIONSAMPLES FROM THE U.S. ARMY CORPSOF ENGINEERS
GUIDANCE FOR PREPARATION, HANDLING, ANDVALIDATION OF PERFORMANCE EVALUATIONSAMPLES
GUIDELINES AND CRITERIA FOR ON-SITEINSPECTION OF COMMERCIAL ANALYTICALCHEMISTRY LABORATORIES
CHECKLISTS FOR ON-SITE LABORATORYINSPECTIONS
I-1
SHORT CHECKLISTS FOR ON-SITE LABORATORYINSPECTIONS
J-1
SAMPLE RECORD OF THE LABORATORYVALIDATION DATABASE
K-1
SUPPLEMENTAL QUESTIONNAIRE FOR VALIDATIONOF USACE DIVISION LABORATORIES
L-1
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Appendices Page
APPENDIX M LIST OF ABBREVIATIONS, ACRONYMS, FORMULAS M-1SYMBOLS, NUMBERS, AND TERMS
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Figures
FIGURE 1-1
Page
1-3/1-4
FIGURE 2-1
FIGURE 2-2
FIGURE 2-3
FIGURE 2-4
FIGURE C-1
FIGURE C-2
FIGURE H-1
FIGURE H-2
FIGURE H-3
FIGURE H-4
FIGURE K-1
FLOW DIAGRAM OF COMMERCIAL LABORATORYVALIDATION PROCEDURES
LABORATORY EVALUATION REQUEST FORMAT
ON-SITE LABORATORY INSPECTION SUMMARY
VALIDATION REVIEW MEETING SUMMARY
LABORATORY PERFORMANCE PROBLEM REPORT
SAMPLE LABORATORY EVALUATION REQUEST
FLOW DIAGRAM OF COMMERCIAL LABORATORYVALIDATION PROCEDURES
PRE-INSPECTION CHECKLIST
ENTRANCE INTERVIEW CHECKLIST
EXIT INTERVIEW CHECKLIST
COOLER RECEIPT CHECKLIST
SAMPLE RECORD OF THE LABORATORYVALIDATION DATABASE
2-2
2-16/2-18
2-20/2-21
2-29/2-30
C-3
C-9/C-10
H-3/H-4
H-5/H-6
H-9
H-12
K-2/K-6
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Tables Page
TABLE 2-1 SAMPLE FORMAT FOR INSPECTION REPORT 2-24/2-25
v
CEMP-RTCECW-E
ManualNo. 200-1-1
DEPARTMENT OF THE ARMYU.S. Army Corps of EngineersWashington, DC 20314-1000
EM 200-1-1
1 July 1994
Environmental QualityVALIDATION OF ANALYTICAL CHEMISTRY LABORATORIES
1. Purpose. This manual implements the USACE policy andrequirements on validation of analytical chemistry laboratoriesas prescribed in the USACE Engineer Regulation 1110-1-263. Thismanual provides detailed procedures, guidance, and criteria forvalidation of commercial and USACE Division analytical chemistrylaboratories. Laboratory validation is required to ensure thatanalytical chemistry laboratories meet the minimum requirementsof the USACE quality assurance/quality control program thatfacilitates the generation of chemical data of known andacceptable quality.
2. Applicability. This manual applies to HQUSACE/OCE elements,major subordinate commands, districts, laboratories, and separatefield operating activities having responsibility for in-house orcontracted projects involving chemical measurements of wasteand/or environmental samples. This includes, but is not limitedto, execution of the following programs: Defense EnvironmentalRestoration Program; Base Realignment and Closure; InstallationEnvironmental Compliance; Military Construction; Superfund; CivilWorks; and Department of Energy.
FOR THE COMMANDER:
WILLIAM D. BROWNColonel, Corps of EngineersChief of Staff
EM 200-1-11 Jul 94
CHAPTER 1
INTRODUCTION
1-1. Purpose. This manual implements policy and providesguidance, procedures, and criteria for the validation ofcommercial and U.S. Army Corps of Engineers (USACE) divisionanalytical chemistry laboratories. Laboratory validation isrequired to ensure that analytical chemistry laboratories meetthe USACE Chemical Data Quality Management (CDQM) requirements asprescribed in the USACE Engineer Regulation (ER) 1110-1-263 forgeneration of chemical data of sufficient quality to meetintended usages within the project.
1-2. Applicability.
a. This manual applies to HQUSACE/OCE elements, majorsubordinate commands, districts, laboratories, and separate fieldoperating activities (FOA) having responsibility for in-house orcontracted projects involving chemical measurements of wasteand/or environmental samples. This includes, but is not limitedto, execution of the following programs: Defense EnvironmentalRestoration Program (DERP); Base Realignment and Closure (BRAC);Installation Environmental Compliance; Military Construction;Superfund; Civil Works; and Department of Energy (DOE).
b. This manual and its prescribed laboratory validationprocess also apply to the validation of USACE divisionlaboratories with minor modifications. USACE divisionlaboratories and commercial laboratories, which perform the QAfunction, shall be evaluated under more stringent criteria thancommercial primary project laboratories.
1.3 References.
a. ER 1110-1-263, Chemical Data Quality Management forHazardous Waste Remedial Activities.
b. “Hazardous, Toxic & Radioactive Waste (HTRW) - PolicyGuidance on Validation of Commercial Analytical ChemistryLaboratories”, CEMP-RT memorandum, (See Appendix A.)
1-4. Overview.
a. The purpose of laboratory validation is to ensure thatanalytical chemistry laboratories meet the minimum requirementsof the USACE quality assurance/quality control (QA/QC) programthat facilitates the generation of chemical data of known and
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acceptable quality. Objectives of commercial laboratoryvalidation are: to communicate USACE QA/QC requirements; toverify that commercial laboratories are performing specifiedanalytical methods with no unacceptable deviations; and to verifythese laboratories meet USACE QA/QC requirements prior to sampleanalysis. In general, all commercial laboratories that supportUSACE HTRW response activities shall obtain a USACE laboratoryvalidation prior to field studies or sample analyses and shallmaintain the validated status throughout the response activities.Appendix B is an introduction to laboratory validation proceduresfor commercial laboratories that express interest in USACElaboratory validation but have not been tasked to executechemical analysis in support of USACE HTRW response activities.
b. The USACE laboratory validation process consists ofthree major sequential steps: (1) review of generalqualifications, (2) analysis of performance evaluation (PE)samples, and (3) on-site laboratory inspection. The validationprovides a parameter, method, and matrix-specific approval. Theperiod of validation is 18 months. For each new contract/project/task order (hereafter referred to as the contract orproject) awarded to a commercial laboratory after its initialvalidation, a project-specific evaluation of the laboratory’scapability and past performance is still required. A simplifiedflow diagram is shown in Figure 1-1 to show the major events in alaboratory validation process.
c. Abbreviations, acronyms, formulas, symbols, numbers,and terms used in this manual are defined in Appendix M.
1-5. Responsibilities. The USACE HTRW Mandatory Center ofExpertise (HTRW MCX) located at the Missouri River Division inOmaha, Nebraska is tasked by HQUSACE with the operation andmanagement responsibilities for this centralized laboratoryvalidation program. A Laboratory Validation Committee (hereafterreferred to as the Committee), composed of staff members from theChemistry Branch of the HTRW MCX, is generally responsible forall aspects of the USACE HTRW laboratory validation program. Oneof the Committee members is designated as the LaboratoryValidation Coordinator (hereafter referred to as the Coordinator)who is the point-of-contact for the Committee and is responsiblefor coordination and execution of the daily activities of thelaboratory validation process. The Committee will meet as neededand is primarily responsible for proposing policy and makingultimate decisions with regard to laboratory-specific validationstatus. Besides the Committee, a number of other parties,including government agencies and private contractors, areinvolved in the USACE HTRW laboratory validation process.
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Figure 1-1. Flow Diagram of Commercial Laboratory ValidationProcedures
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Figure 1-1. Flow Diagram of Commercial Laboratory ValidationProcedures (continued)
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Details on the responsibilities of all involved parties areaddressed below.
a. HQUSACE:
(1) Actively performs oversight for the USACE HTRWlaboratory validation program.
(2) Administers approval authority for the policies andprocedures of the USACE HTRW laboratory validation program.
b. The Committee, HTRW MCX:
(1) Is responsible for all aspects of the USACE HTRWlaboratory validation program including planning, programming,execution, budget, and management.
(2) Coordinates laboratory validation activities andprovides liaison with various government agencies and privatesector parties on laboratory validation issues. Ensures alllaboratory evaluations and/or validations are successfullycompleted in a timely manner.
(3) Identifies the PE samples and analytical methodsrequired for each laboratory validation. Assures that PE samplesuppliers are provided with proper information to prepare andship PE samples.
(4) Monitors the performance of PE sample suppliersthrough review of their most recent analytical results of anyproficiency testing programs and all QA/QC data associated withthe verification of PE samples on a quarterly basis. Alsoconducts on-site audits of PE sample suppliers on a regularbasis.
(5) Reviews the qualification documents of commerciallaboratories, evaluates PE sample results, and conducts ordelegates on-site laboratory inspections.
(6) Trains USACE personnel to perform on-site laboratoryinspections. Monitors the inspector's performance to ensure thatconsistent inspection approach and results of high quality arecarried out within the USACE HTRW laboratory validation program.
(7) Decides the pass/fail status for each step of thelaboratory validation process, additional work required forcompletion of laboratory validation, or the appropriate time toterminate a laboratory validation process or to revoke an activevalidation status.
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(8) Prepares and distributes laboratory inspection andevaluation reports.
(9) Establishes and maintains a performance database forPE sample results from commercial laboratories. Statisticallyevaluates PE sample results to adjust or update the acceptancelimits for PE sample analysis.
(10) Provides technical assistance to USACE TechnicalManagers/Contracting Officer Representatives (TM/CORs) to resolveproblematic issues on laboratory validation and performance.
(11) Upon request, provides technical assistance to USACETM/CORs in selection of contract laboratories prior to nominationfor validation to support USACE HTRW response activities.
(12) Provides liaison with various government agencies andprivate sector parties on national laboratory “accreditation”programs. Revises the USACE HTRW laboratory validation programas needed to meet Federal and/or State regulatory requirements.
c. PE Sample Suppliers (including Waterways ExperimentStation and Missouri River Division Laboratory):
(1) Prepare or purchase PE samples of high quality.Verify the PE samples prior to use. Maintain proper in-housedocumentation on PE sample preparation and verification per theU.S. Environmental Protection Agency (USEPA) and the USACEguidance. Arrange for multiple laboratory analyses of PE samplesand statistically evaluate PE sample results to establish initialacceptance limits.
(2) Supply PE samples to candidate laboratories withovernight express delivery services. Ensure all PE samples arepacked and shipped according to the USEPA, USACE, and theDepartment of Transportation (DOT) regulations and guidelines.Maintain a full chain-of-custody for each shipment of PE samples.Generate and send a sample-specific instruction letter for PEsample analysis with each PE sample shipment. Notify theCommittee of any problems with PE sample preparation,verification, and shipment immediately.
(3) Provide technical assistance in resolving problemswith PE sample analysis to the Committee and commerciallaboratories. Keep the Committee informed of any major problemsor issues on PE sample analysis.
(4) Evaluate PE sample results based on statisticallyestablished confidence limits for precision and accuracy.
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Prepare and send written evaluation reports on PE sample resultsto the Committee within the required time frame. Provide theCommittee with verbal reports on PE sample results, if a quickanswer is needed.
(5) Ensure the availability and readiness of multiple setsof PE samples of different constituents and/or concentrations.Avoid sending same PE samples to same laboratory twice, includingaffiliated laboratories belonging to same parent corporation whenpossible.
(6) Actively participate in proficiency testing programsof State, Federal, and/or private firms. Provide the Committeewith most recent proficiency testing results on a quarterlybasis.
D. USACE TM/CORs:
(1) Submit a fully completed format of “Request forEvaluation of Commercial Laboratory” or an equivalent for eachlaboratory-project case to the Committee in a timely manner.
(2) Inform the Committee of any major changes in projectrequirements related to chemical analyses in a timely manner.
(3) Notify the Committee immediately to terminatevalidation efforts if a commercial laboratory undergoing thevalidation process is replaced by another commercial laboratory.
(4) Provide funding, if appropriate, for laboratoryvalidation.
(5) Inform the Committee of any performance problems withsample analysis.
e. Prime Contractors (including Architect EngineeringFirms, Construction Contractors, and Government Agencies):
(1) Select a subcontract laboratory and notify the USACETM/COR early.
(2) Provide a subcontract laboratory a copy of the finalChemical Data Acquisition Plan (CDAP) for information prior tolaboratory inspection. If a CDAP is not available prior to theinspection, as a minimum, provide a copy of the Scope ofServices.
f. Analytical Chemistry Laboratories (including Commercialand Government Laboratories):
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(1) Respond to the Committee's requirements within therequired time frame.
(2) Follow instructions to analyze and report PE sampleresults.
(3) Inform the Committee immediately of any major changeson the laboratory’s facility, instruments, or key technical staffduring the laboratory's 18-month validation period.
1-6. Expenses and Funding.
In general, “billable” items related to specific laboratoryvalidations include: travel and per diem for on-site inspectionplus time and labor spent on review of documents, inspection oflaboratory, and preparation of inspection report and onpreparation, testing, and shipment of PE samples. Depending onthe program, customer billable items are funded on a yearlyprogram basis or project specifically. Mixed funding for aparticular validation is used if appropriate. Verbalcommunication with the USACE TM/COR will cover the topic offunding for a particular request. For projects under programs ormissions without yearly program funds available at the HTRW MCX,the USACE TM/CORs who request the validation shall be responsiblefor the expense of laboratory validation that is approximately$2,500 per laboratory validated. The cost of laboratoryvalidation may be adjusted as needed, based on updated expenses.
1-7. Effective Date and Amendments.
a. This manual is effective upon approval by the HQUSACEand shall remain in effect until superseded or terminated.
b. These procedures may be modified, revised, or amendedupon approval by the HQUSACE.
c. This manual and any future revisions or amendmentsshall be distributed by the HQUSACE.
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CHAPTER 2
PROCEDURES FOR COMMERCIAL LABORATORIES
Section I. Validation Procedures
2-1. Initiation Procedures. A laboratory validation will beinitiated after a commercial laboratory successfully bids acontract to support USACE HTRW response activities. A writtenrequest from a USACE TM/COR to the Coordinator initiates thelaboratory validation process. A request format as shown inFigure 2-1 or a memorandum with all information contained inFigure 2-1 may be submitted to the Coordinator by mail orfacsimile, as follows:
U.S. Army Corps of EngineersATTN: CEMRD-ED-EC (Laboratory Validation Coordinator)HTRW Mandatory Center of ExpertiseMissouri River Division12565 West Center RoadOmaha, Nebraska 68144-3869
Voice: (402) 221-7494FAX : (402) 221-7403
2-2. Implementation Procedures.
a. Upon receiving the laboratory evaluation request, theCoordinator will immediately check the laboratory’s currentvalidation status. If the laboratory is currently validated bythe USACE for all project-required analytical parameters and hasno performance problems noted, the Coordinator will notify theUSACE TM/COR in writing of the Committee’s approval within tenworking days. If the laboratory is not currently validated bythe USACE for all project-required analytical parameters, theCoordinator will immediately notify the USACE TM/COR by phone andinitiate the laboratory validation process.
b. The laboratory validation process may take up to 12weeks; therefore, the primary contractor and/or the USACE TM/CORshould plan the project schedule to allow adequate time forlaboratory validation and the USACE TM/COR should submit arequest for evaluation to the Coordinator as early as possible.The Committee shall also make a concerted effort to ensure thatthe validation process is completed within the time framerequired by the project. Unless projects require specializedchemical analyses or a quick turnaround of large number ofsamples, normally a minimal number of commercial laboratoriesshould be used for each contract and be requested for validation.
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TO: CEMRD-ED-EC
SUBJECT: REQUEST
Project Name:
FROM:____________________
FOR EVALUATION OF COMMERCIAL
DATE:____/_____/____
LABORATORY
Location:__________________________________________ State:_______Contract No:___________________ Type: POL TANK REMOVAL:___HTRW:___
Program: SF:___ FUDS :____ IRP:____ AF(ACC):_____ OTHER:_____________Phase: PA/SI:____RI/SI:____ RD:____RA:____ RFA :____ RFI:____ CMS:____
Approximate Sampling Dates:______________________________Project-Specific Sample Turnaround Time:___________________
USACE Technical Manager:__________________________________________Address:_________________________________________________________
Phone:___________________________ FAX:_________________________
A-E/Contractor:________________________________________ State:________Lab Name:__________________________________________________________Address:_________________________________________________________
POC:_________________________________________________________Phone:__________________________ FAX:_________________________
Required analytical parameters, methods, and approximate numberof samples to be taken for above project.
No. of No. ofPARAMETERS & METHODS LIQUID SAMPLES SOLID SAMPLES
State or other laboratory certifications that will be requiredfor this project:_________________________________________________
Note: If the laboratory is planning to subcontract any samples to another laboratory or location, all of
these laboratories shall be evaluated separately. This format should be sent for verification of
laboratory status regardless of expiration date on the l ist of validated laboratories.
Figure 2-1 Laboratory Evaluation Request Format
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c. Although three major sequential steps are involved inthe laboratory validation process, the actual steps required foreach laboratory, as determined by the Committee, may bedifferent, based on the following guidelines:
(1) For commercial laboratories that have never beenvalidated under the USACE HTRW Program: A full, three-steplaboratory validation process conducted by the Committeerepresentatives is required.
(2) For commercial laboratories that have expiredlaboratory validation under the USACE HTRW Program: When thenext contract is awarded to support USACE HTRW responseactivities, a revalidation will be required. After consideringthe use of the laboratory and the laboratory’s previousperformance, the Committee will determine which of the threesteps will apply to the revalidation process.
(3) For commercial laboratories that are currentlyvalidated under the USACE HTRW Program: When the laboratoryobtains a new contract(s) to support USACE HTRW responseactivities during its validation period, the capability and pastperformance on USACE HTRW projects shall be verified by theCommittee. If different analytes and/or matrices are involved inthe new contract(s), the laboratory must pass additional PEsamples for those different analytes and/or matrices. If pastperformance has been satisfactory, the USACE TM/COR will benotified that no further actions are required and the laboratoryis validated for all parameters of the new contract(s);otherwise, a full laboratory validation might be required asdetermined by the Committee on a case-by-case basis.
(4) For commercial laboratories whose validations mightexpire while the laboratories are working on ongoing projects: Arevalidation will be required if a USACE TM/COR expects that anongoing project will extend more than six months beyond thevalidation expiration date. The Committee will determine whichvalidation steps are required for the revalidation process on acase-by-case basis. If the completion of an ongoing project isanticipated within six months after the expiration date, noactions are required.
(5) For on-site mobile laboratories: The same proceduresused for validation/revalidation of an off-site “fixed”commercial laboratory will apply to an on-site mobile laboratory.However, no PE samples will be sent to a mobile laboratory untilthe mobile laboratory is mobilized and settled down at theproject site. Due to the timing of PE sample analysis and thequick turnaround nature of mobile laboratory, the laboratory
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inspection for an on-site mobile laboratory can be coordinatedwith project schedule. The validation status of an on-sitemobile laboratory terminates if the laboratory moves to a newlocation prior to the validation expiration date. After anon-site mobile laboratory is mobilized to a new location, anotherfull laboratory validation is required. No laboratory validationis required for an on-site mobile laboratory that only performsfield screening analysis, i.e., Level II data quality.
(6) For commercial laboratories to be used for undergroundstorage tank removal projects:
(a) For projects involving removal of tanks, bothunderground storage tanks (USTs) and aboveground storage tanks(ASTs), that have been used only for storage of petroleum, oils,or lubricants (POL), there are two alternatives to the validationprocess. These two alternatives apply only to predesign samplingof UST organic phase contents and soil sampling during removal.They do not apply to investigations required by groundwatercontamination or extensive soil contamination.
Alternative 1: State certified laboratories may be usedwithout USACE validation, if the state considers itscertification to be applicable to UST removal. When thisalternative is selected, a document in the project file mustidentify the individual responsible for coordination with thestate.
Alternative 2: The HTRW MCX will conduct an abbreviatedlaboratory validation process if a USACE TM/COR submits a requestfor evaluation of commercial laboratory. The laboratory mustsubmit its qualification documents including laboratory qualitymanagement manual (LQMM) and standard operating procedures (SOP)for the required analyses to the Coordinator for review. If thelaboratory has been recently validated for the project-specificanalytical parameters and has no performance problems with USACEprojects, the laboratory may be exempted from PE sample analysis.However, if performance problems with the commercial laboratoriesare noted, a full laboratory validation by the Committeerepresentatives will be performed.
(b) If alternative 2 is selected, an on-site inspection bythe Committee representatives for POL UST/AST removal projects isgenerally exempted. The USACE division laboratory that serves asthe project QA laboratory, the geographic district, and/or FOAare encouraged to perform inspection per the protocols addressedin this manual. If inspections are not conducted by theCommittee representatives, the inspectors must be trained andcertified by the Committee prior to on-site inspections.
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The Committee shalland will be free toany time. The same
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be kept fully informed of these inspectionssend representative(s) to the inspections atinspection approach and checklists as
described in this manual shall also be used by the “non-Committeerepresentative” inspectors.
(c) A commercial laboratory validated for POL UST/ASTremoval projects may not be used to support other HTRW projectsunless a full laboratory validation is performed by the Committeerepresentatives. A full laboratory validation will be requiredfor a UST/AST site investigation if leaking tanks causegroundwater contamination or severe soil contamination. Forprojects involving removal of non-POL tanks that have containedHTRW substances or wastes, a full laboratory validation conductedby the Committee is required.
2-3. Implementation Procedure Steps. A full laboratoryvalidation involves three major sequential steps conducted by theCommittee representatives. Ordinarily, each step in the sequenceis completed before the subsequent step is initiated.
a. Step 1: Review of Qualification Documents.
(1) The Coordinator will inform a commercial laboratory byphone or mail of the upcoming laboratory validation and requestfor review copies of the laboratory's qualification documents,including generic LQMM and other appropriate documents such asSOPs, laboratory certificates, etc. The laboratory shall submitthe required documents within five working days of the request.If the laboratory does not have a LQMM, USACE will not pay forthe preparation of this document. The submittals should provideappropriate information (including personnel, facilities,instrumentation, SOPs, QA/QC policies, etc.) for the Committee toevaluate and assess the laboratory’s technical capabilities onthe project-required chemical analyses.
(2) Upon receiving the qualification documents, one of thecommittee members will be designated to compare the laboratory’sin-house technical capabilities with the project requirements.Within two working days, the designee will verbally convey theresults of this comparison to the Coordinator. If the comparisonidentifies deficiencies, the Coordinator or designee shall:immediately contact the laboratory to verify the deficiencies;coordinate any follow-up actions; and verbally notify the USACETM/COR of the problems. If deficiencies are verified, theCoordinator or designee shall present the findings to theCommittee and recommend termination of the validation. Uponapproval by the Committee, the Coordinator shall immediatelyissue a follow-up letter to notify the USACE TM/COR and the
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commercial laboratory of the problems, the Committee's decisionof termination of the validation process, and the need forselection of another laboratory. If it appears that thecapabilities of the laboratory are adequate to meet the projectrequirements, the Coordinator shall immediately mail thefollowing documents to the laboratory for information and action,and step 2 will be initiated.
- Information for Commercial Analytical ChemistryLaboratories Undergoing Validation by the U.S. ArmyCorps of Engineers (Appendix C),
- Guidelines for Analyzing and Reporting PerformanceEvaluation Samples from the U.S. Army Corps of Engineers(Appendix D), and
- Preliminary Questionnaire for the U.S. Army Corps ofEngineers Validation Program for Analytical Laboratories(Appendix E).
(3) The laboratory shall complete and return a copy of thecompleted preliminary questionnaire within ten working days fromthe date of receipt.
b. Step 2: Analysis of PE Samples.
(1) The Coordinator will arrange to have PE samples sentto the laboratory for analysis. Project-specific PE samples aremandatory and must be passed. In addition to project-specific PEsamples, the laboratory may volunteer for validation ofadditional parameters by requesting non-project-specific PEsamples. The cost for the first set of project-specific PEsamples will be covered by the USACE HTRW program managementfunds. However, for any additional sets or any non-project-specific PE samples, the laboratory will be responsible for theexpense of PE samples which ranges from $100 to $300 per method,per matrix, and per shipment. Appendix F shows the fee schedule,which is subject to annual review and adjustment without noticeto reflect currency value fluctuations or changes in programadministration costs, for PE samples available from the USACE. Acommercial laboratory is not reimbursed for costs involved in theanalysis of the PE samples.
(2) If a nonstandard analytical method or a modifiedstandard analytical method is required, the laboratory shallsubmit its in-house SOP and method validation data (includingmethod detection limits, precision, accuracy, QC limits,chromatograms, etc.) to the Coordinator for review and approval.PE samples for a nonstandard or a modified standard method will
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only be sent after the Committee has reviewed and approved themethod. PE samples for validation of a mobile laboratory shallonly be sent after the laboratory is mobilized to the projectsite and all instruments are calibrated. The Committee mayrequest instrument calibration data for review prior to shippingPE samples to a mobile laboratory.
(3) Analysis of PE Samples.
(a) In general, the PE samples are method- andmatrix-specific. A commercial laboratory may not subcontract PEsamples to another laboratory. A commercial laboratory must useproject-required analytical methods for analyses of allproject-specific PE samples unless otherwise instructed by theCoordinator. The sources of analytical methods usually requiredfor USACE HTRW projects, and therefore for the PE sampleanalysis, in a preferential order are as follows:
- Test Methods for Evaluating Solid Waste, SW-846 (ThirdEdition, Revision 0, September 1986; Revision 1, July1992; or the most recently promulgated revisions.)
- Statements of Work for Organics Analysis, InorganicsAnalysis, and Dioxin Analysis, (USEPA ContractLaboratory Program, Document Number OLM02.0, ILM03.0,DFLMO1.0, and the most recent revisions.)
- Methods for Chemical Analysis of Water and Wastes,EPA-600/4-79-020 (Revised March 1983 or the mostrecently promulgated revisions.)
- Methods for the Determination of Organic Compounds inDrinking Water, EPA-600/4-88/039 (December 1988 or themost recently promulgated revisions.)
- Other standard and published methods of the most recentversions from USEPA, American Society for Testing andMaterials (ASTM), American Public Health Association,American Water Works Association, Water PollutionControl Federation, United States Geological Survey(USGS), National Institute for Occupational Safety andHealth (NIOSH), Department of Energy (DOE), etc.
(b) The parameters and commonly required methods for PEsample analyses are listed in Appendix F. Any changes ormodifications in analytical methods for PE samples must bepreapproved by the Committee. Use of nonstandard or modifiedstandard analytical methods without a proapproval from theCommittee may result in failure of PE sample analysis.
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(c) PE samples will be prepared and sent out from reliablesuppliers by overnight express delivery. All PE samples shall bepreserved and shipped according to USACE, USEPA, and DOTregulations and guidelines. Full chain-of-custody shall bemaintained for each shipment of PE samples. The analyticallaboratory of Waterways Experiment Station (WES) in Vicksburg,Mississippi, and the Missouri River Division Laboratory (MRDL) inOmaha, Nebraska, are currently two of the major USACE PE samplesuppliers. Guidance for PE sample suppliers including WES, MRDL,and commercial vendors on PE sample preparation, handling, andvalidation are described in Appendix G. The general guidelinesfor PE sample analysis and reporting by a commercial laboratoryare described in Appendix D. Special sample-specificinstructions for PE sample analysis will be provided by PE samplesuppliers on the chain-of-custody document enclosed in each PEsample shipment. Any questions on PE sample analyses should bedirected to the Coordinator. A commercial laboratory shall alsoconduct all method-specific QC analyses which include but are notlimited to method blank, replicate, matrix spike, matrix spikeduplicate, and surrogate spike. If the amount of materialconstituting the PE samples is not enough for all QC analyses,the QC analyses shall be performed on spiked reagent water.
(4) Reports of PE Sample Results.
(a) A commercial laboratory shall report theconcentrations of all target analytes listed in the requiredanalytical methods, including estimated values and thequantitation limits for target analytes not detected. Thequantitation limit of each analyte must meet or be less thanthose specified in the method for the particular matrix. Exceptfor petroleum hydrocarbons PE samples, all soil/sediment PEsample analyses shall be reported on a dry-weight basis alongwith percent moisture. For petroleum hydrocarbons PE samples,the results shall be reported on an “as-received” basis (i.e., nocorrection should be made for moisture content). Neither shouldany data be corrected for spike recoveries nor for anycontamination found in trip blank or laboratory’s method blank.
(b) All method-specific QC data associated with the PEsample analysis, including method blank, replicate analysis,spike recovery, etc., shall be reported. Written reports of allPE sample analyses are to be received by the PE sample supplierswithin 20 working days after receipt of the samples. Forprojects requiring quick turnaround for field sample analyses,the turnaround times for the PE samples may be reduced. Forexample, due to the often short lead-time and the quickturnaround nature of most UST removal projects, the turnaround
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time for PE sample analysis needed for UST removal projects willrange from five to ten working days depending on the number ofparameters required. Failure to analyze the PE samples correctlyand within the required time frame may result in termination ofthe validation process. An additional copy of all PE samplereports shall be sent to the Coordinator for review. Uponrequest by the Coordinator, a commercial laboratory shall alsosubmit for review all raw data including sample preparation andrun logs, calibrations, chromatograms, calculations, etc. Acommercial laboratory may use its standard data package to reportPE sample results; however, the data package shall besequentially numbered and contain, as a minimum, the followinginformation:
- Table of contents.
- A case narrative including problems encountered with PEsample analysis.
- A chain-of-custody report.
- Sample preparation information.
- Analytical results for all target analytes plus methodcitations and quantitation limits.
- Summary of method-specific QC results for assessment ofprecision and accuracy.
- Phone conversation records on major issues related to PEsample analysis.
(c) Failure to submit the requested information within arequired time frame will be considered as non-responsive and mayresult in termination of the validation procedure. It is thelaboratory's responsibility to keep the Coordinator informedearly of any problems with PE sample analyses that would affectthe return of results within a required time frame.
(5) Evaluation of PE Sample Results.
(a) After receipt of PE sample data reports, the PE samplesuppliers should immediately evaluate the analytical data qualitybased on statistically established confidence limits andgenerally accepted QC indicators for accuracy and precision. ThePE sample results will be compared in the following manner:
- with the prepared concentrations of PE samples that areused as the absolute recovery comparators, and
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- with the statistical mean and standard deviationsreported by a group of referee and/or peer laboratories.
(b) The general acceptance limits for analyte quantitationwill be established statistically at the 95 percent confidencebased on referee laboratories and/or peer group results. TheCommittee shall review the evaluation reports and determine thepass/fail status for PE sample results. The general criteria foracceptance of PE sample results are as follows:
- All Chemical Analyses:
All method-specific QC data are reported and withinmethod-specified criteria.
- Multianalyte Organic Analyses:
No more than one target compound outside three sigmaconfidence limits and no more than two target compoundsbetween two and three sigma limits. False negatives andfalse positives are considered as outside three sigma.
- Metal Analysis:
No metal elements outside three sigma confidence limitsand no more than two metal elements between two andthree sigma limits. False negatives and false positivesare considered as outside three sigma.
- Classical Chemical Analyses:
All data are within two sigma.
(c) Within ten working days after receipt of PE sampleresults, the PE sample suppliers shall send the Coordinator awritten evaluation report. At a minimum, the report shallcontain the: laboratory name; location (city and state); datesthat PE samples were delivered; laboratory's PE sample results;dates results were received; true values and/or acceptable limitsfor each target analyte; narratives for special problems orissues; follow-ups on failed parameter; and recommendations forpass/fail. If requested by the Coordinator, the PE samplesuppliers shall provide the Committee with verbal reports on PEsample results within five working days after receipt of PEsample results. In addition to a written evaluation report, thePE sample suppliers shall also send a cover memorandum inline-item summary format with the: names of PE samples withinacceptable limits; names of target analytes correctly identified,but quantitated outside acceptable limits; and number of false
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positives and/or negatives reported for each PE sample. Theidentities of false positives and/or negatives shall not bedisclosed in the cover letter or memorandum.
(d) The majority of PE samples available from the USACEare in water and/or soil/sediment matrices. If only water PEsamples are available for certain analytical parameters from theUSACE, a commercial laboratory that passes the water PE sampleswill be considered for a multimedia validation of theseparameters. However, if both water and soil/sediment PE samplesare available for any parameters from USACE, a commerciallaboratory must pass both matrices prior to consideration for amultimedia validation for these parameters. A commerciallaboratory that passes water PE samples but fails thecorresponding soil/sediment PE samples for any parameters will beconsidered for a validation of these parameters in water samplesonly. However, a laboratory that passes soil/sediment PE samplesbut fails the corresponding water PE samples will not beconsidered for validation of the failed parameters in any matrixtype of samples, including soil/sediment samples.
(e) For volatile and semivolatile organic analyses, somecompounds in the water or soil/sediment PE samples may not be themethod-specific target compounds. A laboratory is required touse the NIST/EPA/MSDC or any other USEPA approved mass spectrallibrary to tentatively identify and quantify up to ten non-targetvolatile organic compounds and twenty non-target semivolatileorganic compounds that exhibit the strongest ion current signals.These compounds must not be system monitoring compounds.Identification of these compounds, based on spectralinterpretation procedures, is evaluated and integrated into theevaluation process for volatile and semivolatile organic PEsample results. For metal analysis, the validation will begranted for one of the following four categories based on thenumber of metal elements in the PE samples passed:
- Category I: Eight RCRA metal elements (arsenic, barium,cadmium, chromium, lead, mercury, selenium, and silver.)
- Category II: Fourteen RCRA and Priority Pollutant (PP)metal elements (antimony, arsenic, barium, beryllium,cadmium, chromium, copper, lead, mercury, nickel,selenium, silver, thallium, and zinc.)
- Category III: Twenty-three USEPA CLP Target AnalyteList (TAL) metal elements (aluminum, antimony, arsenic,barium, beryllium, cadmium, calcium, chromium, cobalt,copper, iron, lead, magnesium, manganese, mercury,
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nickel, potassium, selenium, silver, sodium, thallium,vanadium, and zinc.)
- Category IV: Any other metal element(s) including thefour metal elements (arsenic, cadmium, chromium, andlead) usually required for UST removal projects.
(f) Based on project requirements on metal analysis, oneof the above four specific categories of metal PE samples will beselected for laboratory validation. A commercial laboratory mayvolunteer for any one of the four categories of metal PE samplesas long as more metal elements than the project-required areanalyzed. Normally, a commercial laboratory must satisfactorilypass all metal elements in a specific category prior toconsideration for validation of the specific category of metalelements.
(9) If PE samples for a particular parameter such asdioxin, radioactivity, air toxics, etc. are not available fromthe USACE, the analysis of PE samples will be exempted until theappropriate PE samples for these particular parameters becomeavailable. The validation of a commercial laboratory forparameters without PE samples available will be based solely onthe laboratory's qualification documents submitted to theCoordinator for review. The qualification documents shallinclude: copies of the laboratory’s LQMM; laboratorycertificates or licenses; and the most recent two rounds of PEsample results from other government and/or private agencies. Ifthe parameter is the only project-required chemical analysis, anon-site inspection may be waived.
(h) For the analysis of chemical warfare agents, theirdegradation products, and other scheduled compounds in thecomplex matrices, the primary contracts shall select chemicalsurety laboratories that have already been approved by the U.S.Army Edgewood Research, Development and Engineering Center(ERDEC) at Aberdeen Proving Ground, Maryland. The USACE will notsend PE samples to or inspect the approved chemical suretylaboratories. The USACE will contact the ERDEC for technicalassistance and provide a list of approved chemical suretylaboratories if requested.
(i) The acceptance of PE sample results also depends onwhether the results are returned in a timely manner and noprocedural problems are found during a follow-up laboratoryinspection. The Coordinator will send a copy of the cover letteror memorandum from the PE sample suppliers evaluation reports tothe laboratory for information and/or necessary action(s) by thelaboratory. Due to confidentiality requirements, the true values
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and/or two sigma confidence limits for any batch of volatileorganic PE samples and soil/sediment PE samples shall not bereleased to commercial laboratories until the batch isdiscontinued. A commercial laboratory will be allowed to providerevised data for failed parameters if problems such ascalculation or transcription errors can be identified. If acommercial laboratory is requested by the Coordinator to checkits analytical data, the laboratory shall return revised datawithin five working days to the Coordinator.
(j) After data revisions, a commercial laboratory mustpass, as a minimum, more than 50 percent of all PE samples,including project-specific and non-project-specific PE samples,within 40 working days from receipt of the first set of PEsamples, or the validation process will be terminated. TheCoordinator will notify all affected USACE TM/CORs immediatelyand suggest selection of another laboratory by the primecontractor for evaluation. After a commercial laboratory passes50 percent of all PE samples within 40 working days, theCoordinator will contact the laboratory to schedule an on-siteinspection within ten working days. Prior to an on-siteinspection, the laboratory shall submit to the Coordinator aconcise written statement describing the problems, solutions, andcorrective actions taken or to be taken for the analyticalparameters failed in its first attempt.
c. Step 3: On-Site Laboratory Inspection.
(1) Two Committee representatives will normally serve asthe inspectors to inspect a commercial laboratory after Steps 1and 2 have been satisfactorily completed. The inspectors shallcontact and invite the USACE TM/COR(s) who initiated theevaluation request(s) and the USACE division laboratory(s) thatserves as the QA laboratory(s) for the project(s) to sendrepresentatives to the inspection. The PE sample suppliers mayalso be requested to send technical experts if assistance isneeded for the inspection. During an on-site laboratoryinspection, the inspectors shall verify that:
- the organization and personnel are qualified to performassigned tasks,
- adequate facilities and equipment are available,
- complete documentation, including chain-of–custody ofsamples, is being implemented,
- proper analytical methodology is being used withoutdeviations,
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- adequate analytical quality control (including referencesamples, control charts, documented corrective actions,etc.) is being provided,
- acceptable data handling and documentation techniquesare being used,
- adequate facilities and operations are installed toensure laboratory health and safety, and
- proper waste disposal procedures are implemented.
(2) The on-site laboratory inspection helps to ensure thatthe laboratory is technically competent and that all thenecessary quality control is being applied by the laboratory inorder to deliver a quality product. The on-site inspection alsoserves as a mechanism for discussing weaknesses identifiedthrough PE sample analysis or other review of data deliverables.Lastly, the on-site inspection allows the inspector to monitorwhether the laboratory has continuously and successfullyimplemented the recommended and/or required corrective actionsthat were made during previous on-site inspections by the USACE.Failure to have implemented past action items may be grounds fortermination of the current validation process.
(3) Prior to the inspection, the inspectors shall reviewall appropriate project- and laboratory-specific documentsincluding:
- scope of services, specifications, work plans, and/orchemical data acquisition plan, if available,
- LQMM and qualification documents,
- preliminary questionnaire,
- PE sample results and evaluation reports,
- previous inspection reports, if applicable, and
- previous performance on USACE HTRW projects based on thechemical quality assurance reports (CQARS) for projectsthat the laboratory has previously worked on.
(4) The on-site inspection generally takes eight hours andnormally consists of three parts: entrance interview, laboratorytour, and exit interview. The entrance interview will be heldwith the upper laboratory management personnel (includinglaboratory director/managers, QA officer, and project personnel)
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to discuss the upcoming USACE projects, the USACE QA program, theUSACE review comments on the laboratory's LQMM, the PE sampleresults, and the laboratory's previous performance on USACEprojects, if applicable. A copy of written comments on the LQMMshall be presented to the laboratory during the entranceinterview. The inspectors will also present an overview of thelaboratory's performance on PE sample analysis.
(5) A tour of the commercial laboratory will follow toexamine the laboratory facilities, instrumentation, operation,maintenance, documentation, safety, waste compliance, etc. Theaudit tour is generally conducted in a manner that allows thefollowing of a sample through the laboratory, and looking at alloperations that a sample is exposed to during its transfer ofcustody, digestion/extraction, and analysis. This includessample/digestate/extract storage, instrument calibration, SOPS,documentation, data review and reporting, etc. During the tour,the inspectors shall also examine the raw data of the PE samplesand talk with the analysts who performed the analyses of anyfailed PE samples to determine the cause of failure and to decideif additional PE samples are needed for the failed parameters.The inspectors should adhere to the inspection guidelines andcriteria in Appendix H and use the appropriate laboratoryinspection checklists in Appendices I or J.
(6) At the conclusion of the laboratory tour, theinspectors shall request a 30-minute close door session toorganize, review, and document the findings. After the closedoor session, an open exit interview will be held with laboratorypersonnel in which a summary of any deficiencies andrecommendations is discussed. The format in Figure 2-2 can beused to document the meeting summary on deficiencies,recommendations, and/or any other findings, if applicable. Theauthorized representative of the laboratory shall be asked tosign the meeting summary to attest that the laboratoryrepresentative has reviewed the meeting summary with theinspectors. The laboratory has ten working days to submitwritten responses with supporting documentation to thedeficiencies and/or recommendations to prevent possiblevalidation termination. The responses shall address thecorrective actions that have been taken or will be taken withproposed implementation and completion schedules. Alldeficiencies shall be corrected by the laboratory prior toperforming USACE HTRW project work. Recommendations based ongood laboratory practice for operations and management are forthe laboratory's consideration.
2-4. Approval Procedures. Normally, within five working daysafter the inspection, the inspectors shall organize, document,
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U.S. ARMY CORPS OF ENGINEERSON-SITE LABORATORY INSPECTION SUMMARY
LAB NAME/LOCATION:
DATE/TIME:
PURPOSE: This format documents any deficiencies andrecommendations noted during the on-site laboratory inspection.The laboratory has ten working days to submit written responseswith supporting documentation, including an implementationschedule for any corrective actions, to the deficiencies andrecommendations to prevent possible validation termination.
MEETING ATTENDEES:
NAME ORGANIZATION/TITLE PHONE
(Page 1 of 3)
Figure 2-2 On-Site Laboratory Inspection Summary
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ON-SITE INSPECTION SUMMARY:
DEFICIENCIES :
Figure 2-2 On-Site
(Page 2 of 3)
Laboratory Inspection
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Summary (continued)
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ON-SITE INSPECTION
RECOMMENDATIONS:
SUMMARY:
OTHER FINDINGS:
ACKNOWLEDGMENT:
LABORATORY:________________________________________________________
USACE INSPECTION TEAM:_______________________________________________________
Figure 2-2 On-Site
(Page 3 of 3)
Laboratory Inspection Summary (continued)
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and verbally present the findings and the recommended validationstatus for the laboratory to the Committee for approval and/orconcurrence. In the event that supportive documents from alaboratory are needed before a final decision by the Committee,the inspectors shall present a second presentation within fiveworking days after receipt of the requested materials from thelaboratory. A minimum of three members of the Committee must bepresent in the review meeting to determine the validation statusof a commercial laboratory. The decisions of the Committee canbe documented in the format shown in Figure 2-3. Normally, aparameter- and matrix-specific full validation for 18 months willbe granted to a commercial laboratory after the laboratory hassatisfactorily met all USACE HTRW laboratory validation criteria.The 18 months start from the date that the Committee first metafter the inspection and agreed upon the laboratory’s validationstatus. The guidelines for determination of validation statusfor a commercial laboratory are as follows:
a. For a commercial laboratory that passes all PE samplesand has no deficiencies noted during the on-site inspection, afull validation status of 18 months will be granted for allanalytical parameters that the laboratory has passed theassociated PE samples.
b. For a commercial laboratory that passes all PE samplesbut has deficiencies noted during the on-site inspection, a fullvalidation status of 18 months will be granted for all analyticalparameters that the laboratory has passed the associated PEsamples. However, validation will only be granted after theCommittee reviews and accepts the written responses from thelaboratory and the laboratory completes the implementation ofcorrective actions for the deficiencies.
c. For a commercial laboratory that does not pass all PEsamples but has no other deficiencies noted during the on-siteinspection, a full validation status of 18 months will be grantedfor all analytical parameters that the laboratory has passed theassociated PE samples. Validation may also be granted foranalytical parameters if it is determined during the on-siteinspection that the failure was due to minor errors, such aserrors in data calculation, transcription, etc. For any failedparameters caused by major errors (such as errors in analyticalprocedure, spectra interpretation, etc.) or unknown/unsurereasons, the laboratory must pass additional PE samples prior toconsideration for validation of the additional parameters. Inthis case, one set of additional PE samples will be sent to thecommercial laboratory that failed the first set of PE samples.Results of the additional set of PE sample analyses shall bereturned to the PE sample suppliers and the Coordinator within
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U.S. ARMY CORPS OF ENGINEERSLABORATORY EVALUATION COMMITTEE
VALIDATION REVIEW MEETING SUMMARY
LAB NAME/LOCATION:________________________________________________
REVIEW MEETING DATE/TIME:________________________________________
PURPOSE: This format documents the final committee decisions onthe validation status of a contract laboratory inspected by thestaffs of the Army Corps of Engineers.
MEETING ATTENDEES:
NAME ORGANIZATION/TITLE
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
INSPECTOR'S RECOMMENDATIONS TO COMMITTEE:
(Page 1 of 2)
Figure 2-3 Validation Review Meeting Summary
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VALIDATION REVIEW MEETING SUMMARY:
MAJOR FACTORS SUPPORTING COMMITTEE DECISIONS:
FINAL COMMITTEE DECISIONS:
SIGNATURES OF COMMITTEE MEMBERS:
1. 2.
3. 4.
5. 6.
7. 8.
9. 10.
11. 12.
(Page 2 of 2)
Figure 2-3 Validation Review Meeting
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Summary (continued)
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five or ten working days, depending on the number of additionalPE samples required. The Committee will make the final decisionon the pass/fail status of PE sample analysis or any additionalwork needed to pass PE samples. If a commercial laboratory failsto pass the additional set of PE samples, no validation statuswill be granted for the additional parameters.
d. For a commercial laboratory that does not pass all PEsamples and also has other deficiencies noted during the on-siteinspection, similar procedures and criteria as described inparagraph 2-4.c. will be used to determine the laboratory’svalidation status. However, validation will only be grantedafter the Committee reviews and accepts the written responsesfrom the laboratory and the laboratory completes theimplementation of corrective actions for the deficiencies.
e. For a commercial laboratory that has deficiencies notedduring the on-site inspection, but failed to submit acceptableresponses or to satisfactorily complete corrective actions withinthe required time frame, no validation status will be granted. Acommercial laboratory that is considered to have failed onattempted validation shall wait for six months prior to repeatingthe validation process, and then the process is only initiated bya written request from a USACE TM/COR. If a commerciallaboratory fails the laboratory validation process during any ofthe three major steps mentioned previously, another commerciallaboratory or a prevalidated commercial laboratory must beselected by the prime contractor for evaluation. If anothernon-validated laboratory is selected, the prime contractor willbe responsible for the expense of this additional laboratoryvalidation.
f. A commercial laboratory, that is exempted from PEsample analysis due to lack of suitable PE samples from USACE,will be granted a six month conditional validation. Theperformance of a commercial laboratory granted a conditionalvalidation status will be closely monitored by the USACE TM/CORs,the USACE division laboratories that serve as the government QAlaboratories, and the Committee during the conditional period.Prior to the end of the conditional validation, the Committeewill review the case and determine the appropriate actionsrequired for a full validation for an additional 12 months.Normally, if no performance problems are noted during theprobation period, a full validation will be granted. TheCoordinator shall keep all affected USACE TM/CORs informed of anychanges of validation status of commercial laboratories.
g. For a commercial laboratory inspected by a“non-committee representative” inspector for UST removal
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projects, the same guidelines addressed above apply. Theinspector(s) shall send a written inspection report and allappropriate documents to the Committee for technical review andapproval. The Committee will make the final decision on alaboratory validation status based on all information availableincluding the inspectors’ written inspection reports.
h. For a mobile laboratory, the above mentioned guidelinesin paragraphs 2-4.a. through 2-4.f. apply. However, thevalidation status of a mobile laboratory will be terminated whenthe laboratory is demobilized.
2-5. Inspection/Evaluation Report.
a. If no deficiencies were noted, a laboratory inspectionand evaluation report shall be prepared by the inspectors andsubmitted to the HTRW MCX management for approval within tenworking days after the inspection date. If deficiencies werenoted and the laboratory provided satisfactory responses, thereport shall be submitted within five working days after receiptof the satisfactory responses.
b. The inspection and evaluation report shall contain, butnot be limited to, the information listed in Table 2-1. Uponapproval by the HTRW MCX management, a cover letter and theinspection report including review comments on LQMM, PE sampleevaluation reports, and laboratory’s written responses todeficiencies shall be immediately sent to the USACE TM/CORs andthe commercial laboratory. The cover letter shall specify themethods, matrices, time period, and limitations for which thevalidation is granted, and the corrective actions that have to betaken by the laboratory if applicable. A commercial laboratorymust rectify all deficiencies prior to the initiation of fieldstudies and sample analyses. During the 18-month period, theCommittee reserves the right to send additional PE samples or toconduct additional inspections as necessary. The laboratoryvalidation does not guarantee the award of any contracts from aUSACE TM/COR or a prime contractor. For UST removal projects,although the inspections may not be conducted by the Committeerepresentatives, all reports generated by the inspectors shallfollow the format given in this manual. All cover letters shalloriginate from the HTRW MCX.
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Table 2-1. Sample Format for Inspection Report
1. General
a. Date of Inspection.b. Name, office symbol, and phone number of inspector.c. Contract(s) for which the laboratory will be used.d. Description of contract.e. General information of the laboratory (Business name,
street address, phone, how long in business, numberemployed, type of services offered, and otherpertinent information.)
2. Summary of Inspection Results
a. Overall comments on the laboratory’s technicalcapabilities in meeting the project requirements.
b. The validation status and expiration date of thelaboratory.
c. Major deficiencies or concerns to be corrected orbe aware of for USACE HTRW projects.
3. Interviews
a. Entrance
- Introduction to the USACE QA program.- Overview of USACE HTRW laboratory validation
procedures.- Discussion of the upcoming USACE project(s).- Presentation and discussion of the USACE comments
on the laboratory’s LQMM.- Overview and discussion of PE sample results.- Discussion of the laboratory’s past performance on
USACE HTRW projects, if applicable.
b. Exit
- Discussion of deficiencies to be corrected.- Recommendations based on good laboratory practice.- Action items for the laboratory's response.
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Table 2-1. Sample Format for Inspection Report (continued)
4. General On-Site QA Evaluation
a.
b.c.
d.
e.
f.g.
h.i.j.
Adequacy of organizational structure to maintain itsstated capabilities in operation and management.Adequacy and maintenance of facilities and equipment.Quality, age, availability, scheduled maintenance,and performance of instrumentation.Staff qualifications, experience, and trainingprograms.Availability, appropriateness, and utilization ofSOPs .Reagents, standards, and sample storage facility.Bench sheets and analytical logbooks maintenanceand review.Data package and data management.Availability and use of control charts.Waste disposal compliance.
5. Conclusions
a. Deficiencies that must be corrected by the laboratoryprior to approval for validation.
b. Recommendations for laboratory's consideration.c. Other findings of interesting or important nature.d. Concerns from the laboratory on USACE HTRW projects.e. Laboratory's responses to deficiencies and
recommendations, if available.f. Action items for the laboratory’s response.
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Section II. Revalidation, Termination, and Appeal
2-6. Revalidation.
a. A commercial laboratory whose 18-month validationstatus has expired will be considered for revalidation uponreceipt of a written request from a TM/COR based on theanalytical requirements in the upcoming contract(s). TheCommittee will determine which of the three steps are requiredfor the revalidation process based on the laboratory’s previousperformance. Normally, Steps 1 (review of qualifications) and 2(analysis of PE samples) are always required. Step 3 (inspectionof laboratory) could be waived if the following criteria are met.
(1) The laboratory’s performance on PE samples has beensatisfactory,
(2) the laboratory has had no performance problems withprevious USACE HTRW projects,
(3) the laboratory has not moved to a new location or hadmajor facility changes at the current location since the lastUSACE HTRW inspection, and
(4) the laboratory has been inspected by the Committeeduring a validation/revalidation process within the last threeyears.
b. During the 18-month validation period, a commerciallaboratory shall inform the Coordinator immediately of any majorchanges in its personnel, equipment, or facilities that couldimpact the laboratory’s performance on any USACE projects.Depending on the scope of changes, a revalidation may berequired. The Committee will determine which of the three stepswould be needed for the revalidation. The validation status of acommercial laboratory that fails to inform the Coordinator of anymajor changes may be suspended.
c. A revalidation may also be required when a fullyvalidated laboratory obtains another contract(s) within its18-month validation period. Based on the contract requirements,the laboratory’s validation status, and its previous performanceon USACE projects, the Committee will determine which of thethree steps are required for a revalidation. Ordinarily, ifdifferent analytes or matrices are involved in anothercontract(s), analysis of additional PE samples is required. Ifits previous performance has been satisfactory and/or additionalPE sample results are acceptable, no further actions arerequired.
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d. A revalidation is also required for laboratoriesworking on ongoing projects that will extend more than six monthsbeyond the validation expiration date of the laboratory. TheCoordinator will alert the affected USACE TM/CORs of the pendingexpiration three months prior to expiration date. A revalidationprocess should not interfere with the ongoing project unlessperformance problems are noted during the revalidation process.
2-7. Termination.
a. As a means of measuring a commercial laboratory’sperformance after validation, the Committee may send additionalPE samples on a quarterly or as-needed basis. This depends onthe laboratory’s past performance on PE sample and/or fieldsample analyses and on whether the laboratory is currentlyworking on an ongoing USACE HTRW project. The quarterly PEsamples could be either single blind or double blind sent by theCommittee directly or through a prime contractor. As a minimum,the results are evaluated for compound identification,quantitation, and sample contamination. Results from theanalysis of the PE samples will be used by the Committee toverify the laboratory’s continuing ability to produce acceptableanalytical data. A commercial laboratory’s results on thesequarterly PE samples will determine its performance as follows:
(1) Acceptable, No Response Required:
Data meets most or all of evaluation criteria aspreviously described. No response is required.
(2) Acceptable, Response Explaining Deficiencies Required:
Deficiencies exist in the laboratory's performance.Within five working days of receipt of notificationfrom the Coordinator, the laboratory shall sendwritten response to describe the deficiencies and theaction(s) taken to correct the deficiencies to theCoordinator.
(3) Unacceptable Performance, Response ExplainingDeficiencies Required:
Deficiencies exist in the laboratory's performance tothe extent that the Committee has determined that thecommercial laboratory has lost its capability to meetthe USACE project requirements. Within five days ofreceipt of notification from the Coordinator, thelaboratory shall describe the deficiencies and the
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action(s) taken to correct the deficiencies in aletter to the Coordinator.
b. Remedial PE samples may be sent for the failedparameters. It is the sole decision of the Committee to approveor disapprove the quarterly PE sample results and to sendremedial PE samples. If a commercial laboratory fails to passquarterly PE samples, the laboratory may expect, but theCommittee is not limited to the following actions: suspension ofthe laboratory validation status, an additional on-sitelaboratory inspection, data package audit, a remedial PE sample,and/or contract sanctions.
c. During the 18-month validation period, the performanceof the laboratory will be monitored by the USACE TM/CORs, theUSACE division laboratories, and the Committee through review ofappropriate CQARs prepared by the USACE division laboratoriesthat serve as the project QA laboratories. If a commerciallaboratory has performance problems with field sample analysis ordata reporting, the USACE TM/CORs and the USACE DivisionLaboratories should contact the Coordinator immediately to workout necessary corrective and remedial actions. Figure 2-4 can beused to report performance problems with commercial laboratories.Depending on the scope of problems, a commercial laboratory’svalidation status may be suspended such that the laboratory willnot be allowed to analyze any more project samples until thecorrective actions are accepted by the Committee and the problemsare corrected.
d. While a commercial laboratory is in the process ofperforming corrective actions, another validated laboratory shallbe used until the problems are solved. Should a commerciallaboratory fail to solve the problems satisfactorily in a timelymanner, the validation status of the laboratory may be revokedfor default. The validation status of any laboratory suspendedor debarred by other government regulatory agencies may also beterminated by the Committee.
2-8. Appeal. The Coordinator shall advise a commerciallaboratory of its right to appeal adverse validation decisionsincluding suspension or termination of validation status. If acommercial laboratory decides to appeal, it should submit awritten appeal to the Coordinator within 20 working days fromreceipt of the laboratory validation report. The Committee willreview its decision and send a written response to the laboratorywithin 20 working days. All review decisions by the Committeeare final.
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TO: CEMRD-ED-EC FROM :_____________________
SUBJECT: PERFORMANCE PROBLEMS WITH COMMERCIAL LABORATORY
Project Name:______________________________________________________________
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DATE: / /
Location:__________________________________________ State:______Contract No:____________________ TYPE: POL TANK REMOVAL:___HTRW:__
Program: SF:____ FUDS:____ IRP:____ AF(ACC):____ OTHER:______________Phase: PA/SI:____ RI/FS:____RD:____ RA:____ RFA:____ RFI:____ CMS:____
USACE Technical Manager:_____________________________________________________Phone:__________________ Address:___________________________________Government QA Lab:____________________ POC:______________________________Phone:_________________ Address:___________________________________
A-E/Contractor:_________________________________________ State:_______Lab Name:___________________________________________________________Address:_________________________________________________________Phone:_________________________________________________________
POC:_________________________________________________________________
PROBLEMS ENCOUNTERED:
Figure
(Page 1 of 2)
2-4 Laboratory Performance Problem Report
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PERFORMANCE PROBLEMS WITH
CORRECTIVE ACTIONS TAKEN:
COMMERCIAL LABORATORY:
TECHNICAL ASSISTANCE NEEDED FROM THE HTRW MCX:
Figure 2-4 Laboratory
(Page 2 of
Performance
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2)
Problem Report (continued)
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Section III. Information Management
2-9. Record Files:
a. Centralized validation records for commerciallaboratories are kept at the HTRW MCX. The record files include:
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
(10)
(11)
b.
Original laboratory evaluation requests (Figure 2-l),
laboratory qualification documents including LQMM andpreliminary questionnaire,
PE sample evaluation reports,
laboratory's responses to PE sample reports,
inspection report and cover letters,
laboratory inspection checklist,
on-site laboratory inspection summary (Figure 2-2),
laboratory's responses to inspection report,
the Committee's validation review meeting summary(Figure 2-3),
laboratory performance problem reports (Figure 2-4),and
miscellaneous documents (e.g., raw data,chromatograms, correspondences, etc.) that theinspectors deems important for the current and/orfuture laboratory validation.
When there is a potential of litigation against theUSACE on a particular laboratory validation; all documentspertaining to the particular laboratory validation shall beretained in the file until a final settlement or a revalidationrequest is received.
2-10. Database. A laboratory validation database is maintainedat the MCX for program management. An example of a laboratoryrecord in the database is shown in Appendix K. Updated lists ofvalidated commercial laboratories in alphabetical order bylaboratory name and state will be distributed to eachEngineering, Construction, and Contracting office within theUSACE on a monthly basis. Customized reports are also available
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if requested by USACE TM/CORs. These reports are for governmentuse only and will not be distributed to private sector.
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CHAPTER 3
PROCEDURES FOR USACE DIVISION LABORATORIES
3-1. USACE Division Laboratories. Minor modifications to thevalidation procedures as described in Chapters 1 and 2 will bemade for validation/revalidation of USACE division laboratoriesto ensure that all USACE division laboratories are able toprovide analytical data of the highest accuracy and precision forvalidated parameters. The modifications include:
a. The Committee shall invite the HQUSACE to send arepresentative(s) to participate in the inspection of each USACEdivision laboratory and shall keep the HQUSACE informed of thecurrent validation status of each USACE division laboratory on aregular basis. A copy of the inspection report for each USACEdivision laboratory shall be sent to the HQUSACE. The HTRW MCXwill recommend the corrective actions for each USACE divisionlaboratory. The HQUSACE will coordinate with the HTRW MCX toensure that corrective actions for each USACE division laboratoryare planned and implemented appropriately.
b. All USACE division laboratories will be revalidatedevery 18-months. The revalidation shall always include a two–dayon-site inspection. During the 18-month period, at least oneadditional announced and/or unannounced site visit will beperformed by the Committee whenever needed.
c. During the 18-month validation period, additional PEsamples shall be provided to USACE division laboratories on aperiodic basis to monitor the laboratory’s continuing ability toprovide superior analytical performance. Results from these PEsamples would be used primarily for the division laboratories tocheck and improve their method specific performance.
d. All division laboratories' technical SOPS that wouldaffect data quality shall be received, reviewed, and approved bythe Committee prior to implementation.
e. Appendix L, Supplemental Questionnaire for USACEDivision Laboratories, shall be included as an appendix to thepreliminary questionnaire and sent to USACE division laboratoriesfor completion.
f. Upon request by USACE division laboratories, theCommittee will provide technical support to assist USACE divisionlaboratories to obtain a full validation on a continual basis.
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g. All expenses for validation of USACE divisionlaboratories will be covered by USACE HTRW program managementfunds.
3-2. Contract QA Laboratories: Designated commerciallaboratories with contracts to provide technical support to theQA function of USACE division laboratories shall also beevaluated under higher standards and more stringent criteria.However, Appendix L is not needed for commercial laboratories.
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APPENDIX A
REFERENCE
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DEPARTMENT OF THE ARMYU.S. Army Corps of Engineers
WASHINGTON. D.C. 20314-1000
14 SEP 1993
MEMORANDUM FOR SEE DISTRIBUTION
Subject: Hazardous, Toxic & Radioactive Waste (HTRW) - PolicyGuidance on Validation of Commercial Analytical ChemistryLaboratories
1. Reference ER 1110-1-263, Chemical Data Quality Management forHazardous Waste Remedial Activities, 1 Oct 90.
2. The referenced ER requires that all commercial analyticalchemistry laboratories which analyze samples in support of allHTRW projects be validated by CEMRD-ED-EC for project specificparameters prior to the analysis of those samples. This memosupplements the reference by providing policy guidance on:
a. The use of lists of validated laboratories (paragraph3); and
b. Alternative validation procedures for laboratoriessupporting underground storage tank (UST) projects (paragraph 4).
3. A list of validated laboratories, which now includes about160 laboratories, is distributed monthly by the HTRW MCX (CEMRD-ED-EC) to all Divisions and Districts. The followinginformation, regarding laboratory validations and the use ofthese lists, must be provided to potential contractors in CBDannouncements or subsequent solicitation packages:
Laboratories must be validated for project specificparameters prior to analyzing any samples under contract as partof USACE HTRW Program execution. Laboratories must berevalidated every eighteen months if they are actively supportingUSACE projects.
b. Initial laboratory validations require eight to twelveweeks, depending on the responsiveness of the laboratory.Revalidation usually requires less time.
The list of currently validated laboratories and/orinformation (encl 2) on the validation process can be obtainedfrom the contracting office of the procuring district.
d. Potential contractors may use laboratories on theor propose to use laboratories not on the list. Proposedlaboratories not on the list will be validated.
list
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CEMP-RT (200-la)SUBJECT: Hazardous, Toxic & Radioactive Waste (HTRW) - PolicyGuidance on Validation of Commercial Analytical ChemistryLaboratories
A "Request for Evaluation of Commercial Laboratory” form (encl 1)must be submitted to the HTRW MCX (CEMRD-ED-EC) by a contractingOfficer Representative for all projects/contracts, regardless ofwhether the laboratory is on the list. The form must besubmitted as soon as a contract has been awarded to the primecontractor and may be faxed to Ms. Paulette Lewis at 402-221-7403.
4. For projects consisting of the removal of Underground storagetanks (UST) Which have contained only petroleum, oils, orlubricants, there are two alternatives to the validation processdescribed in ER 1110-1-263. The following alternatives applyonly to predesign sampling of UST organic phase contents and soilsampling during removal. They do not apply to investigationsrequired by groundwater contamination or extensive soilcontamination.
a. State certified laboratories may be used without USACEvalidation, if the state considers its certification to beapplicable to UST removal. When this alternative is selected, adocument in the project file must identify the individualresponsible for coordination with the state.
b. The HTRW MCX will follow an abbreviated laboratoryvalidation process if requested on the “Request for Evaluation ofCommercial Laboratory” form (encl 1) and the analyses identifiedare applicable to UST removal. The laboratory’s standardoperating procedure for the required analyses must be submittedto the HTRW MCX for review. Based on the SOPs and otheravailable information, the HTRW MCX will determine the remainderof the validation process. The HTRW MCX may delegate certainvalidation responsibilities to Division Chemistry Laboratories bymutual consent. Note that the SOPs are not copies of printedstandard methods, but rather step-by-step procedures which arefollowed by the laboratories for sample analysis, qualitycontrol, and data reporting. Laboratories validated by thisabbreviated procedure may be used only for the UST projectsdefined above.
5. The CEMP-RT POC is Dr.
2 Encls
DivisionDirectorate of Military programs
2
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CEMP-RT (200-la)SUBJECT: Hazardous, Toxic & Radioactive Waste (HTRW) - PolicyGuidance on Validation of Commercial Analytical ChemistryLaboratories
COMMANDER:HUNTSVILLE DIVISION, ATTN: CEHND-CTHUNTSVILLE DIVISION, ATTN: CEHND-ED-CSHUNTSVILLE DIVISION, ATTN: CEHND-TDHUNTSVILLE DIVISION, ATTN: CEHND-TD-TOLOWER MISSISSIPPI VALLEY DIVISION, ATTN: CELMV-ED-WLOWER MISSISSIPPI VALLEY DIVISION, ATTN: CELMV-CO-CLOWER MISSISSIPPI VALLEY DIVISION, ATTN: CELMV-CTMISSOURI RIVER DIVISION, ATTN: CEMRD-EDMISSOURI RIVER DIVISION, ATTN: CEMRD-ED-LMISSOURI RIVER DIVISION, ATTN: CEMRD-CTNEW ENGLAND DIVISION, ATTN: CENED-CTNEW ENGLAND DIVISION, ATTN: CENED-EDNEW ENGLAND DIVISION, ATTN: CENED-ED-GLNEW ENGLAND DIVISION, ATTN: CENED-PD-LNORTH ATLANTIC DIVISION, ATTN: CENAD-CTNORTH ATLANTIC DIVISION, ATTN: CENAD-EN-TSNORTH ATLANTIC DIVISION, ATTN: CENAD-CO-CENORTH ATLANTIC DIVISION, ATTN: CENAD-PP-PMNORTH CENTRAL DIVISION, ATTN: CENCD-CTNORTH CENTRAL DIVISION, ATTN: CENCD-EDNORTH CENTRAL DIVISION, ATTN: CENCD-CO-CNORTH CENTRAL DIVISION, ATTL: CENCD-TE-ED-WNORTH PACIFIC DIVISION, ATTN: CENPD-CTNORTH PACIFIC DIVISION, ATTN: CENPD-PE-GTNORTH PACIFIC DIVISION, ATTN: CENPD-PE-GT-LNORTH PACIFIC DIVISION, ATTN: CENPD-PM-MPOHIO RIVER DIVISION, ATTN: CEORD-CTOHIO RIVER DIVISION, ATTN: CEORD-EDOHIO RIVER DIVISION, ATTN: CEORD-PE-GLOHIO RIVER DIVISION, ATTN: CEORD-DL-MSPACIFIC OCEAN DIVISION, ATTN: CEPOD-CTPACIFIC OCEAN DIVISION, ATTN: CEPOD-ED-MESOUTHSOUTHSOUTHSOUTHSOUTHSOUTHSOUTHSOUTH
ATLANTIC DIVISION, ATTN:ATLANTIC DIVISION, ATTN:ATLANTIC DIVISION, ATTN:ATLANTIC DIVISION, ATTN:PACIFIC DIVISION, ATTN:PACIFIC DIVISION, ATTN:PACIFIC DIVISION, ATTN:PACIFIC DIVISION, ATTN:
SOUTHWESTERNSOUTHWESTERNSOUTHWESTERNSOUTHWESTERNSOUTHWESTERN
DIVISION,DIVISION,DIVISION,DIVISION,DIVISION,
CESAD-CTCESAD-ENCESAD-EN-FLCESAD-PM-H
CESPD-CTCESPD-EDCESPD-ED-GLCESPD-CO-CM
ATTN : CESWD-CTATTN : CESWD-EDATTN : CESWD-ED-GLATTN : CESWD-PP-MATTN : CESWD-PP-MM
3
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CEMP-RT (200-la)SUBJECT: Hazardous, Toxic & Radioactive Waste (HTRW) - PolicyGuidance on Validation of Commercial Analytical ChemistryLaboratories
CF:CENPA-CTCENPA-EN-G-MCESWA-CTCESWA-EDCENAB-CTCENAB-EN-HTCENCB-CTCENCB-PE-HQCESAC-CTCESAC-EN-DFCENCC-EDCENCE-CTCENCE-ED-DCESWF-CTCESWF-EDCESWG-CTCESWG-ED-DCCEORH-CTCEORH-ED-AECESAJ-CTCESAJ-ENCESAJ-CO-CQCEMRK-CTCEMRK-EDCESWL-CTCESWL-ED-GHCESPL-CTCESPL-ED-GGCEORL-CTCEORL-ED-GCEORL-CD-FBCELMM-CTCELMM-ED-HWCENAN-CL-ME-ECESAM-CTCESAM-ENCESAM-PD-ESCEORN-CTCEORN-EDCELXN-CDCELMN-CD-QMCELMN-CTCELMN-ED-EECENAN-CT
4
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CEMP-RT (200-la)SUBJECT: Hazardous, Toxic & Radioactive Waste (HTRW) - PolicyGuidance on Validation of Commercial Analytical ChemistryLaboratories
CENAN-ENCENAO-CTCENAO-EN-MPCEMRO-CTCEMRO-ED-EGCENAP-CTCENAP-EN-CCEORP-CTCEORP-EDCENPP-CTCENPP-ED-DCCENCR-CTCENCR-ED-DGCESPK-CTCESPK-ED-MCESPK-ED-GCELMS-CTCELMS-ED-HQCENCS-CTCENCS-ENCESPN-CTCESPN-ENCESAS-CTCESAS-ENCENPS-CTCENPS-EDCENPS-EN-GT-HWCESWT-CTCESWT-EDCESWT-OW-ARCELMK-CDCELMK-CTCELMX-ED-DRCEIMK-CD-QMCELMK-OD-MCEWES-EE-ACENPW-CTCENPW-EN-EECESAW-CTCESAW-EN
5
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APPENDIX B
INTRODUCTION
TO
THE U.S. ARMY CORPS OF ENGINEERS
VALIDATION PROGRAM
FOR
COMMERCIAL ANALYTICAL CHEMISTRY LABORATORIES
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(SAMPLE LETTER)
Dear Laboratory Director:
Thank you for your interest in the U.S. Army Corps ofEngineers (USACE) Hazardous, Toxic, and Radioactive Waste (HTRW)laboratory validation program. I hope that the informationenclosed will be helpful to you and answer any questions you mayhave.
If you have any further questions regarding this informationor the USACE HTRW laboratory validation program in general,please contact the USACE Laboratory Validation Coordinator at(402) 221-7494.
Sincerely,
Chief, Environmental, HTRW DivisionHTRW and Engineering Directorate
Enclosure
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INTRODUCTION TO THE U.S. ARMY CORPS OF ENGINEERSVALIDATION PROGRAM FOR COMMERCIAL ANALYTICAL
CHEMISTRY LABORATORIES
WHO NEEDS VALIDATION?
According to USACE Engineer Regulation 1110-1-263, CHEMICALDATA QUALITY MANAGEMENT FOR HAZARDOUS WASTE REMEDIAL ACTIVITIES:
Laboratory validation shall apply to all commerciallaboratories directly or indirectly providing chemicalanalysis support to USACE HTRW investigative and remedialactivities.
All commercial laboratories that support USACE HTRW responseactivities must obtain a USACE laboratory validation prior tofield studies or sample analyses and must maintain the validatedstatus throughout the contract/project/task order(s) (hereafterreferred to as the contract or project) for the HTRW responseactivities.
HOW TO APPLY FOR A VALIDATION
After a prime architect-engineering firm or a constructioncontractor (hereafter referred to as the prime contractor) isawarded with a contract to support USACE HTRW remedialactivities, the prime contractor will select a subcontractcommercial laboratory for this contract and notify the USACETechnical Manager or Contracting Officer Representative (TM/COR)of its selection. The USACE TM/COR will then submit a writtenrequest for evaluation of the subcontract commercial laboratoryto the USACE Laboratory Validation Committee (hereafter referredto as the Committee) to initiate the laboratory validationprocess. After receipt of the request, the Committee willcontact the laboratory shortly. A commercial laboratory, itself,does not apply for a USACE HTRW laboratory validation. TheCommittee will only respond to a validation request from a USACETM/COR.
WHAT IS THE VALIDATION PROCESS?
The laboratory validation process consists of three majorsequential steps: (1) the Committee reviews the laboratory’squalification documents, (2) the laboratory analyzes a set ofperformance evaluation (PE) samples, and (3) the Committeeconducts an on-site laboratory inspection. The Committee is
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responsible for execution and management of the laboratoryvalidation program.
WHAT KIND OF QUALIFICATION DOCUMENTS?
Typical qualification documents may be in the form of anoff-the-shelf laboratory quality management manual (LQMM) or insome other format which includes a laboratory floor plan,organization chart, instrumentation list, staff resumes,certificates, in-house standard operating procedures, etc. Thedocuments should provide proper information for the Committee toassess the laboratory’s technical capabilities. Upon request, alaboratory should promptly submit its qualification statements tothe Committee for review. If it appears that the laboratory hasthe adequate capabilities to meet project requirements, theCommittee will initiate the next step, PE sample analysis.
WHAT KIND OF PE SAMPLES?
The Committee will provide the laboratory with project-specific PE samples for performance evaluation. The PE samplesmay be in water and/or soil/sediment matrices. Arrangements willbe made with the laboratory for analysis and reporting of thesesamples. The results are considered passing if the results of aparticular method are within statistically established acceptancelimits as determined by the USACE and no procedural problems arefound during a follow-up laboratory inspection. A laboratory mayvolunteer for additional non-project-specific PE samples at itsown cost. A laboratory must pass more than 50 percent of all PEsamples within 40 working days from receipt of the PE samples orthe validation process will be terminated.
WHAT ARE INSPECTION PROCEDURES?
Two Committee representatives will inspect the laboratoryonly after Steps 1 and 2 have been satisfactorily completed. Theon-site inspection which generally takes eight hours includes:(1) an entrance interview with the laboratory management todiscuss USACE QA program, review comments on laboratoryqualification submittals including LQMM, PE sample results,upcoming projects, etc., (2) a follow-up laboratory tour toexamine laboratory facility, instrumentation, operation,maintenance, documentation, etc., and (3) an exit interview tosummarize any deficiencies found and corrective actions required.A laboratory must rectify any deficiencies noted during theinspection prior to an approval for a full validation status.
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After inspection, the Committee will meet to review and determinethe validation status of a laboratory.
WHAT ARE VALIDATION CRITERIA?
The USACE basically follows Federal and/or State laws,regulations, and guidelines and good laboratory practices toevaluate laboratory performance. The validation status of alaboratory depends on whether the laboratory’s PE sample resultsare within USACE established acceptance criteria and noprocedural problems are found during a follow-up laboratoryinspection. The laboratory’s PE sample results will be comparedin the following manner: (1) with the prepared concentrations ofPE samples that are used as the absolute recovery comparators,and (2) with the statistical mean and standard deviationsreported by a group of peer laboratories. The acceptable limitsfor analyte quantitation will be established statistically at 95percent confidence based on referee laboratories’ and/or peergroup results.
HOW MUCH TIME DOES VALIDATION TAKE?
The entire process of laboratory validation generally takesup to 12 weeks depending on a laboratory’s performance andresponsiveness. The prime contractors should plan the projectschedule to allow adequate time for laboratory validationprocess.
WILL A CERTIFICATE BE ISSUED?
USACE will not issue a certificate for validatedlaboratories. However, a letter and a copy of inspection reportwill be sent to each validated laboratory. The letter willspecify the methods and matrices, the project(s), and the timeperiod (usually 18 months) for which the validation is granted.
IS THE VALIDATION UNIVERSAL?
The validation is a parameter, method, and matrix-specificapproval and only applies for USACE HTRW program. However, foreach new contract awarded during the 18-month validation period,a project-specific evaluation is still required. The Committeewill check the laboratory’s validation status and previousperformance to determine if any additional actions are needed.If different parameters, methods, and/or matrices are involved,
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only those PE samples will be sent. If work done for the USACEby the laboratory has been satisfactory, no further actions willbe necessary.
HOW ABOUT SUBCONTRACTING?
A validated laboratory may not subcontract any USACE samplesto a second laboratory without the knowledge and approval of theUSACE TM/COR and the concurrence of the Committee. The secondlaboratory must also be validated for methods, parameters, andmatrices corresponding to the subcontract. Subcontract of PEsample analysis is totally prohibited.
WHAT ARE THE FEES REQUIRED FOR VALIDATION?
There are no direct fees for the laboratory besides the costfor additional PE samples required for failed parameters ornon-project-specific parameters. The current cost for anyadditional or any non-project-specific PE samples ranges from$100 to $300 per method, per matrix, and per shipment. The costshall be reviewed annually and adjusted as necessary withoutnotice to reflect currency value fluctuations or changes inprogram administration costs. The USACE will not pay the costsfor analysis of PE samples and preparation of any qualificationdocuments.
WHERE TO GET MORE INFORMATION
The Laboratory Validation Committee at the USACE HTRWMandatory Center of Expertise (MCX) of the USACE is responsiblefor all aspects of the USACE HTRW laboratory validation program.The Committee meets as needed to propose policy on USACE HTRWlaboratory validation program and to make ultimate decisions onlaboratory-specific validation status. Any questions concerningthe validation program can be directed to the LaboratoryValidation Coordinator.
U.S. Army Corps of EngineersHTRW Mandatory Center of ExpertiseATTN: CEMRD-ED-EC (Laboratory Validation Coordinator)12565 West Center RoadOmaha, NE 68144-3869
Voice: (402) 221-7494FAX : (402) 221-7403
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APPENDIX C
INFORMATION
FOR
COMMERCIAL ANALYTICAL CHEMISTRY LABORATORIES
UNDERGOING VALIDATION
BY
THE U.S. ARMY CORPS OF ENGINEERS
C - 1
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(SAMPLE LETTER)
Dear Laboratory Director:
Your laboratory has been submitted as a candidate forvalidation/revalidation in support of the U.S. Army Corps ofEngineers (USACE) hazardous, toxic, and radioactive waste (HTRW)response activities. Prior to the field studies or sampleanalyses, your laboratory must be validated by the USACE.Enclosed for your information and action are:
(1) Information about the USACE Project(s) that leads tothis validation/revalidation process,
(2) Information for Commercial Analytical ChemistryLaboratories Undergoing Validation by the USACE,
(3) Guidelines for Analyzing and Reporting PerformanceEvaluation Samples (Appendix D), and
(4) Preliminary Questionnaire (Appendix E).
If you decide to obtain a USACE HTRW laboratory validation,please be sure that:
(1) All instructions, including all time deadlines, are readand followed carefully.
(2) The preliminary questionnaire is completed and returnedwith original verification signature(s) within tenworking days from receiving date.
I hope that the information provided in this packet will behelpful to you and answer any questions you may have. If youhave any questions regarding this information or the USACE HTRWlaboratory validation program in general, please contact theLaboratory Validation Coordinator at (402) 221-7494.
Sincerely,
Chief, Environmental, HTRW DivisionHTRW and Engineering Directorate
4 Enclosures
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TO: Laboratory Director/Manager
FROM: USACE HTRW MCX
DATE: 01/21/92
SUBJECT: USACE HTRW Projects and Laboratory Validation
Listed below is some basic information about the USACE HTRWproject(s) that your laboratory will provide analyticalchemistry services. For the details, please contact the primarycontractor and/or refer to the approved final Work Plan.
Laboratory Name: ABC Analytical Laboratory State: MD
1. Project Name: Elmwood County Landfill State: NJContract No: DACWO1-91-C-2345
Sampling Date: 09/01/91 (approximate)
AE/Contractor: DEF, Inc. State: PA
USACE TM: John DowPhone No: (222) 333-4444
HTRW Analyses: VOA, BNA, PCB, PEST, TAL METALS, TRPH, CN.
2. Project Name: Any AFB; Fire Fighting Training 2A State: AZContract No: DACAO1-91-B-1234
Sampling Date: 04/15/92 (approximate)
AE/Contractor: Any Environmental Services, Inc. State: CA
USACE TM: Paula SmithPhone No: (333) 444-5555
HTRW Analyses: RCRA METALS, TRPH, AVO, TPH (Mod. 8015) .
Remarks: The HTRW analyses may involve samples of variousmatrices.
Figure C-1 Sample Laboratory Evaluation Request
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INFORMATION FOR COMMERCIAL ANALYTICAL CHEMISTRY LABORATORIESUNDERGOING VALIDATION BY THE U.S. ARMY CORPS OF ENGINEERS
Please retain this information and a copy of your completedpreliminary questionnaire in your file for future reference.
WHO NEEDS VALIDATION?
According to USACE Engineer Regulation 1110-1-263, CHEMICALDATA QUALITY MANAGEMENT FOR HAZARDOUS WASTE REMEDIAL ACTIVITIES:
Laboratory validation shall apply to all commerciallaboratories directly or indirectly providing chemicalanalyses to support USACE HTRW investigative and remedialactivities.
All commercial laboratories that support USACE HTRW responseactivities must obtain a USACE laboratory validation prior tofield studies or sample analyses and must maintain the validatedstatus throughout the contract/project/task order(s) (hereafterreferred to as the contract or project) for the HTRW responseactivities.
WHAT IS THE VALIDATION PROCESS?
The laboratory validation process consists of three majorsequential steps: (1) review of the laboratory’s qualificationdocuments, (2) analysis of performance evaluation (PE) samples,and (3) on-site inspection of laboratory’s facility,instrumentation, operation, and management.
(1) Step 1. Upon request, a commercial laboratory shouldsubmit its qualification documents within five working days tothe USACE Laboratory Validation Committee (hereafter referred toas the Committee) for review. This submittal may be in the formof an off-the-shelf quality assurance manual or in some otherformat that provides proper laboratory-specific information forthe Committee to assess the laborator's technical capabilities.The information includes, but is not limited to, laboratory floorplan, organization chart, list of major instrumentation, copy ofstaff resumes, laboratory certificates, standard operatingprocedures for nonstandard/modified standard chemical testing,quality assurance/quality control (QA/QC) policy and practice,etc. If it appears that a laboratory has the adequatecapabilities to meet project requirements, the Committee willinitiate Step 2.
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(2) Step 2. The Committee will provide a laboratory withproject-specific PE samples for performance evaluation. Alaboratory may volunteer for additional non-project-specific PEsamples at its own cost. Arrangements will be made with thelaboratory for the analysis and reporting of these samples.Enclosure 3 is a general guidance for PE sample analysis andreporting. Sample-specific instructions will be sent along withthe PE samples and should be followed wherever applicable.Failure to analyze these samples correctly or within the requiredtime frame may result in termination of the validation. Theresults are considered passing if the results of a particularmethod are within statistically established acceptance limits asdetermined by the USACE and no procedural problems are foundduring the Step 3 follow-up laboratory inspection. Normally,only one set of PE samples will be sent to each laboratory. Alaboratory must pass more than 50 percent of all PE sampleswithin 40 working days from receipt of the PE samples or thevalidation process will be terminated. Prior to an on-siteinspection, a laboratory shall submit to the Committee a concisewritten statement describing the problems, solutions, andcorrective actions taken or to be taken for the analyticalparameters failed in the first attempt.
(3) Step 3. Two Committee representatives will inspect alaboratory only after Steps 1 and 2 have been successfullycompleted. The on-site inspection which generally takes eighthours involves:
(a)
(b)
(c)
An entrance interview with the upper laboratorymanagement staff (including laboratory director,managers, QA officer, and project personnel) to discussupcoming USACE project(s), the USACE QA program, theUSACE review comments on the laboratory’s qualificationdocuments, the PE sample results, and the laboratory’sprevious performance on USACE projects, if applicable.
A laboratory tour to determine the adequacy oflaboratory organization, personnel, facility, andequipment and the implementation of adequate analyticalquality and document control, including use of properanalytical methodology, control charts, data and samplehandling, documented corrective action measures,chain-of-custody, etc.
An exit interview to discuss any deficiencies notedduring the inspection and recommended correctiveactions with the laboratory management staff. Thecorrective actions may include the analysis of a secondset of PE samples for failed parameters.
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During the exit interview, a laboratory will be requested tosubmit written responses with supporting documentation to thedeficiencies within ten working days from the inspection date.The Committee will evaluate and determine the validation status.A laboratory must rectify any deficiencies noted during theinspection prior to approval for a full validation status.
WHAT ARE VALIDATION CRITERIA?
The USACE basically follows Federal and/or State laws,regulations, and guidelines and good laboratory practices toevaluate laboratory performance. The validation status of alaboratory depends on whether the laboratory's PE sample resultsare within USACE established acceptance criteria and noprocedural problems are found during a follow-up laboratoryinspection. The laboratory's PE sample results will be comparedin the following manner: (1) with the prepared concentrations ofPE samples that are used as the absolute recovery comparators,and (2) with the statistical mean and standard deviationsreported by a group of referee and/or peer laboratories. Theacceptance limits for analyte quantitation will be establishedstatistically at 95 percent confidence based on peer groupresults.
WHAT DOES A LAB NEED TO PREPARE FOR THE INSPECTION?
Prior to the USACE on-site inspection, a laboratory should befamiliar with all the materials that have been provided by theUSACE. Laboratory key personnel including laboratory director/manager, QA officer, group supervisors, etc., should be residingand available for answering questions during the inspection.
Results of any USACE PE samples should be reviewed prior tothe inspection. Special attention should be placed onunacceptable results. Documented corrective actions forunacceptable results should be made available to the USACEinspector(s) during the inspection. Any data or informationrequested in advance by the USACE inspector(s) should be madereadily available.
The preliminary questionnaire should have been filled out andreturned within ten working days from receipt or at least oneweek before the inspection. A map and/or directions for gettingto the laboratory should also be submitted along with thepreliminary questionnaire.
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HOW MUCH TIME DOES VALIDATION TAKE?
process of laboratory validation generally takesdepending on a laboratory's performance and
responsiveness. A simplified flow diagram for the entirevalidation process is shown in Figure C-2 (Pages C-9 thru C-10).
WILL A CERTIFICATE BE ISSUED?
USACE will not issue a certificate for validatedlaboratories. However, a letter and a copy of inspection reportwill be sent to each validated laboratory. The letter willspecify the methods and matrices, the project(s), and the timeperiod (usually 18 months) for which the validation is granted.
IS THE VALIDATION UNIVERSAL?
The validation is a parameter, method, and matrix-specificapproval and only applies for USACE HTRW program. However, foreach new contract awarded during the 18-month validation period,a project-specific evaluation is still required. The Committeewill check the laboratory’s validation status and previousperformance to determine if any additional actions are needed.If different parameters, methods and/or matrices are involved,only those PE samples will be sent. If work done for the USACEby the laboratory has been satisfactory, no further actions willbe necessary.
HOW ABOUT SUBCONTRACTING?
A validated laboratory may not subcontract any USACE samplesto a second laboratory without the knowledge and approval of theUSACE TM/COR and the concurrence of the Committee. The secondlaboratory must also be validated for methods, parameters, andmatrices corresponding to the subcontract. Subcontract of PEsample analysis is totally prohibited.
WHAT ARE THE FEES REQUIRED FOR VALIDATION?
There are no direct fees for the laboratory besides the costfor additional PE samples required for failed parameters ornon-project-specific parameters. The cost for any additional ornon-project-specific PE samples range from $100 to $300 peranalytical parameter, per matrix, and per shipment. The costshall be reviewed annually and adjusted as necessary without
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notice to reflect currency value fluctuations or changes inprogram administration costs. The USACE will not pay the costfor analysis of PE samples and preparation of any qualificationdocuments.
HOW TO RENEW VALIDATION
On a monthly basis, the Committee will notify USACE TM/CORsof laboratories with expiring validation (i.e., within threemonths). If the USACE TM/CORs intend to use those laboratoriesbeyond the expiration dates, the USACE TM/CORs will requestrevalidations. For a commercial laboratory with an expiredvalidation status, its validation will be renewed when nextcontract is awarded. After considering use of the laboratory andits previous performance, the Committee will determine which ofthe three steps will apply to the revalidation process.
WHAT TO DO WITH THE PRELIMINARY QUESTIONNAIRE
The enclosed preliminary questionnaire shall be completed andreturned to the Committee within ten working days from the dateof receipt. Any supporting documents should be attached ifavailable.
WHERE TO GET MORE INFORMATION
The Laboratory Validation Committee at the HTRW MandatoryCenter of Expertise (MCX) of the USACE is responsible for allaspects of the USACE HTRW laboratory validation program. Anyquestions concerning the validation program can be directed tothe Laboratory Validation Coordinator.
U.S. Army Corps of EngineersHTRW Mandatory Center of ExpertiseATTN: CEMRD-ED-EC (Laboratory Validation Coordinator)12565 West Center RoadOmaha, NE 68144-3869
Voice: (402) 221-7494FAX: (402) 221-7403
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Figure C-2. Flow Diagram of Commercial Laboratory ValidationProcedures
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Figure C-2. Flow Diagram of Commercial Laboratory ValidationProcedures (continued)
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APPENDIX D
GUIDELINES
FOR
ANALYZING AND REPORTING
PERFORMANCE EVALUATION SAMPLES
FROM
THE U.S. ARMY CORPS OF ENGINEERS
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GUIDELINESEVALUATION
FOR ANALYZING AND REPORTING PERFORMANCESAMPLES FROM THE U.S. CORPS OF ENGINEERS
Please read and follow these guidelines for analyzing andreporting performance evaluation samples and retain theseguidelines in your file for future reference.
GENERAL INFORMATION
The guidelines addressed below are the general requirementsfor performance evaluation (PE) samples analysis and reporting.Please follow them explicitly. Sample-specific guidelines willbe provided with each shipment of PE samples and shall befollowed wherever applicable. The sample-specific guidelinessupersede these general guidelines.
POINTS OF CONTACT
A Laboratory Validation Committee (hereafter referred to asthe Committee) at the HTRW Mandatory Center of Expertise (MCX) ofthe U.S. Army Corps of Engineers (USACE) is responsible for allaspect of the USACE HTRW laboratory validation program. ALaboratory Validation Coordinator (hereafter referred to as theCoordinator) is the point of contact of the Committee. Anyquestions concerning the USACE HTRW laboratory validation programshould be directed to the Coordinator at the following mailingaddress and phone number:
U.S. Army Corps of EngineersHTRW Mandatory Center of ExpertiseATTN: CEMRD-ED-EC (Laboratory Validation Coordinator)12565 West Center RoadOmaha, NE 68144-3869
Voice: (402) 221-7494FAX: (402) 221-7403
PE SAMPLES
Most PE samples will be sent out from the analyticallaboratory of USACE Waterways Experiment Station (WES) inVicksburg, Mississippi, except for petroleum hydrocarbons, oiland grease, and explosives which will be sent out from the USACEMissouri River Division Laboratory (MRDL) in Omaha, Nebraska. PEsamples are method- and matrix-specific. A laboratory has to
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pass all PE samples of different matrices available from theUSACE to be considered for multimedia approval.
ANALYTICAL METHODS
A commercial laboratory shall use contract-requiredanalytical methods for all PE sample analyses unless otherwiseinstructed by the Coordinator. The contract-required analyticalmethods are usually specified in a project-specific Scope ofServices or Chemical Data Acquisition Plan. The followinganalytical methods from SW-846 (1986 or the most recentlypromulgated version) and EPA-600/4-79-020 (revised 3/1983) arethe most commonly specified methods for the respective analyses.Any changes in analytical methods from the contract-requiredanalytical methods must be pre-approved by the Committee.
PARAMETERS METHODS
Volatile Organic Compounds (VOA)Halogenated Volatile Organic Compounds (HVO)Aromatic Volatile Organic Compounds (AVO)
Semivolatile Organic Compounds (BNA)Organochlorine Pesticides (PEST)Polychlorinated Biphenyls (PCB)Phenols (PHENO)
Chlorinated Herbicides (HERB)Polynuclear Aromatic Hydrocarbons (PAH)Nitroaromatics and Nitramines (EXPLO)
Total Recoverable Petroleum Hydrocarbons (TRPH)Total Recoverable Oil and Grease (O&G)Total Petroleum Hydrocarbons (TPH)
Trace Metals (METAL)ArsenicMercurySelenium
Cyanide (CN)Total Organic Carbon (TOC)Common Anions (ANION)Phenolics (PHENL)
8240A8010A8020
8250/8270A808080808040A
8150A8100/83108330 (draft)
418.1413.1/413.28015 (mod.)
6010A7060/70617470/74717740/7741
9010A/90129060300.0/300s9065/9066/9067
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PARAMETERS METHODS
Total Hardness (HARD) 130sAlkalinity (ALKAL) 310sChemical Oxygen Demand (COD) 410s
Total Dissolved Solids (TDS) 160.1Total Suspended Solids (TSS) 160.2
ANALYSIS OF PE SAMPLES
A laboratory must use project-required analytical methods foranalyses of all project-specific PE samples unless otherwiseinstructed by the Coordinator. A laboratory’s practicalquantitation limits for each analytical method must meet or belower than those specified in the method. The soil/sediment PEsamples could be real world environmental samples which containcertain analytes of high concentrations. Special attention isneeded to reduce or correct the interference caused by theanalytes of high concentrations. Subcontract of PE sampleanalysis is prohibited.
INTERNAL QC ANALYSES
A laboratory shall conduct and report all method-requiredinternal QC analyses. The minimum internal QC analyses requiredfor PE samples include:
- method blanks for all PE sample analyses,
- surrogate spikes for all organic PE sample analyses,
- laboratory control samples (LCSs), second columnconfirmation, etc., whenever applicable,
- replicates, matrix spikes, and matrix spike duplicates forall soil/sediment PE sample analyses, and
- replicates, matrix spikes, and matrix spike duplicates onspiked reagent water for all water PE samples.
DATA REPORTING PACKAGE
A laboratory may use its standard data package to report PEsample results, however, the data package should be sequentiallynumbered and contain as a minimum the following information:
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a. Table of contents
b. A case narrative including a list of PE samplesanalyzed/reported and problems encountered with PE sampleanalysis.
c. A Chain-of-Custody report.
d. Sample preparation information including samplepreparation date, method citations for sample digestion,extraction, solvent exchange, concentration, cleanup, etc.
e. Analytical results for all target analytes plus methodcitations and laboratory practical quantitation limits.
f. Summary of method-specific QC results and assessments ofprecision and accuracy.
g. Phone conversation records on major issues related to PEsample analysis.
The analysis results shall identify and quantify all targetanalytes listed in the required analytical method, includingestimated values and the quantitation limits for target analytesnot detected. Except for petroleum hydrocarbons PE samples, allsoil/sediment PE sample analyses shall be reported on adry-weight basis along with percent moisture. For petroleumhydrocarbons PE samples, the results shall be reported on an“as-received” basis, i.e., no correction should be made formoisture content. Neither should any data be corrected for spikerecoveries nor for any contamination found in trip blank orlaboratory's method blank. Raw data including sample preparationand run log, calibration, chromatograms, calculation, etc., arenormally not required for PE sample data package unless requestedby the Coordinator.
WHEN TO REPORT
Normally, written reports for all PE sample analyses are tobe received by the sample originators at WES and/or MRDL within20 working days after receipt of the samples. For fastturnaround projects or reanalysis of additional PE samples, alaboratory shall return the results within five or ten workingdays, depending on the number of PE samples to be analyzed.Failure to analyze these samples successfully or within therequired time frame may result in termination of the validationprocess. It is a laboratory's responsibility to keep the
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Committee informed of any problems with PE sample analyses thatwould affect return of the results in a required time frame.
WHERE TO REPORT
All PE sample results except for total recoverable petroleumhydrocarbons, total petroleum hydrocarbons, total recoverable oiland grease, and explosives shall be returned to WES:
U.S. Army Corps of EngineersWaterways Experiment StationATTN: CEWES-EE-C (Ann B. Strong)3909 Halls Ferry RoadVicksburg, MS 39180-6199
The PE sample results for total recoverable petroleumhydrocarbons, total petroleum hydrocarbons, total recoverable oiland grease, and explosives shall be returned to MRDL:
U.S. Army Corps of EngineersMissouri River Division LaboratoryATTN: CEMRD-ED-L (Doug Taggart)420 S. 18th StreetOmaha, NE 68102-2586
A complete copy of all PE sample results shall be sent to theCommittee:
U.S. Army Corps of EngineersHTRW Mandatory Center of ExpertiseATTN: CEMRD-ED-EC (Laboratory Validation Coordinator)12565 West Center RoadOmaha, NE 68144-3869
CRITERIA FOR EVALUATION OF PE SAMPLE RESULTS
The laboratory PE sample results will be compared in thefollowing manner: (1) with the prepared concentrations of PEsamples that are used as the absolute recovery comparators, and(2) with the statistical mean and standard deviations reported bya group of referee and/or peer laboratories. The acceptablelimits for analyte quantitation will be established statisticallyat 95 percent confidence based on peer group results. If onlyminor errors which are attributable to data calculation,transcription, etc. appear in PE samples analysis, a laboratorywill have an opportunity to provide revised data. If a
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laboratory is asked to check its analytical data, the laboratoryshould return revised data within five working days.
WHAT IS NEXT AFTER PE SAMPLE ANALYSIS?
Possibly an on-site laboratory inspection. After datarevisions, a commercial laboratory must pass, as a minimum, morethan 50 percent of all PE samples, including project-specific andnon-project-specific PE samples, within 40 working days fromreceipt of the first set of PE samples to trigger the on-sitelaboratory inspection process. Prior to an inspection, alaboratory shall promptly submit to the Coordinator a concisereport about the problems, solutions, and corrective actions onthe PE sample parameters failed on its first attempt. Afterreceipt of this report, the Coordinator will contact thelaboratory to schedule an on-site inspection within two weeks.
During an on-site laboratory inspection, the USACE inspectorswill investigate the problems and solutions for the failed PEsamples. Additional PE samples may be required, as recommendedby the inspectors and concurred by the Committee, for alaboratory to demonstrate that all problems associated with thefailed parameters have been satisfactorily corrected. Ifadditional PE samples are analyzed, a laboratory shall returnanalytical results of the additional PE samples within five orten working days after receipt of the PE samples depending on thenumber and type of the additional PE samples. The cost ofadditional PE samples will be borne by the laboratory (currentlyabout $100 to $300 per method, per matrix, and per shipment.)
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APPENDIX E
PRELIMINARY QUESTIONNAIRE
FOR
THE U.S. ARMY CORPS OF ENGINEERS
VALIDATION PROGRAM FOR
ANALYTICAL CHEMISTRY LABORATORIES
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PRELIMINARY QUESTIONNAIRE
This questionnaire is designed to elicit all the informationrequired prior to an on-site survey. Please make a concertedeffort to furnish the information as accurately and concisely aspossible. For convenience, the questionnaire has been dividedinto seven sections:
Section 1: General Laboratory Information
Section 2: Organization and Personnel
Section 3: Laboratory Facilities and Equipment
Section 4: Analytical Instrumentation
Section 5: Technical Services
Section 6: Chemical Analyses
Section 7: Federal RCRA Compliance
In each section, the questions are styled for the ease of thelaboratory’s response. In many cases only a check ( ) isrequired. Other questions call for a short answer; clarity andbrevity should hallmark your response. If you need more space,please continue on blank sheets and attach them to thequestionnaire.
Each section is independent, so that the different sectionsmay be distributed to the most knowledgeable persons in thelaboratory who can complete their parts independently. Finally,management should assemble and check all responses beforereturning the completed forms. The completed preliminaryquestionnaire shall be returned to the USACE within ten workingdays from the date of receipt or prior to the on-site laboratoryinspection.
The completed questionnaire will be used by the USACElaboratory inspectors to prepare the upcoming on-site laboratoryinspection. The time involved in the on-site inspection can beminimized by a thorough presentation of the information sought inthe questionnaire. Therefore, it is advantageous to both yourlaboratory and the inspection team if these questions areanswered precisely and completely.
Thank you for your cooperation.
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SECTION 1. GENERAL LABORATORY INFORMATION
Laboratory Name:
Street Address:
Mailing Address:
3. Telephone No.: FAX No.:
4. Name of Laboratory Director:
Name of Laboratory Manager:
Name of QA Officer:
5. Does your laboratory routinely participate in any of thefollowing QA programs? If yes, please check the brackets,complete the attached CHART E-1 (Page E-6), and submit copiesof the laboratory certificates, a list of approved analyticalparameters and the two most recent results of any performanceevaluation sample analyses. [ ] Check if attached.
a. Department of Defense QA Programs:
[ ] U.S. Army Corps of Engineers (USACE)[ ] U.S. Army Environmental Center (USAEC)[ ] U.S. Air Force Occupational and Environmental Health
Laboratory QA/QC Audit (USAFOEHL)[ ] U.S. Navy Energy and Environmental Support Activity
(NEESA)[ ] Naval Assessment and Control of Installation
Pollutants (NACIP)
b. USEPA QA Programs:
[ ] EMSL/Cincinnati Water Supply QA Program[ ] EMSL/Cincinnati Water Pollution QA Program[ ] Office of Solid Waste Quarterly Audit Program[ ] Remedial Engineering Management (REM) or Alternative
Remedial Contracts Strategy (ARCS) SubcontractLaboratory
[ ] Radiochemistry Laboratory Intercomparison Study
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[ ] DischargeClients
c. Other Federal
Monitoring Program for NPDES Permitted
Agencies:
[ ][ ][ ][ ][ ][ ][ ]
DOE Hazardous Waste Remedial Action Program (HAZWRAP)USDA Plant Protection and Quarantine ProgramNIST National Voluntary Laboratory Accreditation
Program (NVLAP) for AsbestosU.S. Geological Survey Performance Evaluation ProgramNIOSH Proficiency Analytical Testing Program (PAT)NIOSH Asbestos Analyst RegistryNuclear Regulatory Commission (NRC) Broadscope
Materials License
6. Does your laboratory currently participate in any statecertification/accreditation programs? [ ] Check if yes andcomplete the attached CHART E-2 (Page E-7).
7. List major USEPA or USACE contracts held in the last twoyears that included soil/sediment/sludge analyses forhazardous, toxic, and radioactive wastes.
Approx. No.Agency Project Name of Samples Analytes
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8. Is your laboratory currently approved by the Small BusinessAdministration (SBA) for Section 8(a) program? [ ] Check ifyes and submit copies of the SBA approval letter/documents.
9. This questionnaire is completed/assembled by:
Date / / NAME TITLE
and reviewed/approved by:
NAME TITLE
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1.
2.
3.
4.
5.
6.
7.
SECTION 2. ORGANIZATION AND PERSONNEL
Provide an organization chart of the laboratory, includingany field operations or other internal affiliations to showhow the laboratory fits into the general organizationalstructure. If attached, please check. [ ]
How many years in operation?_________
What is the total number of laboratory employees?______Has this number increased over the past five years?Check if yes [ ]
What portion of the laboratory employees are technical staff?Number__________ Percentage__________
What portion of your technical staff participated in a formaltraining program related to improving work performance duringthe past year? Number_________ Percentage__________
What was your turnover rate during the last 12 months?
(A) Administrative Staff:
Number__________ Percentage_________
(B) Technical Staff:
Number Percentage________
Complete CHART E-3 (Pages E-9 thru E-16) for all technicalstaff. Use a separate block for each employee and makeadditional copies if needed.
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SECTION 3. LABORATORY FACILITIES AND EQUIPMENT
1. Please provide a laboratory floor plan and complete CHARTE-4. (* Note: The adequacy of laboratory facilities will bechecked by USACE inspectors.)
CHART E-4
Lab Name: Page 1 of 2
Ade-* AdditionalItem Description quate Information
Building in Use Total (Sq Ft)
Office Space Total (Sq Ft)
Lab Space Total (Sq Ft)
Bench-top Space Total (Sq Ft)
Bench Hoods No. ____ (Ft/min)
Avai - Ade-* AdditionalItem able quate Information
Storage Space - Chemicals
Sample Storage - General
Secured Space
Refrigerated Space
High Hazardous Samples
Controlled Area - Temperature
Humidity
Shielded
Clean Rooms
Compressed Air
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CHART E-4Page 2 of 2
2
*Avai - Ade- Additional
Item able quate Information
Vacuum
Water Supply - Distilled
Deionized
Ammonia - free
C0 - free
Bacteriologically Suitable
Safety Equipment - Fire Alarm
Fire Extinquishing Equipment
Emergency Showers
Eye Fountains
Safety Glasses & Gloves
Hazardous Area Escape
Flammable Material Storage
OSHA Signs
Glassware Washing Equipment
Disposal Equipment - BrokenGlass, Contaminated Solvent,Material, etc.
Laboratory InformationManagement System (LIMS)
Building Security System
Mobile Laboratories
Facilities as a Whole
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2. FIELD SAMPLING/ANALYSIS. Please complete CHART E-5 if thelaboratory conducts field sampling/analysis. (* Note: Theadequacy of laboratory facilities and equipment shall be checkedby USACE inspectors.)
CHART E-5
Lab Name:________________________ Page 1 of 1
ItemAvai -able
Dedicated Lab Space & Hoods
Bottle Preparation Area
Sample Coolers
Chain-of-Custody Record
Sample Labels and Tags
Sampling Tools - Soil
Sediment
Sludge
Surface Water
Ground Water
Ambient Air
Emission Source
Other (specify)
Field Testing/MonitoringEquipment - Sniffers
Portable GCS
Geiger Counters
Other (specify)
Mobile Laboratories
Ade-* Additionalquate Information
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SECTION 4. ANALYTICAL
CHART E-6
GC INSTRUMENTS:
INSTRUMENTATION
1. SUMMARY OF Page 1 of 1
8000 series GC methods in SW-846 (3rd Edition, 1986).The adequacy of analytical instrument will be checked by USACE inspectors.Detectors, condition, autosamplers, modifications, etc.
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CHART E-6
2. SUMMARY OF GC/MS INSTRUMENTS: Page 1 of 1
Model Age Use for Ade-*No. Manufacturer Number Yrs Method quate Comments
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
Iclude MS, LC/MS, GPC, etc., if available.8000 series GC methods in SW-846 (3rd Edition, 1986).The adequacy of analytical instrument will be checked by USACE inspectors.Detectors, condition, autosamplers, modifications, etc.
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CHART E-6
3. SUMMARY OF AA/ICP INSTRUMENTS: Page 1 of 1
Model AgeNo. Manufacturer Number Yrs
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
Use for Ade-*Method quate Comments
Include ICP/MS, microwave digester, etc., if available.8000 series GC methods in SW-846 (3rd Edition, 1986).The adequacy of analytical instrument will be checked by USACE inspectors.Detectors, condition, autosamplers, modifications, etc.
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CHART E-6
4. SUMMARY OF OTHER INSTRUMENTS: Page 1 of 1
Model Age Use for Ade-*No. Manufacturer Number Yrs Method quate Comments
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
Include autoanalyzer, UV/VIS, IR, HPLC, IC, SEM, X-ray instrument, radioactivitycounter/system, analytical balance, etc.8000 series GC methods in SW-846 (3rd Edition, 1986).The adequacy of analytical instrument will( be checked by USACE inspectors.Detectors, condition, autosamplers, modifications, etc.
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SECTION 5. TECHNICAL SERVICES
1.
2.
3.
4.
Laboratory Name:_____________________________________________
Please check the types of technical services routinelyprovided at this laboratory.
[ ] Environmental [ ] Pharmaceutical [ ] Metallurgical[ ] Ecological [ ] Clinical [ ] R&D[ ] Radiochemical [ ] Agricultural [ ] Other (specify)[ ] Geotechnical [ ] Food Quality
Please check the types of samples routinely analyzed at thislaboratory.
[ ] Drinking Water [ ] Air [ ] Hazardous Waste[ ] Waste Water[ ] Soil/Sludge[ ] Sediment
Please check thethis laboratory.
[ ] Asbestos [ ] Mixed Waste[ ] Fuel Oil [ ] Other (specify)[ ] Wipe Sample
types of analyses routinely conducted at
A. Organics:
Organic Compounds[ ] Volatile[ ] Semivolatile Organic Compounds[ ] Organic compounds using Isotope Dilution Techniques[ ] Organochlorine Pesticides
[ ] Organophosphorus Pesticides[ ] Polychlorinated Biphenyls[ ] Congener Specific Polychlorinated Biphenyls[ ] Polynuclear Aromatic Hydrocarbons
[ ] Chlorinated Herbicides[ ] Dioxins and Furans[ ] Nitroaromatics/Nitramines/Explosives[ ] Other (specify)_____________________________________
[ ] Perform any of the above analyses on an oily matrix.[ ] Perform any of the above analyses on a plant/animal
tissue matrix.[ ] Perform any of the above analyses on dioxin
contaminated samples.[ ] Perform any of the above analyses on mixed waste
samples.
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B. Metals:
[ ][ ][ ][ ][ ][ ]
[ ][ ]
[ ]
[ ]
c. Wet
[ ][ ][ ][ ]
[ ][ ][ ][ ]
[ ][ ][ ]
General Metals AnalysisMicrowave DigestionHexavalent ChromiumOrgano-Lead, Tin and MercuryMetals analyses using neutron activationOther (specify)______________________________________________
Perform any of the above analyses on an oily matrix.Perform any of the above analyses on a plant/animaltissue matrix.Perform any of the above analyses on dioxincontaminated samples.Perform any of the above analyses on mixed wastesamples.
Chemistry:
Anions (C1-, F-, NO2
-, NO3
-,SO4
2-,PO4
3-, etc.)Physical (TDS, TSS, Conductivity, pH, etc.)Oxygen DemandsNutrients
PhenolsOil and GreasePetroleum HydrocarbonsTotal Organic Carbon
Total Organic HalidesRadioactivityOther (specify)______________________________________________
D. RCRA Characteristics:
[ ][ ][ ][ ]
IgnitabilityReactivityCorrosivityToxicity
E. Leaching Procedures:
[ ] Toxicity Characteristic Leaching Procedure[ ] Extraction Procedure Toxicity[ ] California Leach[ ] ASTM Leach
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F. Radiochemical:
[ ][ ][ ][ ]
[ ][ ][ ][ ]
[ ][ ][ ]
Gross Alpha/BetaRadium 226/228TritiumGamma-Emitting Radionuclides
Total/Isotopic UraniumTotal/Isotopic ThoriumTransuranic Alpha-EmittersStrontium 89/90
Isotopic PlutoniumRadonOther (specify)__________________________________
G. Physical:
[ ][ ][ ]
[ ]
[ ][ ][ ][ ]
[ ][ ][ ]
[ ]
[ ]
ViscosityBulk DensityProximate/Ultimate Analysis (percent moisture,percent ash, volatile matter, C, H, S, N, O)Chlorine
Total SulfurForms of SulfurFuel Oil FingerprintingSpecific Gravity
Percent Water (Karl Fisher Test)Heat ContentsOther (specify)___________________________________
Perform any of the above analyses on dioxincontaminated samples.Perform any of the above analyses on mixed wastesamples.
H. Air:
[ ][ ][ ][ ]
[ ][ ][ ]
Summa CanistersTenax TubesCarbon Molecular Sieves/Charcoal TubesTedlar Bags
Polyurethane Foam FiltersXAD Resinsother (specify)____________________________________
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[ ] Performs metals analyses on cellulose membranefilters.
[ ] Performs metals analyses on air samples using anannular denuder.
I. Asbestos:
[ ] Polarized Light or Phase Contrast Microscopy[ ] Scanning Electron Microscopy[ ] Transmission Electron Microscopy[ ] X-Ray Diffraction
J. Biological:
[ ] AMES Mutagenicity Testing[ ] Biological Oxygen Demand[ ] Chlorophyll A[ ] Bacteriological (fecal coliform/streptococcus, etc.)
[ ] Acute Toxicity Bioassay[ ] Chronic Toxicity Bioassay[ ] Other (specify)_____________________________________
K. Geotechnical:
[ ] Atterberg Limits[ ] Permeability[ ] Cation Exchange Capacity[ ] Porosity
[ ] Shear Strength[ ] Grain Size[ ] Other (specify)______________________________________
[ ] Perform any of the above analyses on dioxincontaminated samples.
[ ] Perform any of the above analyses on mixed wastesamples.
5. Do you perform field sampling activities? Yes [ ] N o [ ]
6 . Do you perform field testing activities? Yes [ ] N o [ ]
7. Do you perform field monitoring activities? Yes [ ] N o [ ]If yes, please check nature of field monitoring activity:
[ ] Water Quality [ ] Air-Ambient [ ] Radiation[ ] Estuaries [ ] Air-Source [ ] Other (specify)[ ] Oceans [ ] NPDES
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8. Do you participate in enforcement actions, emergencyepisodes, or special studies? Please specify.
9. Are/were you an USEPA CLP RAS contract laboratory? If yes,please provide the following information.
[ ]
[ ]
[ ]
[ ]
10. Are
Volatile Organics Expiration Date:
Organics
Inorganic
Dioxin
you an USEPA
Expiration Date:
Expiration Date:
Expiration Date:
SAS contract laboratory? Ifprovide the following information.
Approx. No.Project Name of samples
/ /
/ /
/ /
yes, please
Analytes
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11. Is your laboratory an AIHA accredited laboratory and/or haveyour laboratory successfully participated in NIOSHProficiency Analytical Testing (PAT) Program for air sampleanalysis? Yes [ ] No [ ]proficiency testing that yourattach copies of the two most
[ ] METALS [ ] SILICA [ ]
If yes, please check thelaboratory participated in andrecent rounds of PAT results.
ASBESTOS [ ] ORGANIC SOLVENTS
12. Does yourAnalysis?TO-14).
Method
laboratory conduct USEPA Compendium Air Sampling/If yes, please list below which methods (TO-1 thru
Total No.of SamplesProject Name
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SECTION 6. CHEMICAL ANALYSES
All sample analyses of water, soil, sediment, sludge, orwaste shall be performed with standard USEPA methods, ifavailable and appropriate. All method specified procedures mustbe followed exactly with no deviations unless modifications arespecifically authorized by the USACE TM/COR. When a standardUSEPA method is not available, the USACE TM/COR may approve theuse of other methods (USEPA CLP, ASTM, USGS, NIOSH, DOE, andAPHA/AWWA/WPCF methods). The standard USEPA methods refer tomethods in the following publications, including the latestapproved or promulgated revisions from USEPA.
1.
2.
3.
4.
5.
6.
Test Methods for Evaluating Solid Wastes, SW-846, ThirdEdition, Revision 0, September 1986 and Revision 1,July 1992.
Methods for Chemical Analysis of Water and Wastes,EPA-600/4-79-020, March 1983.
Guidelines Establishing Testing Procedures for theAnalysis of Pollutants, 40 CFR Part 136, October 26,1984.
Prescribed Procedures for Measurement of Radioactivity inDrinking Water, EPA-600/4-80-032, August 1980.
Radiochemical Analytical Procedures for Analysis ofEnvironmental Samples, EMSL-LV-0539-17, March 1979.
Compendium of Methods for the Determination of ToxicOrganic Compounds in Ambient Air, EPA/600/4-89/017,June 1988.
The USEPA CLP methods refer to analytical parameters includedin the appropriate USEPA Contract Laboratory Program Statement ofWork and/or the most current revision:
1.
2.
3.
Statement of Work for Organic Analysis, Multi-Media,Multi-Concentration, Document Number 0LM02.0 includingRevision 0LM02.1.
Statement of Work for Organic Analysis, Multi-Media,High-Concentration, SOW Number Revision 9/88 includingRevision 4/89.
Superfund Analytical Methods for Low Concentration Waterfor Organics Analysis, SOW Number Revision 10/92.
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4.
5.
6.
7.
EM 200-1–11 Jul 94
Statement of Work for Inorganics Analysis, Multi-Media,Multi-Concentration, Document Number ILM03.0.
Statement of Work for Inorganics Analysis, Multi-Media,High-Concentration, Document Number IHCO1.3.
Superfund Analytical Methods for Low Concentration Waterfor Inorganics Analysis, SOW Number Revision 10/91.
Statement of Work for Analysis of PolychlorinatedDibenzo-P-Dioxins (PCDD) and PolychlorinatedDibenzofurans (PCDF), Multi-Media, Multi-Concentration,Document Number DFLM01.0 including Revision DFLM01.1,September 1991.
The ASTM methods refer to the Annual Book of ASTM Standards,Section 11, Water and Environmental Technology, 1993 or the mostcurrent revision, published by the American Society for Testingand Materials.
The USGS methods refer to the Techniques of Water-ResourcesInvestigations of the United States Geological Survey, Book 5,Third Edition, 1989 or the latest revised edition, published bythe United States Geological Survey, U.S. Department of Interior.
The NIOSH methods refer to the Manual of Analytical Methods,Third Edition, 1984 and all supplements and revisions, publishedby the National Institute for Occupational Safety and Health,U.S. Department of Health and Human Services.
The DOE methods refer to the DOE Methods for EvaluatingEnvironmental and Waste Management Samples, DOE/EM-0089T,Revision 1, March 1993 and the latest update or addendum,published by the U.S. Department of Energy.
The APHA/AWWA/WPCF methods refer to Standard Methods for theExamination of Water and Wastewater, 18th Edition, 1992 or thelatest published edition, published jointly by the AmericanPublic Health Association, the American Water Works Association,and the Water Pollution Control Federation.
If your laboratory routinely uses an alternate method or amodification of a referenced method above, please provide therequested information for each such case in CHART E-7 (PageE-32), "ALTERNATE OR MODIFIED ANALYTICAL METHODS".
In CHART E-8 (Page E-33), "OTHER ANALYTICAL METHODS", pleaseprovide information on important tests performed by yourlaboratory that are not included in the reference methods above.
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CHART E-7
ALTERNATE OR MODIFIED ANALYTICAL METHODS
Laboratory Name:
1. Test:
2 . If this is a modification of a referenced method,A. Which reference method (give manual name and pages)?
B. Purpose of modification:
C. Brief description of modification:
3. If this an alternate method,A. Purpose of use of alternate method:
B. Brief description of method:
4. Have you applied to USEPA for approval of this procedure?(c.f., FR, Vol. 38, No. 199, October 16, 1973, Page 28760)
5. If alternate or modified methods will be used for USACEprojects, please attach all validation documentation to provethe method works.
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SECTION 7. FEDERAL RCRA COMPLIANCE
1. Lab Name:
Hazardous Waste Coordinator:
2. Was a RCRA inspection ever done at the lab? If yes, whoperformed the inspection?When was the inspection performed?(Attach a copy of the most recent inspection report.)
3. Generally, what were the results of the inspection?
4. Describe the way hazardous waste is stored at the lab:
5. How does the lab dispose of their waste?
6. Describe the way hazardous waste is managed at the lab:
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Citation: 40 CFR 261 USEPAHazardous Waste
Subpart A - General
EM 200-1–11 Jul 94
Regulations for Identifying
1.
2.
3.
4.
5.
Does the lab generate any hazardous waste? ______
Does the lab generate any hazardous wastes that are excludedfrom regulations under 40 CFR 261.4? ______ Provide citationfor exclusion:________________________________________________________
Has the sample exclusion in 40 CFR 261.4(d) been invoked forthe lab?______ If yes, have all the requirements associatedwith this exemption been met? If not, explain:
Are treatability studies conducted by the lab? _____ Has theState adopted the Treatability Exclusion in 40 CFR 261.4(f)?_____ If yes, has the lab met the requirements of 40 CFR261.4(e) and (f)? ______ If the State has not adopted theexclusion, does the lab have a RCRA Part B Permit fortreatment? ______
Is the lab a conditionally exempted small quantity generator(SQG)?_______ Does the lab generate less than 100 kg/mo ofhazardous waste and less than 1 kg/mo of acute hazardouswaste?______ How much waste does the lab produce each month?_____ Are there records available to substantiate the amountof waste generated each month?______ Are there recordsavailable that substantiate how much waste is being storedon-site at any one time?______ If the lab generates less than100 kg/mo of hazardous waste and less than 1 kg/mo of acutehazardous waste, the lab is a conditionally exempted SQG. Toqualify for this exemption, the lab must meet the following(40 CFR 261.5):
a. Hazardous waste is characterized IAW 40 CFR 262.b. There is never more than 1,000 kg stored on site.c. Waste is sent to a TSDF or a facility that beneficially
reuses the waste, or a state permitted facility.
Are there records to substantiate the above claims?
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6. Does the facility do any of the following (40 CFR 261.6):
a. Recycle materials in a manner constituting disposal?_____b. Burn or send to be burned hazardous wastes in a boiler or
industrial furnace for energy recovery?_____c. Recycle waste containing precious metals?_____d. Reclaim spent lead-acid batteries?_____e. Generate used oil?____
If the lab does any of the above, they are regulated by therequirements of 40 CFR 266 (Standards for the Management ofSpecific Hazardous Wastes).
7. Containers previously holding a hazardous wastes may bereused for other purposes or discarded as a solid waste (40CFR 261.7) if they are emptied by pouring, pumping,aspirating, etc. Containers that once contained an acutehazardous wastes must be tripled rinsed prior to reuse. Whathappens to empty hazardous waste containers?
Are there empty hazardous waste containers on site?_____Have all residues been removed from the containers?_____Have all labels been removed from the containers?_____What happens to empty containers that once contained an acutehazardous waste?
Subpart B - Criteria for Identifying the Characteristic ofHazardous Waste and for Listing Hazardous Wastes
1. Does the lab have a Hazardous Waste Management Plan or anequivalent? _______
Subpart C - Characteristics of Hazardous Wastes
1. Does the facility generate any of the following types ofcharacteristic wastes:
a. Ignitable?____b. Corrosive?____
c. Reactive? _____d. TCLP? __________
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Subpart D - Lists of Hazardous Wastes
1. Does the facility lab generate any of the following listedhazardous wastes:
a. F-listed? _____ c. P-listed? _______b. K-listed? _____ d. U-listed? _______
2. Does the facility understand how to characterize their waste?_____ Is there a plan that describes the procedure?______List examples of the types of waste generated by the lab:
Citation: 40 CFR 262 USEPA RegulationsGenerators
Subpart A - General
1.
2.
3.
4.
Does the facility generate less thanwaste and 1 kg/mo of acute hazardousfacility is a conditionally exemptedstore more than 1,000 kg of waste or
for Hazardous Waste
100 kg/mo of hazardouswaste?_______ If yes, theSQG. Does the facility1 kg of acute waste at
any one time?______If yes, the facility is NOT aconditionally exempted SQG.
Does the facility generates between 100 - 1,000 kg/mo ofhazardous waste or store more than 1,000 kg of waste onsite? _______ If yes, the facility is a SQG.
Does the facility generate more than 1,000 kg/mo?______ Ifyes, the facility is a generator.
Does the generator or SQG have a USEPA identification number(40 CFR 262.12)? What is that number?
Has the facility filed USEPA Form 8700-12, “Notification ofHazardous Waste Activity”?______ Does the USEPA number onthis form match the USEPA number on the manifests?_______
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Subpart B - Manifest
1.
2.
3.
4.
Does the SQG or generator use a manifest when shippinghazardous waste (40 CFR 262.20)?______
Are efforts made to use the consignment states’s manifest?_______If the consignment state does not have a statemanifest, are efforts made to secure a manifest from thegenerator's state (40 CFR 262.21)?_______
Does the facility sign the manifests certifying that a wasteminimization program is in place at the facility?________Is there a waste minimization program in place (40 CFR262.20)?_______
Do the following land ban records accompany the manifests:
a. USEPA Hazardous Waste Number?________b. Corresponding Treatment Standard?________c. Waste Analysis?_______d. Certification if waste meets land ban standards or if
the lab is shipping lab packs for disposal (40 CFR268.7)?______
Subpart C - Pre-Transportation Requirements
1. Does the facility label, mark, and placard waste prior totransportation to disposal? ______ What training has beenprovided to those persons?_______________________________________
Who is responsible for labelling, marking, and placarding thewaste leaving your facility?_____________________________________
2. SQG Requirements (40 CFR 262.34(d)):
A SQG may generate between 100 - 1,000 kg/mo of hazardouswaste and store up to 6,000 kg of hazardous waste on sitewithout a permit. If the quantity stored exceeds 6,000 kg or180 days (270 days if waste must be transported over 200miles to disposal), the SQG will need a TSDF permit forstorage.
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a.
b.
c.
d.e.f.g.
h.i.
j.
k.1.
m.
n.
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Does the facility dispose of its waste over 200 milesaway from the facility?_______Does the facility store hazardous waste more than 180days?______Is more than 6,000 kg of waste stored on site at any onetime?________Is the waste stored in containers (40 CFR 265.170)?_______Are containers in good condition?______Is the waste compatible with the containers?______Is the container always kept closed except when adding orremoving waste?_________Are the containers inspected at least weekly?______Is the date of which accumulation began clearly marked oneach container?_______Is the hazardous waste stored in tanks (40 CFR 265.201)?
Are only compatible wastes stored in the tank?_____Is there sufficient freeboard or containment around thetank?_______If the tank is a continuous feed tank, is there a meansto stop inflow?_______Is the tank, discharge control equipment, and monitoringequipment inspected each operating day?_______
Preparedness and Prevention (40 CFR 265 Subpart C)
c.
a.
b.
d.
e.
f.
g.
h.
Does the facility have an internal communications oralarm system?______Does the facility have means to summons emergencyassistance?_________Does the facility have a portable fire extinguisher?_______Is an adequate volume of water available to firefighters?_______Is adequate aisle space provided in container storagearea?_______Have arrangements been made with the local authorities tofamiliarize them with wastes stored at the site?_______Has an emergency coordinator been designated?Name:_____________________________________Is the following information posted next to the phone?
- Name and telephone number of the emergency coordinator?
- Location of spill control equipment, fire alarm, fireextinguishers, etc.?______
- Are all employees familiar with the proper wastehandling and emergency procedures relevant to theirresponsibilities?_______
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3. Generator Requirements (20 CFR 262.34):
A generator is a person who generates more than 1,000of waste. A generator may accumulate hazardous waste90 days or less without a permit.
a. Does the facility store waste over 90 days?____b. Is the waste stored in containers (40 CFR 265.170)? ______c. Are the containers in good condition?______d. Is the waste compatible with the container?______e. Are the containers always kept closed except when adding
or removing waste? _____f. Are the containers inspected at least weekly? _____
kg/moon site
g. Is accumulation start date marked on each container?______h. Is the container labeled “Hazardous Waste”?______i. Is the hazardous waste stored in tanks (40 CFR 265
Subpart J)?______j. Is the tank integrity good?_____k. Has the tank been adequately designed to hold the waste
both structurally and with respect to compatibility?_____l. Has secondary containment been provided around the tank
(40 CFR 265.192)?_____m. Are only compatible wastes stored in the tank?____n. Is there sufficient freeboard or containment around the
tank?____o. If the tank is a continuous feed tank, is there a meansp. to stop inflow?______
Is tank, discharge control equipment and monitoringequipment inspected each operating day?_____
q. Is tank closure anticipated?_____r. During tank closure how was the disposal of contaminated
soil, structures, and debris handled (40 CFR 265.114)?
Preparedness and Prevention (40 CFR 265 Subpart C)a. Does the facility have an internal communications or
alarm system?_______b. Does the facility have means to summons emergency
assistance?________Does the facility have a portable fire extinguisher?______
c. Is an adequate volume of water available to firefighters?______
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e. Is adequate aisle space provided in container storagearea?
f. Have arrangements been made with the local authorities tofamiliarize them with wastes stored at the site? _____
g. Has an emergency coordinator been designated? ______Name: _____________________________________
Contingency Plan and Emergency Procedures (40 CFR 265Subpart D)a. Does the facility have a Contingency Plan? ______b. Does the plan include a list of emergency equipment? _______c. Does the plan include a description of arrangements with
local emergency authorities? ________d. Does the plan include an evacuation plan? ______e. Have copies of the plan been submitted to the local
authorities? ________f. Has an emergency coordinator been designated?_______
Name: __________________________________
Training (40 CFR 265.16)a. Has training been provided to each employee who handles
hazardous waste?________b. Has an annual update been provided?________c. Are the following records maintained at the facility:
- Job title of each position involving hazardouswaste?_______
- Name of person filling that job?_______- Written job description describing hazardous waste
related activities?________- Written description of the type of training that will
be provided?_______- Documentation that the employees had received
training? ________
4. Satellite Accumulation (40 CFR 262.34(c))
a. Does the facility use satellite accumulationspoints?________
b. Are the containers in good condition?________c. Are the containers compatible with the waste stored in
them?________d. Are the containers kept closed except when adding of
removing waste?______e. Are the containers marked "Hazardous Waste" or others
words that identify the contents? _______
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Subpart D - Recordkeeping and reporting requirements
1.
2.
3.
4.
5.
6.
Are manifests kept on file for at least three years?______
Are Biennial (applicable to generators only) and ExceptionReports kept on file for at least three years?_______
Are waste analysis, waste records, etc. kept on file for atleast three years?______
If the lab is a generator, has a Biennial Report been filedby 1 March of each even numbered year?______ If yes, does thereport include the following:
- Name, address, USEPA ID number for the generator?______- Calendar year covered by the report? ______- Name, address and USEPA ID number of each
you shipped waste to?______- Name, address and USEPA ID number of each
used?______- Description of the waste?________
TSDF facility
transporter
- Description of the effort for waste minimization?______- Waste minimization comparison with previous years?_____- Generator’s certification?______
Has the facility filed any exception reports (40 CFR 262.42)?
Recordkeeping and reporting requirements for SQG (40 CFR262.44):
a. Are manifests kept on file for at least three years?_______b. Are waste analysis, waste records, etc. kept on file for
at least three years?______c. Has the lab filed any exception reports (40 CFR 262.42)?
Subpart E - Exports of Hazardous Waste
1. Does the lab export hazardous waste?______262 Subparts E for requirements.
Subpart F - Imports of Hazardous Waste
1. Does the lab import Hazardous waste?______262 Subpart F for requirements.
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If yes, see 40 CFR
If yes, see 40 CFR
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Citation: 40 CFR 266 USEPA Standards for Management of SpecificHazardous Wastes and Facilities
Subpart E - Used Oil Burned for Energy Recovery
1. Does the lab generate used or waste oil?_______
2. Is the used oil sent to disposal?_______ If yes, the used oilmust be sampled and if characteristic or mixed with a listedhazardous waste the used oil must be managed and disposed ofas a hazardous waste.
3. If the used oil exceeds the parameters listed in the tablebelow, the used oil is considered to be off-specification:
Arsenic 5 ppm maximumCadmium 2 ppm maximumChromium 10 ppm maximumLead 100 ppm maximumTotal Halogens 4,000 ppm maximumFlash Point 100 oF minimum
Does analysis of the used oil indicate all levels less thanthose presented in the table? ______ If yes, the used oil isspecification used oil and hence is not regulated under RCRA.If the used oil exceeds the levels presented in the table, itis considered to be off-specification used oil and the oilmust be burned in an industrial furnace (40 CFR 260.10) or aboiler (40 CFR 260.10).
4 . Does the used oil typically contain over 1,000 ppm totalhalogens?______ If yes, the used oil is presumed to be ahazardous waste unless the generator can prove otherwise.Thus, this used oil becomes a hazardous waste fuel and mustbe burned in boilers and furnaces that are permitted under 40CFR 264. If the hazardous waste fuel oil is stored on site,all generator regulations apply to this waste.
5. Is the oil properly disposed of? ______
a. Specification used oil is not regulated under RCRA,however, the state may have special handling and disposalrequirements.
b. Off-specification used oil must be burned in anindustrial furnace or boiler.
c. Hazardous waste fuel must be burned in permitted furnacesand boilers.
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6.
7.
8.
9.
Is the disposal method documented?_____ Are there records tosubstantiate the characterization of the used oil?______ Arethere records identifying the energy recovery facility usedor the disposal facility used?_____
Does the lab sell/distribute their used oil directly to aburner? ______ Does the lab sell/distribute their used oil toanother marketer?_______ If yes to either question, the lab isconsidered a marketer of used oil.
If the lab is a marketer of off-specification used oil, arethe following requirements fulfilled:
a. Analysis of used oil kept on file for both on-spec andoff-spec used oil?_______
b. Notification to USEPA of off-spec used oil managementactivities? ________
c. Invoice system used?_____ The following items must beincluded in the invoice system:
- An invoice number.- The lab's USEPA ID number and the receiving facility's
number.- The names and address of the generator's facility and
the receiving facility.- The quantity of off-spec used oil to be delivered.- The dates of shipment or delivery.- The following statement: “This used oil is subject to
USEPA regulation under 40 CFR Part 266."
d. Has the lab secured a signed notice from the burner ormarketer certifying: that the facility has notifiedUSEPA of their location and management activities; andthat the burner will only burn the off-spec oil in anindustrial furnace or boiler?______
Recordkeeping requirements for generators of used oil thatmeets specifications:
a. Are copies of the analyses kept for three years?_____b. Does the record include the name and address of the
facilities receiving the used oil?_______c. Does the record include the dates of shipment or
delivery? ______
Recordkeeping requirements for generators ofoff-specification used oil:
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a. Are copies of the invoices kept for three years?______b. Are copies of the required notices kept on file for three
years? ________
10. Does the lab burn used oil for energy recovery? ______ If yes,the requirements of 40 CFR 266.44 must also be met. Checkthe regulations to ensure compliance.
Subpart F - Recyclable Materials Utilized for Precious MetalRecovery
1. Does the lab accumulate precious metals for reclamation?______If yes, has the lab notified USEPA of the reclamationactivities?________ Does the lab use a manifest whentransporting precious metals for reclamation?______
2. Does the lab store recyclable materials?________
a. Does the lab maintain records showing the volume ofmaterials stored at the beginning of the calendaryear? _______
b. Does the lab maintain records showing the volume ofmaterials generated during the calendar year?______
c. Does the lab maintain records showing the volume ofmaterials remaining at the end of the calendar year? _______
3. Are these materials being speculatively accumulated?______If yes, all generator standards apply to these materials.Basically the material is being speculatively accumulated ifthe material is being stored and there is no real plans ormarket for reclamation. See 40 CFR 261.1 (c) for exactdefinition.
Subpart G - Spent Lead-Acid Batteries Being Reclaimed
1. Does the lab store spent batteries? ______ If yes, are these batteries destined for disposal? ______ If yes, thesebatteries are to be managed and disposed of as hazardouswaste. If no, are these batteries destined for reclamation?_____ If yes, has the lab notified USEPA of this activity?______ If the lab is storing spent batteries for reclamation,40 CFR Part 264 applies.
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SECTION 7. FEDERAL RCRA COMPLIANCE (continued)
Review the State regulations and list below any differencesbetween the Federal RCRA requirements and the State'srequirements:
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SECTION 7. FEDARAL RCRA COMPLIANCE (continued)
The lab shall prepare to have the following documents, ifapplicable, ready for review during the inspection.
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
USEPA Notification Form 8700-12
USEPA Identification Number
SQG Permit
RCRA Part A Permit
RCRA Part B Permit
NPDES Permit
Manifests
Waste Analysis Records
Land Ban Records
Exception Reports
Biennial Reports
Annual Reports
Training and Personnel Files
Contingency Plan/Spill Prevention Control andCountermeasure (SPCC) Plan
Agreements with Local Emergency Authorities
Used Oil Records
Hazardous Waste Management Plan
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APPENDIX F
ANALYTICAL PARAMETERS, METHODS, AND FEE SCHEDULE
FOR
THE PERFORMANCE EVALUATION SAMPLES
FROM
THE U.S. ARMY CORPS OF ENGINEERS
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ANALYTICAL PARAMETERS, METHODS, AND FEE SCHEDULE FORTHE PERFORMANCE EVALUATION SAMPLES FROM
THE U.S. ARMY CORPS OF ENGINEERS
The USACE PE samples are parameter, matrix, and methodspecific. Listed below are: the common analytical parameters andmatrices for PE samples that are currently available from theUSACE, the analytical methods that are normally required for thePE sample analyses, and the fee schedule that are currentlycharged for additional or non-project-required PE samples. Thefee schedule of the PE samples is on a per method, per matrix,and per shipment basis.
ANALYTICAL PARAMETERS MATRIX METHODS COST
Volatile OrganicsHalogenated Volatile OrganicsAromatic Volatile Organics
Semivolatile OrganicsSemivolatile OrganicsOrganochlorine PesticidesPolychlorinated BiphenylsPolychlorinated Biphenyls
Chlorinated HerbicidesPhenolsPolynuclear Aromatic HydrocarbonsNitroaromatics and NitraminesNitroaromatics and Nitramines
Petroleum HydrocarbonsPetroleum HydrocarbonsPetroleum HydrocarbonsPetroleum HydrocarbonsOil and Grease
Trace MetalsTrace MetalsCyanide
Total Organic CarbonPhenolicsCommon AnionsTotal HardnessAlkalinityChemical Oxygen Demand
waterwaterwater
watersoilwaterwatersoil
waterwaterwaterwatersoil
watersoilwatersoilwater
watersoilwater
waterwaterwaterwaterwaterwater
8240A8010A8020
8250/8270A8250/8270A808080808080
8150A8040A8100/83108330 (draft)8330 (draft)
418.19071/418.18015 (mod.)8015 (mod.)413.1/413.2
6010A/7000s6010A/7000s9010A/9012
90609065/9066/9067300.0/300s130s310s410s
$100$100$100
$150$150$100$100$100
$100$100$100$150$150
$100$100$150$150$100
$100$100$100
$100$100$100$100$100$100
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APPENDIX G
GUIDANCE
FOR
PREPARATION, HANDLING, AND VALIDATION
OF
PERFORMANCE EVALUATION SAMPLES
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GUIDANCE FOR PREPARATION, HANDLING, AND VALIDATION OFPERFORMANCE EVALUATION SAMPLES
G-1. Introduction. PE samples are an integral part of acomprehensive laboratory validation program and are used toevaluate the performance of the entire laboratory system for aspecific parameter and matrix. This includes sample tracking,preparation, analysis, method selection (i.e., selection ofparticular options within specified standard operatingprocedures), record keeping, and data reduction and reporting.The USACE's HTRW Quality Assurance (QA) Program routinely employsPE samples to validate the performance of a contract laboratoryand to evaluate the quality of data produced by a validatedlaboratory. The USACE has developed a number of PE samples inwater, soil, and sediment matrices for various environmentalanalyses. Other new PE samples in the above matrices and airmatrix are under development to fulfill the USACE’s environmentalmission needs.
a. PE samples used for performance evaluation could beeither single blind or double blind. A single blind PE sample isknown to be an audit sample, but its composition is not known tothe analyst. A double blind PE sample is intended to beindistinguishable from a routine field sample such that alaboratory will not devote more attention to produce non-routineanalytical performance. Use of double blind PE samples isperhaps the most ideal approach to the assessment of laboratoryperformance. However, stability considerations for aqueoussamples and homogeneity concerns for soil samples presentsubstantive obstacles to the effective use of double blind PEsamples. Given these concerns, use of single blind PE samples iscurrently the most effective and economical mechanism formonitoring laboratory performance.
b. The preparation process for PE samples should becarefully planned to ensure the precision, accuracy, andreproducibility of each batch of PE samples. Detailedpreparation procedures should be documented and maintainedin-house per proper USEPA and USACE guidance for legaldefensibility. All chemicals, reagents, and solvents used shouldbe pre-analyzed to ensure that they meet high purityrequirements. Each gravimetric and volumetric measurementdevices such as titrant, balance, and calibrant should becertified against the National Institute of Standards andTechnology (NIST) standards whenever available. Only ASTM classA volumetric glassware should be used for PE sample preparation.Each batch of resulting PE samples should be checked to confirmconcentrations. All PE samples should be refrigerated and storedin the dark to ensure maximum storage life.
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c. Ideally, all PE samples should have the followingcharacteristics:
- Physical similarity to field samples.
- Analyte and interference content similar to field samples.
- Analyte concentrations near the levels expected in fieldsamples, or, in absence of this information, concentrations thatspan the range of the analytical method.
- Behavior similar to actual field samples throughoutlaboratory handling and method manipulations.
- Ability to provide useful information on laboratoryperformance as well as documentation of associated data quality.
d. During the design and development of PE samples, theUSACE must ensure that the following goals are considered andmet.
- Suitability of the materials to mimic real worldenvironmental samples for performance evaluation of sampleprocessing and analysis.
- Homogeneity of the materials in terms of the targetanalyte profile.
- Stability of the materials in terms of the target analyteprofile over an extended time no less than specified holdingtime.
- Long-term availability of a sufficient and reliable supplyof PE samples.
- Legal defensibility of the data associated with PEsamples.
- Minimization of the cost and time required to producethese materials.
G-2. Determinig PE Sample Requirements and Specifications. Asaforementioned, ideal PE samples should be site-specific. Theconstituents (analytes and matrices), concentrations, andassociated acceptance limits for PE samples should be selectedbased on certain key aspects of the specific project: projectgoals and objectives, data quality objectives (DQOs), andanalytical methods to be employed. However, due to the greatnumber and broad variety types of environmental projects and
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programs that the USACE is involved in, site-specific PE samplesare not cost effective and may not be available in a timelymanner. Furthermore, the USACE PE samples are mainly used forvalidation of contract laboratories prior to field sampleanalysis. The continuous monitoring of contract laboratory'sperformance during the time period of active field sampleanalysis is mainly achieved through analysis of split field QAsamples by government QA laboratories, with supplemental PEsamples if needed. Therefore, the USACE PE samples are basicallydesigned and prepared on a non-site-specific basis.
a. Matrix. Ideally, the matrix for the PE samples should berelevant to the problem at hand and must be accuratelycharacterized. The matrix can generally be categorized intowater, soil, sediment, sludge, ash, oil, waste, etc. However,significant matrix differences can be found, for example, betweentwo soil or even two water samples. The design of PE samplesshould include consideration of the origin, mineralogy, andpretreatment of the field samples. Because total site-specificPE samples are not cost effective and/or available in a timelymanner, the USACE normally uses reagent water and real world soiland sediment as matrix materials for preparation of PE samples.By special requests, the USACE can also prepare PE samples withsite-specific sample matrices, such as spiked field samples orspiked well-defined field matrices.
b. Methods. The analytical method or instrumentation to beused for analysis must be considered when selecting or preparingPE samples. PE samples prepared for a highly sensitiveinstrument, such as graphite furnace atomic absorption (GFAA)spectrophotometer, may not be appropriate for a less sensitiveinstrument, such as flame atomic absorption (FLAA)spectrophotometer or inductively coupled plasma (ICP) atomicemission spectrometer. Because most USACE environmental projectsrequest USEPA SW-846 methods for sample analysis, the majority ofUSACE PE samples are designed and prepared for evaluation of alaboratory's capability in SW-846 methods. PE samples for theUSEPA CLP or drinking water methods are also available.
c. Quality Assurance/Quality Control. The laboratoryvalidation process is usually focused on certain specificproblems with a laboratory’s quality assurance/quality control(QA/QC). With proper use of different types of PE samples,specific QA/QC problems can be detected and corrected. Forexample, analytical precision could be verified by duplicate PEsamples that are extremely homogeneous (such as water) andcontains many analytes at midrange concentrations. Matrix spikerecovery problems can be verified by sending a spiked fieldsample and a spiked extract or digest of the same field sample.
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Differences in recoveries between pre- and post-extraction/digestion spikes will demonstrate whether the laboratory’sextraction/digestion process is at fault. Precision data basedon PE samples of clean matrices and on PE samples of real worldmatrices provide information about the true laboratory precisionagainst the precision difficulty associated with the method oncomplex matrices.
d. Analytes. A PE sample must contain target analytes, butit also should contain components that cause known interferenceswhen the target analytes are measured. This approach willuncover whether or not the laboratory is performing interferencecorrection and the extent to which the correction is effective.Sometimes the difficulties encountered by a laboratory in theanalysis of PE samples may be due to limitations of a method oran instrument. When considering candidate PE samples, one shouldobtain as much information as possible about the analytes ofinterest, all possible interfering species, and the limitationsof the method or instrument.
(1) It is common to include problematic and non-problematicanalytes and to evaluate a laboratory’s performance proficiencyon an analyte-by-analayte basis. PE samples that containproblematic analytes that are unstable, reactive, or interferingunder optional preparation/analysis conditions can be used tocheck whether a laboratory takes proper precautions andcorrective actions. Examples of these include: breakdown of DDTand endrin in a dirty gas chromatography (GC) injection port; lossof dichlorobenzene (the most volatile of the semivolatilecompounds) by a poor nitrogen blow-down technique; loss ofphenols caused by incomplete acidification of the sample, a lessthan required extraction time, excess drying out of the extract,etc.
(2) False-positive problems can be identified by looking fordetection of analytes that are purposely left absent.False-negative problems can be identified by adding low levelanalytes and watching for non-detects. Or, the PE samples maycontain isomers of analytes that elute close together and share acommon GC/MS ion (for example, 2,4,5 & 2,4,6-trichlorophenol,4-nitrophenol & dibenzofuran, benzo(a)anthracene & chrysene,benzo(b) & benzo(k) fluoranthene, anthracene & phenanthrene), highlevel of transition metals (especially iron) that exhibitpotentially interfering spectral lines, or excess phthalateesters or elemental sulfur that interferes with pesticide or PCBanalysis. These conditions are designed to mimic problems thatwould occur in analyzing routine field samples.
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(3) PE samples should be designed to evaluate the entireanalytical process. Specific modifications of the composition ofPE samples provide additional checks of specific procedures. Forexample, semivolatile PE samples should contain acid, base, andneutral extractable over the full retention time range.However, the addition of isomeric pairs to organic PE sampleswill check GC resolution; the addition of phthalates to pesticidePE samples will test extract cleanup methods; the addition of oilto soil PE samples will verify whether gel permeationchromatographic cleanup was performed as contract required; andthe use of potassium ferricyanide, instead of potassium cyanide,to prepare aqueous cyanide PE samples will check whetherdistillation was conducted. Various other analytes may be addedto gauge instrument performance, such as addition ofchloromethane to volatile PE samples to check for correct purgeflow, addition of di-n-octyl phthalate to semivolatile PE samplesto determine if the GC/MS transfer line temperature was set toolow, use of specific xylene isomers to indicate if properstandards and response factors were used to set up instrumentcriteria, etc.
(4) Certain groups of compounds should not be combined sincethey will react together. For example, semivolatile acids(phenols) should not be combined with bases (anilines), becausethese compounds will react with each other causing subsequentloss of analytes. Silver and low to medium levels of chlorideare incompatible and should not be mixed. Certain compounds maynot even be compatible with some instruments and should not beused. For example, it is difficult to use GFAA to analyze a PEsample with a high concentration of chloride because of analytesignal suppression.
G-3. Preparation of PE Samples. PE samples can be preparedeither by spiking known amounts of analytes into a well definedhomogeneous matrix or by defining well homogenized real worldsamples. The USACE PE samples can generally be categorized intotwo groups based on preparation methods: fortified PE samples and"real world” PE samples. The fortified PE samples are preparedby spiking high purity reagent water or control solid materialswith solvated target analytes of high purity. Fortified PEsamples cost less to prepare and allow qualitative andquantitative variations in the compositions of final PE samples.Real world PE samples are usually soil or sediment collected fromcontaminated sites, which are dried, ground, mixed, and analyzedprior to use. Real world PE samples are used for validation oflaboratory performance in soil analysis for two reasons: (a) itis very difficult to prepare an absolutely homogeneous samplethat can then be subsampled for PE samples and (b) a spikedsample can never truly represent the weathering and complexities
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of a naturally contaminated matrix. Because the constituents areintegrated into the matrices as naturally as possible, the realworld PE samples present special analytical challenges of matrixinterferences. The USACE is continually seeking suitable realworld samples that represent typical environmental samples andcontain a broad spectrum of target analytes at adequateconcentrations.
a. General Preparation Procedure. Regardless of the type ofPE samples, the general USACE procedure for preparing PE samplesis outlined below.
(1) Determine matrix type, analytical method, andinstrumentation.
(2) Calculate the amount of PE samples needed by volume orweight.
(3) Select analytes, interferences, solvents, andpreservatives.
(4) Decide on the concentration of each component.
(5) Select stock materials and calculate appropriate amountsto add.
(6) Write step-by-step instructions (i.e., standardoperating procedures).
(7) Perform an error analysis and determine performancerequirements.
(8) Obtain materials.
(9) Prepare the PE sample.
(l0) Verify the concentration of each component in the PEsamples.
(11) Verify PE samples by multi-laboratory referee analyses.
(12) Establish the performance acceptance limits of PEsamples.
When real world materials are used for preparation offortified or non-fortified PE samples, additional intra- andinterlaboratory analyses are needed to verify the compositions ofthe real world materials. Any indigenous levels of analytes andinterferents that are present in the real world materials must be
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accurately determined. Depending on the levels and types ofanalytes and interferents, the real world materials may be usedfor preparation of fortified or non-fortified PE samples.
b. Starting Materials and Stock Solutions. Startingmaterials and stock solutions must fulfill several criteria inorder to be suitable for preparation of PE samples. All criticalinformation about starting materials and stock solutions shouldbe recorded in logbooks such that the PE samples are traceable toNIST or other reliable reference materials.
(1) Purity is the first requirement, especially if the finalsample’s true values are going to be based on the material addedto the sample. Only chemical sources of known high quality willbe used for PE sample preparation. The purity of all reagents,acids, and solvents should be checked prior to use. Purity isnot as much of a factor if the PE sample is going to becharacterized with consensus values from reputable laboratories.
(a) For inorganic PE samples, contaminant levels should bein the low ppm range if the PE sample is to contain only oneanalyte. Higher purity (low ppb range) starting materials shouldbe used if multianalyte PE samples are prepared (to avoidcontamination) or if sensitive instrumentation is used. Theamount of target analytes in the starting material should becertified to within ±0.5 percent for most cases. Materials thatare sold without certified purity information should not be used.Individual metal solutions are either purchased from NIST or fromvendors whose materials are traceable to NIST.
(b) For organic PE samples, only the highest purity solventshould be used. Purge-and-trap grade methanol is necessary forpreparation of volatile spiking solution because lower gradesfrequently contain toluene and xylene as impurities. Standardsfor use in preparing organic PE samples may be purchased neat, assingle component solutions, or as multiple standard mixes fromreliable vendors.
(2) Stability and chemical compatibility are other importantcriteria for starting materials and stock solutions. Specificreagents for each analyte are selected on the basis ofavailability and chemical characteristics, such as stability andreactivity. An expiration date must be specified for allprepared materials.
(3) For solid PE samples, unless the entire sample is to beanalyzed, homogeneity is one of the most important factors to beconsidered. Natural solid matrices, such as soil or sediment,should always be dried, ground, sieved, and mixed thoroughly
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prior to spiking. For solid PE samples, the smallest samplealiquot that will provide reproducible analysis results could beestimated with Pierre Gy’s sampling theory and confirmed byreplicate analyses. (See F. F. Pitard, Pierre Gy’s SamplingTheory and Sampling Practice, 2 volumes, 1989, CRC press, Inc.,Boca Raton, Florida.) For liquid PE samples, homogeneity isinherent unless adhesion of analytes to the container wall ormultiple phases are present. Normally, multiple phase PE samplesshould be avoided because sampling errors may overwhelm all othererrors, thus limiting a study's usefulness.
(4) Starting materials and stock solutions should also beobtained at appropriate concentration levels to minimize theamounts required and remain in the realm of accurate laboratoryware measurements. For example, weights of solid materialsshould be between 0.1 and 500g and volumes of liquids should bebetween 50 µL and 500 mL. Avoid dilutions that would require oddsizes of volumetric ware. If several levels for a given analyteare available, the more concentrated solution should be chosen tominimize potential contamination from stock materials.
(5) When commercially available reference materials areutilized, only certified reference materials (CRMS) should beused for PE sample preparation. The term “certified” means thatdocumentation supports the reference material. Using a CRM mayassure the capability of the measurement system to determine theanalyte in the sample. NIST is the most widely used supplier ofCRMs. However, using NIST values for solid materials can lead tocomparison errors on data obtained using USEPA inorganic andorganic extraction methods. NIST expresses CRM values as “total”concentrations but many USEPA methods use values based upon“extractable” concentrations. Because of this, certified NISTvalues for solid CRMs usually cannot be used. Using NIST valuesdo not pose a problem in performance evaluation of laboratoriesfor water analysis, where “total” extractables approximate truevalues. The acceptance criteria of the USACE PE samples shouldbe established based on extractable concentrations.
(6) Each lot of standards used for preparation orverification of PE samples should be analyzed by the PE samplesuppliers to verify its concentration prior to use. Reanalysisof the standards is required periodically to verify stability,according to a schedule optimized for each standard. Theprobable error of each step in the preparation of PE samplesshould be evaluated and used to assess the overall probable errorand implications on confidence levels. Details analysis andvalidation procedures should be documented and maintainedin-house per appropriate USEPA and USACE guidance for legaldefensibility.
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(7) All PE sample suppliers must actively participate inState and/or Federal proficiency testing programs and provide theUSACE Laboratory Validation Committee with their most recentresults for review on a quarterly basis.
(8) Safety must also be considered. Material Safety DataSheets (MSDS) should be obtained with each material and should beread and followed carefully. As good laboratory practice, handleand weigh out all toxic materials in a well ventilated fume hood.
c. Calculations. The calculations involved in preparingfortified PE samples are relatively simple. It is best to startwith the final volume or weight of PE samples to be prepared andwork backward to determine the amounts of individual analytestocks needed. Care should be taken in calculations with reagentpurity values, gravimetric factors, dilution and concentrationfactors, significant figures, and unit manipulations. The mostcommon types of concentration units are weight/weight for solidPE samples and weight/volume for liquid PE samples. Reagentbottles should be labeled with specific units, such as µg/mL orµg/kg. Ambiguous units such as ppb or ppm should not be usedbecause these units do not differentiate between weight/weight orweight/volume. Depending on when they are noticed, calculationerrors can have serious ramifications when PE samples areinvolved. Therefore, it is best to double check all calculationsleading up to the final concentrations of PE samples before thesamples are prepared. Good laboratory practice should include asecond person’s review of the calculation.
d. Standard Operating Procedures. In order to preparereliable PE samples, adherence to prescribed preparationprocedures is imperative. In any operation that is performed ona repetitive basis, reproducibility is best accomplished throughthe use of standard operating procedures (SOPs). This isespecially true for preparing PE samples that will be used todetermine laboratory performance. An SOP is defined as awritten, narrative, and stepwise description of laboratoryoperating procedures including examples of laboratorydocumentation. An SOP should accurately describe the actualprocedures used in the laboratory to ensure that reproducibleresults can be achieved by following the SOP. The SOP for PEsample preparation should be prepared as part of the planningprocess and should be at or near completion before PE samplepreparation work begins. The SOP should be reviewed beforepreparing actual PE samples. Ambiguous statements or terminologylike “air dried at ambient temperature” or “1:10 dilution” shouldnot be used when “18 to 22°C” or “ten-fold dilution” is meant.The “l:l0” may be confused with one part concentrate diluted withten parts of diluent, which is really an 11-fold dilution. As a
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PE sample is prepared, changes and observations are documented sothat significant information will be available if needed later.
e. Fortified PE samples. Fortified PE samples are usuallyprepared with spiking techniques. Either large volumes or smallunits of fortified PE samples of any matrix can be prepared byspiking analytes of choice at selected concentrations. Normally,it is preferable to spike a large volume and create individualunits from it, unless there is a major concern of analyte loss tocontainer wall. PE samples should be prepared by designated,experienced senior chemists to improve batch-to-batchreproducibility and reliability.
(1) Fortified aqueous PE samples. Aqueous PE samples shouldbe prepared on the day of shipment, usually early in the week toallow adequate preparation time for the contract laboratory toperform digestions, extractions, cleanups, etc. before theweekend.
(a) Reagent water which is free of contaminants at themethod detection limits is normally used for PE samplespreparation. Reagent water can be prepared by passing tap waterthrough a reverse osmosis water system and then through anultraviolet and activated carbon cartridge or equivalent systemto produce analyte-free reagent water. The quality of reagentwater should be monitored and documented on a routine basis.
(b) ASTM class A pipets and calibrated microsyringes shouldbe used for delivering and spiking during PE sample preparation.Variable pipetters can be used if they are verified to be incalibration; however, glass pipets are preferred. Samplecontainers (high density polyethylene for inorganic and amberglass for organics) are purchased as “certified pre–cleaned”according to USEPA standards.
(c) Gravimetric measurements can be used on less volatileliquids, such as water. If weights are used for calculations,density of the liquid also must be determined so thatweight-to-volume units can be calculated. Volatile liquids haveto be prepared by volume, using minimal headspace and minimalexposure to the atmosphere. Diluents should already contain anyrequired preservatives so that final volumes are not altered bypreservation.
(d) Full-volume PE samples of one liter are normally usedfor aqueous organic PE samples except volatiles which are 40 mL.A trip blank should always accompany volatile samples for eachdifferent analytical method. Volumes for the inorganic analyses
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vary from 200 to 1,000 mL, depending on the target analytes andanalytical methods.
(e) Multiple sets of spiking solutions are maintained withvarying constituents and concentrations to avoid sending the samePE samples to the same laboratory twice or to affiliatedlaboratories of the same parent organization.
(f) Organic spiking solutions (except volatiles) areprepared by dilution of reference stocks. Records andcertificates of all stock solutions and dilutions are maintainedin standard logbooks. Aqueous PE samples for organics (exceptvolatiles) are spiked individually into the sample bottles sincethe entire sample is used for analysis.
(g) Volatile spikes are purchased as mixed solutionsdesigned for laboratory evaluations and certificates aremaintained in laboratory files. Aqueous volatile PE samples areprepared in a volumetric flask with sufficient volume to preparethe day's shipment and then transferred to 40-mL VOA vials forsubmission to contract laboratories.
(h) Aqueous PE samples for inorganic are prepared involumetric flasks and aliquots are then transferred to individualsample bottles for shipment.
(i) All PE samples should be properly preserved per methodrequirements. PE samples with critical holding times should beshipped immediately after preparation to allow adequate time forthe contract laboratory to prepare and analyze the PE samples.
(j) Only one aliquot of each aqueous PE sample will be sentto each contract laboratory. Because the aqueous PE sample isprepared with reagent water, the laboratory will be instructed toperform method-specific QC analyses with its own reagent water.
(2) Fortified solid PE samples. Various types of soilsamples are collected and prepared to serve as a solid matrix.The soil could be clayey, silty, or sandy with differentalkalinity, organic, and metal contents. However, care must betaken to avoid using soils that are very reactive to acids orother reagents used for sample preparation. Except for volatileorganics, solid PE samples can be prepared by solid or liquidaddition. Due to the high volatility of volatile organics, soilPE samples for volatile organics can be prepared by a vaporfortification technique. (See A. D. Hewitt, P. H. Miyares, D. C.Leggett, and T. F. Jenkins, Comparison of Analytical Methods forDetermination of Volatile Organic Compounds in Soils, Environ.
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Sci. Technol., 1992, 26, 1932.) The USACE is looking into thistechnique.
(a) After removal of extraneous materials such as rocks,sticks, etc., the soil will be air dried, ground, and mixed withmills or grinders. Mixing mills or grinders capable of grindingand mixing large volumes of soil (up to 1 gallon) per batch arepreferred. Separate batches can be combined, sieved to pass 150mesh (<100 µm), and blended in a larger container. A 1 g samplealiquot should have a relative sampling error of about twopercent at this particle size if the total batch is 100 g. Thegrinding and mixing times are established by short interval runsand examining the particle size and physical consistency of thesoil. The homogenized soils should be stored in a cool, dark,and dry place. If needed, the potential influence of laboratoryrelative humidity can be removed by conditioning an air dried,sieved, and thoroughly mixed soil with CaSO desiccation.
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(b) The concentrations of any target analytes andinterferents in the homogenized soil should be thoroughly andaccurately determined. It is preferred that the concentrationsof natural contaminants in the soil are below method detectionlimits or relatively low compared with the concentrations ofspiked analytes.
(c) The spiking can be done by solid addition. The twosolids that are to be mixed should be reduced to approximatelythe same small particle size (at least <150 mesh) before mixing.This reduction leads to easier blending and components will beless prone to segregate during storage and transit. Relativeamounts of each component should not be extreme because it isvery difficult to evenly distribute small amounts of one materialwithin large amounts of another. If extremes in relative amountscannot be avoided, the blending can be done in stages. That isa small quantity of the main component can be spiked and blended,then mixed and blended with the rest of the main component.
(d) The spiking can also be done by liquid addition.Analyte solutions (except volatiles) are sprayed over thehomogenized soil in small increments. After vaporization of thesolvent, mix the soil thoroughly and spray again. The aboveprocess is repeated until all analyte solutions are used up.Rinse the spray bottles with more solvent and spray over the soilagain to ensure all target analytes are quantitativelytransferred to the homogenized soil. When liquid spikes are usedto modify solid matrix, the solvent must be removed by drying.Since local deposits of analyte can be left after drying,thorough mixing after drying is crucial. Mixing can be improvedby using enough solvent to form a runny paste or mud. The paste
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is occasionally stirred while drying and, when completely dry,must be re-ground and blended.
(e) Prior to packing the homogenized bulk PE samples intosmall units for use, the homogeneity of the PE samples should bereassessed to determine the minimum subsample size for eachtarget analyte. A general approach is first selecting aliquotsfrom the homogenized bulk PE samples and measuring theconcentrations of target analytes. A two-way analysis ofvariance is then carried out by comparing results from aliquotswithin subsamples with those between subsamples. If the means donot differ significantly at 95 percent confident level, the bulkPE samples is considered homogeneous. Homogeneity could furtherbe assessed by analyzing aliquots from certain percentage of theindividual subsamples at a variability of, say, five percentrelative standard deviation. Not all target analytes need to betested, and a single measurement technique may be used, However,the selected analytes and technique should include berepresentative and conclusive.
f. Real world PE samples. Real world soil and sediment PEsamples are collected from locations that have significant levelsof numerous contaminants of concern. Numerous low levels ofanalytes that may cause problems in assessing laboratoryperformance should be avoided. Large volumes of materials arecollected and shipped to USACE PE sample suppliers forprocessing. The materials are mixed thoroughly and extraneousmaterials are removed. Approximately five to ten gallons ofmaterials are air dried to three to four percent moisture. Thematerials are then ground in a large volume grinder to passthrough a 0.5-mm sieve. Materials are mixed and passed throughthe grinder a second time to desired particle size (i.e., 45-75µm) and stored at 4°C in the dark.
(1) Extraneous materials such as rocks, sticks, etc. shouldfirst be removed from the solid materials. The materials arethen air dried, ground, and mixed with mills or grinders. Mixingmills or grinders capable of grinding and mixing large volumes ofsoil (up to one gallon) per batch are preferred. Separatebatches can be combined, sieved to pass 150 mesh (<100 µm), andblended in a larger container. A l-g sample aliquot should havea relative sampling error of about two percent at this particlesize if the total batch is 100 g. The grinding and mixing timesare established by short interval runs and examining the particlesize and physical consistency of the soil. The homogenized soilsshould be stored in a cool, dark, and dry place.
(2) The content of natural PE samples can be altered byspiking to fulfill special needs. The same spiking technique as
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previously described can be used. After spiking and drying, anadditional blending step is necessary.
(3) Most real world PE samples used by the USACE are verystable. The stability of PE samples should be studied andmonitored by analyzing random PE samples of each production batchaccording to a proper kinetics-based schedule. Some real worldsolid PE samples have been used as long as five years with nosignificant changes in concentrations in metals and semivolatileorganics.
(4) Multiple sets of real world PE samples with differentconstituents and/or concentrations should be available and readyfor use to avoid sending the same PE samples to the samelaboratory twice or to affiliated laboratories belonging to thesame parent organization.
G-4 . Handling. All PE samples should be handled and stored withextreme care to ensure the sample stability, integrity, purity,and authenticity.
a. Generally, containers are selected for their inertness totheir contents and their ability to prevent sample loss. Samplesfor organic analyses are stored in amber glass to avoid theplasticizers and organics found in plastic containers. Amberglass is recommended since some analytes are ultraviolet (UV)light sensitive. Plastic bottles are suggested for metals toavoid leaching of trace impurities from glass containers. Bottlecaps should be tightly closed to avoid leakage during shipment.
b. A PE sample must maintain its stability. If valueschange significantly before the sample can be analyzed, the PEsample is worthless. Short holding times are common practice forunstable species such as mercury, cyanide, and volatile organics.In addition to observance of holding times, preservatives andrefrigeration are used to retard sample degradation. Inaddition, PE samples for cyanides and organic analysis should bekept in the dark to avoid degradation by UV light. PE samplesmust be preserved according to the required analysis. Forexample, aqueous PE samples for volatile organics should only beacid preserved depending on the analytical method to be used.Normally, all PE samples should be preserved and stored at 4°C inthe dark to retard degradation processes. Analytes requiringdifferent preservatives cannot be grouped together in the samesample container. Bottles for volatile organic samples should becompletely filled to retard loss of volatiles.
c. All PE samples should be appropriately preserved, packed,and shipped by overnight express delivery service to commercial
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laboratories according to USEPA, USACE, and DOT regulations andguidelines. Chain-of-custody form should be used for all PEsamples.
d. PE samples are usually provided as single blind, althoughdouble blind are occasionally provided. When double blind PEsamples are shipped, special precautions on labeling and packingshould be taken to make the PE samples indistinguishable fromregular field samples. The packaging and container must beidentical with that used by field personnel sending the samesample type to the contract laboratory. Special arrangements,such as arranging for a “consulting firm” to contract with thelaboratory to be evaluated or using the same bottles, labels,chain-of-custody forms, sample coolers, shipping location, etc.as used in the field, will be made to simulate actualenvironmental samples.
G-5 . Validation. Because PE samples may be used to disqualify alaboratory's performance or to challenge a laboratory's results,the analyte concentrations in PE samples must be validated withlegal defensibility prior to use. All PE samples should bemeticulously tested internally and externally to determine thetrue values and statistically establish the acceptance limitsprior to use.
a. Two approaches, the consensus interlaboratory approachand the multiple techniques/definitive techniques approach, areusually used for validation of PE samples. In the multipletechniques/definitive techniques approach, the PE samples aretested by independent techniques with different measurementprinciples and by definitive techniques whose measurementprinciples are based on or are directly traceable to physicalmeasurements such as weight and radioactive decay to reducerandom or systematic variabilities of chemical measurementtechniques. Nearly all of NIST's environmental standardreference materials are certified by this approach. However,there are few definitive techniques and none for organics. Themajority of USACE PE samples are validated by interlaboratoryconsensus in performing a single methodology where the mean valueapproximates the true value. When there is no definitivetechnique available to check, the mean value obtained byinterlaboratory consensus could be nothing more than astatistical average. Therefore, only reliable laboratories ofhigh performance should be used for validation of PE samples.
b. Fortified PE samples. Depending on the type of fortifiedPE samples, the true concentrations and acceptance limits of eachtarget analyte can be determined by three different methods:
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referee laboratory analysis, error propagation analysis, orperformance data estimation.
(1) Fortified aqueous PE samples. The true values andacceptance limits of fortified aqueous samples can be determinedby all three methods. Normally, consensus values by refereelaboratory analysis should be used. If the other two methods areused, a triplicate for each batch of PE samples should beanalyzed by the USACE PE sample supplier to check the accuracyand precision.
(a) Referee laboratory analysis. For analytes withcritical holding times, PE samples should be sent to the contractlaboratory being tested at the same time they are sent to aminimum of four referee laboratories. The uncertainty of themean value based on referee laboratory’s results decreases withincreasing number of laboratories. Therefore, it is preferred tohave more laboratories (e.g., 12 referee laboratories) to improvethe confidence level of the mean value. The determinedconcentration from each independent referee laboratory should bewithin ten percent of prepared concentrations or the causes ofexcess high/low recovery should be investigated. Consensusvalues within 95 percent confidence level from the refereelaboratories can then be used for evaluation of the contractlaboratories. Stable analytes can be characterized beforeshipment to contract laboratory.
(b) Error propagation analysis. If a material is notcharacterized (i.e., round-robin data not available), acceptancelimits can be calculated. Sometimes calculation is the only wayto determine the true values and acceptance limits. Thecalculation for the expected or true concentration for eachanalyte in fortified aqueous PE samples is very accurate andstraightforward. The acceptance limits of fortified aqueous PEsamples can be determined through an error analysis of the stepscaused by analytical sample preparation and by sample analysis.Error propagation rules are used as guidelines to estimatedeterminate and indeterminate errors that should be experiencedby the laboratory being evaluated. The indeterminate errors arealways judgement calls and should be based on experience. TheFactor-2 criterion (i.e., indeterminate errors = 2 x determinateerrors) can be used as a good approximation for inclusion ofindeterminate errors. The result is a relative error that can bemultiplied by the expected target values for each analyte to getacceptance limits. If biases are known to exist but cannot bereliably accounted for, the PE sample may have to becharacterized by several reputable laboratories and consensusvalues used for acceptance windows.
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(c) Performance data estimation. The performance data for anumber of USEPA methods, based on multiple laboratories testingresults, are published in the methods. The acceptance limits foreach analyte can therefore be estimated by the calculated targetvalues and the precision formula. The estimated acceptancelimits usually are very reliable.
(2) Fortified solid PE samples. A difficulty with fortifiedsolid PE samples is matrix interaction with the analytes.Analyte accuracy of the spiking solution may be very well known,but that accuracy is lost after spiking, when the analytes reactwith the solid matrix. For example, adsorption of metal ions insolution by the clay matrix of a soil is a well known phenomenon.Since most USEPA extractions are designed to remove leachablerather than true totals, all the analyte that was introduced byspiking may or may not be removable by the sample preparationmethod. The result is a reduced recovery for affected analytes.Analytes like antimony, silver, and selenium are especiallysusceptible. To complicate matters further, if indigenous levelsof analytes are present in the solid matrix, their leachablelevels must be known before total levels or percent recovery canbe calculated accurately. Given these difficulties, a fortifiedsolid PE sample is best characterized by consensus rather than bycalculation or estimation of analyte levels from individualcomponents.
c. Real world PE samples. For real world PE samples, thetrue values of target analytes are usually unknown. The mean ofreported values from a round-robin testing is usually considereda "consensus" value and would be used as the true analyticalvalue. Confidence intervals for the consensus values of targetanalytes are based on reported values using standard populationstatistics. The initial acceptance limits for PE samples arestatistically determined by consensus values of the participatinglaboratories which include reputable government and contractlaboratories. The acceptance limits for each target analyte willbe established statistically at 95 percent confidence level. Theacceptance limits for each target analyte are matrix- andmethod-specific.
(1) Any method of evaluating real world PE samples maypresent problems of accuracy that depend upon the amount of dataused to set acceptance limits. Thus, it would be best to sendsplit PE samples to a minimum of four round-robin testinglaboratories. Although a consensus value resulting from a smallnumber of determinations may have significant uncertainties, theconsensus value from the round-robin testing laboratories shouldbe a better estimate of true value than any single measurement.
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(2) A round-robin analysis is used to certify analytes ofinterest. In order to ensure the integrity of PE samples, one ortwo PE samples should periodically be resubmitted to the refereelaboratories to evaluate any possible degradation or trends inthe analyte concentrations. This information is also used toevaluate possible extension of the useful life of real world PEsamples.
d. The pool of PE sample results produced by all contractlaboratories should be carefully analyzed on a regular basis.The mean values and the associated uncertainties of targetanalytes should always be documented. The program-widestatistical results for PE sample analyses by contractlaboratories should also be used to adjust the acceptance limitsin order to observe the relative performance of each laboratoryusing a given protocol against its peers. The USACE may adjustthe acceptance limits on any given PE sample to compensate forunanticipated difficulties with a particular sample or analysis.
e. All PE samples must be analyzed with the same methodology(i.e., USEPA SW-846 of the most recently promulgated revisions)by both the contract laboratories and the referee laboratories.Deviations from the standard methods will make the datanoncomparable. The results of all PE sample analyses should beused to develop control charts displaying the true concentrationand ranges of recovery and bias for each target analyte.
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APPENDIX H
GUIDELINES AND CRITERIA
FOR
ON-SITE INSPECTION
OF
COMMERCIAL ANALYTICAL CHEMISTRY LABORATORIES
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GUIDELINES AND CRITERIA FOR ON-SITE INSPECTION OFCOMMERCIAL ANALYTICAL CHEMISTRY LABORATORIES
H-1. On-Site Laboratory Inspection Procedures. This documentoutlines the procedures to be used by the USACE inspectors toconduct an on-site inspection and evaluation of a commerciallaboratory. On-site laboratory inspections are carried out tomonitor a commercial laboratory's ability to meet selected termsand conditions specified in a USACE HTRW contract and to identifylaboratory problems that adversely impact performance. Thefrequency of on-site inspection is dictated by a commerciallaboratory's performance. An on-site inspection generally takeseight hours and normally consists of three parts: entranceinterview, laboratory tour, and exit interview. Prior to theinspection, the inspectors shall thoroughly review all project-and laboratory-specific documents. The Pre-Inspection Checklistshown in Figure H-1 can be used as a guidance for preparation ofon-site inspection.
a. Entrance Interview. The entrance interview will beheld with the laboratory management personnel, includinglaboratory director/managers, QA officer, and project personnel,to discuss the upcoming USACE projects, USACE Chemical DataQuality Management (CDQM) requirements, PE sample results, USACEreview comments on laboratory quality management manual (LQMM),and laboratory's previous performance on USACE projects, ifapplicable. A copy of written comments on the LQMM should bepresented to the laboratory during the entrance interview. TheEntrance Interview Checklist shown in Figure H-2 can be used aguidance.
b. Laboratory Tour. A tour of the commercial laboratorywill follow to examine the laboratory facilities,instrumentation, operation, maintenance, documentation, safety,waste compliance, etc. The laboratory tour will emphasize on twoseparate aspects: Quality Assurance Evaluation and EvidentiaryAudit. The questionnaire and checklist presented in Appendices Eand I should be used during the laboratory tour.
(1) Quality Assurance Evaluation: The inspectors shallinspect a commercial laboratory's facilities to verify theadequacy and maintenance of instrumentation, the continuity ofpersonnel meeting experience or education requirements, and theacceptable performance of analytical and QC procedures. Theitems to be monitored will include, but not be limited to, thefollowing items:
H-2
1.
2.
3.
4.
5.
6.
7.
EM 200-1-11 Jul 94
PRE-INSPECTION CHECKLIST
Gather all appropriate laboratory information from files.
a. Preliminary questionnaire.
b. Laboratory's LQMM.
c. PE sample results and evaluation reports.
d. Chemical quality assurance reports (CQARs) on pastprojects.
Gather and review project information.
a.
b.
c.
Project summary based on specifications, scope of work,work plans, chemical data acquisition plan, etc.
Analytical parameters and number of samples.
Project data quality objectives (DQOs).
Contact laboratory to set up audit date.
a. Get directions to laboratory by FAX.
b. Suggest tentative on-site inspection date.
c. Briefly review inspection procedures.
Contact USACE TM/CORs and district chemists.
a. Get most current project information.
b. Extend an invitation for them to attend the inspection.
Contact laboratory to confirm inspection date and maketravel arrangements.
Review laboratory’s LQMM, questionnaire, and any otherqualification documents. Generate written comments.
Review laboratory's PE sample results.
a. Review and confirm all PE sample results.
Figure H-1 Pre-Inspection Checklist
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8.
9.
10.
b. Gather any missing information.
c. Update database with current information.
d. Prepare a summary of PE sample status for review at thelaboratory.
Review the CQARs on past USACE projects that laboratorypreviously worked on.
a. Check with QA laboratory(s) for any detail or missinginformation.
b. Extend an invitation for QA laboratory(s) to attend theinspection.
Prepare a list of problem areas in laboratory.
a. Based on PE sample results.
b. Based on past performance on USACE projects.
Gather general information and forms for distribution at thelaboratory.
a.
b.
c.
d.
e.
f.
g.
h.
i.
ER 1110-1-263.
Copy of laboratory evaluation request(s).
"On-site Inspection Summary" format.
Entrance interview checklist.
Laboratory inspection checklist.
Exit interview checklist.
Cooler receipt checklist.
USACE minimum data reporting requirements.
Sample CQAR and data comparison table.
j. Your business card.
Figure H-1 Pre-Inspection Checklist (continued)
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ENTRANCE INTERVIEW CHECKLIST
1.
2.
3.
Personnel introductions.
a. Give background of inspectors and USACE HTRW MCX.
b. Pass out/gather business cards.
c. Pass out and have everyone sign "On-site InspectionSummary" format.
Validation process.
a. Describe USACE laboratory validation process.
- Step 1: Preliminary review and screening based onqualification submittals.
- Step 2: Performance evaluation based on PE sampleanalysis.
- Step 3: On-site inspection.
b. Explain the approval process after on-site inspection.
c. Emphasize that laboratory validation ismatrix, and method-specific approval.
d. A project-specific evaluation is neededproject.
Project information.
a.
b.
Is laboratory aware of the project?
- Is CDAP available? Laboratory shouldCDAPs for upcoming projects.
a parameter,
for
get
each new
copies of
- Are DQOs available?
- Make available to laboratory a copy of evaluationrequest(s).
Describe projects.
Figure H-2 Entrance Interview Checklist
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4.
5.
6.
7.
USACE QA Program.
a. Pass out a copy of ER 1110-1-263.
- Describe USACE QA program and special features.
- It is consistent and complies with Federal and Stateregulations.
b. Describe field split QA sample program
c. Describe government QA Laboratory and its role:
- Examines incoming field samples against CDAP. Pass outcopy of "Cooler Receipt Checklist". Notify TM/CORsimmediately if errors noted.
- Analyzes QA samples. QA Laboratory can be used as aresource to answer questions.
- Reviews project laboratory's data. Pass out a copy of"USACE Minimum Data Reporting Requirements."
- Generates CQAR. Describe this report. Pass out a copyof sample "Data Comparison Table" and describe the keyelements that are focused on.)
Review comments on laboratory's LQMM.
a. Pass out and review comments.
b. Discuss corrective actions, if needed.
Status of PE sample results.
a. Summarize current status of all PE samples.
b. Discuss deficiencies and corrective actions, if needed.
Laboratory's performance on past USACE projects.
a. Discuss data quality based on precision, accuracy,representativeness, comparability, completeness, andsensitivity (PARCCS).
b. Discuss corrective actions, if needed.
Figure H-2 Entrance Interview Checklist (continued)
H-6
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
(2)
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Size and appearance of the facility.
Quantity, age, availability, scheduled maintenance,and performance of instrumentation.
Availability, appropriateness, and utilization ofSOPs.
Staff qualifications, experience, and personneltraining programs.
Reagents, standards, and sample storage facilities.
Standard preparation logbooks and traceability.
Sample analysis, raw data, bench sheets, andanalytical logbooks maintenance and review.
Data package review and data management procedures.
Evidentiary Audit: The inspectors conducts an evidentiary audit to determine if the laboratory's QA/QC policiesand SOPS are implemented to warrant required data quality andlegal defensibility. The evidentiary audit is comprised of thefollowing three activities:
(a) Procedural Audit: The procedural audit consists ofreview and examination of actual operating procedures andaccompanying documentation for the following laboratoryoperations: sample receiving, storage, identification, security,tracking (from receipt to completion of analysis), and analyticalproject file organization and assembly.
(b) Written SOPs Audit: The written SOPs audit consistsof review and examination of the written SOPs to determine ifthey are accurate and complete for the following laboratoryoperations: sample receiving, storage, identification, security,tracking (from receipt to completion of analysis), and analyticalproject file organization and assembly.
(c) Analytical Project File Audit: The analytical projectfile audit consists of review and examination of the analyticalproject file documentation. The inspectors shall review thefiles to determine:
- the accuracy of the document inventory,
- the completeness of the file,
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the traceability of sample activity,
the identification of activity recorded on thedocuments, and
the error correction methods.
c. Exit Interview. At the conclusion of the laboratorytour, the inspectors discuss their findings and recommendationsfor any corrective actions with the laboratory management staffduring an exit interview. A commercial laboratory shall preparea written report regarding the corrective actions implemented orto be implemented with schedule for completion to the Committeefor review and approval. The written report must provide detailon corrective actions for all deficiencies discussed during theexit interview and must be sent within ten working days from theon-site inspection. The Exit Interview Checklist shown in FigureH-3 can be used as guidance.
H-2 . Guidance and Criteria for Sample Management, DataManagement, Document Control, and Standard Operating Procedure
a. Sample Management. Sample management procedures aredefined as procedures specifying the sample receiving, log-in,storage, and disposal. A sample is a physical evidence collectedfrom a facility or from the environment. Controlling evidence isan essential part of the hazardous waste investigation effort. Acommercial laboratory shall establish SOPs to maintain theintegrity, authenticity, and legal defensibility of samples frominitial receiving to proper disposal. To accomplish this,laboratories are required to develop and implement the followingsample identification, chain-of-custody, sample receiving, andsample tracking procedures:
(1) Sample Identification: To assure traceability of thesamples while in possession of a laboratory, the laboratory shallhave a specified method for maintaining identification of samplesthroughout the laboratory. Each sample and sample preparationcontainer shall be labeled with a USACE field sample ID number ora unique laboratory identifier. If a unique laboratoryidentifier is used, it shall be cross-referenced to the USACEfield sample ID number.
(2) Chain-of-Custody Procedures: The custody of USACEsamples must be traceable from the time the samples are collecteduntil they are introduced as evidence in legal proceedings. Acommercial laboratory shall have procedures ensuring that USACEsample custody is maintained and documented. A sample is undercustody if:
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EXIT INTERVIEW CHECKLIST
1. Express gratitude for laboratory's efforts, cooperation andtime
2. Present inspection findings
a. Strong and weak areas.
b. Deficiencies and corrective actions.
c. Recommendations for improvements.
3. Complete the "Inspection Summary" sheets
a. Ask laboratory director/manager to review and signsummary sheet.
b. Pass out a copy of signed summary sheet.
b. Request written responses within ten working days.
4. Invite questions and comments
5. Meeting adjourned
Figure H-3 Exit Interview Checklist
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- it is in your possession,
- it is in your view after being in your possession,
- it was in your possession and you locked it up, or
- it is in a designated secure area that is accessibleonly to authorized personnel.
(3) Sample Receiving Procedures:
(a) A commercial laboratory must designate a samplecustodian responsible for receiving all samples. Arepresentative should also be designated to receive samples inthe event that the sample custodian is not available. The samplecustodian must inspect the condition of the shipping containers,sample bottles, and the custody seals (intact/not intact) uponreceipt. The sample custodian shall also check for the presenceor absence of the following documents accompanying each sampleshipment:
- Airbills or airbill stickers
- Chain-of-Custody forms
- Sample labels
- Sample tags (if required for a project)
(b) The sample custodian must sign and date all forms(e.g., custody records, packing lists, and airbills) accompanyingthe samples at the time of sample receipt. A commerciallaboratory must immediately contact the prime contractor and/orUSACE TM/COR to resolve any discrepancies and problems such asabsent documents, conflicting information, broken custody seals,and unsatisfactory sample condition (e.g., leaking sample bottle,improper preservation, etc.) A commercial laboratory shallrecord the resolution of discrepancies and problems on a phoneconversation log. All records and logs shall become part of theproject file records.
(c) The following information shall be recorded in samplelogbook by the sample custodian or his/her representative assamples are received and inspected:
- Condition of the shipping container
- Presence or absence and condition of custody seals onshipping and/or sample containers
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- Custody seal numbers, when present
- Condition of the sample bottles
- Presence or absence of airbills or airbill stickers
- Airbill or airbill sticker numbers, when present
- Presence or absence of packing lists
- Presence or absence of sample tags
- Sample tag identification numbers, when present
- Verification of agreement or non-agreement ofinformation recorded on shipping documents and samplecontainers
- Problems or discrepancies
- Resolutions for problems or discrepancies
(d) The Cooler Receipt Checklist as shown in Figure H-4 ora similar one is strongly recommended.
(4) Sample Tracking Procedures: A commercial laboratoryshall maintain records documenting all phases of sample handlingfrom receipt, analysis, and final sample disposal.
(5) Sample Disposal Procedures: A commercial laboratoryshall treat all USACE samples, including residual samples,digested or extracted samples, samples with analyses cancelled,sample containers, waste generated during sample preparation oranalysis, etc., as potential hazardous and toxic material orsubstance until proven otherwise. SOPs for disposal USACEsamples shall comply with all Federal and State regulations suchthat the USACE will not be legally liable for improper sample orwaste disposal by the laboratory.
b. Data Management. Data management procedures aredefined as procedures specifying the acquisition or entry,update, correction, deletion, storage, and security of computerreadable data and files. These procedures should be in writtenform and contain a clear definition for all databases and filesused to generate or submit deliverables. Key areas of concerninclude: system organization (including personnel and security),documentation operations, and traceability. The system shouldprevent entry of incorrect or out-of-range data and alert dataentry personnel of errors through a multilevel review process.
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LIMS #: _____________________ Chain-of-Custody No: _______________ Date received: ___________________
Project: ________________________________________________________________________________________________
A .
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
B.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
USE OTHER SIDE OF THIS FORMAT TO NOTE DETAILS CONCERNING CHECK-IN PROBLEMS.
PRELIMINARY EXAMINATION PHASE: Date cooler was opened: ______________________
by (print): _________________________________ (sign): ________________________________________
Did cooler come with a shipping slip (airbill, etc.)? ................................ YES NO
If YES, enter carrier name & airbill nunber here: ____________________________________________
Here custody seals on outside of cooler? ....................................... YES NO
How many & where: ________________________, seal date: ____________, seal name: _____________
Were custody seals unbroken and intact at the date and time of arrival? ...................... YES NO
Did you screen samples for radioactivity using a Geiger Counter ........................ YES NO
Were custody papers sealed in a plastic bag & taped inside to the lid? ................. YES NO
Were custody papers filled out properly (ink, signed, etc.)? .......................... YES NO
Did you sign custody papers in the appropriate place? ............................... YES NO
Was project identifiable from custody papers? ....................................... YES NOIf YES, enter project name at the top of this form.
If required, was enough ice used? ............. Type of ice: ______________________ ............ YES NO
Have designated person initial here to acknowledge receipt of cooler: _______________ (date): _________
LOG-IN PHASE: Date samples were logged-in: _________________________
by (print): ____________________________________________ (sign): ___________________________________
Describe type of packing in cooler: ____________________________________________________________
Were all bottles sealed in separate plastic bags? ..................................... YES NO
Did all bottles arrive unbroken and were labels in good condition? ....................... YES NO
Were all bottle labels complete (ID, date, time, signature, preservative, etc.)? ............ YES NO
Did all bottle labels agree with custody papers? ................................ YES NO
Were correct containers used for the tests indicated? ............................ YES NO
Were correct preservatives added to samples? ...................................... YES NO
Was a sufficient amount of sample sent for tests indicated? .......................... YES NO
Were bubbles absent in VOA samples? If No, list by sample #:......................... YES NO
Was the USACE Technical Manager called and status discussed? ................................. YES NOIf YES, give details on the back of this form.
Who was called? _________________________ By whom? _________________ date: ____________
F i g u r e H - 4 C o o l e r R e c e i p t C h e c k l i s t
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The record of changes in the form of corrections and updates todata originally generated, submitted, and/or resubmitted must bedocumented to allow traceability of updates. Documentation mustinclude the following for each change:
- Justification or rationale for the change.
- Initials of the person making the change or changes.Data changes must be implemented and reviewed by aperson or group independent of the source generating thedeliverable.
- The laboratory manager must approve changes tooriginally submitted deliverables.
c. Document Control. The goal of a laboratory documentcontrol program is to assure that all documents for a specifiedproject will be accounted for when the project is completed.Accountable documents used by commercial laboratories shallinclude, but not be limited to, logbooks, chain-of-custodyrecords, sample work sheets, bench sheets, and other documentsrelating to the sample or sample analyses. The followingdocument control procedures should be established to assure thatall laboratory records are assembled, stored, and ready fordelivery to USACE when requested by USACE:
(1) Preprinted Laboratory Forms and Logbooks:
(a) All observations and results recorded by a commerciallaboratory but not on preprinted laboratory forms shall beentered into permanent laboratory logbooks. The laboratory shallidentify the activity recorded on all laboratory documents thatare directly related to the preparation and analysis of USACEsamples.
(b) Preprinted laboratory forms shall contain the name ofthe commercial laboratory and be dated (month/day/year) andsigned by the person responsible for performing the activity atthe time an activity is performed. Logbook entries shall also bedated, signed, and entered in chronological order. Pages in bothbound and unbound logbooks shall be sequentially numbered.Instrument run logs shall be maintained so as to enable areconstruction of the run sequence of individual instruments.
(c) Corrections to raw data and supporting documents shallbe made by drawing a single line through the error and enteringthe correct information. Corrections and additions to raw dataand supporting documents shall be dated and initialed. Noinformation shall be obliterated or rendered unreadable. All
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notations shall be recorded in ink. Unused portions of documentsshall be crossed out.
(2) Consistency of Documentation: A commercial laboratoryshould assign a document control officer responsible for theorganization and assembly of all project related files. Allcopies of laboratory documents shall be complete and legible.Before releasing analytical results, the document control officershall assemble and cross-check the information on sample tags,custody records, laboratory bench sheets, personal and instrumentlogs, and other relevant deliverables to ensure that datapertaining to each particular sample is consistent throughout thespecific USACE project.
(3) Storage of USACE Files: A commercial laboratory shallmaintain USACE laboratory documents in a secure location that hasa limited access. All documents that are directly related to thepreparation and analysis of USACE samples shall be stored andmade available to USACE upon request within a contract specifiedtime limit.
d. Specifications for SOPs. In order to obtain reliableresults, adherence to prescribed analytical methodology isimperative. In any operation that is performed on a repetitivebasis, reproducibility is best accomplished through the use ofSOPs . An SOP shall be functional: i.e., clear, comprehensive,up-to-date , and sufficiently detailed to permit duplication ofresults by qualified analysts. All SOPs must accurately reflectactual procedures used in the laboratory, and copies of thewritten SOPs shall be available to the appropriate laboratorypersonnel. In addition, all SOPs must be consistent withappropriate, current Federal and/or State regulations andguidelines and with manufacturer's specific instruction manuals.
(1) SOP Format: An SOP is defined as a written documentthat provides step-by-step description of a laboratory operation,analysis, or actions. The format of an SOP may vary dependingupon the kind of activity for which they are prepared; however,at a minimum, the following sections must be included:
(a) Title page
(b) Scope and Application
(c) Definitions
(d) Procedures
(e) QC Criteria
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(f) Corrective Action Procedures, including secondaryreview of information being generated
(g) Documentation description and example forms
(h) Miscellaneous notes and precautions
(i) References
(2) SOPs Required: The followings are the minimum numberof SOPs required:
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
(i)
(j)
(k)
(l)
Sample receipt and logging
Chain-of-custody procedures
Sample storage
Prevention of sample contamination
Security for laboratory and samples
Standard purity and preparation
Instrument maintenance records and logbooks
Sample analysis and data control system
Glassware cleaning
Internal review of QA/QC data for each data package
Data reduction and reporting
Laboratory data validation
- Data flow and chain-of-command for data review.
- Procedures for measuring precision and accuracy.
- Control chart generation and utilization.
- Evaluation parameters for identifying systematicerrors.
- Internal QA inspection procedures.
- Documentation of problem identification, correctiveactions, and resumption of analytical processing.
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(m) Data management and handling
e. Handling of Confidential Information. A commerciallaboratory conducting work under the USACE HTRW contract mayreceive USACE-designated confidential information. Confidentialinformation must be handled separately from other documentation.To accomplish this, a commercial laboratory should establish thefollowing procedures for the handling of confidentialinformation:
(1) All confidential documents shall be under thesupervision of a designated document control officer. In orderto provide document accountability of the confidential documents,each item in a specific USACE project file should be inventoriedand assigned a serialized number. All documents relevant to eachsample delivery group should be inventoried. This includes:logbook pages, bench sheets, mass spectra, chromatograms,screening records, re-preparation records, re-analysis records,records of failed or attempted analysis, custody records, libraryresearch results, etc. The designated document control officershall be responsible for ensuring that all documents generatedare placed in the specified project file for inventory.
(2) Any samples or information received with a request ofconfidentiality shall be handled as "confidential." A separatelocked file shall be maintained to store this information andshall be segregated from other nonconfidential information. Datagenerated from confidential samples shall be treated asconfidential. Upon receipt of confidential information, thedocument control officer will log these documents into aConfidential Inventory Log. The information will then beavailable to authorized personnel but only after it has beensigned out to that person by the document control officer. Thedocuments shall be returned to the locked file at the end of eachworking day.
(3) Confidential information may not be reproduced exceptupon approval by the USACE TM/COR. The document control officershall enter all copies into the document control system describedabove. In addition, this information may not be disposed ofexcept upon approval by the USACE TM/COR. The document controlofficer shall remove and retain the cover page of anyconfidential information disposed of for one year and shall keepa record on the disposition in a Confidential Inventory Log.
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APPENDIX I
CHECKLISTS
FOR
ON-SITE LABORATORY INSPECTIONS
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CHECKLISTS FOR ON-SITE LABORATORY INSPECTION
CHARTS I-1 through I-36 contain checklists on which theadequacy of laboratory organization, facility, equipment,operation, and QA/QC policy and practice shall be checked by theinspector(s) during an on-site inspection. The titles of thesechecklists are:
CHART I-1CHART I-2CHART I-3CHART I-4CHART I-5CHART I-6CHART I-7CHART I-8CHART I-9CHART 1-10
CHART I-11CHART I-12CHART I-13CHART I-14CHART I-15CHART I-16CHART I-17CHART I-18CHART I-19CHART I-20
CHART I-21CHART I-22CHART I-23CHART I-24CHART I-25CHART I-26CHART I-27CHART I-28CHART I-29CHART I-30
CHART I-31CHART I-32CHART I-33CHART I-34CHART I-35CHART I-36
Organization and PersonnelFacilitiesEquipmentGeneral QA/QCReport GenerationField SamplingSample Receipt and StorageSample Preparation for Organic AnalysisGeneral QA/QC for Organic Analysis by GCOrganic Analysis by GC: HVO (8010A)
Organic Analysis by GC: TPH (Modified 8015)Organic Analysis by GC: AVO (8020)Organic Analysis by GC: PHENOLS (8040A)Organic Analysis by GC: PEST/PCB (8080)Organic Analysis by GC: PAH (8100)Organic Analysis by GC: HERB (8150A)General QA/QC for Organic Analysis by GC/MSOrganic Analysis by GC/MS: VOA (8240A)Organic Analysis by GC/MS: BNA (8270A)Organic Analysis by GC/MS: DIOXINS (8280)
Organic Analysis by HPLC: PAH (8310)Organic Analysis by HPLC: EXPLOSIVES (8330)Sample Preparation for Metal AnalysisGeneral QA/QC for Metal AnalysisMetal Analysis by ICP: METALS (6010A)Metal Analysis by AA: METALS (7000s)General QA/QC for Classical AnalysisClassical Analysis: COMMON ANIONS (300s)Classical Analysis: OIL AND GREASE (413.1)Classical Analysis: TRPH (418.1)
Classical Analysis: CYANIDE (9010A)Classical Analysis: TOC (9060)Waste Characteristics: Ignitability (1010/1020)Waste Characteristics: Corrosivity (1110)Waste Characteristics: Reactivity (Section 7.3)Waste Characteristics: Toxicity (1311)
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An inspector(s) should use those checklists that areapplicable to the laboratory to be inspected. Depending on theprojects and/or the laboratory, an inspector(s) shall determinewhich sections of each checklist should be used. Theinspector(s) should check those items, under the “YES” column,which he/she believes to be adequately practiced and documentedin the laboratory. Additional information should be entered inthe “COMMENT” columns with an “N/A” for items not applicable tothe work for the USACE. The detail of any observations,comments, or problems should be recorded in the blank spaceprovided at the end of each checklist. Any deficiences noted onthe checklist shall be discussed with and acknowledged by thelaboratory management staff during an Exit Interview.
The checklists will be revised or augmented when revised ornew analytical methods are officially approved by the USEPA orother regulatory agencies. All revisions of the checklists shallbe approved by the HQUSACE.
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CHART I-1
ORGANIZATION AND PERSONNEL:
ITEM
Is the lab legally identifiable?
Has the lab provided supervision by personsfamiliar with the test methods, theobjective of the test, and the assessmentof the results?
Has the lab specified and documented theresponsibility, authority, and relationshipof all personnel who manage, perform, orverify work affecting the quality of tests?
Does the lab have a QA Officer who hasresponsibility for the quality system andits implementation?
Is the QA Officer familiar with all testprocedures and QC requirements?
Does the QA Officer have direct access tothe highest level of management at whichdecisions are taken on lab policy orresources?
Does the lab nominate deputies in case ofabsence of the QA Officer?
lees the lab have documented protocol fortraining in QC methods?
Do personnel assigned to this project havethe appropriate background to successfullyaccomplish the objectives of tests?
Is each analyst accountable for performingtasks in any of the following areas meetthe specified minimum experience:
a. Inorganic sample preparation – 6months?
b. Organic sample preparation – 1 year?
Page 1 of 3
YES COMMENT
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CHART I-1
ORGANIZATION AND PERSONNEL: Page 2 of 3
ITEM YES COMMENT
c. Classical analysis – 1 year?
d. Trace metal analysis – 1 year?
e. Gas chromatography – 1 year?
f. Pesticide residue analysis – 2 years?
g. Mass spectrometry – 1 year?
h. Spectrum interpretation – 2 years?
i. Radiochemical analysis – 2 years?
Is each analyst’s performance audited andapproved prior to work without closesupervision by a senior chemist?
Is there documented evidence of analystproficiency for each test method performed?
Does the lab have an in-house trainingprogram or send staff to training schools?
Are staff’s qualification, training, andexperience recorded?
Is backup provided for technical staff?
Does the lab have documented policy andprocedures to ensure the protection ofclients’ confidential information andproprietary right?
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CHART I-1
ORGANIZATION AND PERSONNEL: Page 3 of 3
ITEM
Additional observations, comments, or problems:
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CHART I-2
FACILITIES: Page 1 of 3
ITEM YES COMMENT
Does the lab building have a securitysystem?
Is access to the test and sample storagearea controlled?
Is a guest logbook available and used?
Is equipment protected and environmentmonitored as needed?
Does the lab have adequate work space,ventilation, light, and access to stablepower sources at workstations?
Is the lab clean and organized?
Is the lab free of dust, drifts, andtemperature extremes?
Is reagent water free of contaminationused for preparation of standards andblanks?
Is the conductivity of water routinelychecked and recorded on a daily basis?
Is a separate conductivity meter (capableof being calibrated) used to measure theconductivity of the reagent water? (Metersbuilt into the water purification systemare not acceptable.)
Is a corrective action taken when theconductivity of the reagent water is twomicromho or greater at 25°C?
Are exhaust hoods provided to allowcontamination-free work with volatileand hazardous materials?
I-7
EM 200-1-11 Jul 94
CHART I-2
FACILITIES: Page 2 of 3
ITEM YES COMMENT
Is the air flow of the hoods periodicallychecked and recorded?
Are adequate facilities, including coldstorage, provided for separate storage ofsamples, extracts, reagents, solvents,reference materials and standards topreserve their identity, concentration,purity, and stability?
Is adequate chemical storage spaceavailable and are chemicals properlysegregated according to class?
Are solvent storage cabinets properlyvented as appropriate for the preventionof possible lab contamination?
Does the lab have adequate safety devicessuch as eye wash stations, spill controlstations, showers, first-aid stations,etc.?
Are these safety devices checked routinelyto ensure they are still working properly?
Are special facilities (e.g., glove box,controlled air) provided for handlingextremely toxic materials such as dioxin?
Are adequate filing space available forstorage of manuals, SOPs, raw data, andreports?
Are chemical waste disposal policies andprocedures well-defined and followed bythe lab?
I-8
EM 200-1-11 Jul 94
CHART I-2
FACILITIES: Page 3
ITEM
Additional observations, comments, or problems:
of 3
I-9
EM 200-1-11 Jul 94
CHART I-3
EQUIPMENT: Page 1 of 8
ITEM YES COMMENT
Is appropriate equipment available for usein accordance with required methodology?
Is equipment adequately maintained withsufficient spare parts and are maintenanceinstructions available?
Is out-of-service equipment clearlylabelled?
Are equipment maintenance logs maintained?
Are standard curves prepared to cover theexpected concentration ranges of samples?
Are calibration logs maintained?
Is a new curve prepared annually (or morefrequently if specified by the method) orwhenever new reagents are prepared,whichever is more frequent?
Are calibration labels used as applicable?
Is proper backup equipment available?
Balances:
a. Analytical Balances:
(1) Are analytical balances capable ofweighing 0.1 mg in use?
(2) Is there a record of balancecalibration in two ranges withClass S weights? (Please specifiythe ranges.)
(3) Do records show daily functionaland calibration checks (<±0.1%) foranalytical balances?
I-10
EM 200-1-11 Jul 94
CHART I-3
EQUIPMENT: Page 2 of 8
ITEM YES COMMENT
(4) Have the balances been calibratedat least annually?
b. Top Loading and/or Pan Balances:
(1) Is a top loading and/or panbalances capable of accuratelydetecting a 100 mg weight at a loadof 150 g available?
(2) Is there a record of the balancehaving been serviced within theprevious 12 months?
(3) Is there a record of balancecalibration in two ranges withClass S weights? (Please specifythe ranges.)
(4) Do records show weekly functionaland calibration checks (<±0.1%) forpan balances?
(5) Have the balances been calibratedat least annually?
Thermometers:
a. Certified Thermometer:
(1) Does the lab have, or have accessto, an NIST-traceable factorycertified thermometer?
(2) Is a copy of factory certificatefor the thermometer available forinspection?
(3) Is there a record of the annualcheck of the certified thermometerat the ice point?
I-11
EM 200-1-11 Jul 94
CHART I-3
EQUIPMENT:
ITEM
b. Working Thermometers:
(1) Are sufficient working thermometersavailable so that each has adedicated use?
(2) Does each working thermometer havea unique identifying number?
(3) Is the calibration of each workingmercury thermometer checkedannually against an NIST-traceablethermometer?
(4) Is the calibration of each dialtype thermometer checked at leastquarterly against an NIST-traceablethermometer?
(5) Are digital thermometers calibratedquarterly at their temperature ofuse against an NIST-traceablethermometer?
(6) Is a record of thermometercalibration maintained?
pH Meters:
a. Is a clean pH meter with appropriateelectrode with scale graduations atleast 0.1 pH units in use?
b. Is a thermometer or temperature sensorfor automatic compensation in use?
c. Do records show daily, or before eachuse, calibration, whichever is lessfrequent?
d. Are three standard buffers used for thecalibration?
YES
Page 3 of 8
COMMENT
I-12
EM 200-1-11 Jul 94
CHART I-3
EQUIPMENT: Page 4 of 8
ITEM YES COMMENT
e. Are aliquots of standards of pH 4,pH 7, and pH 10 used only once?
f. Are acceptance limits in place?
g. Is the meter recalibrated if not withinthe limits of 0.05 for two pointcalibration and within 0.2 for onepoint calibration?
h. If the limits cannot be achieved, isthe problem determined and resolved?
Conductivity Meters:
a. Are a conductivity meter and probe ofsufficient sensitivity in use?
b. Do records show a daily, or beforeeach use, calibration check, whicheveris less frequent?
c. Do records show cell constant isdetermined annually?
d. If the cell constant has a largedeviation from the expected value, isthe cause determined and corrected?
Refrigerators/Walk-in Coolers:
a. Is a thermometer in each refrigeratorwith bulb immersed in liquid?
b. Are thermometers graduated inincrements no larger than 1°C?
c. Are temperatures for each refrigeratorrecorded daily?
I–13
EM 200-1-11 Jul 94
CHART I-3
EQUIPMENT: Page 5 of 8
ITEM YES COMMENT
d. Do records show that refrigeratortemperatures are maintained in therange of 2 to 6°C?
Ovens:
a. Are thermometers graduated inincrements no larger than 1°C?
b. If the oven temperature cannot be readwithout opening the door, is the bulbof the thermometer in a sand bath?
c. Is oven temperature adequatelymonitored (e.g., beginning and end ofeach use cycle)?
d. Is a record documenting date, time ofuse, nature of use, and temperaturemaintained?
e. Do the records indicate the oven holdstemperature at the appropriate dryingtemperature?
Glassware:
a. Is the lab stocked with sufficientvolumetric glassware for the analysesperformed?
b. Is Class A volumetric glasswareavailable for standard preparation?
c. Is glassware cleaned in a mannerappropriate for the analyticalprocedures for which it is to be used?
d. Is glassware cleaning procedure postednext to the cleaning station?
I-14
CHART I-3
EQUIPMENT:
EM 200-1-11 Jul 94
Page 6 of 8
ITEM
e. For organics, are the following basiccleaning steps used?
(1)
(2)
(3)
(3)
(4)
(5)
(6)
(7)
(8)
Removal of surface residualsimmediately after use?
Flush with methanol before it isplaced in hot detergent soak?
Hot soak (>50°C) in a syntheticdetergent bath to loosen andfloat most particulate material?
Hot-water rinse to flush awayfloated particulates?
Soak with oxidizing agent such aschromic acid solution made up ofsulfuric acid and potassium orsodium bichromate at 40-50°C todestroy traces of organiccompounds?
Hot-water rinse to flush awaymaterials loosened by the deeppenetrant soak?
Distilled-water rinse to removemetallic deposits from the tapwater?
Methanol or isopropanol rinse toflush off any final traces oforganic materials and remove thewater?
Flushing the item immediatelybefore use with some of the samesolvent that will be used in theanalysis?
YES COMMENT
I-15
EM 200-1-11 Jul 94
CHART I-3
EQUIPMENT: Page 7 of 8
ITEM YES COMMENT
f. Is glassware for organics dried at100°C?
g. As an alternative to solvent rinsing,is glassware for organics heated to aminimum of 300°C to vaporize anyorganics?
h. Is volumetric glassware, glassware withground glass joints, or sinteredglassware not heated to hightemperature to avoid deformation?
i. For trace metals, is the plastic orglassware cleaned with detergent, tapwater, 1:1 nitric acid, tap water, 1:1hydrochloric acid, tap water, andreagent water?
j. Is chromic acid not used to cleanglassware and plastic bottles for tracemetal analysis?
k. Is clean glassware properly covered andstored to prevent recontamination bydust?
I-16
EM 200-1-11 Jul 94
CHART I-3
EQUIPMENT: Page 8 of 8
ITEM
Additional observations, comments, or problems:
I-17
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC: Page 1 of 10
ITEM YES COMMENT
Does the lab maintain a QA Manual?
Does the manual address the importantelements of a QA/QC program, includingthe following:
a. QA Policy and Objectives?
b. organization?
c. Personnel?
d. Facilities and Equipment?
e. Document Control?
f. Sample Receiving and Storage?
g. Analytical Methodology?
h. Instrument Operation?
i. Instrument Calibration?
j. Preventive Maintenance?
k. Certification of Regents/Standards?
l. Data Generation/Reduction/Validation?
m. Data Reliability?
n. Feedback and Corrective Action?
o. Recordkeeping and Archives?
p. Internal QC Audits?
q. Performance and External Audits?
r. Training/Certification of Personnel?
I-18
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC: Page 2 of 10
ITEM YES COMMENT
Is the manual available to all laboratorypersonnel?
Is the manual updated regularly?
Is line authority for all referencedorganizations explained by including anorganization chart?
Is the organizational structure appropriateto accomplish the project QA objectives?
Are QA/QC responsibilities and reportingrelationships clearly defined?
Are all staff aware of QA/QC and itsapplication?
Is the QA Officer a full-time employee?
Does the QA Officer operate independentlyof the analyses?
Does the QA Officer report directly to asenior officer?
Are internal QA reviews conducted at leastannually and recorded including anycorrective action taken?
QA Objectives and Criteria:
a. Are the terms and definitions forprecision, accuracy, comparability,representativeness, and completenessproperly used?
b. Have the following been defined foreach parameter and matrix:
(1) Level of QA effort (frequency andtype of QC, etc.)?
I-19
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC: Page 3 of 10
ITEM YES COMMENT
(2) Accuracy (matrix spikes, surrogatespikes, reference samples, etc.)?
(3) Precision (replicate samples)?
(4) Sensitivity or MDL?
(5) Statistical reporting units?
c. Are quantitative limits established foreach parameter and matrix?
d. Are field and lab both covered?
e. If appropriate, are completenessobjectives quantitatively stated?
f. Are representativeness andcomparability appropriately addressed?
Is a sample batch clearly defined anddetermined as a group of samples of < 20,with similar matrix, prepared and analyzedwith same technique and reagents at sametime or within same time sequence?
Is at least the following minimum QCpracticed in the lab?
a. For Inorganic/Classical Analysis:
(1) Minimum three concentrations ofstandards plus blank, and one checkstandard in ten; the lab shallrepeat all samples if checkstandard is outside ±10%.
(2) One method blank per batch.
(3) One matrix spike per batch.
(4) One lab duplicate per batch.
I-20
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CHART I-4
GENERAL QA/QC: Page 4 of 10
ITEM YES COMMENT
(5) One control (consists of a controlmatrix spiked with analytesrepresentative of the targetanalytes) per batch.
b. For Organic Analysis:
(1) Minimum five concentrations ofstandards plus blank and one checkstandard in ten; if any are outsidecontrol limits repeat all samples.
(2) One method blank per batch.
(3) One matrix spike per batch.
(4) One lab duplicate/matrix spikeduplicate per batch.
(5) One control (consists of a controlmatrix spiked with analytesrepresentative of the targetanalytes) per batch.
(6) Surrogates for all samples.
Are there any exceptions to the aboveminimum QC practice in the lab?
Has the lab established control limits forall the above types of QC samples?(Control limits should be at least as tightas those stated in the methods.)
Are quality control data (e.g., standardcurve, results of duplicates and spikes)accessible for all analytical results?
Are method detection limits empiricallydetermined and documented?
I-21
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC:
ITEM
Are control charts maintained for eachroutine analysis?
Do lab records indicate what correctiveaction has been taken when results fail tomeet QC criteria?
Are documented methods/procedures availablefor assurance of field and lab equipmentfunctioning optionally?
Is a program of initial and periodiccalibration established for each method?
Does the QA Manual include calibrationdocumentation requirements:
a. Date of calibration?
b. Identification of standards used?
c. Personnel performing calibration?
d. Results of calibration (raw data andsummary statistics)?
e. Corrective actions taken?
Are primary reference standards used forcalibration only?
Are all working standards versus primarystandards verified and documented?
Are reference materials traceable to NISTstandards?
Are reagent grade or higher puritychemicals used to prepare standards?
Page 5 of 10
YES COMMENT
I-22
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC: Page 6 of 10
ITEM YES COMMENT
Are fresh analytical standards prepared ata frequency consistent with good QC?
Are reference materials/reagents properlylabeled with concentrations, dates ofpreparation and expiration, and identityof the person preparing the reagent?
Are updated equipment operatinginstructions available?
Are analytical procedures written as SOPsavailable for review?
Are all procedural steps and optionsdescribed?
Are the criteria of method selectionincluded (e.g., in order to obtain aspecific data quality objective?)
If method choice is governed by regulatoryrequirement (e.g., NPDES, SDWA, RCRA), havethe appropriate methods been chosen?
Are approved methods being used asspecified?
Are procedures documented for data handling, reporting, and recordkeeping?
Are documented validation proceduresapplied at appropriate levels for allmeasurement procedures?
Are documented procedures available forchecking the validity of reported analysisvalues?
I-23
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC: Page 7 of 10
ITEM YES COMMENT
Are predetermined limits available for dataacceptability beyond which correctiveaction is required?
Are documented procedures available forcorrecting erroneously reported results?
Are the following SOPs available forreview?
a. Sample collection, preservation,storage, and handling.
b. Sample preparation and analysis.
c. Purity and preparation of standards.
d. Instrument operation and calibration.
e. Preventive maintenance and correctiveactions.
f. Quality control for each type of test.
g. Quality control chart.
h. Data reduction and reporting.
i. Recordkeeping and archives.
j. Personnel training/certification.
k. Procurement and inventory procedures.
l. Glassware cleaning.
m. Waste disposal.
n. Technical and managerial review of laboperation.
I-24
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC: Page 8 of 10
ITEM YES COMMENT
Are procedures in place for making andcontrolling revisions to in-house SOPs?
Are there internal audits for both fieldand lab activities?
Are there designated persons who willconduct the audits?Auditor’s Name:
Is there a documented protocol which willbe used for audit?
Are acceptance criteria defined?
Are audit reports prepared and distributed?To whom?
Are the type and frequency of audit reportsspecified?Type/frequency:
Do the reports address:
a. status of project (time table)?
b. results of performance and systemaudits?
c. data quality assessment?
d. significant QA problems and proposedcorrective action?
I-25
EM 200-1-11 Jul 94
CHART 1-4
GENERAL QA/QC: Page 9 of 10
ITEM YES COMMENT
Does the lab participate in any externalproficiency testing programs such as EPAperformance evaluation studies for watersupply and water pollution?
Are there corrective actions taken anddocumented?
Does the lab have a laboratory informationmanagement system (LIMS) currently in use?
If yes, manufacturer:Model No.:
Brief description of hardware & software:
Does the LIMS have an audit trail feature?
I-26
EM 200-1-11 Jul 94
CHART I-4
GENERAL QA/QC: Page 10 of 10
ITEM
Additional observations, comments, or problems:
I-27
EM 200-1-11 Jul 94
CHART I-5
REPORT GENERATION: Page 1 of 4
ITEM YES COMMENT
Are there documented procedures forinternal field and lab checks of:
a. precision and accuracy?
b. routine duplicates, spikes, andstandard samples?
c. statistical methods, including controlchart and computer methods?
Is there a written description of the labrecord system including data management,review, validation, and audit?
Is there written description of the labreporting system?
Is there a system in place that providesfor retrievability and traceability of thesample source, analytical methods, results,person performing analysis, and date?
Are records and reports adequately securedfor the required amount of time to ensurethe integrity per regulatory requirements?
Are permanently bound notebooks withconsecutively numbered pages being used?
Is a unique serial number clearly displayedon each notebook cover or spine?
Are logbook entries made in permanentfashion with indelible ink?
Are logbook entries legible?
Are all raw data signed and dated by thechemist who performed the analysis?
I-28
EM 200-1-11 Jul 94
CHART I-5
REPORT GENERATION: Page 2 of 4
ITEM YES COMMENT
Are there evidence of entries beingtampered with?
Has data been altered?
If yes, was a single line drawn through theentry and corrections made withoutobliterating original entries?
Was the new entry initialed and dated?
Were technical reviews conducted on alllogbook entries and deliverables?
Was a minimum of three-levels of technicalreviews conducted by chemist, supervisor,QA Officer?
Have QC measures been utilized to ensurethe quality of the work performed?
Can all signatures be clearly identified?
Is a central file being maintained for allproject documents?
Is a system of document control numbers inplace?
Are all completed lab notebooks, raw data,analytical reports, electronic tapes anddisks, and other pertinent documentationfiled in a secure, controlled archivesarea?
Has the supervisor personally examined andreviewed each notebook periodically andsigned and dated the review?
Do the lab’s reports accurately, clearly,and unambiguously present results and allother relevant information?
I-29
EM 200-1-11 Jul 94
CHART I-5
REPORT GENERATION: Page 3 of 4
ITEM YES COMMENT
Does each test report include the followinginformation:
a. Names and addresses of laboratory andclient?
b. Unique identification and page number?
c. Case narrative?
d. Sample identification and description?
e. Dates of sample receipt and testperformed, as appropriate?
f. Identification of sample preparationand analysis methods used?
g. Description of any deviations fromtest method?
h. Disclosure of any subcontractor used?
i. Results including all method requiredQC data?
j. Description of any problems or failuresidentified?
k. Measurement uncertainty, if relevant?
Is the lab's report format acceptable?
Does the length of storage time for allsample related information comply withregulatory requirements, organizationalpolicy, or project requirements, whicheveris more stringent? (It is recommended thatdocumentation be stored for a minimum ofthree years from submission of the projectfinal report.)
I-30
EM 200-1-11 Jul 94
CHART I-5
REPORT GENERATION: Page 4 of 4
ITEM
Additional observations, comments, or problems:
I-31
EM 200-1-11 Jul 94
CHART I-6
FIELD SAMPLING: (Complete if this lab conductsfield sampling for USACE projects.) Page 1 of 3
ITEM YES COMMENT
Is a site specific Chemical DataAcquisition Plan (CDAP) available to labpersonnel?
Are lab personnel familiar with the QCrequirements of the CDAP?
Do sampling procedures follow contractspecifications?
Do field documentation procedures:
a. document the sources and lot numbers ofreagents and supplies?
b. include procedures/forms for recordingthe exact location and specificconsiderations associated with sampleacquisition?
c. document specific preservative methods?
d. include labels containing all necessaryinformation?
e. include forms for tracking custody?
Is there a unique identification on eachsample?
Is sampling information properly recordedsuch as sample ID numbers, type (grabversus composite), preservatives, analytes,location, date and time of collection,and name of sample collector?
Are written chain-of-custody proceduresavailable for review? Are they inaccordance with USACE/EPA guidelines?
I-32
EM 200-1-11 Jul 94
CHART I-6
FIELD SAMPLING: Page 2 of 3
ITEM YES COMMENT
Are there written sampling SOPs coveringsampling plan, sampling equipment, samplecollection, preservation, identification,storage, and lab handling?
Are there written descriptions of chain-of-custody of samples? (Attach a copy ofchain-of-custody form.)
Are there written procedures for fieldmeasurement of flow, dissolved oxygen,residual chlorine, etc.?
Are there written procedures for monitoringwater supply, effluent, ambient air,stacks, radiation, etc.?
Are proper preservation techniques beingused for the analytical methods and sampletypes concerned?
Are provisions made for the collection ofQA/QC split samples?
Are provisions made for field blanks andduplicate samples at an appropriate rate(normally 10% or minimum of one per matrixtype, whichever is greater, or as specifiedin contract?)
Are adequate facilities available to docompatibility testing?
I-33
EM 200-1-11 Jul 94
CHART I-6
FIELD SAMPLING: Page 3 of 3
ITEM
Additional observations, comments, or problems:
I-34
EM 200-1-11 Jul 94
CHART I-7
SAMPLE RECEIPT AND STORAGE: Page 1 of 3
ITEM YES COMMENT
Are there adequate written procedures forreceipt and storage of samples to ensuresample integrity?
Do the written procedures address samplehandling, storage, and dispersement foranalysis and disposal?
Do the written procedures accuratelyreflect procedures in use?
Is separate area and facility includinghoods available for sample receipt?
Is a dedicated sample custodian available?Custodian’s name:
Are appropriate chain-of-custody proceduresdocumented and followed in the lab?
Does the lab maintain internal custodyprocedures?
Does a permanent record exist for samplelog-in?
Are samples assigned unambiguous sample IDnumbers when logged in?
Is a checklist used to document problems ordeficiencies noted during sample log-in?
Is sample temperature properly measuredand recorded during log-in?
Are pH values of aqueous samples for thefollowing analyses checked and adjusted ina hood during log-in? (Metals, phenols, oiland grease, TRPH, TOC, TOX, COD, hardness,ammonia, nitrate-nitrite, total phosphorus,Kjeldahl and organic nitrogen, radiologicaltesting, cyanide, and sulfide.)
I-35
EM 200-1-11 Jul 94
CHART I-7
SAMPLE RECEIPT AND STORAGE: Page 2 of 3
ITEM YES COMMENT
Is the pH value properly measured to avoidsample contamination and to minimize wastegeneration?
Are corrective actions properly documented?
Are clients notified if problems are noted?
Are there adequate facilities for samplestorage?
Are samples stored in such a way as tomaintain their identity, integrity,stability, and concentration?
Are volatile organic samples stored inseparate refrigerators from other samples?
Are temperature logs of storage coolers andrefrigerators properly maintained?
Are acceptable temperature ranges used andposted? (4 ± 2°C)
Are coolers and refrigerators locked whenunattended?
Is final disposition of samples documented?
I-36
EM 200-1-11 Jul 94
CHART I-7
SAMPLE RECEIPT AND STORAGE: Page 3 of 3
ITEM
Additional observations, comments, or problems:
I-37
EM 200-1-11 Jul 94
CHART I-8
SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 1 of 12
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor sample preparation?
b. Do these SOPs accurately reflectprocedures in use?
c. Are all sample preparations conductedin a hood?
d. Are a group of samples (up to a maximumof 20) which behave similarly withrespect to the procedures beingemployed and which are processed as aunit with the same method sequence andthe same lots of reagents and with thereagents and with the manipulationsmanipulations common to each sampleswithin the same time period or incontinuous sequential time periodsconsidered as a batch?
e. Are the following lab internal QCsamples prepared for each batch ofsamples?
(1) Method blanks?
(2) Matrix spikes?
(3) Matrix spike duplicates?
(4) Matrix duplicates?
(5) Laboratory control samples?
f. If the quantity of field samples is notsufficient for internal QC analyses,are blank spike/blank spike duplicateor duplicate laboratory control samplesanalyzed?
I-38
EM 200-1-11 Jul 94
CHART I-8
SAMPLE PREPARATION FOR ORGANIC ANALYSIS:
ITEM YES
g.
h.
i.
j.
k.
l.
m.
n.
o.
p.
Is a purified solid matrix used forpreparation of method blanks for soiland sediment volatile organics?
Is a purified sodium sulfate used forpreparation of method blanks for soiland sediment semivolatile organicsincluding pesticides, herbicides, andPCBs?
If sample extracts are cleaned up withMethods 3600s, are the associated QCsamples also processed through thecorresponding cleanup methods?
Is the water meniscus of aqueoussamples marked on the side of samplecontainer for later determination ofsample volume?
Are the rates of internal QC samplesconsistent with method requirements or,at a minimum, 5% per batch of no morethan 20 samples with similar matrix,whichever is greater?
Is the appropriateness of a particularpreparation for a specific sample typedetermined by the completeness ofextraction and by spike recoveries?
Are logbooks for sample preparationused and well maintained?
Are permanently bound notebooks withconsecutively numbered pages used?
Is a unique serial number clearlydisplayed on each notebook?
Are critical times entered in logbooks?
I-39
Page 2 of 12
COMMENT
EM 200-1-11 Jul 94
CHART I-8
SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 3 of 12
ITEM YES COMMENT
q. Are spiking solutions traceable to NISTor other reliable standards?
r. Are spiking solutions labeled properlywith date of preparation, composition,concentration and identity ofpreparer?
s. Have entries been made in permanentfashion and corrections made withoutobliterating original entries?
t. Are corrections reviewed and initialedby a supervisor?
u. Does the logbook of sample preparationcontain the following information?
(1) Date/time?
(2) Sample ID number?
(3) Sample preparer?
(4) Matrix noted?
(5) Spiking standards?
(6) Pretreatment?
(7) Volume/weight of sample?
(8) Final volume?
(9) Preparation methods?
Separatory Funnel Liquid-Liquid ExtractionMethod 3510A):
a. Is the following equipment available?
I-40
EM 200-1-11 Jul 94
CHART I-8
SAMPLE PREPARATION FOR ORGANIC ANALYSIS:
ITEM
b.
c.
d.
(1) Separator funnel (2-L with Teflonstopcock)?
(2) Drying tube with Pyrex glass wool at bottom and a Teflon stopcock?
(3) Sets of Kuderna-Danish glassware(including concentration tubes,evaporation flasks, and macro andmicro Snyder columns)?
(4) Water bath capable of temperaturecontrol within 5°C?
Are enough sets of separator funnels(2,000 mL with Teflon stopcock) andKuderna-Danish apparatuses availablefor simultaneous extraction of allbatch samples?
Are
(1)
(2)
(3)
(4)
(5)
the following reagents available?
Sodium hydroxide solution (10 N)?
Sulfuric acid solution (1:1)?
Anhydrous
Methylene
Hexane?
sodium sulfate?
chloride?
(6)
(7)
(8)
Aresolutions added to the samples in theseparator funnel prior to the additionof methylene chloride?
2-Propanol?
Cyclohexane?
Acetonitrile?
surrogate standards and spiking
YES
Page 4 of 12
COMMENT
I-41
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CHART I-8
SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 5 of 12
ITEM YES COMMENT
e. Is the Kuderna-Danish concentrationprocess conducted with a hot water bathat 80-90°C?
f. If concentrated extracts are to bestored more than two days are theytransferred to Teflon-1ined screw-capor crimp-top vials, labeledappropriately, and refrigerated?
Continuous Liquid-Liquid Extraction(Method 3520A):
a. Is the following equipment available?
(1) Continuous liquid-liquid extractorequipped with Teflon or glassconnecting joints and stopcocksrequiring no lubrication?
(2) Drying column with Pyrex glass woolat bottom and a Teflon stopcock?
(3) Sets of Kuderna-Danish glassware(including concentration tubes,evaporation flasks, and macro andmicro Snyder columns)?
(4) Water bath capable of temperaturecontrol within 5°C?
(5) Heating mantle (Rheostatcontrolled)?
b. Are enough sets of continuous liquid-liquid extractors and Kuderna-Danishapparatuses available for simultaneousextraction of all batch samples?
c. Are the following reagents available?
(1) Sodium hydroxide solution (10 N)?
I-42
EM 200-1-11 Jul 94
CHART I-8
SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 6 of 12
ITEM YES COMMENT
(2) Sulfuric acid solution (1:1)?
(3) Anhydrous sodium sulfate?
(4) Methylene chloride?
(5) Hexane?
(6) 2-Propanol?
(7) Cyclohexane?
(8) Acetonitrile?
d. Are surrogate standards and spikingsolutions added to the samples prior toextraction?
e. Is twice the volume of spiking solutionadded when GPC cleanup will be used?
f. Are samples extracted for 18-24 hoursat a specific pH value?
g. Is the Kuderna-Danish concentrationprocess conducted with a hot water bathat 80-90°C?
h. If concentrated extracts are to bestored more than two days are theytransferred to Teflon-lined screw-capor crimp-top vials, labeledappropriately and refrigerated?
Soxhlet Extraction (Method 3540A):
a. Is the following equipment available?
(1) Soxhlet extractor with 500-mL roundbottom flask?
I-43
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CHART I-8
SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 7 of 12
ITEM YES COMMENT
(2) Drying column with Pyrex glass woolat bottom and a Teflon stopcock?
(3) Sets of Kuderna-Danish glassware(including concentration tubes,evaporation flasks, and macro andmicro Snyder columns)?
(4) Heating mantle (Rheostatcontrolled)?
(5) Grinding apparatus?
b. Are enough sets of Soxhlet extractorsand Kuderna-Danish apparatusesavailable for simultaneous extractionof all batch samples?
c. Are the following reagents available?
(1) Anhydrous sodium sulfate?
(2) Toluene/Methanol (10:1) solvent?
(3) Acetone/Hexane (1:1) solvent?
(4) Methylene chloride?
(5) Hexane?
(6) 2-Propanol?
(7) Cyclohexane?
(8) Acetonitrile?
d. If a dry waste sample will not passthrough a l-mm standard sieve or cannotbe extruded through a l-mm opening, isit processed into a homogeneous samplethat meet these requirements?
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SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 8 of 12
ITEM YES COMMENT
e. Are surrogate standards and spikingsolutions added to the samples prior toextraction?
f. Is twice the volume of spiking solutionadded when GPC cleanup will be used?
g. Are samples extracted for 16-24 hours?
h. Is the Kuderna-Danish concentrationprocess conducted with a hot water bathat 80-90°C?
i. If concentrated extracts are to bestored more than two days are theytransferred to Teflon-lined screw-capor crimp-top vials, labeledappropriately and refrigerated?
Sonication Extraction (Method 3550):
a. Is the following equipment available?
(1) Grinding apparatus?
(2) Horn-type sonicator equipped with atitanium tip (475 W)?
(3) Sets of Kuderna-Danish glassware(including concentration tubes,evaporation flasks, and macro andmicro Snyder columns)?
(4) Drying column with Pyrex glass woolat bottom and a Teflon stopcock?
(5) Water bath capable of temperaturecontrol within 5°C?
b. Are the following reagents available?
(1) Anhydrous sodium sulfate?
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SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 9 of 12
ITEM YES COMMENT
(2) Methylene chloride/Acetone (1:1)?
(3) Methylene chloride?
(4) Hexane?
(5) 2-Propanol?
(6) Cyclohexane?
(7) Acetonitrile?
c. If the sample will not pass through al-mm standard sieve or cannot beextruded through a l-mm opening, is itprocessed into a homogeneous samplethat meet these requirements?
d. Are samples mixed with anhydroussodium sulfate to form a free flowingpowder?
e. Are surrogate standards and spikingsolutions added to the samples prior tothe addition of the extraction solvent?
f. Is twice the volume of spiking solutionadded when GPC cleanup will be used?
g. Are samples that are expected tocontain low concentrations of organicssonicated three times for three minuteswith fresh solvent each time?
h. Are samples that are expected tocontain high concentrations of organicssonicated once for two minutes?
i. Is the Kuderna-Danish concentrationprocess conducted with a hot water bathat 80-90°C?
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SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 10 of 12
ITEM YES COMMENT
j. If concentrated extracts are to bestored more than two days are theytransferred to Teflon-lined screw-capor crimp-top vials, labeledappropriately and refrigerated?
Purge-and-Trap (Method 5030A):
a. Is a purge-and-trap device available?
b. Are purge-and-trap systems subjected toa periodic bake-out and cleaningprocess and are these actionsdocumented?
c. Is a purge chamber designed to accept5-mL samples available?
d. Is a 25-mL all glass purge chamberavailable for GC/MS Methods 524.1,524.2, and 8260 (optional)?
e. Is the gaseous headspace less than15 mL?
f. Is the trap a minimum of 25-cm long?
g. For Method 8010A, is the trap packedwith 1.0-cm 3% OV-1 on Chromosorb-W60/80 mesh, 7.7-cm Tenax GC, 7.7-cmsilica gel, and 7.7-cm charcoal orequivalent?
h. For Method 8015A, is the trap packedwith l.0-cm 3% OV-1, 15-cm Tenax GC,and 7.7-cm silica gel or equivalent?
i. For Methods 8020 and 8030A, is the trappacked with l.0-cm 3% OV-1 onChromosorb-W and 23-cm Tenax GC orequivalent?
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SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 11 of 12
ITEM YES COMMENT
j. Is methanolic extraction of purge-and-trap only used for medium-concentrationsoils or sediments?
k. Is the methanol purge-and-trap qualityor equivalent?
l. Are surrogate standards and spikingsolutions added to the purging chamberalong with the sample?
m. Is a method blank carried through allof sample preparation and measurementbefore any sample are processed?
Headspace (Method 3810):
a. Is this method only used as a screeningprocedure?
b. Is a hot bath capable of maintaining a90°C temperature available?
c. Are 125-mL hype-vials with seals andsepta used for the equilibration?
d. Are both a 1-ppm spike and a 1-ppmstandard analyzed along with samples?
e. Are the vials with the samples (the1-ppm spike and the 1-ppm standard)equilibrated in a 90°C water bath forone hour?
f. Are the vials maintained at 90°C while2-mL of headspace gas is withdrawn fordirect injection into a GC?
g. Is the GC operated using the same GCconditions listed in the method beingscreened (8010A, 8015A, 8020, 8030A, or8040A)?
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SAMPLE PREPARATION FOR ORGANIC ANALYSIS: Page 12 of 12
ITEM
Additional observations, comments, or problems:
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CHART I-9
GENERAL QA/QC FOR ORGANIC ANALYSIS BY GC: Page 1 of 4
ITEM YES COMMENT
Are the following detectors available andare they used appropriately?
a. Flame Ionization (603, 604, 609, 610,8015A, 8030A, 8040A, 8060, 8090, 8100)?
b. Photoionization (602, 8020)?
c. Electron Capture (604, 606, 608, 609,612, 8040A, 8060, 8080, 8090, 8120,8150A)?
d. Electrolytic Conductivity (601, 611,801OA, 8080, 8140)?
e. Microcoulometric (601, 611, 8140)?
f. Thermal Energy Analyzer (607)?
g. Nitrogen/Phosphorus (607, 8140)?
h. Flame Photometric (8140)?
Are the column ovens, at a minimum, capableof temperature control within ±0.2°C at220oC?
Are the injection ports glass lined?
Are manufacturer's operating manualsreadily available to bench chemists?
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Have any instruments been modified in anyway?
Are the instruments properly vented?
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CHART I-9
GENERAL QA/QC FOR ORGANIC ANALYSIS BY GC: Page 2 of 4
ITEM YES COMMENT
Is glassware for organics solvent rinsed orheated to a minimum of 300oC to vaporizeany organics in a muffle furnace aftercareful cleaning?
Is this high temperature treatment avoidedfor volumetric glassware, glassware withground joints, or sintered glassware?
Is there a calibration protocol availableto bench chemists?
Is there a calibration protocol availableto bench chemists?
Is a 5-point calibration used?
Is the calibration curve or calibrationfactor verified each working day?
Are calibration results kept in a permanentlogbook?
Is the MDL for each analyte and matrix typedetermined every six months or wheneverthere is a significant change in backgroundor instrument response?
Is the linear calibration range determinedfor each analyte when there is significantchange in instrument response and every sixmonths for those analytes that periodicallyapproach their linear limits?
Is a method blank included with each samplebatch and carried through the entirepreparation and analysis?
Is a matrix spike and a matrix spikeduplicate run with each batch at a rate of5% or one per batch, whichever is greater?
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GENERAL QA/QC FOR ORGANIC ANALYSIS BY GC: Page 3 of 4
ITEM YES COMMENT
Is corrective action taken if matrix spikerecoveries exceed QC limits?
Is a matrix duplicate run with each batchat a rate of 5% or one per batch, whicheveris greater?
Is corrective action taken if percentdifferences based on duplicated analysesexceed QC limits?
Are surrogate recoveries run on eachsample?
Is corrective action taken if surrogaterecoveries exceed QC limits?
Is an LCS prepared with standardsindependent of calibration standardsanalyzed for each batch of samples?
Is corrective action taken if the LCSrecovery exceeds QC limits?
Are QC data statistically analyzed andcharted for quality control?
Are control charts maintained and readilyavailable to bench chemists?
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CHART I-9
GENERAL QA/QC FOR ORGANIC ANALYSIS BY GC: Page 4 of 4
ITEM
Additional observations, comments, or problems:
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CHART I-10
ORGANIC ANALYSIS BY GC: HVO (8010A) Page 1 of 13
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor HVO sample preparation/analysis?
b. Do these SOPs accurately reflectprocedures in use?
c. Are all target analytes, at a minimum,that have retention times published inTable 1 of Method 8010A, routinelyanalyzed at the lab?
d. Are manufacturer's operating manualsreadily available to bench chemists?
e. Are prenumbered, bound notebooks usedfor data entry?
f. Are all records written in indelibleink?
g. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible?
h. Are corrections initialed and dated bythe responsible individual?
i. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of apurge-and-trap and GC system and ininterpretation of chromatograms?
b. Are backup bench chemists available?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 2 of 13
ITEM YES COMMENT
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Does the lab have adequate air handlingsystem to avoid cross contamination ofsamples?
c. Is a temperature-programmable gaschromatography equipped with anpurge-and-trap device and electrolyticconductivity detector available?
d. Is oven temperature stable to ±0.5°C orbetter at desired setting?
e. Is one of the following GC columnavailable?
(1) 8-ft x 0.1-in ID SS or glass columnpacked with 1% SP-1OOO onCarbopack-B 60/80 mesh orequivalent?
(2) 6-ft x 0.1-in ID SS or glass columnpacked with chemically bondedn-octane on Porasil-C 100/200 meshor equivalent?
f. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
g. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 3 of 13
ITEM YES COMMENT
h. Is helium used as carrier gas?
i. Is a hood available for samplepreparation?
j. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
k. Are backup instruments available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. For standard preparation, is a waitingperiod of ten minutes allowed fordrying the alcohol-wetted surfacebefore measuring the weight ofmethanol?
d. Are stock standards stored in bottleswith minimal headspace and Teflon-linedscrew-cap at -10 to -20°C and protectedfrom light?
e. Are stock standards replaced after sixmonths, or sooner if comparison withcheck standards indicates a problem?
f. Are stock standards for target analytesof low boiling points (<30°C) andhigh reactivity prepared fresh everytwo months or sooner?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 4 of 13
ITEM YES COMMENT
g. Are secondary standards stored with minimal headspace and check frequentlyfor degradation or evaporation?
h. For the initial calibration, areaqueous calibration standards, at aminimum of five concentrations,prepared fresh and discarded after onehour, unless properly sealed in a vialand stored at 4°C with no headspace(up to 24 hours)?
i. Is a 25-µL Hamilton 702N microsyringeor equivalent used for standardpreparation? (Pipets should never beused to dilute or transfer volatilesamples or aqueous standards.)
j. Are volatile organic standards storedin a separated freezer/refrigeratorfrom samples or other standards?
k. Is “purge-and trap”, “pesticidequality” or equivalent methanol storedaway from other solvents?
l. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are volatile organic samples stored at4°C in separate refrigerators fromother samples?
b. Are low concentration volatile organicsamples stored separately from highconcentration volatile organic samples?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 5 of 13
ITEM YES COMMENT
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
d. Is one of the calibration standards ata concentration near, but above, theMDL?
e. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
f. Is a linear calibration curve with acorrelation coefficient > 0.995 preparedfor each analyte?
g. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working ranges?
h. Is the calibration curve or factorverified at the beginning and end ofeach analysis sequence with amid-concentration standard?
i. Is a new calibration curve prepared forany target analyte when the responsefor the target analyte varies from thepredicted response by more than ±15% orexceeds the acceptance criteria listedin the Table 3 of Method 8010A?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 6 of 13
ITEM YES COMMENT
j. Is the retention time windowestablished with three injections ofall target analytes throughout thecourse of a 72-hour period?
k. Is the retention time window checked ona quarterly basis or whenever a new GCcolumn is installed?
Sample Preparation:
a. Is a combination of bromochloromethane,2-bromo-l-chloropropane, and1,4-dichlorobutane used as surrogatestandards?
b. Are samples routinely introduced intothe GC using purge-and-trap (Method5 030)?
c. Is methanolic extraction of purge-and-trap only used for medium-concentrationsoils or sediments?
d. Is direct injection used only for watersoluble compounds that do not purge orwhen concentrations are expected toexceed 10,000 µg/L?
e. Is the percent solid of solid samplesdetermined by drying overnight at 105oCin a vented drying oven?
Sample Analysis:
a. Is daily calibration checked with amid-concentration standard at thebeginning and the end of an analysissequence?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 7 of 13
ITEM YES COMMENT
b. If the calibration factor calculatedfrom daily calibration check at the endof an analysis sequence exceeds ±15%when compared with the initial standardof the analysis sequence, is the GCsystem recalibrated and reanalysisperformed for all samples, in thesequence, that contain target analytesthat exceed the criteria?
c. Are daily retention time windowsestablished for each analyte prior tosample analysis?
d. Is the retention time for each analytein the daily mid-concentration standardused as the midpoint of the window forthat day?
e. Is the same sample introduction methodused for calibration standards andsamples? (i.e., either purge-and-trapor direct injection, but not mixedmethods.)
f. If a peak response exceeds the linearrange of the system, is a dilutionperformed on a second aliquot of thesample that has been properly sealedand stored prior to use?
g. Are peak height measurements used forquantitation when overlapping peakscaused errors in area integration?
h. Is a second GC column used to resolvethe analytes from co-eluting non-targetcompounds?
i. Are positive hits routinely confirmedby a second GC column?
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CHART I-10
ORGANIC ANALYSIS BY GC: HVO (8010A) Page 8 of 13
ITEM YES COMMENT
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Is the lab specific MDL equal to orlower than the method specified MDL?
e. Is a mid-concentration standardanalyzed for each group of ten samplesin the analysis sequence?
f. Is a method blank run at a minimum rateof 5% or one per batch, whichever isgreater?
g. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) Is an LCS, prepared with standardsindependent of calibrationstandards, analyzed for each batch?
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 9 of 13
ITEM YES COMMENT
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
h. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever is higher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever is higher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 10 of 13
ITEM YES COMMENT
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) Is the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
i. Is the performance of purge-and-trap,analytical system, and theeffectiveness of the method in dealingwith sample matrix monitored by spikingeach sample, standard, and blank withsurrogates that encompass the methodspecified temperature range?
j. Are the average percent recovery andstandard deviation of the percentrecovery for each surrogate calculated,when surrogate data from 25 to 30samples for each matrix is available?
k. Are control limits for each surrogatein a given matrix calculated based onthe above data?
l. Do the control limits fall within thecontrol limits of Method 8240 ifapplicable?
m. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 11 of 13
ITEM YES COMMENT
n. Are corrective actions of reanalysisor reextraction/reanalysis taken ifany surrogates for a sample are out ofcontrol limits?
o. Are control charts for internal QC dataplotted and available to benchchemists?
p. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 12 of 13
ITEM YES COMMENT
b. Are lab wastes disposed of properlysuch that no secondary pollution isgenerated from sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for HVO analysis?
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: _______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forHVO analysis?
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ORGANIC ANALYSIS BY GC: HVO (8010A) Page 13 of 13
ITEM
Additional observations, comments, or problems:
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CHART I-11
ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015) Page 1 of 15
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor TPH sample preparation and analysisas gasoline range organics (GRO) anddiesel range organics (DRO)?
b. Do these SOPs accurately reflectprocedures in use?
c. Are manufacturer’s operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of apurge-and-trap and GC system and ininterpretation of chromatograms?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
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CHART I-11
ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015) Page 2 of 15
ITEM YES COMMENT
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Does the lab have adequate air handlingsystem to avoid cross contamination ofsamples?
c. Is a temperature-programmable gaschromatography equipped with apurge-and-trap device and flameionization detector available for GRO?
d. Is oven temperature stable to ±0.5°C orbetter at desired setting?
e. Is a data system available fordetermination of peak area sums usingforced baseline and baselineprojection?
f. Are the following GC columns available?
GRO Analysis:(1) 105-m x 0.53-mm ID Restek RTX 502.2
0.3-micron film thickness?
(2) Other capillary columns which canresolve 2-methylpentane from themethanol solvent front in a 25 µg/LLCS and to resolve ethylbenzenefrom m/p-xylene (<25% valley)?
DRO Analysis:(1) 25-m x 0.25-mm Quadrex 007 5%
methyl phenyl 0.5-micron filmthickness?
(2) 30-m x 0.53-mm ID Quadrex RTX-5,1.5-micron film thickness?
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CHART I-11
ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015) Page 3 of 15
ITEM YES COMMENT
(3) Other capillary columns which canresolve C17/pristane and C 1 8/phytane (>50% resolution)?
g. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
h. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
i. Has any instrument been modified in anyway?
j. Is a hood available for samplepreparation?
k. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
l. Is a horn-type sonicator equipped witha titanium tip and 475 Watt availablein the lab?
m. Are backup apparatus available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Are "pesticide quality" or equivalentsolvents used for TPH analysis?
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CHART I-11
ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015)
ITEM
d. Is granular, anhydrous sodium sulfatepurified by heating at 400oC for fourhours prior to use?
e. Does the lab use a calibration standardcomposed of a blend of the followingtypical ten gasoline compounds for GRO?
2-methylpentane 15% wt.2,2,4-trimethylpentane 15%heptane 5%benzene 5%toluene 15%
ethylbenzene 5%m-xylene 10%p-xylene 10%o-xylene 10%l,2,4-trimethylbenzene 10%
f. Does the lab use a calibration standardcomposed of a blend of the followingtypical 14 C10-C28 even normal alkanestandards, plus n-C17, pristane, andphytane for DRO?
decanedodecanetetradecanehexadecaneheptadecane
≈ 7%≈ 7%≈ 7%≈ 7%≈ 7%
pristaneoctadecanephytaneeicosanedecosane
≈ 7%≈ 7%≈ 7%≈ 7%≈ 7%
tetracosanehexacosaneoctacosane5 −α − androstane (I.S.)
wt.
YES
Page 4 of 15
COMMENT
≈ 7%≈ 7%≈ 7%≈ 7%
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ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015) Page 5 of 15
ITEM YES COMMENT
g. Are the materials of interest, ifavailable, or the same type ofpetroleum fraction, if it is known andoriginal sample is unavailable, usedfor preparation of calibrationstandards?
h. Is an internal standard used for DROsamples to correct for injectionvariances and matrix interferences?
i. Does the lab have, at a minimum, thefollowing Pattern Recognition Standardsfor identification of petroleumhydrocarbons? Gasoline, aviation fuel,(JP-4), kerosene, and diesel fuel (#2).
j. Does the lab use a well characterizedgasoline (e.g., API PS-6 or equivalent)and a commercial diesel #2 as LCSs forGRO and DRO, respectively?
k. Are stock standards for GRO prepared inmethanol and replaced after six months,or sooner, if comparison with checkstandards indicates a problem?
l. Are stock standards for DRO prepared inacetone and replaced after six months,or sooner, if comparison with checkstandards indicates a problem?
m. Are secondary dilution standards in methanol stored with minimum headspacefor volatiles and frequently checkedfor signs of degradation/evaporation?
n. Are working standards at a minimum offive concentration levels prepared inreagent water?
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ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015)
ITEM
o. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a.
b.
c.
d.
e.
f.
g.
h.
Are triplicate water samples in 40 mLVOA vials received for GRO analysis?
Are water GRO samples inverted andchecked for existence of air bubbles?
Are soil GRO samples in wide mouthglass jars with Teflon-lined septachecked (without opening the container)for existence of excess headspace?
Are duplicate samples collected for thealternate methanol extraction method?
Are low level GRO samples stored at 4°Cin a separate refrigerators from highlevel GRO samples?
Are GRO samples analyzed within 14 daysfrom collection?
Are water DRO samples stored at 4°C,and extracted within seven days fromcollection and analyzed within 40 daysfrom extraction?
Are soil DRO samples stored at 4°C, andextracted within 14 days fromcollection and analyzed within 40 daysfrom extraction?
YES
Page 6 of 15
COMMENT
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ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015) Page 7 of 15
ITEM YES COMMENT
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Is the GC system calibrated with aminimum of five concentration levelsof calibration standard blenders?
d. Is one of the calibration standards ata concentration near, but above, theMDL?
e. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
f. Are the calibration standards for GROinjected using a purge-and-trap?
g. For DRO, is a methylene chloride blankrun in every batch to determine thearea generated on normal baseline bleedbetween C10
and C28and subtracted from
the total areas of DR0 standards andsamples?
h. Is a linear calibration curve with acorrelation coefficient > 0.995 preparedfor each analyte?
i. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working ranges?
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ITEM YES COMMENT
j. Is the calibration curve or factorverified with, at a minimum, a midpointcalibration standard at the beginningand end of each analysis sequence?
k. Is a new calibration curve prepared forany target analyte when the responsefactors for the daily calibrationsvary from the initial response factorsby more than 15%?
l. Is the retention time windowestablished with three injections ofeach calibration standard over thecourse of a 72-hour period?
m. Are the retention time windows,specially for surrogates, internalstandards, and the first and the lastcomponents in calibration standards,checked on a quarterly basis orwhenever a new GC column is installed?
n. Are the retention times for surrogates,internal standards, and the first andthe last components in the dailymid-concentration standard used as themidpoints of the windows for that day?
Sample Preparation:
a. Is a purge-and-trap device used toinject water GRO samples to a GC?
b. Are soil and solid GRO samplesextracted by methanol extraction,diluted in water and injected withpurge-and-trap to a GC?
c. Are all supernatant liquids retainedin methanol extraction process for GROsamples?
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CHART I-11
ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015)
ITEM
d.
e.
f.
g.
h.
i.
j.
k.
Are water DRO samples extracted by EPAMethods 3510/3520 and soil DRO samplesby EPA
Is thebottleof the
Is the
Methods 3540/3550?
water meniscus on the side ofmarked for later determinationsample volume?
pH of water DRO samples checkedand adjusted with 10 N NaOH or 1:1H2SO4 to 5-9?
Is the water DRO sample containersrinsed with methylene chloride? (Donot cap and shake the bottle.)
Is continuous extraction method used ifemulsion forms and cannot be brokenduring separatory funnel method suchthat the recovery of methylene chlorideis less than 80% after correction forwater volubility of methylene chloride?
For soil DRO samples, are large rocksor foreign materials removed and anyvegetation chopped into small pieces?
Are soil DRO samples sonicated for1.5 minutes at 475 watts, one secondpulse mode with a 50% duty cycle?
IS the percent solid of solid samplesdetermined by drying overnight at 105oCin a vented drying oven?
Sample Analysis:
a. Are the concentrations of all analyteswithin the initial calibration ranges?
YES
Page 9 of 15
COMMENT
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ORGANIC ANALYSIS BY GC: TPH (MODIFIED 8015)
ITEM
b.
c.
d.
e.
f.
g.
h.
i.
j.
Is a method/instrument blank analyzedafter a sample that produces asaturated response from a compound?
If the method/instrument blank is notfree from interferences, is the systemdecontaminated before sample analysis?
Is the quantitation of GRO based on thearea summation of all peaks that areabove instrument blank baseline andelute between 2-methylpentane andl,2,4-trimethylbenzene?
Are non-petroleum hydrocarbons, such aschlorinated solvents, ketones, andesters, excluded from the GROquantitation?
Is the total peak area for C10-C28 frombaseline-to-baseline used for DROquantitation?
Are non-petroleum hydrocarbons, such aschlorinated solvents, phenols, andphthalates, excluded from the DROquantitation?
Are retention times and patterns of thepeaks used in identification of thetype of petroleum hydrocarbons?
Are comments provided for contaminantsthat appear in the GRO and DRO windowsbut do not match the reference fuels?
Is internal standard, 5 −α− androstane,used as a retention time marker forDRO samples?
YES
Page 10 of 15
COMMENT
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ITEM YES COMMENT
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab before data release?
c. Are lab specific MDL or PQL empiricallyestablished and updated on asemiannually basis?
d. Is the lab specific PQL equal to orlower than the method specified PQL?
GRO: water 100 µg/Lsoil 5 mg/kg
DRO: water 100 µg/L (diesel #2)soil 4 mg/kg (diesel #2)
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
f. For GRO/GRO samples, are duplicate LCSsanalyzed at a minimum rate of 5% or oneper batch, whichever is more frequent?
g. Is the percent recovery of LCS largerthan 50% and the percent differenceless than 20%?
h. Is a column bleed profile run for eachbatch of DRO samples to determine thearea from normal baseline bleeding andsubtracted from the area of DROsamples?
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ITEM YES COMMENT
i. Is a methylene chloride blank run aftersamples of highly concentrated toprevent carryover?
j. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever concentration would behigher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
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ITEM YES COMMENT
(5) IS the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
k. Does the lab use one or two surrogatecompounds, p-chlorofluorobenzene,bromofluorobenzene, or trifluoro-toluene, to monitor the systemperformance and effectiveness of theof the GRO method in dealing with eachmatrix?
l. Does the lab use one or two surrogatecompounds, n-pentacosane (n-C25) orortho-terphenyl, to monitor the systemperformance and effectiveness of theof the DRO method in dealing with eachmatrix?
m. Has the lab established control limitsfor surrogate recoveries?
n. Are corrective actions of reanalysisor reextraction/reanalysis taken ifsurrogate(s) for a sample are out ofcontrol limits?
o. Are control charts for internal QC dataplotted and available to benchchemists?
p. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
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ITEM YES COMMENT
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for TPH analysis?
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ITEM
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: ______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forTPH analysis?
Additional observations, comments, or
YES COMMENT
problems:
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ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor AVO sample preparation/analysis?
b. Do these SOPs accurately reflectprocedures in use?
c. Are manufacturer's operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible?
g. Are corrections initialed and dated bythe responsible individual?
h. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of apurge-and-trap and GC system and ininterpretation of chromatograms?
b. Are backup bench chemists available?
c. Are bench chemists' performance auditedand approved prior to work withoutclose supervision by a senior chemist?
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ITEM YES COMMENT
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Does the lab have adequate air handlingsystem to avoid cross contamination ofsamples?
c. Is a temperature-programmable gaschromatography equipped with anpurge-and-trap device and photo-ionization detector available?
d. Is oven temperature stable to ±0.5°C orbetter at desired setting?
e. Is one of the following GC columnavailable?
(1) 6-ft x 0.082-in ID SS or glasscolumn packed with 5% SP-1OOO and1.75% Bentone-34 on 100/120 meshSupelcoport or equivalent?
(2) 8-ft x 0.1-in ID SS or glass columnpacked with 5% l,2,3-Tris(2-cyano-ethoxy)propane on 60/80 meshChromosorb W-AW or equivalent?
(3) IS column one used as the primaryanalytical column and column two asa confirmation column?
f. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
g. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
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ITEM YES COMMENT
h. Has any instrument been modified in anyway?
i. Is a hood available for samplepreparation?
j. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
k. Are backup instruments available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. For standard preparation, is a waitingperiod of ten minutes allowed fordrying the alcohol-wetted surfacebefore measuring the weight ofmethanol?
d. Are stock standards stored in bottleswith minimal headspace and Teflon-linedscrew-cap at -4°C and protected fromlight?
e. Are stock standards replaced after sixmonths, or sooner if comparison withcheck standards indicates a problem?
f. Are secondary standards stored withminimal headspace and check frequentlyfor degradation or evaporation?
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ITEM YES COMMENT
g. For the initial calibration, areaqueous calibration standards, at aminimum of five concentrations,prepared fresh and discarded after onehour, unless properly sealed in a vialand stored at 4°C with no headspace(up to 24 hours)?
h. Is a 25 µL Hamilton 702N microsyringeor equivalent used for standardpreparation? (Pipets should never beused to dilute or transfer volatilesamples or aqueous standards.)
i. Are volatile organic standards storedin a separated freezer/refrigeratorfrom samples or other standards?
j. Is “purge-and-trap”, “pesticidequality”, or equivalent methanol storedaway from other solvents?
k. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are volatile organic samples stored at4°C in separate refrigerators fromother samples?
b. Are low concentration volatile organicsamples stored separately from highconcentration volatile organic samples?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
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ITEM YES COMMENT
b. Are calibration results kept inpermanent logbooks?
c. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
d. Is one of the calibration standards ata concentration near, but above, theMDL?
e. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
f. Is a linear calibration curve with acorrelation coefficient > 0.995 preparedfor each analyte?
g. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working range?
h. Is the calibration curve or factorverified at the beginning and end ofeach analysis sequence with amid-concentration standard?
i. Is a new calibration curve prepared forany target analyte when the responsefor the target analyte varies from thepredicted response by more than ±15% orexceeds the acceptance criteria listedin the Table 3 of Method 8020?
j. Is the retention time windowestablished with three injections ofall target analytes throughout thecourse of a 72-hour period?
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ITEM YES COMMENT
k. Is the retention time window checked ona quarterly basis or whenever a new GCcolumn is installed?
Sample Preparation:
a. Are surrogate compounds, bromochloro-benzene, bromofluorobenzene, 1,1,1-trifluorotoluene, fluorobenzene, anddifluorobenzene, which encompass thetemperature range of this method usedfor all samples?
b. Are samples routinely introduced intothe GC using purge-and-trap (Method5030)?
c. Is methanolic extraction of purge-and-trap only used for medium-concentrationsoils or sediments?
d. Is direct injection used only for watersoluble compounds that do not purge orwhen concentrations are expected toexceed 10,000 µg/L?
e. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Is daily calibration performed with amid-concentration standard at thebeginning and the end of an analysissequence?
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ITEM YES COMMENT
b. If the calibration factor calculatedfrom daily calibration check at the endof an analysis sequence exceeds ±15%when compared with the initial standardof the analysis sequence, is the GCsystem recalibrated and reanalysisperformed for all samples, in thesequence, which contain target analytesthat exceed the criteria?
c. Are daily retention time windowsestablished for each analyte prior tosample analysis?
d. Is the retention time for each analytein the daily mid-concentration standardused as the midpoint of the window forthat day?
e. Is the same sample introduction methodused for calibration standards andsamples? (i.e., either purge-and-trapor direct injection, but not mixedmethods.)
f. If a peak response exceeds the linearrange of the system, is a dilutionperformed on a second aliquot of thesample that has been properly sealedand stored prior to use?
g. Are peak height measurements used forquantitation when overlapping peakscaused errors in area integration?
h. Is a second GC column used to resolvethe analytes from co-eluting non-targetcompounds?
i. Are positive hits routinely confirmedby a second GC column?
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ITEM YES COMMENT
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Is the lab specific MDL equal to orlower than the method specified MDL?
e. Is a mid-concentration standardanalyzed for each group of 10 samplesin the analysis sequence?
f. Is a method blank run at a minimum rateof 5% or one per batch, whichever isgreater?
g. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) Is an LCS prepared with standardsindependent of calibrationstandards analyzed for each batch?
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
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ITEM YES COMMENT
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
h. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever concentration would behigher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
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ITEM YES COMMENT
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) IS the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
i. Is the performance of purge-and-trap,analytical system, and theeffectiveness of the method in dealingwith sample matrix monitored by spikingeach sample, standard, and blank withsurrogates which encompass the methodspecified temperature range?
j. Are the average percent recovery andstandard deviation of the percentrecovery for each surrogate calculated,once a minimum of 30 samples of thesame matrix have been analyzed?
k. Are control limits for each surrogatein a given matrix calculated based onthe above data?
l. Do the control limits fall within thecontrol limits of Method 8240 ifapplicable?
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ITEM YES COMMENT
m. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
n. Are corrective actions of reanalysisor reextraction/reanalysis taken ifany surrogates for a sample are out ofcontrol limits?
o. Are control charts for internal QC dataplotted and available to benchchemists?
p. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
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ITEM YES COMMENT
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for AVO analysis?
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: ______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forAVO analysis?
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ITEM
Additional observations, comments, or problems:
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ORGANIC ANALYSIS BY GC: PHENOLS (8040A) Page 1 of 13
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor phenols sample preparation andanalysis?
b. Do these SOPs accurately reflectprocedures in use?
c. Are manufacturers operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of a GCsystem and interpretation ofchromatograms?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
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ITEM YES COMMENT
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Are enough sets of separator funnels,continuous liquid-liquid extractors,Soxhlet extractors, and Kuderna-Danishapparatuses available for simultaneousextraction of all batch samples?
c. Is oven temperature stable to ±0.5°C orbetter at desired setting?
d. Is a 1.8-m x 2-mm ID glass columnpacked with 1% SP-1240 DA onSupercoport (80/100 mesh) or anequivalent column in use for thedetermination of underivatized phenols?
e. Is a flame ionization detectoravailable for the determination ofunderivatized phenols?
f. Is nitrogen carrier gas available foruse with the FID?
g. Is a 1.8-m x 2-mm ID glass columnpacked with 5% OV-17 on Chromosorb W-AW-DMCS (80/100 mesh) or an equivalentcolumn in use for the determination ofderivatized phenols?
h. Is an electron capture detector (ECD)available for the determination ofderivatized phenols?
i. Is 5% methane/95% argon carrier gasavailable for use with the ECD?
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ORGANIC ANALYSIS BY GC: PHENOLS (8040A)
ITEM
j.
k.
l.
m.
n.
o.
p.
If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Has any instrument been modified in anyway?
Is a hood available for samplepreparation?
Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
Are backup apparatus available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
c. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Are the following reagents availablefor use in derivatization:
(1) Pentafluorobenzene bromide(α − Bromopentafluorotoluene)?
I-97
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Page 3 of 13
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ITEM YES COMMENT
(2) 18-crown-6-ether (1,4,7,10,13,16-Hexaoxacyclooctadecane)?
d. Are derivatization reagents preparedfresh weekly and stored at 4°C fromlight?
e. Are “pesticide quality” or equivalentsolvents used for sample analysis?
f. Does the lab have calibration standardsfor all method specified targetanalytes?
g. Are calibration standards prepared with2-propanol as a solvent?
h. Are stock standard solutions stored at4°C and protected from light?
i. Are stock standard solutions replacedafter one year, or sooner if comparisonwith check standards indicates aproblems?
j. Are working standards replaced aftersix months, or sooner if comparisonwith calibration standards indicates aproblems?
k. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are aqueous samples stored at 4°C, andextracted within seven days fromcollection and analyzed within 40 daysfrom extraction?
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ITEM YES COMMENT
b. Are soil samples stored at 4°C, andextracted within 14 days fromcollection and analyzed within 40 daysfrom extraction?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
d. Is one of the calibration standards ata concentration near, but above, theMDL?
e. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
f. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working range?
g. Is the calibration curve or factorverified at the beginning and end ofeach analysis sequence with amid-concentration standard?
h. Is a new calibration curve prepared forany target analyte when the responsefor the target analyte varies from thepredicted response by more than ±15%?
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ITEM YES COMMENT
i. Is the retention time windowestablished with three injections ofall target analytes throughout thecourse of a 72-hour period?
j. Is the retention time window checked ona quarterly basis or whenever a new GCcolumn is installed?
Sample Preparation:
a. Are aqueous samples extracted at a pH≤2 with methylene chloride, usingMethod 351OA or 3520A?
b. Are solid samples extracted usingeither Method 3540A or 3550?
c. Are extracts from either Method 3520Aor 3550 undergone acid-base partitioncleanup, using Method 3650A?
d. Is the extraction solvent exchanged to2-propanol prior to GC analysis?
e. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Is daily calibration performed with amid-concentration standard prior tosample analysis?
b. Is daily calibration checked at the endof an analysis sequence?
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ITEM YES COMMENT
c. If the calibration factor calculatedfrom daily calibration check at the endof an analysis sequence exceeds ±15%when compared with the initial standardof the analysis sequence, is the GCsystem recalibrated and reanalysisperformed for all samples, in thesequence, which contain target analytesthat exceed the criteria?
d. Are daily retention time windowsestablished for each analyte prior tosample analysis?
e. Is the retention time for each analytein the daily mid-concentration standardused as the midpoint of the window forthat day?
f. Is solvent flush technique used toinject samples to GC?
g. If interferences prevent measurement ofpeak area during analysis by an FID, isthe phenol extract derivatized bypentafluorobenzylbromide (PFB) and thederivatized extract cleaned up usingMethod 3630A (silica gel cleanup) andanalyzed by an ECD?
h. If the peak areas exceed the linearrange of the system, is the extractdiluted and reanalyzed?
i. Are peak height measurements used forquantitation when overlapping peakscaused errors in area integration?
j. Are any positive hits confirmed by asecond GC column (or by GC/MS if theconcentration of each positive hitexceeds 10 ng/µL in the final extract)?
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ITEM YES COMMENT
k. If sample extracts are cleaned up withMethods 3630A/3650A, are the associatedQC samples processed through the samemethods?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Is the lab specific MDL equal to orlower than the method specified MDL?
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
f. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) IS an LCS prepared with standardsindependent of calibrationstandards analyzed for each batch?
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
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ITEM YES COMMENT
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the sampleanalysis halted until the systemperformance is back in control?
g. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever concentration would behigher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
– the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
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ITEM YES COMMENT
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) Is the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
h. Is the performance of extraction,cleanup (when used), analytical system,and the effectiveness of the method indealing with sample matrix monitored byspiking each sample, standard, andblank with phenolic surrogates using2-fluorophenol and 2,4, 6-tribromophenolto encompass the range of temperatureused in this method?
i. Are the average percent recovery andstandard deviation of the percentrecovery for each surrogate calculated,when surrogate data from 25 to 30samples for each matrix is available?
j. Are control limits for each surrogatein a given matrix calculated based onthe above data?
k. Do the control limits fall within thecontrol limits of Method 8270 ifapplicable?
l. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
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ORGANIC ANALYSIS BY GC: PHENOLS (8040A) Page 11 of 13
ITEM YES COMMENT
m. Are corrective actions of reanalysisor reextraction/reanalysis taken ifsurrogates for a sample are out ofcontrol limits?
n. Are control charts for internal QC dataplotted and available to benchchemists?
o. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
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ORGANIC ANALYSIS BY GC: PHENOLS (8040A)
ITEM
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a.
b.
c.
d.
Does the lab have sound technicalcapability for phenols analysis?
Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month:
Could the lab handle quick turnaroundsamples?
Overall, is the lab acceptable forphenols analysis?
YES
Additional observations, comments, or problems:
Page 12 of 13
COMMENT
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 1 of 15
ITEM YES COMMENT
General:
a. Are written SOPS available and adequatefor PEST/PCB sample preparation andanalysis?
b. Do these SOPS accurately reflectprocedures in use?
c. Are manufacturer's operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of a GCsystem and interpretation ofchromatograms?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
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ITEM YES COMMENT
d. Does the lab have experienced residueanalysis experts on staff?
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Are enough sets of separatory funnels(2,000 mL with Teflon stopcock),Soxhlet extractors, and Kuderna-Danishapparatuses available for simultaneousextraction of all batch samples?
c. Is gas chromatography equipped with anglass-lined injection port, and anelectron capture or electrolyticconductivity detector available?
d. Is oven temperature stable to ±0.5°C orbetter at desired setting?
e. Is carrier-gas line equipped with amolecular sieve drying cartridge and atrap for removal of oxygen from thecarrier gas?
f. Is one of the following glass GC columnavailable?
(1) 1.8-m x 4-mm ID glass, packed with1.5% SP-2250/l.95% SP-2401 onSupelcoport (100/120 mesh) orequivalent?
(2) 1.8-m x 4-mm ID glass, packed with3% OV-1 on Supelcoport (100/120mesh) or equivalent?
g. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 3 of 15
ITEM YES COMMENT
h. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
i. Has any instrument been modified in anyway?
j. Is a hood available for samplepreparation?
k. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
l. Are backup apparatus available?
m. Is glassware properly cleaned andfinally rinsed with pesiticide-qualityhexane?
n. Is volumetric glassware cleaned with“No Chromix” or equivalent?
o. Is heavily contaminated glasswareheated in a muffle furnace at 400°C for15 to 30 minutes?
p. Is glassware contaminated with high-boiling-point materials, such as PCBS,heated at 500°C overnight?(Borosilicate glassware shall not beheated above this temperature.)
q. Is high temperature treatment onvolumetric glassware, glassware withground joints, or sintered glasswareavoid?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 4 of 15
ITEM YES COMMENT
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Are all chemical reagents for pesticideand PCB analyses stored in glasscontainers?
d. Are “pesticide quality” or equivalentsolvents used for pesticide analysis?
e. Are all solvents stored in glasscontainers and transferred with allglass system?
f. Is 5% methane/95% argon carrier gasavailable?
g. Are solvent extracted silicon carbideor equivalent used as boiling chips?
h. Does the lab have calibration standardsfor all method specified target PCBs?
i. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are aqueous samples stored at 4°C, andextracted within seven days fromcollection and analyzed within 40 daysfrom extraction?
b. Are soil samples stored at 4°C, andextracted within 14 days fromcollection and analyzed within 40 daysfrom extraction?
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 5 of 15
ITEM YES COMMENT
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. If the GC is not used for a day ormore, is the GC column primed ordeactivated by injecting a PCB orpesticide standard mixture about 20times more concentrated than themid-level standard, prior to instrumentcalibration?
d. Is a calibration blank run followingthe system prime to ensure no carryovercontamination?
e. Is a mid-level standard contain only4,4'-DDT and endrin injected to checkthe degradation problem at injectionport or front of the column prior tocalibration?
f. If the degradation of either DDT orendrin exceeds 20% (or 15% forcapillary column) based on peak areas,is corrective action taken beforeproceeding with calibration?
g. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
h. Is one of the external standards at aconcentration near, but above, the MDL?
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ITEM YES COMMENT
i. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
j. Is a linear calibration curve with acorrelation coefficient ≥ 0.995 preparedfor each analyte?
k. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working range?
l. Is the total area of all peaks measuredfrom the common baseline under allpeaks used for quantitation ofmultiresponse analytes?
m. Is the calibration curve or factorverified at the beginning and end ofeach analysis sequence with amid-concentration standard?
n. Is a new calibration curve prepared forany target analyte when the responseor the target analyte varies from thepredicted response by more than ±5%?
o. Is the retention time windowestablished with three injections ofall single component standard mixturesand multiple response productsthroughout the course of a 72-hourperiod?
p. Is the retention time window checked ona quarterly basis or whenever a new GCcolumn is installed?
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080)
ITEM
Sample Preparation:
a.
b.
c.
d.
e.
Are aqueous samples extracted at aneutral, or as is, pH with methylenechloride, using Method 3510 or 3520?
Are solid samples extracted usingeither Method 3540 or 3550?
Is entire aqueous sample consumed foranalysis and no analysis performed onaliquots of samples?
Is sample bottle rinsed with extractionsolvent and the rinsate combined withextract?
Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Is daily calibration performed with amid-concentration standard prior tosample analysis?
b. Is daily calibration checked at the endof an analysis sequence?
c. If the calibration factor based ondaily calibration check at the end ofan analysis sequence exceeds ±15% whencompared with the initial standard ofthe analysis sequence, is the GC systemrecalibrated and reanalysis performedfor all samples which contain targetanalytes that exceed the criteria?
d. Are daily retention time windowsestablished for each analyte prior tosample analysis?
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COMMENT
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 8 of 15
ITEM YES COMMENT
e. Is the retention time for each analytein the daily mid-concentration standardused as the midpoint of the window forthat day?
f. Is the volume of sample injectedrecorded to the nearest 0.05 µL?
g. If the peak areas exceed the linearrange of the system, is the extractdiluted and reanalyzed?
h. Are peak height measurements used forquantitation when overlapping peakscaused errors in area integration?
i. If peak detection and identificationare prevented due to interference, doesthe extract routinely undergo aFlorisil column cleanup (Method 3620A)and/or sulfur cleanup (Method 3660A)to eliminate interferences?
j. Is mercury, activated copper powder, ortetrabutylammonium (TBA)-sulfitereagent used for sulfur cleanup?
k. Is microcoulometric or halogen specific(i.e., electrolytic conductivity)detector used to eliminate interferencecaused by phthalate esters?
l. Are any positive hits confirmed bya second GC column (or by GC/MS if theconcentration of each positive hitexceeds 10 ng/µL in the final extract)?
m . If the early portion of toxaphenechromatogram is interfered with byother substances, is area of the lastfour peaks in both sample and standardused for quantitation?
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 9 of 15
ITEM YES COMMENT
n. If chlordane residue does not resembletechnical chlordane, but insteadconsists primarily of individual,identifiable peaks, is each peakquantitated separately againstappropriate reference materials andreported as individual residues?
o. Is the total area of all peaks measuredfrom the common baseline under allpeaks used for PCB quantitation?
p. Are only those peaks that can beattributed to chlorobiphenyls used forPCB quantitation?
q. If there are interference peaks withinthe Aroclor pattern, is the PCBquantitation determined with three tofive major peaks that are ≥ 25% of theheight of the largest Aroclor peak inthe Aroclor standards?
r. Is the amount of Aroclor calculatedwith the individual response factor foreach of the major peaks and are theresults of the three to fivedeterminations averaged?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
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ITEM YES COMMENT
d. Is the lab specific MDL equal to orlower than the method specified MDL?
e. Is a separate set of internal QCsamples including method blanks, LCS,matrix spikes, matrix spike duplicatesand matrix duplicates run for eachanalytical batch of pesticides or PCB?
f. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
g. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) Is an LCS prepared with standardsindependent of calibrationstandards analyzed for each batch?
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 11 of 15
ITEM YES COMMENT
h. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever concentration would behigher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) Is the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
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ITEM YES COMMENT
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
i. Is the performance of extraction,cleanup (when used), analytical system,and the effectiveness of the method indealing with sample matrix monitored byspiking each sample, standard, andblank with pesticide surrogates using2,4,5,6-tetrachloro-meta-xylene (TCMX)and decachlorobiphenyl (DCBP) asspecified by the method?
j. Are the average percent recovery andstandard deviation of the percentrecovery for each surrogate calculated,when surrogate data from 25 to 30samples for each matrix is available?
k. Are control limits for each surrogatein a given matrix calculated based onthe above data?
l. Do the control limits fall within thecontrol limits of Method 8270 ifapplicable?
m. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
n. Are corrective actions of reanalysisor reextraction/reanalysis taken ifboth surrogates for a sample are out ofcontrol limits?
o. Are control charts for internal QC dataplotted and available to benchchemists?
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ITEM YES COMMENT
p. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
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ITEM YES COMMENT
Overall Evaluation:
a. Does the lab have sound technicalcapability for PEST/PCB analyses?
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month:
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forPEST/PCB analyses?
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ORGANIC ANALYSIS BY GC: PEST/PCB (8080) Page 15 of 15
ITEM
Additional observations, comments, or problems:
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ORGANIC ANALYSIS BY GC: PAH (8100) Page 1 of 12
ITEM YES COMMENT
General:
a. Are written SOPS available and adequatefor PAH sample preparation/analysis?
b. Do these SOPS accurately reflectprocedures in use?
c. Are manufacturer’s operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of a GCsystem and interpretation ofchromatograms?
b. Are backup bench chemists available?
c. Are bench chemists' performance auditedand approved prior to work withoutclose supervision by a senior chemist?
I-122
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CHART I-15
ORGANIC ANALYSIS BY GC: PAH (8100)
ITEM
Apparatus and Facilities:
a.
b.
c.
d.
e.
f.
g.
h.
Is working space adequate and clean?
Are enough sets of separatory funnels,continuous liquid-liquid extractors,Soxhlet extractors, and Kuderna-Danishapparatuses available for simultaneousextraction of all batch samples?
Is oven temperature stable to ±0.5°C orbetter at desired setting?
Is one of the following glass GC columnavailable?
(1) 1.8-m x 2-mm ID glass column packedwith 3% OV-17 on-Chromosorb W-AW-DCMS (100/120 mesh) or equivalent?
(2) 30-m x 0.25-mm ID SE-54 fusedsilica capillary column?
(3) 30-m x 0.32-mm ID SE-54 fusedsilica capillary column?
If capillary column is in use, ishelium used as the carrier gas?
If packed column is in use, is nitrogenused as the carrier gas?
Is a flame ionization detectoravailable?
If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
YES
Page 2 of 12
COMMENT
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ORGANIC ANALYSIS BY GC: PAH (8100) Page 3 of 12
ITEM YES COMMENT
i. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
j. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
k. Has any instrument been modified in anyway?
l. Is a hood available for samplepreparation?
m. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
n. Are backup apparatus available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Are reagent grade chemicals usedconform to the specifications of theCommittee on Analytical Reagents of theAmerican Chemical Society, where suchspecifications are available?
c. Are "pesticide quality" or equivalentsolvents used for sample analysis?
d. Does the lab have calibration standardsfor all method specified targetanalytes?
e. Are calibration standards prepared withisooctane as a solvent?
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ITEM YES COMMENT
f. Are stock standard solutions stored at4°C and protected from light?
g. Are stock standard solutions replacedafter one year, or sooner if comparisonwith check standards indicates aproblem?
h. Are working standards replaced aftersix months, or sooner if comparisonwith check standards indicates aproblem?
i. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are aqueous samples stored at 4°C, andextracted within seven days fromcollection and analyzed within 40 daysfrom extraction?
b. Are soil samples stored at 4°C, andextracted within 14 days fromcollection and analyzed within 40 daysfrom extraction?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
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ITEM YES COMMENT
d. Is one of the external standards at aconcentration near, but above, the MDL?
e. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
f. Is a linear calibration curve with acorrelation coefficient ≥ O.995 preparedfor each analyte?
g. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working range?
h. Is the calibration curve or factorverified at the beginning and end ofeach analysis sequence with amid-concentration standard?
i. Is a new calibration curve prepared forany target analyte when the responsefor the target analyte varies from thepredicted response by more than ±15%?
j. Is retention time window establishedwith three injections of all singlecomponent standard mixtures andmultiple response products throughoutthe course of a 72-hour period?
k. Is retention time window checked on aquarterly basis or whenever a new GCcolumn is installed?
Sample Preparation:
a. Are aqueous samples extracted at aneutral pH with methylene chloride,using Method 3510 or 3520?
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ITEM YES COMMENT
b. Are solid samples extracted usingeither Method 3540 or 3550?
c. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Is daily calibration performed with amid-concentration standard prior tosample analysis?
b. Is daily calibration checked at the endof an analysis sequence?
c. If the calibration factor calculatedfrom daily calibration check at the endof an analysis sequence exceeds ±15%when compared with the initial standardof the analysis sequence, is the GCsystem recalibrated and reanalysisperformed for all samples, in thesequence, which contain target analytesthat exceed the criteria?
d. Are daily retention time windowsestablished for each analyte prior tosample analysis?
e. Is the retention time for each analytein the daily mid-concentration standardused as the midpoint of the window forthat day?
f. If peak detection and identificationare prevented due to interferences, isthe extract undergone Method 3630(Silica Gel Cleanup)?
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ITEM YES COMMENT
g. If the peak areas exceed the linearrange of the system, is the extractdiluted and reanalyzed?
h. Is peak height measurement used forquantitation when overlapping peakscaused errors in area integration?
i. Are any positive hits confirmed by asecond GC column (or by GC/MS if theconcentration of each positive hitexceeds 10 ng/µL in the final extract)?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
e. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) IS an LCS prepared with standardsindependent of calibrationstandards analyzed for each batch?
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ITEM YES COMMENT
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
f. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever concentration would behigher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever would be higher?
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ITEM YES COMMENT
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) IS the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
g. Is the performance of extraction,cleanup (when used), analytical system,and the effectiveness of the method indealing with sample matrix monitored byspiking each sample, standard, andblank with one or two surrogates, e.g.,2-fluorobiphenyl & l-fluoronaphthalene,to encompass the range of temperatureused in this method?
h. Are the average percent recovery andstandard deviation of the percentrecovery for each surrogate calculatedto establish control limits, whensurrogate data from 25 to 30 samplesfor each matrix is available?
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ORGANIC ANALYSIS BY GC: PAH (8100) Page 10 of 12
ITEM YES COMMENT
i. Do the control limits fall within thoseof Method 8270 if applicable?
j. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
k. Are corrective actions of reanalysisor reextraction/reanalysis taken ifsurrogates for a sample are out ofcontrol limits?
l. Are control charts for internal QC dataplotted and available to benchchemists?
m. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
n. Because of coelution problems, is theuse of this method avoided and thesample analyzed by either HPLC or GC/MSwhen the four pairs of compounds listedbelow are encountered?
(1) Anthracene and phenanthrene
(2) Chrysene and benzo(a)anthracene
(3) Benzo(b) fluoroanthene andbenzo(k) fluoranthene
(4) Dibenzo(a,h) anthracene andindeno(l,2,3-cd)pyrene
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CHART I-15
ORGANIC ANALYSIS BY GC: PAH (8200)
ITEM
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for PAH analysis?
YES
Page 11 of 12
COMMENT
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CHART I-15
ORGANIC ANALYSIS BY GC: PAH (8100)
ITEM
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month:
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forPAH analysis?
YES
Page 12 of 12
COMMENT
Additional observations, comments, or problems:
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 1 of 14
ITEM YES COMMENT
General:
a. Are written SOPS available and adequatefor HERB sample preparation/analysis?
b. Do these SOPS accurately reflectprocedures in use?
c. Are manufacturer’s operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrection written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of a GCsystem and interpretation ofchromatograms?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
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ORGANIC ANALYSIS BY GC: HERB (8150A) Page 2 of 14
ITEM YES COMMENT
d. Do bench chemists have properexperience in working with diazomethanewhich is explosive and carcinogenic?
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Is a temperature-programmable gaschromatography equipped with anelectron capture detector, microcoulo-metric detector, or electrolyticconductivity detectors?
c. Is oven temperature stable to ±0.5°C orbetter at desired setting?
d. Is one of the following glass GC columnavailable?
(1) 1.8-m x 4-mm ID glass, packed with1.5% SP-2250/l.95% SP-2401 onSupelcoport (100/120 mesh) orequivalent?
(2) 1.8-m x 4-mm ID glass, packed with5% OV-21O on Gas Chrom Q (100/120mesh) or equivalent?
(3) 1.98-m x 2-mm ID glass, packed with0.1% SP-1OOO on Carbopack C (80/100 mesh) or equivalent?
(4) Is column one used as the primaryanalytical column and columns twoor three as a confirmation column?
e. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 3 of 14
ITEM YES COMMENT
f. Is a diazomethane generator availableat the lab?
g. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
h. Has any instrument been modified in anyway?
i. Are glassware and glass wool acidrinsed prior to use?
j. Are boiling chips solvent extracted?
k. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
l. Are backup instruments available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Are pesticide-quality or equivalentsolvents (i.e., acetone, methanol, andhexane) used?
d. Is diethyl ether of pesticide qualityor equivalent and free of peroxidesused?
I-136
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 4 of 14
ITEM YES COMMENT
e. Is 20 mL of ethyl alcohol preservativeadded to each liter of cleaned diethylether?
f. Is sodium sulfate purified by heatingat 400°C for four hours or byprecleaning with methylene chloride?
g. Is sodium sulfate acidified withsulfuric acid prior to use to avoidreaction with herbicides?
h. Are stock standards stored in bottleswith Teflon-lined screw caps or crimptops at 4°C and protected from light?
i. Are stock standards replaced after oneyear, or sooner if comparison withcheck standards indicates a problem?
j. Are working standards replaced aftersix months or sooner, if comparisonwith check standards indicates aproblem?
k. Does the lab use one or two herbicides,that are not expected to be presentedin the sample and that elute over thetemperature range of this method, assurrogate(s)?
l. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are herbicide samples stored at 4°C andextracted within seven days (water) or14 days (soil) from collection?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 5 of 14
ITEM YES COMMENT
b. Are extracts stored under refrigerationand analyzed within 40 days fromextraction?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
d. Is one of the calibration standards ata concentration near, but above, theMDL?
e. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
f. Is a linear calibration curve with acorrelation coefficient ≥ 0.995 preparedfor each analyte?
g. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working range?
h. Is the calibration curve or factorverified at the beginning and end ofeach analysis sequence with amid-concentration standard?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 6 of 14
ITEM YES COMMENT
i. Is a new calibration curve prepared forany target analyte when the responsefor the target analyte varies from thepredicted response by more than ±15%?
j. Is the retention time windowestablished with three injections ofall target analytes throughout thecourse of a 72-hour period?
k. Is the retention time window checked ona quarterly basis or whenever a new GCcolumn is installed?
Sample Preparation:
a. Is the pH of aqueous samples adjustedto <2 with sulfuric acid prior toextraction?
b. Is diethyl ether of pesticide-qualityor equivalent and free of peroxidesused for extraction of aqueous samples?
c. For soil/sediment samples, is the pHof sample adjusted to two with HC1 andmonitored and adjusted, if needed, for15 minutes prior to extraction?
d. Are multiple extractions with acetoneand diethyl ether used for soil andsediment samples?
e. Is cold (4°C) sulfuric acid used toadjust the pH to two prior to solventcleanup?
f. Is acidified sodium sulfate used to drythe diethyl ether for a minimum of twohours prior to esterification?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 7 of 14
ITEM YES COMMENT
g. Is a bubble method or a Diazald kitmethod used at the lab to generatediazomethane?
h. Are the following precautions takenduring esterification withdiazomethane?
(1) Use a safety screen?
(2) Use mechanical pipetting aides?
(3) Do not heat above 90°C?
(4) Avoid grinding surfaces, groundglass joint, sleeve bearing, glassstirrers?
(5) Store away from alkali metals?
(6) Avoid contact with copper powder,calcium chloride, and boilingchips?
i. Is methylated extracts analyzedimmediately to minimize trans-esteri-fication and other potential reactions?
Sample Analysis:
a. Is GC column 1 selected for majority ofherbicide analysis, except for Dalaponwhich is analyzed with GC column 3?
b. Is daily calibration performed with amid-concentration standard at thebeginning and the end of an analysissequence?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 8 of 14
ITEM YES COMMENT
c. If the calibration factor calculatedfrom injection of a mid-concentrationstandard at the end of an analysissequence exceeds ±15% when comparedwith the initial standard of theanalysis sequence, is the GC systemrecalibrated and reanalysis performedfor all samples, in the sequence,which contain target analytes exceedthe criteria?
d. Are daily retention time windowsestablished for each analyte prior tosample analysis?
e. Is the retention time for each analytein the daily mid-concentration standardused as the midpoint of the window forthat day?
f. Have calibration standards undergonethe same hydrolysis and esterificationprocesses as the samples?
g. If calibration is done with standardsmade from methyl ester compounds, isthe final concentration corrected formolecular weight of methyl ester versusthe acid herbicides?
h. If a peak response exceeds the linearrange of the system, is a dilutionperformed on a second aliquot of thesample which has been properly sealedand stored prior to use?
i. Is peak height measurement used forquantitation when overlapping peakscaused errors in area integration?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 9 of 14
ITEM YES COMMENT
j. Is further extract cleanup routinelyconducted if interferences preventpeak detection and identification?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Is the lab specific MDL equal to orlower than the method specified MDL?
e. Are GC/MS techniques routinely used toconfirm positive hits?
f. If GC/MS fails, are additional stepsincluding alternative packed orcapillary GC columns or additionalcleanup routinely taken for qualitativeconfirmation?
g. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
h. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) Is an LCS prepared with standardsindependent of calibrationstandards analyzed for each batch?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A)
ITEM
(2)
(3)
Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
i. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1)
(2)
If, as in compliance monitoring,the concentration of a specificanalyte in the sample is checkedagainst a regulatory limit, is thespike at that regulatory limit orone to five times higher than thebackground concentration, whicheverconcentration would be higher?
If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
YES
Page 10 of 14
COMMENT
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ORGANIC ANALYSIS BY GC: HERB (8150A) Page 11 of 14
ITEM YES COMMENT
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) Is the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
j. Is the performance of extraction,cleanup, analytical system, and theeffectiveness of the method in dealingwith sample matrix monitored by spikingeach sample, standard, and blank withsurrogates which encompass the methodspecified temperature range?
k. Are the average percent recovery andstandard deviation of the percentrecovery for each surrogate calculated,when surrogate data from 25 to 30samples for each matrix is available?
l. Are control limits for each surrogatein a given matrix calculated based onthe above data?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 12 of 14
ITEM YES COMMENT
m. Do the control limits fall within thecontrol limits of Method 8270 ifapplicable?
n. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
o. Are corrective actions of reanalysisor reextraction/reanalysis taken ifany surrogates for a sample are out ofcontrol limits?
p. Are control charts for internal QC dataplotted and available to benchchemists?
q. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational poilicy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 13 of 14
ITEM YES COMMENT
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for HERB analysis?
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: _______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forHERB analysis?
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CHART I-16
ORGANIC ANALYSIS BY GC: HERB (8150A) Page 14 of 14
ITEM
Additional observations, comments, or problems:
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EM 200-1-11 Jul 94
CHART I-17
GENERAL QA/QC FOR ORGANIC ANALYSIS BY GC/MS: Page 1 of 3
ITEM YES COMMENT
Is the MS capable of scanning from 35 to450 amu every seven seconds or less?
Is tuning compound, FC-43, used to verifymass calibration?
Do the mass spectra of BFP and DFTPP meetall criteria before each batch of volatileand semivolatile samples is run?
Are standards containing all of theanalytes of interest analyzed to verifyresponse factors and update retention time?
Is glassware for organics solvent rinsed orheated to a minimum of 300°C to vaporizeany organics in a muffle furnace aftercareful cleaning?
Is this high temperature treatment avoidedfor volumetric glassware, glassware withground joints, or sintered glassware?
Is glassware sealed and stored in a cleanenvironment?
Are magnetic tapes stored in a secure area?
Are extensive in-house replacement partsavailable?
Are manufacturer’s operating manualsreadily available to bench chemists?
Is there a calibration protocol availableto the bench chemists?
Are calibration results kept in a permanentlogbook?
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CHART I-17
GENERAL QA/QC FOR ORGANIC ANALYSIS BY GC/MS: Page 2 of 3
ITEM YES COMMENT
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Has the instrument been modified in anyway?
Are the instruments properly vented?
Is a 5-point calibration used?
Are continuing calibration checks done ona 12-hour basis?
Are system performance response factorschecked on a 12-hour basis?
Are BFB and DFTPP tuning checks done on a12-hour basis?
Is low-level method routinely used forenvironmental soil/sediment samples?
For tentatively identified compounds, arelibrary searches done for the ten volatileorganics and the 20 semivolatile organicsof highest concentration?
Are surrogate recoveries run on eachsample?
Is a corrective action taken if surrogaterecoveries exceed QC limits?
Is a method blank included with each batchof samples and carried through the entirepreparation and analysis?
Is a lab duplicate run at a rate of 5% orone per batch, whichever is greater?
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CHART I-17
GENERAL QA/QC FOR ORGANIC ANALYSIS BY GC/MS: Page 3 of 3
ITEM YES COMMENT
Is a corrective action taken if matrixspike recoveries exceed QC limits?
Is a spiked sample run at a rate of 5% orone per batch, whichever is greater?
Is an LCS analyzed with every tenth sampleor each batch?
Additional observations, comments, or problems:
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A) Page 1 of 18
ITEM YES COMMENT
General:
a. Are written SOPS available and adequatefor VOA sample preparation/analysis?
b. Do these SOPS accurately reflectprocedures in use?
c. Are all target analytes, at a minimum,listed in Table 2 of Method 8240Aroutinely analyzed at the lab?
d. Are manufacturer's operating manualsreadily available to bench chemists?
e. Are prenumbered, bound notebooks usedfor data entry?
f. Are all records written in indelibleink?
g. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
h. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of apurge-and-trap and GC/MS system and ininterpretation of chromatograms andmass spectra?
b. Are backup bench chemists available?
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A) Page 2 of 18
ITEM YES COMMENT
c. Are bench chemists' performance auditedand approved prior to work withoutclose supervision by a senior chemist?
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Does the lab have adequate air handlingsystem to avoid cross contamination ofsamples?
c. Is a temperature-programmable gaschromatography equipped with apurge-and-trap device available?
d. Is oven temperature stable to ±0.5°C orbetter at desired setting?
e. Is a GC column of 6-ft x O.1-in IDglass, packed with 1% SP-1OOO onCarbopack-B (60/80 mesh) or equivalent,available?
f. If an "equivalent" column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
g. Are enough sets of purge-and-trapdevices available for all samples in ananalytical batch?
h. Is the mass spectrometer capable ofscanning from 35 - 260 amu every threeseconds or less, using 70-volt electronenergy in the electron impact mode?
i. Is a computer data system that allowscontinuous acquisition and storage onmachine-readable media of all massspectra available?
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A)
ITEM YES
j. Is the most recent version of the EPA/NIST Mass Spectral Library available?
k. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
l. Is sample preparation conducted in ahood?
m. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
n. Are backup instruments available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. For standard preparation, is a waitingperiod of ten minutes allowed fordrying the alcohol-wetted surfacebefore measuring the weight of methanolto the nearest 0.1 mg?
d. Are stock standards stored in bottleswith minimal headspace and Teflon-linedscrew cap at -10 to -20°C and protectedfrom light?
e. Are stock standards replaced after sixmonths, or sooner if comparison withcheck standards indicates a program?
Page 3 of 18
COMMENT
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A) Page 4 of 18
ITEM YES COMMENT
f. Are stock standards for target analytesof low boiling points (<30°C) and highreactivity prepared fresh every twomonths or sooner?
g. Are secondary standards stored withminimal headspace and check frequentlyfor degradation or evaporation?
h. Is 2 mL of GC/MS system tuningstandard, containing 25 ng/µL of4-bromofluorobenzene (BFB) in methanolinjected or purged for hardware tuning?
i. Are method recommended surrogates,toluene-d8’ 4-bromofluorobenzene, and1,2-dichlgroethane-d 4 spiked into eachsample undergoing GC/MS analysis?
j. Are method recommended internalstandards, bromochloromethane,1,4-dichlorobenzene, and chlorobenzene-d5 or other compounds with retentiontimes similar to the compounds beingdetected by GC/MS?
k. For the initial calibration, areaqueous calibration standards, at aminimum of five concentrations,prepared fresh and discarded after onehour, unless properly sealed in a vialand stored at 4°C with no headspace(up to one week)?
l. Are method recommended matrix spikestandards (1,1-dichloroethene, tri-chloroethene, chlorobenzene, toluene,and benzene in methanol at 25 µg/mL)available?
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A)
ITEM
m. Are all non-aqueous standard solutionsstored at -10 to -20°C in screw-capamber bottles with Teflon liners?
n. Are volatile organic standards storedin a separated freezer/refrigeratorfrom samples or other standards?
o. IS “purge-and-trap”, “pesticidequality”, or equivalent methanol storedaway from other solvents?
p. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
YES
Sample Handling and Storage:
a. Are volatile organic samples stored at4°C in separate refrigerators fromother samples?
b. Are low concentration volatile organicsamples stored separately from highconcentration volatile organic samples?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Is the trap of a purge-and-trap deviceconditioned overnight at 180°C in thepurge mode with an inert gas flow ofat least 20 mL/min?
EM 200-1-11 Jul 94
Page 5 of 18
COMMENT
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A)
ITEM
d.
e.
f.
Prior to use, is the trap conditioneddaily for 10 minutes while backflushingat 180°C with the column at 220°C?
Is manufacturer’s recommendations usedfor conditioning of the purge-and trapdevice?
Initial Calibration:
(1) Is each GC/MS systemto meet the criteriainjection or purgingto sample analysis?
hardware-tunedfor 50-ngof BFB prior
Mass Ion Abundance Criteria50 15% to 45% of mass 9575 30% to 60% of mass 9595 base peak, 100% relative
abundance96 5% to 9% of mass 95
173 O% to <2% of mass 174174 >50% of mass 95175 5% to 9% of mass 174176 >95% but <101% of mass 174177 5% to 9% of mass 176
(2) Is the initial calibrationperformed with a minimum of fiveconcentration levels for eachtarget analyte?
(3) Is one of the calibration standardsat a concentration near, but above,the MDL?
(4) Do concentrations of otherstandards cover the expectedconcentration ranges of realsamples or define the working rangeof the detector?
YES
Page 6 of 18
COMMENT
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A)
ITEM
(5) IS a system performance check madewith five System Performance CheckCompounds (SPCCs) for a minimalaverage response factor (RF) of0.300 for each SPPC (0.250 forbromoform)?
The
(a)
(b)
(c)
SPCCs are:Chloromethane,1,1-Dichloroethane,Bromoform,1,1,2, 2-Tetrachloroethane, andChlorobenzene.
Chloromethane will be lost ifthe purge flow is too fast.
Bromoform will be purged verypoorly if purge flow is tooslow. Cold spots and/or activesites may adversely affectresponse.
Tetrachloroethane and1,1-dichloroethane are degradedby contaminated transfer linesand/or active sites.
(6) IS percent relative standarddeviation for each CalibrationCheck Compound (CCC), less than30%, based on the RFs from theinitial calibration?
The CCCs are:1,1-Dichloroethene,Chloroform,1,2-Dichloropropane,Toluene,Ethylbenzene, andVinyl chloride.
YES
Page 7 of 18
COMMENT
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CHART I-18
ORGANIC ANALYSIS BY GC/MS: VOA (8240A)
ITEM
g . Daily Calibration:
(1)
(2)
(3)
(4)
(5)
(6)
(7)
Is each GC/MS system hardware-tunedto meet BFB tuning criteria foreach 12-hour shift prior to sampleanalysis?
Is the initial calibration curvefor each target analyte checked andverified by checking SPCC and CCCof a midpoint calibration standardevery 12-hour shift?
Do the RFs of SPCCs meet theinitial SPCC criteria for each12-hour shift?
Is the percent difference on RFsless than 25% for any one CCC?
If the criteria in (3) and (4) arenot met, is corrective action takento solve possible problems such asstandard mixture degradation,injection port inlet contamination,contamination at the front end ofthe analytical column, and activesites in the column or GC system?
If no source of problem can bedetermined after corrective actionhas been taken, is a new 5-pointcalibration generated?
Are the retention times of theinternal standards in the checkcalibration standard within 30seconds from the last dailycalibration check (12 hour)?
YES
Page 8 of 18
COMMENT
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ORGANIC ANALYSIS BY GC/MS: VOA (8240A) Page 9 of 18
ITEM YES COMMENT
(8) Is the response of the internalstandards in the check calibrationstandard within a factor of two(-50% to +100%) from the last dailycalibration standard check (12hour)?
(9) If the criteria in (7) and (8) arenot met, is the mass spectrometerinspected and corrected?
(10) If corrections are made, isreanalysis conducted for samplesanalyzed while the system wasmalfunctioning?
Sample Preparation:
a. Are purge-and-trap (Method 5030) usedfor the extraction and injection ofstandards and samples?
b. Before initial use, is the trapconditioned overnight at 180°C by backflushing with an inert gas flow of atleast 20 mL per minute?
c. Prior to daily use, is the trapconditioned for 10 minutes at 180°Cwith back flushing?
Sample Analysis:
a. Are all samples and standard solutionsallowed to warm to ambient temperaturebefore analysis?
b. Is the flow rate of helium purgefor best response for chloromethane andbromoform? (≈ 30-40 mL per minute)
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ORGANIC ANALYSIS BY GC/MS: VOA (8240A) Page 10 of 18
ITEM YES COMMENT
c. If a second analysis is needed fromsample stored in a syringe, is theanalysis completed within 24 hours?
d. Is the purging chamber washed with two5-mL flushes of reagent water ormethanol followed by reagent water toavoid carryover?
e. If the concentration of analytes in asample exceeds the calibration ranges,is the sample diluted and reanalyzed?(Diluted to upper half of curve.)
f. If sample dilution is needed, is analiquot of sample which is not lessthan 1 mL used for dilution and themixture only inverted and shake threetimes to minimize loss?
g. Is proper dilution conducted to keepthe response of the major constituents(previously saturated peaks) in theupper half of the linear range ofcalibration curve?
h. Is secondary ion quantitation used onlywhen there are sample interferenceswith primary ion quantitation?
i. Is there a method blank analyzed aftera sample that has saturated ions from acompound?
j. If the blank is not free ofinterferences, is the system cleanedprior to resuming sample analysis?
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ITEM YES COMMENT
k. Are sediment/soil and waste samplesscreened by headspace (Method 3810) orhexadecane extraction (Method 3820) todetermine whether the high-level methodshould be used?
l. Is the low-level method used forsamples containing individual compoundsof < 1 mg/kg and the high-level methodused only for samples with an expectedconcentration of >1 mg/kg?
m. Is a 5-g sample used if the expectedconcentration is <0.1 mg/kg or a l-gsample for expected concentrationbetween 0.1 and 1 mg/kg?
n. Is a heated purge calibration curve(40°C) prepared and used for thequantitation of all low-level sediment/soil samples?
o. Do the standards and method blank forhigh-level method contain 100 µL ofmethanol to simulate the sampleconditions?
Data Interpretations:
a. Is the relative retention window (RRT)for each compound set at ±O.06 RRTunits of the RRT of the standardcompound analyzed within the same12 hours as the sample?
b. Are major ions in the standard massspectra at a relative intensity >10%present in the sample spectra?
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ITEM YES COMMENT
c. Do the relative intensities of themajor ions agree within 20% between thestandard and sample spectra?
d. Are molecular ions present in thereference spectrum also present inthe sample spectrum?
e. Is the lab capable to conduct acomputer library search to identify andquantify tentatively identifiedcompounds (TICs)?
f. Is the identification of TICSdetermined only after visual comparisonof a sample with the closest librarysearch?
g . Is the internal standard of nearestretention time of that of a givencompound used for quantification?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Are lab specific MDL and PQLempirically established and updated ona semiannually basis?
d. Is the lab specific PQL equal to orlower than the method specified PQL?
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ORGANIC ANALYSIS BY GC/MS: VOA (8240A)
ITEM
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
YES
f. To demonstrate that the lab cangenerate data of acceptable accuracyandthe
(1)
(2)
(3)
precision, does the analyst performfollowing operations?
Is an LCS prepared with standardsindependent from calibrationstandards analyzed for each batch?
Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
g. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples? (If a labanalyzes one to ten samples per month,at least one spiked sample per month isrequired.)
Page 13 of 18
COMMENT
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ORGANIC ANALYSIS BY GC/MS: VOA (8240A)
ITEM
(1)
(2)
(3)
(4)
(5)
If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimit or one to five times higherthan the background concentration,whichever concentration would behigher?
If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
For other matrices, is the spikeconcentration at ten times theestimated quantitation limit?
Is the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
YES
Page 14 of 18
COMMENT
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Page 15 of 18
ITEM
h.
i.
j.
k.
l.
m.
n.
o.
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
Is the performance of purge-and-trap,analytical system, and theeffectiveness of the method in dealingwith sample matrix monitored by spikingeach sample, standard, and blank withsurrogates which encompass the methodspecified temperature range?
Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
Are lab's control limits for surrogateswithin the method specified limits?
At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
Are the average percent recovery andstandard deviation of percent recoveryfor each surrogate standard calculatedonce a minimum of 30 samples of samematrix have been analyzed?
Is the method accuracy for each matrixstudied assessed and recorded afterthe analysis of five spiked samples?
Is the accuracy assessment for eachanalyte updated after each five to tennew accuracy measurements?
Are control charts for internal QC dateplotted and available to benchchemists?
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ITEM YES COMMENT
p. Are corrective actions of reanalysisor reextraction/reanalysis taken ifany surrogates for a sample are out ofcontrol limits?
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
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ORGANIC ANALYSIS BY GC/MS: VOA (8240A) Page 17 of 18
ITEM YES COMMENT
Overall Evaluation:
a. Does the lab have sound technicalcapability for VOA analysis?
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: _______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forVOA analysis?
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ORGANIC ANALYSIS BY GC/MS: VOA (8240A) Page 18 of 18
ITEM
Additional observation, comments, or problems:
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CHART I-19
ORGANIC ANALYSIS BY GC/MS: BNA (8270A) Page 1 of 16
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor BNA sample preparation/analysis?
b. Do these SOPs accurately reflectprocedures in use?
c. Are all target analytes, at a minimum,listed in Table 2 of Method 8270Aroutinely analyzed at the lab?
d. Are manufacturer's operating manualsreadily available to bench chemists?
e. Are prenumbered, bound notebooks usedfor data entry?
f. Are all records written in indelibleink?
g. Are all errors corrected by drawing asingle line through the error withcorrection written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
h. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of a GC/MSsystem and in interpretation ofchromatograms and mass spectra?
b. Are backup bench chemists available?
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ITEM YES COMMENT
c. Are bench chemists' performance auditedand approved prior to work withoutclose supervision by a senior chemist?
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Are enough sets of separator funnels,continuous liquid-liquid extractors,Soxhlet extractors, and Kuderna-Danishapparatuses available for simultaneousextraction of all batch samples?
c. Is a temperature-programmable gaschromatography equipped available?
d. Is oven temperature stable to ±0.5°C orbetter at desired setting?
e. Is the following GC column available?
30-m x 0.25-mm ID (or 0.32-mm ID) l-µmfilm thickness silicone-coated fusedsilica capillary column or equivalent.
f. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
g. Is the mass spectrometer capable ofscanning from 35 - 500 amu every onesecond or less, using 70-volt electronenergy in the electron impact mode?
h. Is a computer data system that allowscontinuous acquisition and storage onmachine-readable media of all massspectra available?
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ORGANIC ANALYSIS BY GC/MS: BNA (8270A)
ITEM
i.
j.
k.
l.
m.
n.
Is the most recent version of the EPA/NIST Mass Spectral Library available?
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Has any instrument been modified in anyway?
Is sample preparation conducted in ahood?
Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
Are backup instruments available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Are stock standards stored in bottleswith minimal headspace and Teflon linescrew-cap at 4°C and protected fromlight?
d. Are stock standards replaced after oneyear, or sooner if comparison withcheck standards indicates a program?
YES
Page 3 of 16
COMMENT
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ITEM YES COMMENT
e. Is a GC/MS system tuning standard,containing 50 ng/µL of decafluorotri-phenylphhosphine (DFTPP) in methylenechloride, prepared?
f. Are method recommended surrogates,phenol-d 5, 2-fluorophenol, 2,4,6-tri-bromophenol, nitrobenzene-d 5, 2-fluoro-biphenyl, and d-terphenyl14-dinto each sample undergoing GC/MSanalysis?
g. Are method recommended internalstandards, 1,4-dichlorobenzene-d4,naphthalene-d 8, acenaphthene-d10
phenanthrene-d 1 0 chrysene-d 12, andperylene-d12 or other compounds withretention times similar to thecompounds (within ±20% of internalstandards’) being detected by GC/MS?
h. Are daily calibration standards, ata minimum of five concentrations,stored at 4°C and freshly preparedweekly or sooner if comparison withcheck standards indicates a problem?
i. Are method recommended matrix spikestandards (pentachlorophenol, phenol,2-chlorophenol, 4-nitrophenol,4-chloro-3-methylphenol, l,2,4-tri-chlorobenzene, acenaphthene, pyrene,2,4-dinitrotoluene, N-nitroso-di-n-propylamine, and 1,4-dichlorobenzene)in methanol available?
j. Are all non-aqueous standard solutionsstored at -lO°C to -20°C in screw-capamber bottles with Teflon liners?
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ORGANIC ANALYSIS BY GC/MS: BNA (8270A) Page 5 of 16
ITEM YES COMMENT
k. Are “pesticide quality” or equivalentmethanol stored away from othersolvents?
l. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are aqueous samples stored at 4°C, andextracted within seven days fromcollection and analyzed within 40 daysfrom extraction?
b. Are soil samples stored at 4°C, andextracted within 14 days fromcollection and analyzed within 40 daysfrom extraction?
c. Are all samples and sample extractsstored in the dark at 4°C?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Initial Calibration:
(1) IS each GC/MS system hardware-tunedto meet the criteria for 50-nginjection or purging of DFTPP priorto sample analysis?
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ITEM YES COMMENT
Mass Ion Abundance Criteria51 30% to 60% of mass 19868 <2% of mass 6970 <2% of mass 69
127 40% to 60% of mass 198197 <1% of mass 198198 Base peak, 100% relative
abundance
195 5% to 9% of mass 198275 10% to 30% of mass 198365 >1% of mass 198
441 Present but less than mass 443442 >40% of mass 198443 17% to 23% of mass 442
(2) Does the DFTPP tuning standard alsocontain 50 ng/µL each of 4,4'-DDT,pentachlorophenol, and benzidine toverify injection port inertness andGC column performance?(<20% of DDT degradation and novisible peak tailing for benzidineand pentachlorophenol.)
(3) Is the initial calibrationperformed with a minimum of fiveconcentration levels for eachtarget analyte?
(4) Is one of the calibration standardsat a concentration near, but above,the MDL?
(5) Do concentrations of otherstandards cover the expectedconcentration ranges of realsamples or define the working rangeof the detector?
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ORGANIC ANALYSIS BY GC/MS: BNA (8270A) Page 7 of 16
ITEM YES COMMENT
(6) Is a system performance check madewith four System Performance CheckCompounds (SPPCs) for a minimalaverage response factor (RF) of0.050 for each compound?
The SPCCS are:N-nitroso-di-n-propylamine,hexachlorocyclopentadiene,2,4-dinitrophenol, and4-nitrophenol.
(a) Degradation of DDT to DDE andDDD should not exceed 20%.
(b) Benzidine and pentachlorophenolshould be present at theirnormal responses, and no peaktailing should be visible.
(7) IS percent relative standarddeviation for each CalibrationCheck Compound (CCC), less than30%, based on the RFs from theinitial calibration?
The CCCs are:4-chloro–3-methylphenol,2,4-dichlorophenol,2-nitrophenol,phenol,pentachlorophenol,2,4, 6-trichlorophenol,
acenaphthene,1,4-dichlorobenzene,hexachlorobutadiene,N-nitroso-di-n-phenylamine,di-n-octylphthalate,fluoranthene,benzo(a)pyrene.
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ORGANIC ANALYSIS BY GC/MS: BNA (8270A) Page 8 of 16
ITEM YES COMMENT
d. Daily Calibration:
(1) Is each GC/MS system hardware-tunedto meet DFTPP tuning criteria foreach 12-hour shift prior to sampleanalysis?
(2) Is the initial calibration curvefor each target analyte checked andverified by checking SPCC and CCCof a midpoint calibration standardevery 12-hour shift?
(3) Do the RFs of SPCCs meet theinitial SPCC criteria for each12-hour shift?
(4) Is the percent difference on RFsless than 30% for any one CCC?
(5) If the criteria in (3) and (4) arenot met, is corrective action takento solve possible problems such asstandard mixture degradation,injection port inlet contamination,contamination at the front end ofthe analytical column, and activesites in the column or GC system?
(6) If no source of problem can bedetermined after corrective actionhas been taken, is a new five-pointcalibration generated?
(7) Are the retention times of theinternal standards in the checkcalibration standard within 30seconds from the last dailycalibration check (12 hours)?
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ITEM YES COMMENT
(8) Is the response of the internalstandards in the check calibrationstandard within a factor of two(-50% to +100%) from the last dailycalibration standard check (12hours)?
(9) If the criteria in (7) and (8) arenot met, is the mass spectrometerinspected and corrected?
(10) If corrections are made, isreanalysis conducted for samplesanalyzed while the system wasmalfunctioning?
e. Is the retention time windowestablished with three injections ofall target analytes throughout thecourse of a 72-hour period?
f. Is the retention time window checked ona quarterly basis or whenever a new GCcolumn is installed?
Sample Preparation:
a. Are samples extracted by Methods 3510,3520, 3540, 3550, or 3580 prior toanalysis?
b. Are proper extract cleanup methodsroutinely used prior to analysis?
c. Is direct injection used only forsamples with concentrations in excessof 10,000 µg/L?
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ITEM YES COMMENT
Sample Analysis:
a. Is the extract screened on a GC/FID orGC/PID using the same type of capillarycolumn to minimize contamination ofGC/MS system from unexpected highconcentrations of organic compounds?
b. If the concentration of analytes in asample exceeds the calibration ranges,is the sample diluted and reanalyzed?
c. Is additional internal standard addedto the diluted extract to maintain therequired 40 ng/µL of each internalstandard in the extract volume?
d. Is secondary ion quantitation used onlywhen there are sample interferenceswith primary ion quantitation?
e. Is there a method blank analyzed aftera sample that has saturated ions from acompound?
f. If the blank is not free ofinterferences, is the system cleanedprior to resuming sample analysis?
Data Interpretations:
a. Is the relative retention window (RRT)for each compound set at ±0.06 RRTunits of the RRT of the standardcompound analyzed within the same12 hours as the sample?
b. Are major ions in the standard massspectra at a relative intensity >10%present in the sample spectra?
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ITEM YES COMMENT
c. Do the relative intensities of themajor ions agree within 20% between thestandard and sample spectra?
d. Are molecular ions present in thereference spectrum also present in thesample spectrum?
e. Is the lab capable to conduct acomputer library search to identify andquantify tentatively identifiedcompounds (TICs)?
f. Is the identification of TICsdetermined only after visual comparisonof a sample with the closest librarysearch?
g. Is the internal standard of nearestretention time of that of a givencompound used for quantification?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Are lab specific MDL and PQLempirically established and updated ona semiannually basis?
d. Is the lab specific PQL equal to orlower than the method specified PQL?
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
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ORGANIC ANALYSIS BY GC/MS: BNA (8270A) Page 12 of 16
ITEM YES COMMENT
f. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) Is an LCS prepared with standardsindependent from calibrationstandards analyzed for each batch?
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the sampleanalysis halted until the systemperformance is back in control?
g. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples? (If a labanalyzes one to ten samples per month,at least one spiked sample per monthis required.)
(1) If the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimit or one to five times higherthan the background concentration,whichever concentration would behigher?
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ITEM YES COMMENT
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 10 times theestimated quantitation limit?
(5) Is the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
h. Is the performance of sampleextraction, analytical system, and theeffectiveness of the method in dealingwith sample matrix monitored by spikingeach sample, standard, and blank withsurrogates which encompass the methodspecified temperature range?
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ORGANIC ANALYSIS BY GC/MS: BNA (8270A) Page 14 of 16
ITEM YES COMMENT
i. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
j. Are lab's control limits for surrogateswithin the method specified limits?
k. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
l. Are the average percent recovery andstandard deviation of percent recoveryfor each surrogate standard calculatedonce a minimum of 30 samples of samematrix have been analyzed?
m. Is the method accuracy for each matrixstudied assessed and recorded afterthe analysis of five spiked samples?
n. Is the accuracy assessment for eachanalyte updated after each five to tennew accuracy measurements?
o. Are control charts for internal QC dataplotted and available to benchchemists?
p. Are corrective actions of reanalysisor reextraction/reanalysis taken ifany surrogates for a sample are out ofcontrol limits?
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ORGANIC ANALYSIS BY GC/MS: BNA (8270A) Page 15 of 16
ITEM YES COMMENT
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for BNA analysis?
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ITEM YES COMMENT
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month _______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forBNA analysis?
Additional observations, comments, or problems:
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CHART I-20
ORGANIC ANALYSIS BY GC/MS: DIOXINS (8280) Page 1 of 3
ITEM YES COMMENT
Is a HRGC/LRMS system available for Method8280?
Does the lab have a HRGC/HRMS system?
Is the column oven temperatureprogrammable?
Is the GC column 60-m long x 0.025-cm IDglass or fused silica, coated with a 0.2micron film of SP-2330?
Is the MS low or high resolution with anion source of 70 volts (norminal)?
Is a data system interfaced with the massspectrometer?
Is the mass spectrometer capable ofselected ion monitoring (SIM)?
If operating conditions such as GC columnhave changed, has the acceptance criteriafor the start up QC been met?
Are all samples preserved by cooling at4°C?
Are all samples extracted within seven daysof collection and analyzed within 40 days?
Is the standard 2,3,7,8-TCDD available?
Is labeled 2,3,7,8-TCDD available (either3 7C l4 or
1 3C 1 2) ?
Is a record of standard preparationavailable?
Are stock standard solutions stored inTeflon sealed screw cap bottles, at 4°C,protected from light?
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ORGANIC ANALYSIS BY GC/MS: DIOXINS (8280) Page 2 of 3
ITEM YES COMMENT
Are stock standard solutions prepared freshevery six months?
Is a standard curve available?
Is a method blank included with each samplebatch and carried through the entirepreparation and analysis?
Is a lab duplicate run at a rate of 5% orone per batch, whichever is greater?
Is a spiked sample run at a rate of 5% orone per batch, whichever is greater?
Is an LCS analyzed with every tenth sample?
Are results for LCSs charted?
Are control limits for LCSs established?
Are charts for LCSs current?
Are results for spiked sample charted?
Are control limits established for spikedsamples?
Are charts for spiked samples current?
Is a temperature controlled (±2°C) hotwater bath available?
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Page 3 of 3
ITEM
Additional observations, comments, or problems:
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 1 of 11
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor PAH sample preparation/analysis?
b. Do these SOPs accurately reflectprocedures in use?
c. Are manufacturer's operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of an HPLCand interpretation of chromatograms?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
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ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 2 of 11
ITEM YES COMMENT
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Are enough sets of separator funnels,continuous liquid-liquid extractors,Soxhlet extractors, and Kuderna-Danishapparatuses available for simultaneousextraction of all batch samples?
c. Is an HPLC equipped with a pump capableof achieving 4,000 psi available?
d. Can the pump produce a gradient?
e. Is a fluorescence detector forexcitation at 280 nm and emissiongreater than 389 nm cutoff available?
f. Is a UV detector at 254 nm coupled tothe fluorescence detector available?
g. Is a reverse phase column, HC-ODS Si-X,5-micron particle size diameter, ina 250-mm x 2.6-mm ID SS column orequivalent available?
h. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
i. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
j. Has any instrument been modified in anyway?
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ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 3 of 11
ITEM YES COMMENT
k. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
l. Are backup apparatus available?
Reagents:
a. Is reagent water used free frominterferents at the MDL of targetanalytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Is “HPLC grade” or equivalent solvent,acetonitrile, used for PAH analysis?
d. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are aqueous samples stored at 4°C, andextracted within seven days fromcollection and analyzed within 40 daysfrom extraction?
b. Are soil samples stored at 4°C, andextracted within 14 days fromcollection and analyzed within 40 daysfrom extraction?
c. Are all samples and sample extractsstored in the dark at 4°C?
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 4 of 11
ITEM YES COMMENT
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Are stock standards stored in bottleswith Teflon-lined screw caps or crimptops at 4°C and protected from light?
d. Are stock solutions replaced after oneyear, or sooner if comparison withcheck standards indicates a problem?
e. Are working standards replaced aftersix months or sooner, if comparisonwith check standards indicates aproblem?
f. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
g. Is one of the calibration standards ata concentration near, but above, theMDL?
h. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
i. Is a linear calibration curve with acorrelation coefficient > 0.995 preparedfor each analyte?
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 5 of 11
ITEM YES COMMENT
j. Is an average calibration factor usedonly when the percent relative standarddeviation of the calibration factor isless than 20% over the working range?
k. Is the calibration curve or factorverified at the beginning and end ofeach analysis sequence with amid-concentration standard?
l. Is a new calibration curve prepared forany target analyte when the responsefor the target analyte varies from thepredicted response by more than 15%?
m. Is the retention time windowestablished with three injections ofall target analytes throughout thecourse of a 72-hour period?
n. Is the retention time window checked ona quarterly basis or whenever a new GCcolumn is installed?
Sample Preparation:
a. Are aqueous samples extracted at aneutral, or as is, pH with methylenechloride, using Method 3510 or 3520?
b. Are solid samples extracted usingeither Method 3540 or 3550?
c. Is the entire aqueous sample consumedfor analysis and no analysis performedon aliquots of samples?
d. Is the sample bottle rinsed withextraction solvent and the rinsatecombined with extract?
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 6 of 11
ITEM YES COMMENT
e. Is the extraction solvent exchanged toacetonitrile and concentrated to 1 mLwith Kuderna-Danish apparatuses andmicro-Snyder column prior to HPLCanalysis?
f. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Is the HPLC elution isocratic withacetonitrile/water (4:6 by volume) forfive minutes, then linear gradient to100% acetonitrile for 25 minutes?
b. Is a daily calibration performed witha mid-concentration standard prior toanalysis?
c. Are daily retention windows establishedfor each analyte prior to sampleanalysis?
d. If the peak areas/heights exceed thelinear range of the system, is theextract diluted and reanalyzed?
e. Is peak height measurement used forquantitation when overlapping peakscaused errors in area integration?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
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ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 7 of 11
ITEM YES COMMENT
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Is the lab specific MDL equal to orlower than the method specified MDL?
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
f. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) Is an LCS prepared with standardsindependent from calibrationstandards analyzed for each batch?
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
g. Does the matrix spike solution containall target analytes?
I-194
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 8 of 11
ITEM YES COMMENT
h. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever concentration would behigher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) Is the percent recovery for eachanalyte in water samples checkedwith the method specified QCacceptance criteria?
I-195
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310)
ITEM
i.
j.
k.
l.
m.
n.
o.
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
Does the lab use one or two analyteswhich are not expected to be presentedin the sample as surrogates? (e.g.,decafluorobiphenyl or other PAHs whichencompass the retention time ranges.)
Are the average percent recovery andstandard deviation of percent recoveryfor each surrogate standard calculatedwhen surrogate data from 25 to 30samples for each matrix is available?
Are control limits for each surrogatein a given matrix calculated based onthe above data?
At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
Are corrective actions of reanalysisor reextraction/reanalysis taken ifsurrogate(s) for a sample are out ofcontrol limits?
Are control charts for internal QC dataplotted and available to operators?
Are control limits for internal qualitycontrol empirically established and updated on a regular basis?
YES
Page 9 of 11
COMMENT
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 10 of 11
ITEM YES COMMENT
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for PAH analysis?
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CHART I-21
ORGANIC ANALYSIS BY HPLC: PAH (8310) Page 11 of 11
ITEM YES COMMENT
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: ______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forPAH analysis?
Additional observations, comments, or problems:
I-198
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 1 of 12
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor explosives sample preparation andanalysis?
b. Are the SOPs consistent with the EPA’sdraft SW-846 Method 8330, Revision 0,November 1992?
c. Do these SOPs accurately reflectprocedures in use?
d. Are manufacturer's operating manualsreadily available to bench chemists?
e. Are prenumbered, bound notebooks usedfor data entry?
f. Are all records written in indelibleink?
g. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror so that it remains legible, andinitialed and dated by the responsibleindividual?
h. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in operation of an HPLCand interpretation of chromatograms?
b. Are backup bench chemists available?
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 2 of 12
ITEM YES COMMENT
c. Are bench chemists? performance auditedand approved prior to work withoutclose supervision by a senior chemist?
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Is an HPLC equipped with a pump capableof achieving 4,000 psi, a 100 µL loopinjector, and 254-nm UV detectoravailable?
c. Is the detector capable to achieve astable baseline at 0.001 absorbanceunits full scale?
d. Are the following HPLC columnsavailable?
(1) C-18 reverse phase HPLC column,25-cm x 4.6-mm (5-µm), SupelcoLC-18 or equivalent?
(2) CN reverse phase HPLC column, 25-cmx 4.6-cm (5-µm), Supelco LC-CN orequivalent?
e. If an “equivalent” column is in use,has its ability to generate data ofacceptable accuracy and precision beendemonstrated?
f. Is the HPLC column temperaturecontrolled? If not, is special caretaken to ensure that temperature shiftsdo not cause peak misidentification?
g. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
I-200
CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330)
ITEM YES
h.
i.
j.
k.
Has any instrument been modified in anyway?
Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
Is a temperature controlled ultrasonicbath available?
Are backup apparatus available?
Reagents:
a.
b.
c.
d.
e.
f.
g.
Is reagent water used free frominterferents at the MDL of targetanalytes?
Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
Are “HPLC grade” or equivalent solventsused for explosives analysis?
Is sodium chloride stored in glasscontainer?
Are all solvents stored in glasscontainers and transferred with allglass system?
Does the lab have calibration standardsfor all method specified targetanalytes?
Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
EM 200-1-11 Jul 94
Page 3 of 12
COMMENT
I–201
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 4 of 12
ITEM YES COMMENT
Sample Handling and Storage:
a. Are aqueous samples stored at 4°C, andextracted within seven days fromcollection and analyzed within 40 daysfrom extraction?
b. Are soil samples stored at 4°C, andextracted within 14 days fromcollection and analyzed within 40 daysfrom extraction?
c. Are all samples and sample extractsstored in the dark at 4°C?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Are solid analyte standards dried toconstant weight in a vacuum desiccatorin the dark prior to use?
d. Are stock standard solutions stored inrefrigerator at 4°C in the dark andreplaced after one year or sooner, ifcomparison with check standardsindicates a problem?
e. Are intermediate standard solutionsprepared in acetonitrile for bothwater and soil samples?
f. Are intermediate standard solutionsstored in refrigerator at 4°C in thedark and replaced after six months orsooner, if comparison with checkstandards indicates a problem?
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ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 5 of 12
ITEM YES COMMENT
g. Are standards for low level methods andworking standards prepared fresh on theday of calibration and stored in thedark?
h. Is a 5 g/L calcium chloride solutionadded to each working standard?
i. Is one of the calibration standards ata concentration near, but above, theMDL?
j. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
k. Is an initial calibration performedwith a minimum of five concentrationlevels for each target analyte?
l. Does the initial calibration containtriplicate injections of eachcalibration standard?
m. Is the response factor for each analytetaken as the slope of the best-fitlinear regression line with correlationcoefficient > 0.995?
n. Is the calibration curve or factorverified with, at a minimum, a midpointcalibration standard in triplicate atthe beginning of the day, singly at themidpoint of the run and after the lastsample of the day, assuming a samplegroup of ten or less?
o. Is an additional mid-level standardchecked after each ten samples in theanalytical batch?
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 6 of 12
ITEM YES COMMENT
p. Is a new calibration curve prepared forany target analyte when the responsefactors for the daily calibrationsvary from the initial response factorsby more than 15%?
q. Is the retention time windowestablished with three injections oftwo standard mixtures, (1) HMX, RDX,135-TNB, 13-DNB, NB, 246-TNT, and24-DNT, and (2) Tetryl, 26-DNT, 2-NT,3-NT, and 4-NT, through the course of a72-hour period?
r. Is the retention time window checked ona quarterly basis or whenever a newHPLC column is installed?
s. Is the retention time for each analytein the daily mid-concentration standardused as the midpoint of the window forthat day?
Sample Preparation:
a. Are process waste samples screened withthe high-level method to determine ifthe low-level method (1-50 µg/L) isrequired?
b. Is low-level method routinely used formost groundwater samples?
c. Are soil samples dried in air at roomtemperature or colder to a constantweight without exposure to directsunlight?
d. Are dried soil samples ground andhomogenized to pass a 30 mesh sieve?
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 7 of 12
ITEM YES COMMENT
e. Are soil samples extracted in a cooledultrasonic bath (<30°C) for 18 hours?
f. Is a salting-out procedure used forextraction and concentration of watersamples?
g. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Does the mobile phase consist of 50/50(v/v) methanol/organic-free reagentwater?
b. Are peak heights used for quantitationof target analytes? (Peak height isrecommended to improve thereproducibility of low level samples.)
c. Are all positive measurements observedon the C-18 column confirmed with theCN column?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Is the lab specific MDL equal to orlower than the method specified MDL?
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 8 of 12
ITEM YES COMMENT
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
f. To demonstrate that the lab cangenerate data of acceptable accuracyand precision, does the analyst performthe following operations?
(1) Is an LCS prepared with standardsindependent from calibrationstandards analyzed for each batch?
(2) Are replicate aliquots (at leastfour) of LCS analyzed, and averagerecovery and standard deviation ofthe recovery calculated for eachtarget analyte using the fourresults to check the systemperformance?
(3) If any individual standarddeviation of recovery exceeds themethod specified precision limitsor any individual average recoveryfalls outside the method specifiedrange for accuracy, is the analysisof actual samples halted until thesystem performance is back incontrol?
g. Does the matrix spike solution containat least one isomer of all targetanalytes?
h. Does the lab routinely perform matrixspike and either one matrix duplicateor one matrix spike duplicate per batchof no more than 20 samples?
I-206
EM 200-1-11 Jul 94
CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330)
ITEM C O M M E N T
(1) If, as in compliance monitoring,the concentration of a specificanalyte in the sample is beingchecked against a regulatory limit,is the spike at that regulatorylimits or one to five times higherthan the background concentration,whichever concentration would behigher?
(2) If the concentration of a specificanalyte in a water sample is notchecked against a limit, is thespike at the same concentration asthe LCS or one to five times higherthan the background concentration,whichever concentration would behigher?
(3) If it is not possible to determinethe background concentration, isthe spike concentration
- the regulatory limit, if any; or
- the larger of either five timesthe expected background or LCSconcentrations?
(4) For other matrices, is the spikeconcentration at 20 times theestimated quantitation limit?
(5) Is the percent recovery for each
YES
Page 9 of 12
analyte in water samples checkedwith the method specified QCacceptance criteria?
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ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 10 of 12
ITEM YES COMMENT
(6) If the spike to background ratio isless than 5:1, does the lab useoptional QC acceptance criteriacalculated for the specific spikeconcentration?
i. Does the lab use one or two analyteswhich are not expected to be presentedin the sample as surrogates?
j. Are the average percent recovery andstandard deviation of percent recoveryfor each surrogate standard calculatedwhen surrogate data from 25 to 30samples for each matrix is available?
k. Are control limits for each surrogatein a given matrix calculated based onthe above data?
l. At a minimum, are surrogate recoverylimits updated annually on a matrix-by-matrix basis?
m. Are corrective actions of reanalysisor reextraction/reanalysis taken ifsurrogate(s) for a sample are out ofcontrol limits?
o. Are control charts for internal QC dataplotted and available to operators?
p. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 11 of 12
ITEM YES COMMENT
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for explosives analysis?
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CHART I-22
ORGANIC ANALYSIS BY HPLC: EXPLOSIVES (8330) Page 12 of 12
ITEM YES COMMENT
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: _______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forexplosives analysis?
Additional observations, comments, or problems:
I-210
CHART I-23
SAMPLE PREPARATION FOR METAL ANALYSIS:
ITEM
General:
a.
b.
c.
d.
e.
f.
Are written SOPs available and adequatefor sample preparation?
Do these SOPs accurately reflectprocedures in use?
Are all sample preparations conductedin a hood?
Are a group of samples (up to a maximumof 20) which behave similarly withrespect to the procedures beingemployed and which are processed as aunit with the same method sequence andthe same lots of reagents and with thereagents and with the manipulationsmanipulations common to each sampleswithin the same time period or incontinuous sequential time periodsconsidered as a batch?
Are the following lab internal QCsamples prepared for each batch ofsamples?
(1) Method blanks?
(2) Matrix spikes?
(3) Matrix spike duplicates?
(4) Matrix duplicates?
(5) Laboratory control samples?
If the quantity of field samples is notsufficient for internal QC analyses,are blank spike/blank spike duplicateor duplicate laboratory control sample:analyzed?
YES
EM 200-1-11 Jul 94
Page 1 of 8
COMMENT
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CHART I-23
SAMPLE PREPARATION FOR METAL ANALYSIS: Page 2 of 8
ITEM YES COMMENT
g. Are the rates of internal QC samplesconsistent with method requirements or,at a minimum, 5% per batch of no morethan 20 samples with similar matrix,whichever is greater?
h. Is the appropriateness of a particularpreparation for a specific sample typedetermined by the completeness ofextraction and by spike recoveries?
i. Are logbooks for sample preparationused and well maintained?
j. Are permanently bound notebooks withconsecutively numbered pages used?
k. Is a unique serial number clearlydisplayed on each notebook?
l. Are critical times entered in logbooks?
m. Are spiking solutions traceable toNIST or other reliable standards?
n. Are spiking solutions labeled properlywith date of preparation, composition,concentration, and identity ofpreparer?
o. Have entries been made in permanentfashion and corrections made withoutobliterating original entries?
p. Are corrections reviewed and initialedby a supervisor?
q. Does the logbook of sample preparationcontain the following information?
(1) Date/time?
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CHART I-23
SAMPLE PREPARATION FOR METAL ANALYSIS: Page 3 of 8
ITEM YES COMMENT
(2) Sample ID number?
(3) Sample preparer?
(4) Matrix noted?
(5) Spiking standards?
(6) Pretreatment?
(7) Volume/weight of sample?
(8) Final volume?
(9) Preparation methods?
Acid Digestion of Mercury Samples for CVAA:
a. Are mercury in liquid samples preparedaccording to Method 7470?
b. Are mercury in solid or semisolidsamples prepared according to Method7471?
c. Are all blanks, spiked samples, andlaboratory control samples carriedthrough the same digestion process?
Acid Digestion of Aqueous Samples for FLAAand ICP (Method 3005A):
a. Is this digestion used to preparesurface and ground water samples foranalysis of total recoverable metalsand dissolved metals by FLAA and ICP?
b. For dissolved metals, is the samplesfiltered through a 0.5-µm filter at thetime of collection, prior toacidification with nitric acid?
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ITEM YES COMMENT
c. Are samples digested with a mixture ofconcentrated nitric acid andhydrochloric acid?
d. Is the sample heated at 90 to 95°C toavoid boiling and loss of antimony?
e. Is filtration of digestate done onlythere is concern of insoluble materialsmay clog the nebulizer?
f. Are the reagent water, nitric acid,and hydrochloric acid monitored todetermine levels of impurities?
g. Are all method blanks, spiked samples,and laboratory control samples carriedthrough the same digestion process?
Acid Digestion of Aqueous and ExtractSamples for FLAA and ICP (Method 3010A):
a. Is this digestion used to prepareaqueous samples, TCLP extracts, andwastes that contain suspended solid foranalysis of total metals by FLAA andICP?
b. Are samples digested with concentratednitric acid?
c. After the digestion is complete, is thesample warmed with 1:1 hydrochloricacid to dissolve any precipitate orresidue?
d. Is filtration of digestate done onlythere is concern of insoluble materialsmay clog the nebulizer?
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ITEM YES COMMENT
e. Are the reagent water, nitric acid,and hydrochloric acid monitored todetermine levels of impurities?
f. Are all method blanks, spiked samples,and laboratory control samples carriedthrough the same digestion process?
g. Is the use of this digestion methodavoided when samples are to be analyzedby the GFAA technique?
Acid Digestion of Aqueous and ExtractSamples by GFAA (Method 3020A):
a. Is this digestion used to prepareaqueous samples, TCLP extracts, andwastes that contain suspended solid foranalysis of total metals by GFAA?
b. Is the digestion based on the use ofnitric acid alone?
c. Are the reagent water and nitric acidmonitored to determine levels ofimpurities?
d. Are all method blanks, spiked samplesand laboratory control samples carriedthrough the same digestion process?
e. Are aqueous samples of arsenic andselenium prepared according to Methods7060 and 7740, respectively?
Acid Digestion of Oils, Greases, or WaxesICP (Method 3040):
a. Is the use of this preparation methodlimited to samples being analyzed onlyfor Sb, Be, Cd, Cr, Cu, Fe, Mn, Ni,and V?
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CHART I-23
SAMPLE PREPARATION FOR METAL ANALYSIS: Page 6 of 8
ITEM YES COMMENT
b. Is xylene or methyl isobutyl ketoneused as the solvent in this method?
c. Are organic metallic standards used?
d. Are method blanks (e.g., Conostan baseoil or mineral oil plus reagents)spike samples, and laboratory controlsamples carried through the samepreparation and analytical processes?
e. Are samples and standards diluted asclosely as possible to the time ofanalysis?
f. Is the method of standard additionsemployed for all samples?
g. Is background correction employed toaccount for additive interferences?
Acid Digestion of Sediments, Sludges, andSoils (Method 3050A):
a. Are nonaqueous samples refrigeratedupon receipt and analyzed as soon aspossible?
b. Are the samples mixed thoroughly toachieve homogeneity prior to digestion?
c. Is the initial phase of the digestionaccomplished with nitric acid andhydrogen peroxide?
d. Is hydrochloric acid used as the finalreflux acid for (1) the ICP analysisof As and Se, and (2) the FLAA and ICPanalyses of Al, Ba, Be, Ca, Cd, Cr, Co,Cu, Fe, Mo, Pb, Ni, K, Na, Tl, V, andZn?
I-216
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CHART I-23
SAMPLE PREPARATION FOR METAL ANALYSIS: Page 7 of 8
ITEM YES COMMENT
e. Is the use of hydrochloric acid avoidedand nitric acid employed as the finaldilution acid for GFAA analysis of As,Be, Cd, Cr, Co, Pb, Mo, Se, Tl, and V?
f. Are the reagent water, nitric acid,hydrochloric acid, and hydrogenperoxide monitored to determine levelsof impurities?
g. Are all method blanks, spiked samples,and laboratory control samples carriedthrough the same digestion process?
h. Is the method of standard additionsemployed whenever a new sample matrixis analyzed?
Alkaline Digestion for Hexavalent Chromium(Method 3060):
a. Are samples digested with 3% sodiumcarbonate and 2% sodium hydroxidesolution?
b. Is the digestion solution stored in atightly capped polyethylene bottle andprepared fresh monthly?
c. Are the sample and digestate stored at4°C until analyzed?
d. Are all positive samples spiked withCr (VI) to double the concentrationfound in the original aliquot, but withthe increase no less than 0.10 mg/g?
e. If spike recovery is not within 85% and115%, is an interference regarded to bepresented and the results invalid?
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CHART I-23
SAMPLE PREPARATION FOR METAL ANALYSIS: Page 8 of 8
ITEM
Additional observations, comments, or problems:
I-218
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CHART I-24
GENERAL QA/QC FOR METAL ANALYSIS:
ITEM
Atomic Absorption Spectrophotometer:
a.
b.
c.
d.
e.
f.
g.
h.
i.
Are fuels and oxidants commercialgrade?
Is there a filter moisture trap betweenthe air source and the spectrometer?
Is nitrous oxide reagent grade?
Are flash-back arrestors and heaters inuse where needed?
Are all lamps dated when first put intouse?
Are lamps available for all elementsanalyzed?
Does the lab have a Zeeman backgroundcorrection system?
Does the lab have a deuteriumbackground correction system?
Does the lab have a Smith-Hieftjebackground correction system?
ICP-Atomic Emission Spectrometer:
a. Is a background correction techniquein use and documented according tosample matrix at least quarterly?
b. Has the instrument detection limit andmethod detection limit for each elementbeen established and documented atleast semiannually?
c. Where required, has the effect of highdissolved solids and/or acidconcentration been controlled?
I-219
YES
Page 1 of 4
COMMENT
EM 200-1-11 Jul 94
CHART I-24
GENERAL QA/QC FOR METAL ANALYSIS: Page 2 of 4
ITEM YES COMMENT
d. Has salt buildup on the nebulizer beencontrolled?
f. When a new matrix is encountered, is aserial dilution, spike addition, or analternate method technique in use toeliminate potential interference?
g. Is the spectrometer equipped with anargon gas supply?
h. Are ultra high purity grade nitricacid, hydrochloric acid, and deionizedor distilled water used for sampleprocessing and preparation?
Are manufacturer's operating manualsreadily available to bench chemists?
Is there a calibration protocol availableto bench chemists?
Are calibration results kept in permanentlogbooks?
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Is ICP calibration checked using a blankand the highest mixed calibration standardprior to sample analysis?
Is ICP calibration verified every tensamples and at the end of the analyticalrun, using a calibration blank and a checkstandard?
Does the result of check standard agreewithin ±10% of expected value?
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GENERAL QA/QC FOR METAL ANALYSIS: Page 3 of 4
ITEM YES COMMENT
Are interelement and background correctionfactors at the beginning and end of ananalytical run or twice during every 8-hourwork shift, whichever is more frequent?
Does the result of interelement checksample agree within ±20% of expected value?
Has the instrument been modified in anyway?
Are the instruments properly vented?
Is an initial 5-point calibration run tocheck instrument linearity?
Is the MDL for each element and matrix typedetermined every six months or wheneverthere is a significant change in backgroundor instrument response?
Is the linear calibration range determinedfor each element when there is significantchange in instrument response and every sixmonths for those elements that periodicallyapproach their linear limits?
Is a matrix spike run at a rate of 5% witheach batch of samples?
Is a corrective action taken if matrixspike recoveries exceed QC limits?
Is an internal QC duplicate run at a rateof 5% with each batch of samples?
Is a corrective action taken if theinternal QC duplicate exceed QC limits?
Is the method of standard addition in usewhere needed?
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GENERAL QA/QC FOR METAL ANALYSIS: Page 4 of 4
ITEM
Additional observations, comments, or problems:
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CHART I-25
METAL ANALYSIS BY ICP: METALS (6010A)
ITEM
General:
a.
b.
c.
d.
e.
f.
g.
Are written SOPs available and adequatefor ICP sample preparation/analysis?
Do these SOPs accurately reflectprocedures in use?
Are manufacturer’s operating manualsreadily available to bench chemists?
Are prenumbered, bound notebooks usedfor data entry?
Are all records written in indelibleink?
Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a.
b.
c.
Do bench chemists appear experiencedwith operation of an ICP system andknowledgeable in the correction ofspectral, chemical, and physicalinterferences?
Are backup bench chemists available?
Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
YES
Page 1 of 11
COMMENT
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METAL ANALYSIS BY ICP: METALS (6010A) Page 2 of 11
ITEM YES COMMENT
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Does the lab have a simultaneousmultielement ICP?
c. Does the lab have a sequential multi-element ICP?
d. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
e. Has any instrument been modified in anyway?
f. Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
g. Are backup instruments available?
h. Are hoods used in sample preparationareas free of rust?
Reagents:
a. Is reagent water used free frominterferents at the MDLs of targetanalytes?
b. Is reagent grade water of at least 16mega-ohm quality used for metalanalysis?
c. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
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CHART I-25
METAL ANALYSIS BY ICP: METALS (6010A) Page 3 of 11
ITEM YES COMMENT
d. Are ultra-high purity chemicals ormetals (99.99 to 99.999% pure) used forin-house preparation of standard stocksolutions?
e. Are all salts used for preparation ofstandard stock solutions dried for onehour at 105°C, unless otherwisespecified?
f. If standard stock solutions arepurchased, are the concentrations ofthe analytes verified in-house?
g. Are stock standards replaced after oneyear, or sooner if comparison withcheck standards indicates a problem?
h. Are calibration standards initiallyverified using check standards andmonitored weekly for stability?
i. Are silver standards limited to 2 mg/Land prevented from exposure to light?
j. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are aqueous samples preserved at pH < 2with nitric acid?
b. Are solid samples stored at 4°C?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
I-225
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CHART I-25
METAL ANALYSIS BY ICP: METALS (601OA)
ITEM
b.
c.
d.
e.
f.
g.
h.
i.
Are calibration results kept inpermanent logbooks?
Is the linearity of ICP calibrationrange established with a minimum offive levels of calibration standards?
Is an initial calibration performedwith a minimum of three concentrationlevels for each target analyte?
Does the lab empirically establish thedetection limits, sensitivity, andoptimum ranges of the metals for eachmodel of spectrometer and type ofmatrices?
Are multiple exposures conducted tosecure a reliable averageeach solution?
Is one of the calibrationa concentration near, butMDL?
reading for
standards atabove, the
Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
Are all mixed calibration standardsolutions scanned with a sequentialspectrometer to verify the absence ofinterelement spectral interference?
Sample Preparation:
a. Is an appropriate sample preparationmethod, Methods 3005A, 3010A, 3020A,3040, or 3050A, used for sampledigestion?
YES
Page 4 of 11
COMMENT
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METAL ANALYSIS BY ICP: METALS (6010A) Page 5 of 11
ITEM YES COMMENT
b. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Is an ICP allowed to become thermallystable before beginning calibrationor analysis (usually requiring atleast 30 minutes)?
b. Are the average intensity of multipleexposures for both standardization andsample analysis used to reduce randomerror?
c. Before beginning the sample run, isthe highest mixed calibration standardreanalyzed to check if the deviation iswithin 5% from actual value?
d. Is daily calibration checked with amid-concentration standard at thebeginning and the end of an analysissequence?
e. Is sufficient quantity of calibrationblank solution used to flush the systemfor at least one minute before theanalysis of each standard or sample?
f. If a peak response exceeds the linearrange of the system, is a dilutionperformed with calibration blanksolution on a second aliquot of thesample that has been properly sealedand stored prior to use?
g. Is an alternate less sensitive spectralline used only when all QC data arealready established?
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CHART I-25
METAL ANALYSIS BY ICP: METALS (6010A) Page 6 of 11
ITEM YES COMMENT
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
c. Are lab specific IDL and MDLempirically established and updated ona semiannually basis?
d. Is the lab specific IDL or MDL equalto or lower than the method specifiedIDL or MDL, respectively?
e. Is a calibration blank used inestablishing the calibration curve?
(A calibration blank is prepared byacidifying reagent water to the sameconcentrations of the acids found inthe standards and samples.)
f. Is a minimum of one method blank persample batch used to determine anymemory effects or possiblecontaminations resulting from varyingamounts of the acids used in the sampleprocessing?
(A method blank must contain allreagents in the same volumes as usedin the processing of the samples andmust be carried through the completeprocedure and contain the same acidin the final solution as the samplesolution used for analysis.)
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METAL ANALYSIS BY ICP: METALS (6010A) Page 7 of 11
ITEM YES COMMENT
g. When a new or unusual sample matrix isencountered, are the following seriesof tests conducted to checkinterferences?
(1) Serial Dilution: If the analyteconcentration is minimally 50 timeshigher than the IDL, is a fivefolddilution analyzed and compared withthe original determinations withinl0%?
(2) Post Digestion Spike Addition: Isan analyte spike added to aprepared sample, or its dilution toproduce a minimum level of tentimes and a maximum of 100 timesof the IDL recovered to within 25%of the known value?
h. If the above tests fail andinterferences are suspected, arecorrective actions such as use ofa standard-addition analysis,computerized compensation, analternate wavelength, or comparisonwith an alternative method used?
i. Is the ICP calibration checked using acalibration blank and two appropriatestandards?
j. Is ICP calibration verified every tensamples and at the end of theanalytical run, using a calibrationblank and a check standard?
k. Is the check standard prepared withreference materials independent ofcalibration standards analyzed for eachbatch?
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METAL ANALYSIS BY ICP: METALS (6010A) Page 8 of 11
ITEM YES COMMENT
l. Does the result of the calibrationblank agree within 30 of mean blankvalue? If not, are the blank analysisrepeated twice and the results averagedand checked against the 30 of thebackground mean?
m. If the check standard is not within 10%of the expected value or the averagebackground is not within 30, is theanalysis terminated, the problemcorrected, the instrument recalibrated,and the analysis of previous tensamples repeated?
n. Are the interelement and backgroundcorrection factors verified at thebeginning and end of an analytical runor twice during every 8-hour workshift, whichever is more frequent?(The results should be within 20% oftrue values.)
o. To demonstrate that a lab can generatedata of acceptable accuracy andprecision, does the lab routinelyperform matrix spike, matrix spikeduplicate, and matrix duplicate perbatch of no more than 20 samples?
p. Is a control limit of ±20% RPD used forsample values greater than ten timesthe IDL?
q. Is the control limit for spikeduplicate sample within 20% of theactual value?
r. Are control charts for internal QC dataplotted and available to benchchemists?
I-230
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CHART I-25
METAL ANALYSIS BY ICP: METALS (6010A) Page 9 of 11
ITEM YES COMMENT
s. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
t. Are all results reported with up tothree significant figures?
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
I-231
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CHART I-25
METAL ANALYSIS BY ICP: METALS (6010A) Page 10 of 11
ITEM YES COMMENT
Overall Evaluation:
a. Does the lab have sound technicalcapability for ICP analysis?
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month:________
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forICP analysis?
I-232
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CHART I-25
METAL ANALYSIS BY ICP: METALS (6010A) Page 11 of 11
ITEM
Additional observations, comments, or problems:
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s) Page 1 of 12
ITEM YES COMMENT
General:
a. Are written SOPS available and adequatefor AA sample preparation and analysis?
b. Do these SOPS accurately reflectprocedures in use?
c. Are manufacturer's operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear experiencedwith operation of an AA system andknowledgeable in the correction ofspectral, chemical, and physicalinterferences?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
I-234
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s)
ITEM
Apparatus and Facilities:
a.
b.
c.
d.
e.
f.
g.
h.
i.
j.
Is working space adequate and clean?
Does the lab have in-house capabilityfor metal analysis by FLAA, GFAA, CVAA,and HGAA?
Does the lab have a Zeeman backgroundcorrection system for GFAA?
Does the lab have other backgroundcorrection systems for GFAA (e.g.,deuterium and/or Smith-Hieftje)?
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Has any instrument been modified in anyway?
Are analytical balance (0.0001 g) andtop loading balance (0.01 g) available?
Are backup instruments available?
Are all glassware, polypropylene/ orTeflon containers, including samplebottles and flasks, washed in thefollowing sequence: detergent, tapwater, 1:1 nitric acid, tap water, 1:1hydrochloric acid, tap water, andreagent water?
Are pipet tips acid soaked with 1:5HNO3 and rinsed thoroughly with tap anddeionized water (Type II ASTM D1193)?
YES
Page 2 of 12
COMMENT
I-235
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s)
ITEM
Reagents:
a.
b.
c.
d.
e.
f.
g.
h.
i.
Is reagent water used free frominterferents at the MDLs of targetanalytes?
Is reagent grademega-ohm qualityanalysis?
Do reagent grade
water of at least 16used for metal
chemicals used confornto the-specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
Are all reagents analyzed to prove thatall constituents are below the MDLs?
Are spectrograde hydrochloric andnitric acids certified for AA analysisused for metal analysis?
Are redistilled nitric or hydrochloricacids used for preparation of stockstandard metal solutions?
Are sulfuric or phosphoric acidsavoided for standard preparation?
If standard stock solutions areprepared in-house, are all salts driedfor one hour at 105°C, unless otherwisespecified?
If standard stock solutions arepurchased, are the concentrations ofthe analytes verified in-house?
YES
Page 3 of 12
COMMENT
I-236
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s) Page 4 of 12
ITEM YES COMMENT
j. Are stock standards replaced after oneyear, or sooner if comparison withcheck standards indicates a problem?
k. Are calibration standards initiallyverified using check standards andmonitored weekly for stability?
l. Is the check standard prepared withreference materials independent ofcalibration standards analyzed for eachbatch?
m. Are silver standards limited to 2 mg/Land prevented from exposure to light?
n. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
o. Is the acetylene tank grounded, safelystrapped, and >100 psi?
Sample Handling and Storage:
a. Are aqueous samples preserved at pH < 2with nitric acid?
b. Are solid samples stored at 4°C?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolreadily available to bench chemists?
b. Are calibration results kept inpermanent logbooks?
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s) Page 5 of 12
ITEM YES COMMENT
c. Is a calibration curve prepared eachday with a minimum of three (exceptfive for mercury) concentration levelsfor each analyte?
d. Are equal amounts of permanganatereagents added to mercury calibrationstandards and blanks?
e. Is a calibration curve made for everyhour of continuous sample analysis ofmercury, arsenic, or selenium by CVAAor GFAA, respectively?
f. Are freshly prepared calibrationstandards used each time a batch ofsamples is analyzed?
g. Are the absorbance readings ofcalibration standards within 0.0 and0.7?
h. Are multiple exposures conducted tosecure a reliable average reading foreach solution?
i. Is one of the calibration standards ata concentration near, but above, theMDL?
j. Do concentrations of other standardscover the expected concentration rangesof real samples or define the workingrange of the detector?
Sample Preparation:
a. Is an appropriate sample preparationmethod, Methods 3005A, 3010A, 3020A,3040, or 3050A, used for sampledigestion?
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METAL ANALYSIS BY AA: METALS (7000s) Page 6 of 12
ITEM YES COMMENT
b. Are the digestion procedures in Section7.1 of Methods 7060 and 7740 used forpreparation of aqueous arsenic andselenium samples, respectively?
c. Are the digestion procedures in Section7.0 of Methods 7470 and 7471 used forpreparation of aqueous and solidmercury samples, respectively?
d. For seawater, brines, and industrialeffluents high in chlorides, areadditional hydroxylamine sulfate andpermanganate reagents (25 mL) used toprevent chlorine interference?
e. Are soil samples dried at ambienttemperature, ground, and sieved, priorto subsampling?
f. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
Sample Analysis:
a. Are the instructions provided by themanufacturer followed for each AA?
b. After choosing the proper lamp foranalysis, is the lamp allowed to warmup for a minimum of 15 minutes, unlessoperated in a double-beam mode?
c. Is an instrument blank run and theinstrument zeroed?
d. Is a lanthanum solution added tosamples that are to be analyze forcalcium and magnesium?
I-239
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s)
ITEM YES
e.
f.
g.
h.
i.
j.
k.
l.
m.
Is a calcium solution added to samplesthat are to be analyzed for iron andmagnesium?
Is a potassium chloride solution addedto samples before atomization in thedetermination of aluminum, barium, andtitanium?
Is an aluminum nitrate solution addedto samples before atomization in thedetermination of molybdenum andvanadium?
Is a cyanogen iodide solution added tosamples that are to be analyzed forsilver?
Is an unused cyanogen iodide solutiondiscarded after two weeks and freshsolution prepared?
Is a cyanogen iodide solution kept awayfrom any acid solution?
If a nitrous oxide/acetylene flame isused, is the nitrous oxide cylinderfitted with a non-freezable regulatoror is a heating coil wrapped around anordinary regulator?
After a nitrous oxide/acetylene flamehas been ignited, is the burner allowedto come to thermal equilibrium beforethe analysis is begun?
Are the average intensity of multipleexposures for both standardization andsample analysis used to reduce randomerror?
Page 7 of 12
COMMENT
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s)
ITEM
n. If the concentration found is greaterthan the highest standard, is thesample diluted in the same acid matrixand reanalyzed?
o. Is same injection volumes used forsamples and standards?
p. Is a magnesium perchlorate drying tubeor a small 60-W light bulb used toprevent condensation of moisture insidea mercury absorption cell?
Quality Control:
a.
b.
c.
d.
e.
f.
Are all QC data maintained andavailable for easy reference andinspection?
Is a three-level data review carriedout within the lab prior to datarelease?
Are lab specific IDL and MDLempirically established and updated ona semiannually basis?
Is the lab specific IDL or MDL equalto or lower than the method specifiedIDL or MDL, respectively?
Is a calibration curve prepared eachday with a minimum of a calibrationblank and three standards?
Is the calibration curve verified withat least a calibration blank and amid-range check standard made fromreference material or other independentstandard material? (The check standardmust be within 10% of its value for thecurve to be considered valid.)
YES
Page 8 of 12
COMMENT
I-241
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s) Page 9 of 12
ITEM YES COMMENT
g. If more than ten samples per day areanalyzed, is the calibration curveverified with a mid-range calibrationstandard or check standard after everyten samples? (This sample value mustbe within 20% of the true value, or theprevious ten samples need to bereanalyzed.)
h. For mercury, arsenic, or seleniumanalysis by CVAA or GFAA, is thecalibration curve verified with amid-range, independently prepared checkcheck standard every 15 samples?
i. For mercury, arsenic, or seleniumanalysis by CVAA or GFAA, are thesamples diluted if they are moreconcentrated than the highest standardor if they fall on the plateau of acalibration curve?
j. Are the following interference testsconducted for each analytical batch?
(1) Dilution Test: Select one typicalsample with concentration ofanalytes at > 25 times of the MDL.Dilute the sample by a minimum offivefold and analyze. If theconcentrations between the dilutedand the undiluted are within 10%,the absence of interferences canbe assumed and samples may beanalyzed without using method ofstandard additions.
I-242
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s)
ITEM
(2) Recovery Test: If all samples in
k.
l.
m.
n.
o.
p.
the batch are below ten times theMDL or the Dilution Test fails, aspiked sample should be analyzed.Add a known amount of analyte tobring the concentration to two tofive times the originalconcentration or to 20 times ofthe MDL if all analytes in thebatch are below MDL. The spikerecovery should be within 15%,otherwise the method of standardadditions shall be used for allsamples in the batch.
To demonstrate that a lab can generatedata of acceptable accuracy andprecision, does the lab routinelyperform matrix spike,duplicate, and matrixminimum rate of 5% orwhichever is greater?
Is a control limit ofsample values greaterthe IDL?
matrix spikeduplicate at aone per batch,
±20% RPDthan ten
Is the control limit for spikeduplicate sample within 20% ofactual value?
Are control charts for internalplotted and available to benchchemists?
Are control limits for internalcontrol empirically establishedupdated on a regular basis?
used fortimes
the
QC data
qualityand
Are all results reported with up tothree significant figures?
YES
Page 10 of 12
COMMENT
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CHART I-26
METAL ANALYSIS BY AA: METALS (7000s) Page 11 of 12
ITEM YES COMMENT
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for AA analysis?
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METAL ANALYSIS BY AA: METALS (7000s) Page 12 of 12
ITEM YES COMMENT
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: ________
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forAA analysis?
Additional observations, comments, or problems:
I-245
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CHART I-27
GENERAL QA/QC FOR CLASSICAL ANALYSIS: Page 1 of 2
ITEM YES COMMENT
Is the wavelength accuracy andrepeatability of all spectrophotometerschecked at several wavelengths for eachbatch of samples?
Is photometric accuracy and repeatabilitychecked and documented with NIST-traceablestandards?
Is acid washed glassware retained forphosphorus analyses only?
Is ammonia free water used in preparationof standards and samples for nitrogenanalyses?
Are manufacturer's operating manualsavailable to bench chemists?
Is there a calibration protocol availableto bench chemists?
Are calibration results kept in permanentlogbooks?
Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Has any instrument been modified in anyway?
Is a minimum of 4-point calibration used?
Are continuing calibration checks done on aregular basis?
Is the MDL for each analyte and matrix typedetermined every six months or wheneverthere is a significant change in backgroundor instrument response?
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CHART I-27
GENERAL QA/QC FOR CLASSICAL ANALYSIS: Page 2 of 2
ITEM YES COMMENT
Is the linear calibration range determinedfor each analyte when there is significantchange in instrument response and every sixmonths for those analytes that periodicallyapproach their linear limits?
Are internal QC samples run per methodrequirements?
Is a method blank run for each batch?
Additional observations, comments, or problems:
I-247
EM 200-1-11 Jul 94
CHART I-28
CLASSICAL ANALYSIS: COMMON ANIONS (300s)
ITEM
Does the lab use an ion chromatography (IC)to analyze chloride, fluoride, nitrate,nitrite, ortho-phosphate, and sulfate?
Does the IC system have appropriate anionguard column, separator column, suppressorcolumn, and conductivity detector?
Is the maximum loading to a separatorcolumn kept below 400 µg/L to avoid columnoverloading and nonlinear response?
Are nitrate, nitrite, ortho-phosphate, andsulfate samples stored at 4°C?
Are the lab's holding times for nitrate,nitrite, and ortho-phosphate by IC method48 hours from sampling to analysis? (28days for chloride, fluoride, and sulfate.)
Is the eluent solution made of sodiumbicarbonate (0.003 M) and sodium carbonate(0.0024 M)?
Is the regeneration solution made ofsulfuric acid (0.025 N)?
Is a filtration conducted on samples thatcontain particles larger than 0.45 micronsand reagent solutions that containparticles larger than 0.20 microns?
Is a reagent water analyzed beforeprocessing any standards or samples todemonstrate that all glassware and reagentinterferences are under control?
Is a reagent blank processed each timethere is a change in reagents?
YES
Page 1 of 7
COMMENT
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CHART I-28
CLASSICAL ANALYSIS: COMMON ANIONS (300s) Page 2 of 7
ITEM YES COMMENT
Are calibration standards prepared fromsodium chloride, sodium fluoride, sodiumnitrate, sodium nitrite, potassium sulfate,and potassium dihydrogen phosphate dried at105°C for 30 minutes?
Are stock standards stored at 4°C?
Are working standards prepared at aminimum on a weekly basis, except thosefor nitrite and phosphate which should beprepared fresh daily?
Is a minimum of three concentration levelsand a blank used for calibration of eachanalyte of interest?
Is one of the calibration standards near,but above, the MDL?
Is the injection loop flush thoroughlyusing each new standard or sample?
Is the same size of injection loop used forstandards and samples?
Unless the attenuator range settings areproven to be linear, is each settingcalibrated individually?
If the working range exceeds the linearrange of the system, is a sufficient numberof standards analyzed to allow an accuratecalibration curve to be established?
Is the water dip or negative peak thatelutes near and interferes with fluoridepeak eliminated by the addition ofconcentrated eluent to each standard andsample?
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CLASSICAL ANALYSIS: COMMON ANIONS (300s) Page 3 of 7
ITEM YES COMMENT
Are the retention times of each analytedocumented during the calibration?(Retention time is inversely proportionalconcentration.)
Is the working calibration curve verifiedon each working day, or when the anioneluent is changed, and after every 20samples?
If the response or retention time for anyanalyte varies from the expected values bymore than ±l0%, is the test repeated withfresh calibration standards?
If the results are still more than ±l0%, isan entirely new calibration curve preparedfor that analyte?
Is the width of retention time windowdetermined based upon three times ofstandard deviation of measurements ofactual retention time variations over thecourse of a day?
If the response of a peak exceeds theworking range of the system, is the samplediluted with reagent water and reanalyzed?
Is an initial demonstration of laboratorycapability conducted with a minimum of fourLCS?
Is a continuing check on laboratoryperformance conducted with spiked samplesat a minimum rate of 10% of all samples?
Are LCS, lab duplicates, and other QC checksamples routinely analyzed for each samplebatch?
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CHART I-28
CLASSICAL ANALYSIS: COMMON ANIONS (300s) Page 4 of 7
ITEM YES COMMENT
Are method performance criteria empiricallydetermined for each spike concentration ofanalyte being measured?
Does the lab develop and maintain separateaccuracy statements, %R ± , for water andwastewater samples? (The average percentrecovery, % R , and the standard deviation ofof the percent recovery, , are developedby analyses of four aliquots of water andwastewater.)
Is a confirmatory technique such as sampledilution and spiking used to confirm anionidentification?
Fluoride:
a. Distillation:
(1) Before a sample is run, is thedistillation apparatus flushed bydistilling the sulfuric acid-distilled water mixture until thetemperature reaches 180°C?
(2) Is the sample and acid-watermixture distilled until the flasktemperature reaches 180°C?
(3) Is the heating the contents of thedistilling flask above 180°Cavoided?
(4) Are all water and wastewater sampledistilled?
b. Calorimetric-SPADNS:
(1) If residual chlorine is present, isit removed with sodium arsenitesolution?
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CLASSICAL ANALYSIS: COMMON ANIONS (300s) Page 5 of 7
ITEM YES COMMENT
(2) Are all samples (including potablewater) subjected to preliminarydistillation?
(3) Are standards prepared in the rangeof 0 to 1.40 mg/L?
(4) Are samples and standards at thesame temperature for colordevelopment?
(5) Is color development carried outwith SPADNS solution and zirconyl-acid reagent (or, alternativelyacid-zirconyl-SPADNS reagent)?
(6) Is the absorbance of samples andstandards read at 570 nm?
(7) Is a standard curve drawn based onthe absorbance of the standards?
(8) Are the fluoride concentrations ofthe samples read directly from thecurve without extrapolation?
(9) Are standard curves retained aspart of the record?
c. Potentiometric Ion Selective Electrode:
(1) Is a series of fluoride standardscovering the range of 0 to 2.0 mg/Lfluoride prepared?
(2) IS an equal volume of total ionicstrength adjustment buffer mixedwith the sample or standard to bemeasured?
(3) Are samples and standards measuredat room temperature?
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CHART I-28
CLASSICAL ANALYSIS: COMMON ANIONS (300s) Page 6 of 7
ITEM YES COMMENT
(4) When a measurement is made, are theelectrodes allowed to remain in thesolution for three minutes (orlonger if necessary) before areading is made?
(5) When an electrometer is used, is astandard curve prepared on semi-logarithmic graph paper with thefluoride concentration in mg/L onthe log axis and the electrodepotential developed in the standardon the linear axis?
(6) Are the samples diluted andremeasured if they fall outsidethe working range of the standardcurve?
(7) Is a 1.00 mg/L fluoride standardread after each known sample andeach standard?
(8) If a selective-ion meter is used,is it calibrated in accordance withthe manufacturer’s instruction?
(9) Are all standard curves andcalibration data retained as partof the record?
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CHART I-28
CLASSICAL ANALYSIS: COMMON ANIONS (300s) Page 7 of 7
ITEM
Additional observations, comments, or problems:
I-254
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CHART I-29
CLASSICAL ANALYSIS: OIL AND GREASE (413.1) Page 1 of 2
ITEM YES COMMENT
Are samples collected in glass containers?
Are samples preserved at the time ofcollection by adjusting the pH to two orless with hydrochloric acid or sulfuricacid and cooling to 4°C?
Are samples analyzed within 28 days ofcollection?
Are the samples at a pH of two or less whenthe analysis is begun?
Is the sample level marked on the samplecontainer for later determination of samplevolume?
Is the entire sample transferred to aseparator funnel?
Is the sample bottle carefully rinsed withfluorocarbon 113 for two minutes and thelayers allow to separate?
Is the solvent layer drained through afunnel containing solvent moistened filterpaper and (if necessary) anhydrous sodiumsulfate into clean tared distilling flask?
Is the extraction repeated twice more andthe extracts combined in the distillingflask?
Is the solvent distilled from thedistilling flask using a 70°C water bathas a source of heat?
After the distillation is completed, is thedistilling flask swept out with air byinserting a glass tube connected to avacuum source?
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CHART I-29
CLASSICAL ANALYSIS: OIL AND GREASE (413.1) Page 2 of 2
ITEM YES COMMENT
Is the flask wiped clean and dry on theoutside, cooled in a desiccator for 30minutes, and then weighted?
Is a solvent blank run with each set ofsamples?
Quality Control Requirements:
a. Is a laboratory blank analyzed dailyor with each batch of sample run?
b. Is a reference standard analyzed withevery tenth sample?
c. Is a spiked sample analyzed with every20th sample?
d. Are duplicate analyses performed on aminimum of 10% of all positive samples?
Additional observations, comments, or problems:
I-256
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 1 of 9
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor TRPH sample preparation/analysis?
b. Do these SOPs accurately reflectprocedures in use?
c. Are manufacturer’s operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are notebooks reviewed and initialed bysupervisors on a regular basis?
d. Is an error crossed out with a line andcorrection entered, dated, andinitialed?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in TRPH analysis?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Are enough sets of separator funnels(2,000 mL with Teflon stopcock) andSoxhlet extractors available forsimultaneous extraction of all batchsamples?
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 2 of 9
ITEM YES COMMENT
c. Is a hood available for samplepreparation?
d. Are IR spectrophotometers suitable formeasurements around 2930 cm¯¹?
e. Does lab have sodium chloride or IRgrade optical cells of 1-cm, 5-cm, and10-cm pathlength?
f. Are backup apparatuses available?
Reagents:
a. Is reagent water used free frominterferents at the method detectionlimits of target analytes?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Is magnesium sulfate monohydrateprepared by drying the heptahydratesalt in an oven at 150°C overnight?
d. Is granular, anhydrous sodium sulfatepurified by heating at 400°C for fourhours, or by precleaning with Freon-113(1,1,2-trichloro-1,2,2-trifluoro-ethane)?
e. Is silica gel, 60-200 mesh, containing1-2% water as defined by residue testat 130°C available? (Dried at 110°Cfor 24 hours and stored in a tightlysealed container.)
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 3 of 9
ITEM YES COMMENT
f. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Is the pH of aqueous and sludge sampleschecked and adjusted to <2 duringsample log-in?
b. Are aqueous and sludge samples storedat 4°C and analyzed within 28 days?
c. Are soil samples stored at 4°C andanalyzed with minimum delay uponreceipt in the lab?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolavailable to the bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Are IR spectrophotometric accuracy andrepeatability checked and documentedwith NIST-traceable standards?
d. Are the materials of interest, ifavailable, or the same type ofpetroleum fraction, if it is known andoriginal sample is unavailable, usedfor preparation of calibrationstandards?
I-259
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 4 of 9
ITEM YES COMMENT
e. Does the lab normally attempt todetermine the petroleum fraction typefor unknowns prior to instrumentcalibration? (Reference oil is to beused as a last resort for unknowns, asit generates low values for diesel,kerosene, and other known petroleumhydrocarbon types.)
f. Does reference oil contain a mixture ofn-hexadecane, isooctane, and chloro-benzene in the appropriate proportions?(i.e., 15.0 mL + 15.0 mL + 10.0 mL)
g. Is Freon-113, b.p. 48°C, used forstandard and sample preparation?
h. Is a minimum of a four-pointcalibration curve (a blank plus threestandards) prepared for calibration?
i. Do working ranges and cell pathlengthscomply with method requirements?
j. Is a calibration plot prepared forabsorbance versus mg petroleumhydrocarbons in 100 mL solution?
k. Are standards scanned from 3200 cm¯¹ to2700 cm¯¹ with solvent in the referenceand results recorded on absorbancepaper?
l. Are absorbance of standards measuredby constructing a base line over thescan range and measuring absorbance ofthe peak maximum at 2930 cm¯¹ andsubtracting absorbance at that point?
m. Are continuing calibration checks doneon a regular basis for each batch ofsamples?
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 5 of 9
ITEM YES COMMENT
n. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
Sample Preparation:
a. For aqueous samples, are the samplebottles marked at the water meniscusfor later determination of samplevolume?
b. Is the entire aqueous sample consumedfor analysis and no analysis performedon aliquots of samples?
c. Is the pH value of aqueous sampleschecked and adjusted to < 2 prior toextraction?
d. Are sample bottle, tip of separatorfunnel, filter paper, and funnel rinsedwith solvent and the rinsate combinedwith extract?
e. Is the aqueous sample sequentiallyextracted with three 30 mL portion offresh Freon-113?
f. Is sodium sulfate, anhydrous crystal,used when emulsion occurs?
g. Is the percent solid of solid samplesdetermined by drying overnight at 105°Cin a vented drying oven?
h. Are sludge samples acidified to a pH oftwo and dried with magnesium sulfatemonohydrate?
i. Are sediment/soil samples decanted anddried with anhydrous sodium sulfate?
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 6 of 9
ITEM YES COMMENT
j. For solid samples, is Soxhlet method(Method 9071, steps 7.1 thru 7.11),instead of sonication method, used forsample extraction?
k. Is Soxhlet extraction conducted at arate of 20 cycles per hour for fourhours?
l. Is the water bath kept at 70°C?
m. Is extract filtered with grease-freecotton or glass wool that is cleanedwith solvent?
n. Is 3-g silica gel used to remove polarfatty matter by stirring the solutionwith a Teflon coated magnetic stirrerfor a minimum of five minutes?
o. Is the absorptive capacity of silicagel checked by repeating the silica geltreatment procedure?
Sample Analysis:
a. Are samples scanned from 3200 cm¯¹ to2700 cm¯¹ with solvent in the referencebeam and results recorded on absorbancepaper?
b. Is a straight baseline constructed overthe scan range and subtracted from thepeak maximum at 2930 cm¯¹?
c. If the absorbance exceeds 0.8, is ashorter pathlength cell or a dilutedextract used?
d. Does the lab strictly adhere to themethod without any deviations?
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 7 of 9
ITEM YES COMMENT
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review conductedwithin the lab prior to data release?
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Does the lab specific MDL meet orexceed the method specified MDL?
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
f. Is calibration curve verified within±10% of an independent, mid-range checkstandard for each batch?
g. Are duplicate analyses performed at aminimum rate of 5% or one per batch,whichever is more frequent?
h. Is one pair of matrix spike and matrixspike duplicate samples run at aminimum rate of 5% or one per batch,whichever is more frequent?
i. Are control charts for internal QC dataplotted and available to benchchemists?
j. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 8 of 9
ITEM YES COMMENT
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
c. Does the lab recycle Freon-113?
Overall Evaluation:
a. Does the lab have sound technicalcapability for TRPH analysis?
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CHART I-30
CLASSICAL ANALYSIS: TRPH (418.1) Page 9 of 9
ITEM YES COMMENT
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: ______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forTRPH analysis?
Additional observations, comments, or problems:
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 1 of 10
ITEM YES COMMENT
General:
a. Are written SOPs available and adequatefor cyanide sample preparation andanalysis?
b. Do these SOPs accurately reflectprocedures in use?
c. Are manufacturer’s operating manualsreadily available to bench chemists?
d. Are prenumbered, bound notebooks usedfor data entry?
e. Are all records written in indelibleink?
f. Are all errors corrected by drawing asingle line through the error withcorrections written adjacent to theerror, so that it remains legible, andinitialed and dated by the responsibleindividual?
g. Are notebooks reviewed, initialed, anddated by supervisors on a regularbasis?
Technical Staff:
a. Do bench chemists appear knowledgeableand experienced in cyanide analysis?
b. Are backup bench chemists available?
c. Are bench chemists’ performance auditedand approved prior to work withoutclose supervision by a senior chemist?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 2 of 10
ITEM YES COMMENT
Apparatus and Facilities:
a. Is working space adequate and clean?
b. Are enough sets of reflux distillationapparatuses available for simultaneousdistillation for all batch samples?
c. Is a hood available for samplepreparation?
d. Are spectrophotometers suitable formeasurements at 578 nm with a 1.0-cmcell or larger?
e. Are backup apparatus available?
Reagents:
a. Is ASTM Type II water (ASTM D1193)monitored and used for analysis?
b. Do reagent grade chemicals used conformto the specifications of the Committeeon Analytical Reagents of the AmericanChemical Society, where suchspecifications are available?
c. Is KCN used for standard preparationin good physical condition?
d. Is chloramine-T solution prepared freshdaily and refrigerated until ready touse?
e. Is pyridine-barbituric acid reagentstored in a cool, dark place anddiscarded after six months (one monthif stored at room temperature in thelight) or upon formation of aprecipitate?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 3 of 10
ITEM YES COMMENT
f. Are all reagents and standards labeled,dated, initialed, and documented suchthat composition and expiration datecan be verified?
Sample Handling and Storage:
a. Are the pH values of aqueous sampleschecked and adjusted to > 12 in a hoodduring log-in?
b. If aqueous samples are not runimmediately, are oxidizing agents, suchas chlorine, in the samples checkedwith acidified KI-starch paper andpreserved with ascorbic acid duringsample log-in?
c. Are samples stored at 4°C and preparedwithin 14 days?
Instrument Calibration and Maintenance:
a. Is there a calibration protocolavailable to the bench chemists?
b. Are calibration results kept inpermanent logbooks?
c. Are photometric accuracy andrepeatability checked and documentedwith NIST-traceable standards?
d. Are calibration standards traceableto NIST or other reliable standards?
e. Is a minimum of one 7-point calibrationcurve (a blank plus six standards)prepared for calibration?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 4 of 10
ITEM YES COMMENT
f. Is method blank, consisting of sodiumhydroxide dilution solution (1.25 N)and all reagents, used to adjust thephotometer zero?
g. Is a calibration curve ranging from 20to 400 µg/L prepared?
h. Are the cyanide standards preparedfresh daily and kept in glass-stopperedbottles?
i. Are all calibration standards preparedwith sodium hydroxide dilution solutionfor all dilution?
j. Is a calibration curve preparedcovering the range of the method byplotting absorbance of standardsagainst cyanide concentrations (0-1.0mg/L?)
k. For samples without sulfide, is aminimum of two standards (a high andlow) distilled and compared withsimilar values on the curve to test thedistillation technique?
l. Do the distilled standards agree within±10% of the undistilled standards?
m. For samples with sulfide, are allstandards distilled in the same manneras the samples?
n. Are continuing calibration checks doneon a regular basis?
o. Is a permanent logbook kept for eachinstrument that summarizes instrumentproblems and servicing records?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 5 of 10
ITEM YES COMMENT
p. Has any instrument been modified in anyway?
Sample Preparation:
a. Is pretreatment for cyanides amenableto chlorination performed in a hoodto avoid the very toxic gas cyanogenchloride and under amber light to avoidfalse positive from K3 [Fe(CN)6]decomposed by UV light?
b. During the chlorination procedure, isthe pH maintained between 11 and 12,and residual chlorine checked andmaintained for one hour while thesamples are agitated by magneticstirring bars?
c. After chlorination, is excess reducingagent, ascorbic acid or sodiumarsenite, added to remove chlorine?
d. Are all samples distilled beforecyanide determination?
e. Is a 500 mL aliquot (or small aliquotdiluted to 500 mL if necessary)containing not more than 100 mg/L ofcyanide taken for distillation?
f. Is sodium hydroxide used as theabsorbing solution?
g. Is a fritted glass disc used todisperse HCN in absorbing solution?
h. Is the vacuum adjusted so that abouttwo air bubbles per second enter theboiling flask?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 6 of 10
ITEM YES COMMENT
i. Is lead acetate paper used to check thesample for the presence of sulfide?
j. If the test is positive, is bismuthnitrate solution used to removesulfide?
k. If samples are known or suspected tocontain nitrate/nitrite, is adequateamount of sulfamic acid solution added,after the air rate is set, to removenitrate/nitrite?
l. Are sulfuric acid and magnesiumchloride added, with washing, throughthe air inlet tube?
m. Is the sample heated to boiling andthen refluxed for one hour?
n. After the reflux period is completed,is heat turned off and the airflowcontinued for at least 15 minutes?
o. Are the contents of the gas absorberdrained into a 250 mL volumetric flask?
p. Are the gas absorber and the tubeconnecting the reflux condenser withthe gas absorber rinsed with distilledwater and combined with the drainedliquid in the volumetric flask and thecontents diluted to 250 mL?
q. If incomplete recovery is suspected,is a fresh charge of sodium hydroxideplaced in the gas washer and the samplerefluxed for one more hour?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 7 of 10
ITEM YES COMMENT
r. If samples contain appreciable amountof solid, oil, or grease to interferewith homogenization and agitation ofthe sample mixture in the distillationflask, is Method 9013 used to extractcyanide?
s. Is Method 9013 used for the extractionof soluble cyanides from oil, solid,and multiphase samples?
Sample Analysis:
a. Is the amount of sodium hydroxide inthe standards and the samples analyzedthe same?
b. Is the chlorine demand of any compoundsin the distillate tested with KI-starchpaper?
c. Do standards bracket the concentrationof the samples?
d. If dilution is required, is distillatediluted with method blank solution?
e. If pyridine-bartituric acid is used,are the reagents mixed and the colorallowed to develop for 8 minutes beforereading being taken within 15 minutes?
Quality Control:
a. Are all QC data maintained andavailable for easy reference andinspection?
b. Is a three-level data review carriedout within the lab prior to datarelease?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A)
ITEM
c. Is a lab specific MDL empiricallyestablished and updated on asemiannually basis?
d. Does the lab specific MDL meet orexceed the method specified MDL?
e. Is a method blank run at a minimum rateof 5% or one per batch, whichever ismore frequent?
f. Is calibration curve verified within±15% of an independent, mid-range checkstandard for each batch?
g. Is a matrix spike sample at a levelof 40 µg/L analyzed per batch to checkthe efficiency of distillation?
h. Are duplicate analyses performed at aminimum rate of 5% or one per batch,whichever is more frequent?
i. Is one pair of matrix spike and matrixspike duplicate samples run at aminimum rate of 5% or one per batch,whichever is more frequent?
j. Is method of standard additions usedfor the analysis of all samples thatsuffer from matrix interferences?
k. Are control charts for internal QC dataplotted and available to benchchemists?
l. Are control limits for internal qualitycontrol empirically established andupdated on a regular basis?
YES
Page 8 of 10
COMMENT
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 9 of 10
ITEM YES COMMENT
Data Package:
a. Does the length of storage time for allsample related information, includingchain-of-custody, instrumentcalibration, sample preparation andanalysis, etc., comply with regulatoryrequirements, organizational policy, orproject requirements, whichever is morestringent? (It is recommended thatdocumentation be stored for a minimumof three years from submission of theproject final report.)
b. Does the data package contain allmethod required QC data and meet theUSACE contract requirements?
c. Are all raw data signed and dated bythe persons who performed the sampleanalysis and data review?
Waste Disposal:
a. Does the lab use a contractor todispose of residual and preparedsamples, and samples with analysiscancelled?
b. Are lab wastes disposed of properlysuch that no secondary pollution isproduced by sample analysis and theUSACE will not be liable for anypollution problems in the future?
Overall Evaluation:
a. Does the lab have sound technicalcapability for cyanide analysis?
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CHART I-31
CLASSICAL ANALYSIS: CYANIDE (9010A) Page 10 of 10
ITEM YES COMMENT
b. Does the lab have appropriate capacityto handle the contract load?Average number of samples analyzed andreported per month: ______
c. Could the lab handle quick turnaroundsamples?
d. Overall, is the lab acceptable forcyanide analysis?
Additional observations, comments, or problems:
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CHART I-32
CLASSICAL ANALYSIS: TOC (9060) Page 1 of 2
ITEM YES COMMENT
Are samples preserved on collection byadjusting the pH to two or less withsulfuric acid or hydrochloric acid andcooling to 4°C?
Are samples analyzed within 28 days ofcollection?
Based on the preliminary treatment of thesamples prior to analysis, is a notationmade defining the type of carbon toanalysis?
Is carbon dioxide-free double distilledwater used on the preparation of standardsand dilution of samples?
Is the use of ion exchanged water avoided?
Is the potassium hydrogen phthalate stocksolution prepared using primary standardgrade reagent?
Is the hypodermic needle size selected soas to obtain the most reproducible results?
Are injections repeated until threeconsecutive peaks are obtained that arereproducible to within ±3%?
Does the series of standards run encompassthe expected concentration range of thesamples to be run?
Is a dilution water blank run?
Quality Control Requirements:
a. Is a laboratory blank analyzed dailyor with each sample run?
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CHART I-32
CLASSICAL ANALYSIS: TOC (9060)
ITEM
b. Is a reference standard analyzed withevery tenth sample?
c. Is a spiked sample analyzed with every20th sample?
d. Are duplicate analyses performed on aminimum of 10% of all positive samples?
YES
Page 2 of 2
COMMENT
Additional observations, comments, or problems:
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CHART I-33
WASTE CHARACTERISTICS: IGNITABILITY (1010/1020) Page 1 of 3
ITEM
Pensky-Martins Closed Method (1010):
a.
b.
c.
d.
e.
f.
g.
Is the Pensky-Martins closed-cup methodused to determine the flash point ofliquids that tend to form surface filmsunder test conditions or containnon-filterable suspended solids?
Are two standard thermometersavailable?
Is a barometer capable of measuringambient pressure available (barometersprecorrected to give sea-level readingare not acceptable)?
Are results documented with thefollowing information?
(1) Observed flash point?
(2) Ambient barometric pressure?
(3) Corrected flash point?
Is a duplicate sample included withevery tenth sample?
Is a p-xylene reference standarddetermined in duplicate with everysample batch?
Is the average of the duplicatep-xylene reference standard flash pointdetermination 27 ± 0.8°C (81 ± 1.5°F)?
YES COMMENT
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CHART I-33
WASTE CHARACTERISTICS: IGNITABILITY (1010/1020) Page 2 of 3
ITEM
Setaflash Closed-Cup Method (1020):
a.
b.
c.
d.
e.
f.
g.
h.
Is the Setaflash closed-cup method usedto determine the flash point of liquidsthat have flash points between 0° andllO°C (32° and 230°F) and viscositieslower than 150 stokes at 25°C (77°F)?
Are ASTM grade thermometers available?
Is heat transfer paste available?
Is a barometer capable of measuringambient pressure available (barometersprecorrected to give sea-level readingare not acceptable)?
Are results documented with thefollowing information?
(1) Observed flash point?
(2) Ambient barometric pressure?
(3) Corrected flash point?
Is a duplicate sample included withevery tenth sample?
Is a p-xylene reference standarddetermined in duplicate with everysample batch?
Is the average of the duplicatep-xylene reference standard flash pointdetermination 27 ± 0.8°C (81 ± 1.5°F)?
YES COMMENT
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CHART I-33
WASTE CHARACTERISTICS: IGNITABILITY (1010/1020) Page 3 of 3
ITEM
Additional observations, comments, or problems:
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CHART I-34
WASTE CHARACTERISTICS: CORROSIVITY (1110) Page 1 of 1
ITEM YES COMMENT
Are the steel coupons of SAE Type 1020steel?
Are the steel coupons suspended andsupported with a non-conducting materialsuch as glass, fluorocarbon, or coatedmetal?
Are the areas of coupons known to ±l%?
Is a blank run with each test sample?
Are duplicates run with every tenth sample?
Is cleaning done by either mechanical,chemical, or electrolytic means?
Additional observations, comments, or problems:
I-281
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CHART I-35
WASTE CHARACTERISTICS : Toxicity (1311) Page 1 of 5
ITEM YES COMMENT
Is reactivity determined by the writtencriteria and an impact apparatus based onan 8-lb weight?
Total Reactive Cyanide:
a. Is the approved test method (Method901OA) in place?
b. Are the samples collected with minimumaeration and headspace, kept in a cooldark place, and analyzed as soon aspossible?
c. Equipment: Are the following pieces ofequipment available?
(1) Three neck round bottom flask of500-mL capacity?
(2) Separator funnel with pressureequalizing tube and 24/80 groundglass joint and Teflon sleeve?
(3) Water pumped or oil pumped nitrogengas?
(4) Rotometer?
d. Method Verification:
(1) Has the system been checked witha reference solution yielding arecovery greater than 50%?
(2) Has this been documented?
Total Reactive Sulfides:
a. Is the approved test method (Method9030) in place?
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CHART I-35
WASTE CHARACTERISTICS: REACTIVITY (SECTION 7.3)
ITEM
b.
c.
d.
Are the samples collected with minimumaeration and headspace, kept in a cooldark place,and analyzed as soon aspossible?
Equipment:
(1) Is the apparatus required forMethod 9030 available?
(2) Has the absorber been replacedan “Industrial Hygiene” type
with
detection tube for sulfide (100 to2,000 ppm)?
Method Verification:
(1) Has the system been checked with areference solution yielding arecovery greater than 50%?
(2) Has this been documented?
YES
Additional observations, comments, or problems:
Page 2 of 2
COMMENT
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CHART I-36
WASTE CHARACTERISTICS: TOXICITY (1311) Page 1 of 5
ITEM YES COMMENT
Are approved methods in place for analysisof toxicity characteristic leachingprocedure (TCLP) extracts for volatiles,BNAs , RCRA metals, pesticides, andherbicides?
Are zero-headspace extraction (ZHE) vesselsavailable?
Is the piston within the ZHE able to movewith approximately 15 Psi or less?
Are enough sets of ZHE and bottleextractors available for simultaneousextraction of all samples in one batch?
Are borosilicate glass bottles used forTCLP extraction bottles?
Is borosilicate glass filter containing nobinder materials used for TCLP extraction?
Are enough aliquots of samples collectedfor preliminary evaluation of whichextraction fluid to be used, actualextraction of nonvolatiles, ZHE ofvolatiles, and QC measures?
Is a separation procedure used for thesolid and liquid phase?
For liquid wastes containing less than 0.5%dry solid materials, are the liquid wastes,after filtration through a 0.6 to 0.8-µmglass fiber filter defined as the TCLPextract?
Is an agitation apparatus capable ofrotating the extraction vessels in an end-over-end fashion at 30 ± 2 rpm available?
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CHART I-36
WASTE CHARACTERISTICS: TOXICITY (1311) Page 2 of 5
ITEM YES COMMENT
Is vacuum filtration used for wastes withlow solid content (<10%) and for highlygranular, liquid-containing wastes?(Positive pressure filtration should beused for all other types of wastes.)
Are filters for determination of mobilityof metals acid washed prior to use with 1 Nnitric acid followed by consecutive rinseswith deionized distilled water? (A minimumof 1 L per rinse is recommended.)
Are preservatives not added to samplesbefore TCLP extraction?
Are TCLP extracts analyzed as soon aspossible following extraction?
Are TCLP extracts for metal analysisacidified with nitric acid to pH<2, unlessprecipitation occurs?
Are TCLP extracts for organic analysespreserved at 4°C without headspace toprevent loss?
Are solid samples passed through a 9.5 mmstandard sieve?
If not, are solid samples crushed, cut, orground to meet the size criteria?
Is the method specified procedure followedto determine the appropriate extractionfluid for nonvolatile TCLP target analytes?
Is extraction fluid Number 1 always usedfor TCLP volatiles?
Is a minimum of 100 g samples extracted fornonvolatile?
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CHART I-36
WASTE CHARACTERISTICS: TOXICITY (1311)
ITEM
Is a maximum of 25 g samples used for a 500mL ZHE vessel?
Is the pH meter used accurate t, ±O.05units at 25°C?
Is the balance used accurate to within±O.01 g? (All weight measurements are tobe within ±O.1 g.)
Is TCLP extraction procedure carried outfor 18 ± 2 hours at 22 ± 3°C?
Are TCLP extractor bottles for nonvolatilesperiodically opened to relieve excesspressure?
Is TCLP extract filtered and combined withany liquid from the original separation, ifcompatible (i.e., no multiple phases form)?
If the initial liquid phase is not or maynot be compatible with the filtered liquid,are these liquids analyzed separately andresults combined mathematically?
Is TCLP toxicity determined by comparisonwith the levels identified in theappropriate regulations?
Is a method blank run with each batch ofextractions?
Is a matrix spike performed for each wastetype?
Are matrix spikes added after filtration ofthe TCLP extract and before preservation?(Matrix pikes should not be added prior toTCLP extraction of samples.)
YES
Page 3 of 5
COMMENT
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WASTE CHARACTERISTICS: TOXICITY (1311) Page 4 of 5
ITEM YES COMMENT
Are matrix spikes at the a concentrationequivalent to the corresponding regulatorylevel but not less than five times the MDL?
When the recovery of matrix spike is belowthe expected analytical method performance,is the use of internal calibration methods,modification of the analytical methods, oruse of alternative analytical methodsemployed to accurately measure theconcentration of the TCLP extract?
Is the method of standard additionsemployed as the internal calibrationquantitation methods for each metalliccontaminant if:
(1) Matrix spike recovery from the TCLPextract is less than 50% and theconcentration does not exceed theregulatory level, and
(2) The contaminant concentration in theTCLP extract is within 20% of theappropriate regulatory level?
Is the method of standard additions usedfor analysis of all EP extracts, on allanalyses submitted as part of a delistingpetition, and whenever a new sample matrixis being analyzed?
Are four identical aliquots of TCLPsolution used for the method of standardadditions?
Is the holding time from TCLP extraction topreparative extraction for semivolatilesless than or equal to seven days?
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CHART I-36
WASTE CHARACTERISTICS: TOXICITY (1311) Page 5 of 5
ITEM
Additional observations, comments, or problems:
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APPENDIX J
SHORT CHECKLISTS
FOR
ON-SITE LABORATORY INSPECTIONS
J-1
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SHORT CHECKLISTS FOR ON-SITE LABORATORY INSPECTIONS
CHARTS J-1 through J-10 contains a short version oflaboratory inspection checklists. The short checklists aredeveloped to reduce the amount of paper work to be brought to anon-site laboratory inspection. Only the major areas to beexamined are listed in the short checklists. They serve as areminder for an experienced inspector to check the adequacy oflaboratory facility, equipment, operation, and QA/QC policy andpractice during an on-site inspection. Depending on alaboratory's performance and an inspector's preference, theinspector may choose the long checklists (Appendix I), the shortchecklists, or a hybrid of both to perform an on-site laboratoryinspection.
J-2
EM 200-1-11 Jul 94
Short Laboratory Inspection Checklists
CHART J-1 Lab Organization, Personnel, and Management
1. Organizationa. Organization chartb. Management structurec. Principal officers
(1) Lab Director - ten years(2) Lab Manager - seven years(3) Organic Lab Manager - five years(4) Inorganic Lab Manager - five years(5) QA Officer - five years
d. Reporting relationships
2. Personnela. Resumesb. Job descriptionsc. Training program
(1) Initial training and evaluation(2) Continuing training and auditing(3) Documentation
d. Minimum Experience without supervision(1)(2)(3)(4)(5)(6)(7)(8)
(9)(10)(11)(12)(13)(14)(15)(16)
(17)(18)(19)
GC supervisor - three yearsGC analysis - one yearPesticide residue analysis - two yearsGC/MS supervisor - three yearsGC/MS analysis - one yearGC/MS spectral interpretation - two yearsHPLC analysis (explosives) - one yearOrganic sample preparation - one year
AA/ICP supervisor - three yearsAA/ICP analysis - one yearMetal sample preparation - six monthsWet chemistry supervisor - three yearsUV/VIS analysis (cyanide) - one yearIR analysis (TRPH) - one yearIC analysis (common anions) - one yearClassical analysis - one year
Radiochemistry supervisor - five yearsRadionuclides analyst - two yearsGross alpha/beta analysis - six months
J-3
EM 200-1-11 Jul 94
CHART J-2 Lab Facility, Equipment, and Instrumentation
1. Facilitya. Securityb. Sample storagec. Chemical storaged. Bench spacee. Number of hoodsf. Ventilationg. Document archives
2. Equipmenta.
b.
c.
d.
e.
f.
g.h.i.j.k.
l.
m.n.
o.
p.q.r.s.
Reagent water system (Free from interferents at MDL;resistivity ≥ 16M Ω.)
Conductivity meters (Daily or before-use calibrationcheck; cell constant determined annually.)
pH meters (Scaled to ≤ 0.1 pH unit; standardized daily attwo pH units that bracket the expected pH range and areno more than three to four pH units apart; temperaturecompensated.)
Analytical balance (Capable of weighing to 0.1 mg; dailyor before-use check with a minimum of one Class Sweight in the range to be used and monthly with aseries of Class S weights; ≤ 0.1%)
Class S weights (50 mg to 4 kg; calibrated within fiveyears and traceable to NIST.)
Drying ovens (Temperature checked before and after eachusage.)
Muffle furnace (Temperature verified annually.)Hotplates (Capable of temperature control within ±5°C.)Water bath (Capable of temperature control within ±5°C.)Refrigerators (Temperature checked twice daily.)Thermometers (Mercury type: scaled to ≤ 1°C; checked
annually against NIST traceable thermometer at twoseparate temperatures; Dial-type: calibrated quarterlyagainst NIST traceable thermometer.)
Autopipetors (Daily or before-use check of deliveryvolume gravimetrically.)
Volumetric glassware (Class A segregated from others.)Glassware cleaning station (Metals, ammonia, phosphorus,volatiles, and semivolatiles.)
Sonicator (Titanium horn; 475 watts with pulsingcapability.)
TCLP (ZHE)LIMS (Audit trail and security.)Safety equipmentWaste disposal
J-4
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CHART J-2 Lab Facility, Equipment, and instrumentation(continued)
3. Instrumentationa. AA: Metals (7000s)
(1) GFAA with Zeeman correction (As, Pb, Sb, Se, Tl)(2) CVAA (Hg)(3) FLAA
b. ICP: Metals (6010A)c. GC:
(1) ECD (8080, 8150A)(2) ELCD (801OA, 8140)(3) FID (8015A, 8040A, 8100)(4) PID (8020)
d. GC/MS:(1) VOA (8240A, 8260)(2) BNA (8250, 8270A)
e. HPLC:(1) PAH (8310)(2) Explosives (draft 8330)
f. IC: Common Anions (300s)g. IR: TRPH (418.1)h. UV/VIS: Cyanide (9010A, 9012)i. Autoanalyzers
4. Backup Instrumentation and Preventive Maintenance
J-5
EM 200-1-11 Jul 94
CHART J-3 Sample Receipt, Storage, and Preservation
1. SOPs
2. Sample Receipta. Cooler receipt checklistb. Ventilation hoodc. External chain-of-custodyd. Internal chain-of-custodye. Unambiguous sample numberf. Documentation of problems and resolutionsg. Coordination with the primary contractor and the USACE
3. Sample Storagea. Temperature controlled (4±2°C; thermometer in liquid.)b. Security (Locked storage.)c. Segregation for volatiles and standards
4. Sample Preservationa. Cold storageb. pH preservations (Check and adjust.)
(1) pH<2: Ammonia, COD, hardness, Kjedahl and organicnitrogen, metals, nitrate-nitrite, oil & grease,organic carbon, total phosphorus, TOX, radiologicaltests, gross alpha and beta, and total radium.
(2) pH< 4: Phenolics.(3) pH> 9: Sulfide.(4) pH ≥ 12: Cyanide.
5. Scheduling and Tracking (Sample holding times and clientrequested suspense dates.)
J-6
EM 200-1-11 Jul 94
CHART J-4 Sample Preparation
1.
2.
3.
4.
5.
6.
SOPs
Chemicals and Reagents:a. Reagent-grade chemicals shall meet the current Committee
on Analytical Reagents of the ACS specifications orbetter and with minimum purity >90%.
b. All chemicals and reagents shall be labelled and signedwith the date of receipt or preparation.
c. All reference materials and measurements shall betraceable to NIST.
d. All acids shall be reagent grade or better, excepthigh-purity grade or equivalent for ICP work.
e. All solvent shall be chromatographic grade or better.f. All reagent documentation shall indicate:
(1) Solvent(2) Concentration(3) Date(4) Preparer’s name(5) Expiration date
Definition of Batch: Samples of ≤ 20 with similar matrixprepared and analyzed with same technique and reagents atsame time or time sequence. Each batch should have acomplete set of method required laboratory QC samples.
Matrix Types:a. Surface water b. Groundwater c. Wastewaterd. Soil e. Sediment f. Sludgeg. Incineration ash h. TCLP extract i. Leachatej. Oil k. Product m. Wasten. Other (Plant, biological, etc.)
Field QC Samples (Blind to analysts.)a. Trip blanksb. Rinsate blanksc. Field duplicates
Laboratory QC Samples (5% per batch.)a. Method blanksb. Matrix duplicatesc. Matrix spikesd. Matrix spike duplicatese. Lab control samplesf. Any other method specific QC samples
J-7
EM 200-1-11 Jul 94
CHART J-5 Sample Analysis
1.
2.
3.
4.
5.
6.
SOPs
Method Validationa. New method or instrument
(1) Accuracy(2) Precision(3) Detection limits(4) Linear calibration ranges
b. Modified method or instrument(1) Accuracy(2) Precision(3) Detection limits(4) Linear calibration ranges
Instrument Calibration
General QA/QCa. System performance auditb. Analyst’s performance auditc. Blind QA samplesd. Documentation
Method Specific Laboratory QC Samplesa. Method blanksb. Matrix duplicatesc. Matrix spikesd. Matrix spike duplicatese. Laboratory control samples (LCS)f. Other method specific QC samples (ICS, CCS, etc.)
Method References: (Promulgated.)a. USEPA SW-846, Revision 0, September 1986:
7000s, 7040/7041, 8020, 8080, 9060.b. USEPA SW-846, Revision 1, July 1992:
6010A, 8010A, 8150A, 8240A, 8270A, 9010A.c. USEPA-600/44-79-020, March 1983:
418.1.
J-8
EM 200-1-11 Jul 94
CHART J-5.1 Halogenated Volatile Organic Compounds by GC (8010A)
1.2.3.4.5.
6.
7.
8.
9.
Number of Analytes: 34Preservation/Storage Conditions: Na2S2O3 if chlorine present (aqueous); stored at 4°C.Holding Time: 14 days.Amount for Extraction: 5 mL (aqueous) and 5 grams (solid) by 5030A.Method of Validation:
(1) Extract and analyze four replicates of QC check standard. Compare results with Table 3.(2) MDL (Table 1) shall be empirically established and verified semiannually for each matrix.(3) Linear calibration range shall be established and verified semiannually.
Standards:(1) Standard Solution Expiration: Stock standards (except gases): six months; stock gas standards:
two months; calibration standards: 24 hours if no headspace(2) Internal Standards: Optional; no internal standards specified.(3) Surrogate Standards: Add surrogates (bromochloromethane, 2-bromo-l-chloropropane, and
1,4-dichlorobutane) to encompass range of temperature program. Results within lab establishedcontrol limits.
(4) QC Check Standards: If MS/MSD results fall outside control limits, a QC check standard must beanalyzed and fall within those ranges designated in Table 3.
Calibration:(1) Initial Calibration: Minimum of five levels with the lowest near but above MDL; linear
correlation coefficient ≥ 0.995. If %RSD<20, linearity is assumed and average RF may be used.(2) Continuing Calibration: Mid-level calibration standard run every ten samples and at the end of
the analytical run. If not within ±15% of predicted response, recalibrate.Analysis: An example of run log is listed below.
(1) Initial Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ± 15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ± 15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)
(2) Middle Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ± 15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ± 15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)
(3) Final Batch: (≤ 20 samples of similar matrix.)- BFB- CCV (≤ ± 15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ± 15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)- CCV (≤ ± 15%)
Other Criteria:(1) When doubt exists in compound identification, second column or GC/MS confirmation should be used.(2) Establish retention time windows at ± 3σ with three injections throughout 72 hours.(3) Establish %R for surrogates, LCS, BS, and MS, and RPD for BD, MD, and MSD.
J-9
EM 200-1-11 Jul 94
CHART J-5.2 Aromatic Volatile Organic Compounds by GC (8020)
1. Number of Analytes: 82. Preservation/Storage Conditions: pH<2 with HCl, H2S04, or NaHS04 (aqueous). Na2S203 if chlorine
present (aqueous); stored at 4°C.3. Holding Time: 14 days.4. Amount for Extraction: 5 mL (aqueous) and 5 grams (solid) by 5030A.5. Method of Validation:
(1) Extract and analyze four replicates of QC check standard. Compare results with Table 3.(2) MDL (Table 1) shall be empirically established and verified semiannually for each matrix.(3) Linear calibration range shall be established and verified semiannually.
6. Standards:(1) Standard Solution Expiration: Stock standards: six months; calibration standards: 24 hours if no
headspace(2) Internal Standards: Optional. If used, α,α,α -trifluorotoluene is recommended.(3) Surrogate Standards: Add surrogates (bromochlorobenzene, bromofluorobenzene, fluorobenzene,
difluorobenzene, and α,α,α -trifluorotoluene are recommended) to encompass range of temperatureprogram. Results within lab established control limits.
(4) QC Check Standards: If MS/MSD results fall outside control limits, a QC check standard must beanalyzed and fall within those ranges designated in Table 3.
7. Calibration:(1) Initial Calibration: Minimum of five levels with the lowest near but above MDL; linear
correlation coefficient ≥ O.995. If %RSD<20, linearity is assumed and average RF may be used.(2) Continuing Calibration: Mid-level calibration standard run every ten samples and at the end of
the analytical run. If not within ±15% of predicted response, recalibrate.8. Analysis: An example of run log is listed below.
(1) Initial Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ±l5%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)
(2) Middle Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ±15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)
(3) Final Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ±15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)- CCV (≤ ±15%)
9. Other Criteria:(1) When doubt exists in compound identification, second column or GC/MS confirmation should be used.(2) Establish retention time windows at ±3σ with three injections throughout 72 hours.(3) Establish %R for surrogates, LCS, BS, and MS, and RPD for BD, MD, and MSD.
J-10
EM 200-1-11 Jul 94
CHART J-5.3 Organochlorine Pesticides and PCBS by GC (8080)
1.2.3.4.
5.
6.
7.
8.
9.
Number of Analytes: 26Preservation/Storage Conditions: Na2S2O3 if chlorine present (aqueous); stored at 4°C.Holding Time: Extraction: seven days (aqueous) and 14 days (solid). Analysis: 40 days after extraction.Amount for Extraction: One liter (aqueous) by 351OA or 3520A. 30 grams (low level solid) or two grams(medium level solid) by 3540A or 3550.Method of Validation:
(1) Extract and analyze four replicates of QC check standard. Compare results with Table 3.(2) MDL (Table 1) shall be empirically established and verified semiannually for each matrix.(3) Linear calibration range shall be established and verified semiannually.
Standards:(1) Standard Solution Expiration: Stock standards: one year; calibration standards: six months.(2) Internal Standards: Optional; no internal standards specified.(3) Surrogate Standards: Two surrogates, decachlorobiphenyl (DCBP) and 2,4,5,6-tetrachloro-m-xylene
(TCMX). Results must fall within laboratory established limits.(4) QC Check Standards: If MS/MSD results fall outside control limits, a QC check standard must be
analyzed and fall within those ranges designated in Table 3.Calibration:
(1) Initial Calibration: Minimum of five levels with the lowest near but above MDL; linearcorrelation coefficient ≥ 0.995. If %RSD<20, linearity is assumed and average RF may be used.
(2) Continuing Calibration: Mid-level calibration standard run every ten samples and at the end ofthe analytical run. If not within ±15% of predicted response, recalibrate.
Analysis: An example of run log is listed below.(1) Initial Batch: (≤ 20 samples of similar matrix.)
GC Column deactivation (GC not used for one day or more; primed at 20x mid-level standard.)Instrument blankDDT and Endrin degradation check standard (Breakdown <20%.)CCV (≤ ±15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)- MSD (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)
(2) Middle Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ±15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)- MSD (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)
(3) Final Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ±15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)- MSD (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)- CCV (≤ ±15 %)
Other Criteria:(1) Check for DDT and Endrin degradation. Breakdown must be <20% for packed column GC or <15% for
capillary GC.(2) Second column confirmation is required for all hits. If compound concentration in the extract
>10 ng/mL, GC/MS confirmation could be used.(3) Establish retention time windows at ±3σ with three injections throughout 72 hours.(4) Establish %R for surrogates, LCS, BS, and MS, and RPD for BD, MD, and MSD.
J-11
EM 200-1-11 Jul 94
CHART J-5.4 Chlorinated Herbicides by GC (8150A)
2.3.4.5.
6.
7.
8.
9.
1. Number of Analytes: 10Preservation/Storage Conditions: Na2S2O3 if chlorine present (aqueous); stored at 4°C.Holding Time: Extraction: seven days (aqueous) and 14 days (solid). Analysis: 40 days after extraction.Amount for Extraction: One liter (aqueous) and 50 grams (solid) by 8150A.Method of Validation:(1) Extract and analyze four replicates of QC check standard. Compare results with Table 3.(2) MDL (Table 1) shall be empirically established and verified semiannually for each matrix.(3) Linear calibration range shall be established and verified semiannually.
Standards:(1) Standard Solution Expiration: Stock standards: one year;(2) Internal Standards:
calibration standards: six months.Optional; no internal standards specified.
(3) Surrogate Standards: One/two surrogates added to each sample (avoid use of deuterated analogs.)Results must fall within laboratory established limits.
(4) QC Check Standards: If MS/MSD results fall outside control limits, a QC check standard must beanalyzed and fall within those ranges designated in Table 3.
Calibration:(1) Initial Calibration: Minimum of five levels with the lowest near but above MDL; linear
correlation coefficient ≥ 0.995. If %RSD<20, linearity is assumed and average RF may be used.(2) Continuing Calibration: Mid-level calibration standard run every ten samples and at the end of
the analytical run. If not within ±15% of predicted response, recalibrate.Analysis: An example of run log is listed below.(1) Initial Batch: (≤ 20 samples of similar matrix.)
- CCV (≤ ±15%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)
(2) Middle Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ±15 %)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)
(3) Final Batch: (≤ 20 samples of similar matrix.)- CCV (≤ ±l5%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 3 or manufacturer/lab established limits.)- Samples (≤ 10)- CCV (≤ ±15%)- Samples (≤ 7)- MD (Compare results with lab established limits.)- MS (Compare results with lab established limits.)- MSD (Compare results with lab established limits.)- CCV (≤ ±15%)
Other Criteria:(1) When doubt exists in compound identification, GC/MS or second column confirmation should be used.(2) Establish retention time windows at ±3σ with three injections throughout 72 hours.(3) Establish %R for surrogates, LCS, BS, and MS, and RPD for BD, MD, and MSD.
J-12
CHART J-5.5 Volatile Organic Compounds by GC/MS (8240A)
1.2.
3.4.5.
6.
7.
8.
9.
Number of Analytes: 74 (Minimum: 35 in Table 2 of 8240, Rev. 0, 1986
EM 200-1-11 Jul 94
Preservation/Storage Conditions: pH<2 with HC1, H2S04, or NaHS04 (aqueous). Na2S203 if chlorinepresent (aqueous); stored at 4°C.
Holding Time: 14 days.Amount for Extraction: 5 mL (aqueous) and 5 grams (solid) by 5030A.Method of Validation:
(1) Extract and analyze four replicates of QC check standard. Compare results with Table 6.(2) EQLs (Table 2) shall be empirically established and verified semiannually for each matrix.(3) Linear calibration range shall be established and verified semiannually.
Standards:(1) Standard Solution Expiration: Stock standards (except gases): six months; stock gas standards:
two months; calibration standards: daily.(2) Internal Standards: Bromochloromethane, l,4-difluorobenzene, and chlorobenzene-d5. RT must be
within ±30 seconds from last calibration; area must be -50 to +100%.(3) Surrogate Standards: 4-Bromofluorobenzene, 1,2-dichloroethane-d4, and toluene-d8. Recover limits
in Table 8.(4) QC Check Standards: If MS/MSD results fall outside control limits, a QC check standard must be
analyzed and fall within those ranges designated in Table 6.Calibration:
(1) GC/MS Tuning: 50 ng of 4-bromofluorobenzene (BFB) which meets the criteria given in Table 3.(2) Initial Calibration: Minimum of five levels with the lowest near but above MDL. %RSD should be
<30% for each CCC (1,1-dichloroethene, chloroform, 1,2-dichloropropane, toluene, ethylbenzene,and vinyl chloride). RF>O.30 for SPCCs (chloromethane, l,l-dichloroethane, chlorobenzene, and1,1,2,2-tetrachloro-ethane) except 0.25 for bromoform.
(3) Continuing Calibration: Mid-level calibration standard run every 12 hours. RF>O.30 for SPCCsexcept 0.25 for bromoform. RF for each CCC must be <25% difference from initial calibration.
Analysis: An example of run log is listed below.(1) Initial Batch: (≤ 20 samples of similar matrix.)
- BFB tuning to meet criteria in Table 3- CCV (Mid-concentration calibration standard every 12 hours.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 6 or manufacturer/lab established limits.)- Samples- BFB (Table 3; every 12 hours.)- CCV (Mid-concentration calibration standard every 12 hours.)- MD (Compare results with lab established limits.)- MS (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)- MSD (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)
(2) Middle or Final Batch: (≤ 20 samples of similar matrix.)- BFB (Table 3; every 12 hours.)- CCV (Mid-concentration calibration standard every 12 hours.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 6 or manufacturer/lab established limits.)- Samples- BFB (Table 3; every 12 hours.)- CCV (Mid-concentration calibration standard every 12 hours.)- MD (Compare results with lab established limits.)- MS (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)- MSD (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)
Other Criteria:(1) Compound ID: All ions >10% intensity must be ±20% of standard; ±0.06 RRT units of standard RRT.(2) Establish %R for surrogates, LCS, BS, and MS, and RPD for BD, MD, and MSD.(3) The most recent version of the EPA/NIST Mass Spectral Library or equivalent should be available.
J-13
EM 200-1-11 Jul 94
CHART J-5.6 Semivolatile Organic Compounds by GC/MS (8270A)
1.2.3.4.
5.
6.
7.
8.
9.
Nunber of Analytes: 233 (Minimun: 65 in Table 2, 8270, Rev. O, 1986.)Preservation/Storage Conditions: Na2 S2 O3 if chlorine present (aqueous); stored at 4°C.Holding Time: Extraction: seven days (aqueous) and 14 days (solid). Analysis: 40 days after extraction.Amount for Extraction: One liter (aqueous) by 351OA or 3520A at pH>11 and pH<2. 30 grams (low levelsolid) or two grams (medium level solid) by 3540A or 3550.Method of Validation:
(1) Extract and analyze four replicates of QC check standard. Compare results with Table 6.(2) EQLs (Table 2) shall be empirically established and verified semiannually for each matrix.(3) Linear calibration range shall be established and verified semiannually.
Standards:(1) Standard Solution Expiration: Stock standards: one year; calibration standards: one year;
daily continuing calibration standards: one week.(2) Internal Standards: 1,4-Dichlorobenzene-d4, naphthalene-d8,
iacenaphthene-d10’ crysene-d12, and
perylene-d 12. RT must be within ±30 seconds from last cal bration; area must be -50 to Standards: Nitrobenzene-d5,(3) Surrogate 2-fluorobiphenyl, p-terphenyl-d14, phenol-d5,2-fluorophenol, and 2,4,6-tribromophenol. Recover limits in Table 8.
(4) QC Check Standards: If MS/MSD results fall outside control limits, a QC check standard must beanalyzed and fall within those ranges designated in Table 6.
Calibration:(1) GC/MS Tuning: 50 ng of decafluorotriphenylphosphine (DFTPP) which meets the criteria given in
Table 3. The standard should also contain 4,4’-DDT, pentachlorophenol, and benzidine to verifyinjection port inertness and GC column performance. (Degradation of DDT <20%. No peak tailing.)
(2) Initial Calibration: Minimum of five levels with the lowest near but above MDL. %RSD should be<30% for each compound and must be <30% for each CCC (Table 4). Retention time for each compoundagrees within 0.06 relative retention time unit. RF>O.05 for SPCCs (N-nitroso-di-n-propylamine,hexachlorocyclopentadiene, 2,4-dinitro-phenol, and 4-nitrophenol.)
(3) Continuing Calibration: Mid-level calibration standard run every 12 hours. RF>O.05 for SPCCs.RF for each CCC must be <30% difference from initial calibration.
Analysis: An example of run log is listed below.(1) Initial Batch: ( < 20 samples of similar matrix.)
DFTPP tuning to meet-criteria in Table 3CCV (Mid-concentration calibration standard.)MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)LCS (Table 6 or manufacturer/lab established limits.)SamplesDFTPP (Table 3; every 12 hours.)CCV (Mid-concentration calibration standard every 12 hours.)MD (Compare results with lab established limits.)MS (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)MSD (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)
(2) Middle or Final Batch: ( < 20 samples of similar matrix.)- DFTPP (Table 3; every 12 hours.)- CCV (Mid-concentration calibration standard every 12 hours.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Table 6 or manufacturer/lab established limits.)- Samples- DFTPP (Table 3; every 12 hours.)- CCV (Mid-concentration calibration standard every 12 hours.)- MD (Compare results with lab established limits.)- MS (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)- MSD (Compare results with Tables ONE-39, 40 of SW-846, Rev. O or lab established limits.)
Other Criteria:(1) Compound ID: All ions >1O% intensity must be ±20% of standard; ±O.06 RRT units of standard RRT.(2) Establish %R for surrogates, LCS, BS, and MS, and RPD for BD, MD, and MSD.(3) The most recent Version of the EPA/NIST Mass Spectral Library or equivalent should be available.
J-14
EM 200-1-11 Jul 94
CHART J-5.7 Metals by ICP (6010A)
1.2.3.4.
5.
6.
7.
8.
Number of Analytes: 26 metalsPreservation/Storage Conditions: pH<2 with HN03; stored at 4°C (solid).Holding Time: Six months.Amount for Digestion: 100 mL (aqueous) by 3005A (aqueous total recoverable or dissolved metals), 3010A(aqueous total metals), 3040 (dissolution procedures); and 1.00-2.00 grams (solid) by 3050A (solid totalmetals).Method of Validation: IDL (listed in Table 1 of Method 6010A) shall be empirically established andverified for each matrix.Standards:
(1) Standard Solution Expiration: Stock standards: specified by manufacturer; must be monitoredweekly; calibration standards: prepare fresh at time of use.
Calibration:(1) Initial Calibration: Per instrument manufacturer’s specifications (should consist of a daily
minimum of three levels plus a calibration blank.) Before beginning the sample run, reanalyzethe highest mixed calibration standard. Concentration values should be ≤ ±5% of the true valuesor the established control limits, whichever is lower.
(2) Continuing Calibration: A mid-level, second source CCV run every ten samples and at the end ofthe analytical run; %R=9O-11O.
(3) Interference check solution (ICS): Used to spike sample with the element of interest atconcentrations of 10x IDL. Run at the beginning and the end of an analytical run or twice duringevery 8-hour work shift, whichever is more frequent.
Analysis: An example of run log is listed below.(1) Initial Batch: (≤ 20 samples of similar matrix.)
- Minimum of three level calibration plus a calibration blank- Highest mixed standard (<±5% of true value)- ICS (<±20% of true value)- LCS (Based on control chart or <±20% prior to establishment of control chart.)- Samples (≤ 10)- Calibration blank ( <3σ of the mean blank value.)- CCV (<±l0%)- Samples (≤ 6)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- MD (RPD<20)- MS (%R=80-120)- MSD (RPD<20, %R=80-120.)
(2) Middle Batch: (≤ 20 samples of similar matrix.)- Calibration blank (<3σ of the mean blank value.)- CCV (<±1O%)- LCS (Based on control chart or <±20% prior to establishment of control chart.)- Samples (≤ 10)- Calibration blank (<3σ of the mean blank value.)- CCV (<±l0%)- Samples (≤ 6)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- MD (RPD<20)- MS (%R=80-120)- MSD (RPD<20, %R=80-120.)
(3) Final Batch: (20 samples of similar matrix.)- Calibration blank (<3σ of the mean blank value.)- CCV (<±1O%)- LCS (Based on control chart or <±20% prior to establishment of control chart.)- Samples (≤ 10)- Calibration blank (<3σ of the mean blank value.)- CCV (<±1O%)- ICS (Additional ICS, if more than eight hours.)- Samples (≤ 6)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- MD (RPD<20)- MS (%R=80-120)- MSD (RPD<20, %R=80-120)- Calibration blank (<3σ of the mean blank value.)- ICS (<±20%)- CCV (<±10%)
J-15
EM 200-1-11 Jul 94
CHART J-5.7 Metals by ICP (6010A) (continued)
9. Other Criteria:(1) Test for matrix interference with each matrix using a 5-fold serial dilution test (if >50x IDL),
Percent difference <±1O%; or a (10-1OOx IDL) post-digestion spike test, %R=75-125.(2) Use MSA to compensate for matrix interferences.(3) Use multiple exposures for both calibration and sample analysis.(4) Establish %R for LCS, BS, and MS, and RPD for BD, MD, and MSD.
J-16
EM 200-1-11 Jul 94
CHART J-5.8 Metals by Flame and Graphite Furnace AA (7000s)
1.2.3.4.
5.
6.
7.
8.
9.
Number of Analytes: 27 metalsPreservation/Storage Conditions: pH<2 with HN03; stored at 4°C (solid).Holding Time: Six months.Amount for Digestion: 100 mL (aqueous) by 3005A (aqueous total recoverable metals or dissolved metalsby FLAA), 301OA (aqueous total metals by FLAA), 3020 (aqueous total metals by GFAA, except As by 7060and Se by 7740), 3040 (dissolution procedures for AA); and 1.00-2.00 grams (solid) by 3050A (solid totalmetals by FLAA and GFAA).Method of Validation: MDL (listed in Table 1 of Method 7000A) shall be empirically established andverified semiannually for each matrix.Standards:
(1) Standard Solution Expiration: Stock standards: specified by manufacturer; must be monitoredweekly; calibration standards: prepare fresh at time of use.
Calibration:(1) Initial Calibration: Minimum of a daily three level calibration plus a calibration blank. Verify
with a calibration blank and a mid-level ICV from a second source; %R=90-110.(2) Continuing Calibration: A mid-level, second source CCV or QC check standard run every ten samples
and at the end of the analytical run; %R=80-120.Analysis: An example of run log is listed below.
(1) Initial Batch: (≤ 20 samples of similar matrix.)- Minimun of a three level calibration plus a calibration blank- Calibration blank (<IDL)- ICV (<±1O%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on control chart or <±20% prior to establishment of control chart.)- Samples (≤ 10)- CCV (<±20%)- Samples (≤ 7)- MD (RPD<20)- MS (%R=75-125)- MSD (RPD<20, %R=75-125.)
(2) Middle Batch: (≤ 20 samples of similar matrix.)- CCV (<±20%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on control chart or <±20% prior to establishment of control chart.)- Samples (≤ 10)- CCV (<±20%)- Samples (≤ 7)- MD (RPD<20)- MS (%R=75-125)- MSD (RPD<20, %R=75-125.)
(3) Final Batch: (≤ 20 samples of similar matrix.)CCV (<±20%)MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)LCS (Based on control chart or <±20% prior to establishment of control chart.)Samples (≤ 10)CCV (<±20%)Samples (≤ 7)MD (RPD<20)MS (%R=75-125)MSD (RPD<20, %R=75-125.)MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)CCV (<±20%)
Other Criteria:(1)
(2)(3)
(4)
Test for matrix interference with each batch using a 5-fold (1+4) dilution test (if sample >25xMDL); percent difference <10%. If dilution test fails or all samples in the batch <1Ox MDL,perform a (2-5x sample or 20x MDL) spike recovery test; %R=85-115.Use MSA to compensate for multiplicative interferences, i.e., matrix or physical interferences.Use Zeeman background correction for additive interferences, i.e., nonspecific absorption andscattering.Establish %R for LCS, BS, and MS, and RPD for BD, MD, and MSD.
J-17
EM 200-1-11 Jul 94
CHART J-5.9 Mercury by Cold Vapor AA (7470/7471)
1.2.3.4.5.
6.
7.
8.
9.
Number of Analytes: Mercury (Hg)Preservation/Storage Conditions: pH<2 with HN03; stored at 4°C (solid).Holding Time: 28 days.Amount for Digestion: 100 mL (aqueous) and 0.2 grams (solid) by 7470 (aqueous) and 7471 (solid).Method of Validation: MDL (0.0002 mg/L listed in Section 1.0) shall be empirically established andverified semiannually for each matrix.Standards:
(1) Standard Solution Expiration: Stock standards: specified by manufacturer; must be monitoredweekly; calibration standards: prepare fresh at time of use.
Calibration:(1) Initial Calibration: Minimum of a daily five level calibration plus a calibration blank.
Verify with a calibration blank and a mid-level ICV from a second source; %R=90-110.(2) Continuing Calibration: A mid-level, second source CCV or QC check standard run every ten samples
and at the end of the analytical run; %R=80-120.Analysis: An example of run log is listed below.
(1) Initial Batch: ( ≤ 20 samples of similar matrix.)Minimum of a five level calibration plus a calibration blankCalibration blank (<IDL)ICV (<±1O%)MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)LCS (Based on control chart or <±20% prior to establishment of control chart.)Samples ( ≤ 10)CCV (<±20%)Samples ( ≤ 7)MD (RPD<20)MS (%R=75-125)MSD (RPD<20, %R=75-125.)
(2) Middle Batch: ( ≤ 20 samples of similar matrix.)- CCV (<±20%)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on control chart or <±20% prior to establishment of control chart.)- Samples ( ≤ 10)- CCV (<±20%)- SampLes ( ≤ 7)- MD (RPD<20)- MS (%R=75-125)- MSD (RPD<20, %R=75-125.)
(3) Final Batch: ( ≤ 20 samples of similar matrix.)CCV (<±20%)MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)LCS (Based on control chart or <±20% prior to establishment of control chart.)Samples ( ≤ 10)CCV (<±20%)Samples ( ≤ 7)MD (RPD<20)MS (%R=75-125)MSD (RPDx20, %R=75-125.)MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)CCV (<±20%)
Other Criteria:(1) Test for matrix interference with each batch using a 5-fold (1+4) dilution test (if >25x MDL);
percent difference <10%. If dilution test fails or all samples in the batch <1OX MDL, perform a(2-5x sample or 20x MDL) spike recovery test; %R=85-115.
(2) Use MSA to compensate for matrix interferences.(3) Establish %R for LCS, BS, and MS, and RPD for BD, MD, and MSD.
J-18
CHART J-5.10 Total and
1.2.
3.4.
5.
6.7.
8.
EM 200-1-11 Jul 94
Amenable Cyanide by Calorimetry (9010A)
amenable to chlorinationNumber of Analytes: Total CN and CNPreservation/Storage Conditions: pH ≥ 12 with NaOH. NaAsO2 or ascorbic acid if oxidizing agents present;
stored at 4°C.Holding Time: 14 days.Amount for Preparation: 500 mL (1,000 mL if both total and amenable CN) (aqueous) and 1-5 grams (2-10grams if both total and amenable CN) (solid) by distillation procedures in 9010.Method of Validation: MDL (0.02 mg/L listed in Section 1.0) shall be empirically established andverified semiannually for each matrix.Standards: Stock standards expiration: not specified; calibration standards expiration: daily.Calibration:
(1) Samples contain no sulfides:(a) Initial Calibration: Daily minimum of six levels and a calibration blank, plus a minimum of
two of the above standards (high and low) distilled. The distilled ones should be <±lO% ofundistilled ones.
(b) Continuing Calibration: Mid-level calibration standard run every batch and should be <±15%of expected value.
(2) Samples contain sulfides:(a) Initial calibration: Daily six standards and calibration blank. All standards are distilled
as the samples using the method of standard additions.(b) Continuing Calibration: Mid-level calibration standard run every batch and should be <±15%
of expected value.Analysis: An example of run log is listed below.
(1) Samples contain no sulfides:(a) Initial Batch: ( ≤ 20 samples of similar matrix.)
- Minimum of six level plus blank calibration- Check standards (Second source, middle level, no distillation, <±15%.)- MB (Distilled; <MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Distilled; compare results with manufacturer/lab established limits.)- Samples (Distilled.)- MS (Distilled; compare results with lab established limits.)- MD (Distilled, <±20%)
(b) Middle Batch: ( ≤ 20 samples of similar matrix.)- Check standards (Second source, middle level, no distillation, <±15%.)- MB (Distilled; <MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (distilled; compare results with manufacturer/lab established limits.)- Samples (Distilled.)- MS (Distilled; compare results with lab established limits.)- MD (Distilled, <±20%)
(c) Final Batch: ( ≤ 20 samples of similar matrix.)- Check standards (Second source, middle level, no distillation, <±15%.)- MB (Distilled; <MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Distilled; compare results with manufacturer/lab established limits.)- Samples (Distilled.)- MS (Distilled; compare results with lab established limits.)- MD (Distilled, <±20%)- Check standards (Second source, middle level, no distillation, <±15%.)
(2) Samples contain sulfides:(a) Initial Batch: ( ≤ 20 samples of similar matrix.)
- Minimum of six level plus blank calibration using MSD- Check standards (Second source, middle level, no distillation, <±15%.)- MB (Distilled; <MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Distilled; compare results with manufacturer/lab established limits.)- Samples (Distilled.)- MS (Distilled; compare results with lab established limits.)- MD (Distilled, <±20%)
(b) Middle Batch: ( ≤ 20 samples of similar matrix.)- Check standards (Second source, middle level, no distillation, <±15%.)- MB (Distilled; <MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Distilled; compare results with manufacturer/lab established limits.)- Samples (Distilled.)- MS (Distilled; compare results with lab established limits.)- MD (Distilled, <±20%)
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CHART J-5.10 Total and Amenable Cyanide by Calorimetry (9010A)(continued)
(c) Final Batch: ( ≤ 20 samples of similar matrix.)- Check standards (Second source, middle level, no distillation, <±15%.)- MB (Distilled; <MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Distilled; compare results with manufacturer/lab established limits.)- Samples (Distilled.)- MS (Distilled; compare results with lab established limits.)- MD (Distilled, <±20%)- Check standards (Second source, middle level, no distillation, <±15%.)
9. Other Criteria:(1) Use MSA to compensate for matrix interferences.(2) Establish %R for check standards, LCS, BS, and MS, and RPD for BD and MD.
J-20
EM 200-1-11 Jul 94
CHART J-5.11 Total Organic Carbon by a Carbonaceous Analyzer(9060)
1.2.
3.4.5.
6.7.
8.
9.
Number of Analytes: No specificPreservation/Storage Conditions:at 4°C.
compounds.pH<2 with HCL or H2SO4. Protect from light and atmospheric O2; stored
Holding Time: 28 days.Amount for Extraction: 50 mL.Method of Validation: MDL (1 mg/L listed in Section 1.0) shall be empirically established and verifiedsemiannually for each matrix.Standards: Standard Solution Expiration: Not specified.Calibration:
(1) Initial Calibration: Per instrument manufacturer’s specifications, correlation coefficient≥ 0 .995.
(2) Continuing calibration: Percent difference <10% of initial calibration.Analysis: An example of run log is listed below.
(1) Initial Batch: ( ≤ 20 samples of similar matrix.)Initial calibration CCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)LCS (Based on lab established control limits and should be <10% difference.)SamplesMS (Based on lab established control limits.)MD (Based on lab established control limits.)
(2) Middle Batch: ( ≤ 20 samples of similar matrix.)- CCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on lab established control limits and should be <10% difference.)- Samples- MS (Based on lab established control limits.)- MD (Based on lab established control limits.)
(3) Final Batch: ( ≤ 20 samples of similar matrix.)- CCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on lab established control limits and should be <10% difference.)- Samples- MS (Based on lab established control limits.)- MD (Based on lab established control limits.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- CCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)
Other Criteria: Establish %R for LCS, BS, and MS, and RPD for BD and MD.
J-21
EM 200-1-11 Jul 94
CHART J-5.12 Total Recoverable Petroleum Hydrocarbons by IR(418.1)
1.2.3.4.
5.
6.
7.
8.
9.
Nunber of Analytes: Non-polar petroleum hydrocarbons. No specific compounds.Preservation/Storage Conditions: pH<2 with HCL (aqueous); stored at [email protected] Time: 28 days.Amount for Extraction: 1,000 mL (aqueous) by 418.1 and 20 grams (solid) by 9071 steps 7.1 thru 7.11(Soxhlet extraction, 3540A.)Method of Validation: MDL (1 mg/L listed in Section 1.0) shall be empirically established and verifiedannually for each matrix.Standards:
(1) Reference oil: Mixture of 15.0 mL n-hexadecane, 15.0 mL isooctane, and 10.0 mL chlorobenzene.(2) Standard Solution Expiration: Stock Standards: six months; working standards: one week.
Calibration:(1) Initial Calibration: Daily minimum of four levels plus a calibration blank; correlation
coefficient >0.995.(2) Continuing calibration: Percent difference <10% of initial calibration.
Analysis: An example of run log is listed below.(1) Initial Batch: ( ≤ 20 samples of similar matrix.)
- Initial calibrationCCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)
- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on lab established control limits and should be <10% difference.)- Samples- MS (Based on lab established limits.)- MD (Based on lab established limits.)
(2) Middle Batch: ( ≤ 20 samples of similar matrix.)- CCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on lab established control limits and should be <10% difference.)- Samples- MS (Based on lab established limits.)- MD (Based on lab established limits.)
(3) Final Batch: ( ≤ 20 samples of similar matrix.)- CCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- LCS (Based on lab established control limits and should be <10% difference.)- Samples- MS (Based on lab established limits.)- MD (Based on lab established limits.)- MB (<MDL, <5% of regulatory limits, or <5% of measured sample concentration.)- CCV (Mid-level; independently prepared; percent difference <10% of initial calibration.)
Other Criteria:(1) Acidify solid samples to pH=2 with HCL.(2) Use MgSO6 •H2O for solid samples.(3) Establish %R for LCS, BS, and MS, and RPD for BD and MD.
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CHART J-6 Data Reduction, Validation, and Reporting
1.
2.
3.
4.
5.
6.
SOPs
Computerized Data Reduction (Manually checked.)
Multiple Levels of Data Reviewa. Analyst or peer (100%)b. Supervisor (≥ 10%)c. QA Officer (≥ 10%)d. Lab Manager/Director (≥ 10%)
Data Qualifier Flags
Report Generation and Archivesa. Prenumbered, permanently bound notebooks.b. Corrections do not obliterate original data.c. Revised entry is signed or initialed and dated.d. Records are traceable, retrievable, legible, and
complete.e. All data and reports stored in a secured area for a
minimum of three years after final reports.
Corrective Actions and Documentation
J-23
EM 200-1-11 Jul 94
CHART J-7 Performance and System Audits
1.
2.
3.
4.
5.
SOPs
Designated Internal Auditor
Performance Audita. External QAb. Internal QA
(1) Initial evaluation of new analysts(2) Periodical audit of experienced analysts(3) Single blind PE samples(4) Double blind PE samples
c. Round robin testingd. Corrective actionse. Documentation
System Audita. Methodologies
(1) New method(2) Modified method(3) New instrument
b. Documentation
Control Charts: Established for each type of QC parameters,methodologies, and matrices; updated quarterly or when 20 newdata points are obtained.a. MBb. LCSc. MDd. MSe. MSDf. Surrogateg. Others
J-24
EM 200-1-11 Jul 94
CHART J-8 Laboratory Safety
1. Safety and Chemical Hygiene Plana. Safety meetingb. Safety inspectionc. Fire drill
2. Safety Equipmenta. Eyewash fountainb. Emergency showerc. Safety glasses and glovesd. Fire alarme. Fire Extinguisherf. Emergency lightg. Flammable material storageh. Hazardous area escapei. OSHA signsj. First aid kit
J-25
EM 200-1-11 Jul 94
CHART J-9 Waste Management
1.
2.
3.
4.
5.
6.
7.
8.
SOPsa. Waste stream analysisb. Waste segregation programc. Waste recycle program
Are residual USACE samples properly disposed of?
Does the lab have a Hazardous Waste Coordinator? (FederalRCRA Compliance Checklist, Appendix E, Section 7.)
Is the lab a conditionally exempted small quantitygenerator?a. The lab generates less than 100 kg per month of
hazardous waste or less than 1 kg per month of acutehazardous waste.
b. There is never more than 1,000 kg stored on site.c. Waste is sent to a TSDF, a facility that beneficially
reuse the waste, or a state permitted facility.
Are there records to substantiate the above claims?
Does the lab use a manifest when shipping hazardous waste?
Is aqueous waste disposed of into a sanitary sewer only ifit is neutralized and approved in writing by the sewerauthority?
Does the lab have the following documents for review?
c.
a.b.
d.e.f.g.h.i.j.k.l.m.n.o.p.q.
USEPA Notification Form 8700-12USEPA Identification NumberSmall Quantity Generator PermitRCRA Part A PermitRCRA Part B permitNPDES PermitManifestsWaste Analysis RecordsLand Ban RecordsException ReportsBiennial ReportsAnnual ReportsTraining and Personnel FilesContingency Plan/SPCC PlanAgreements with Local Emergency AuthoritiesUsed Oil RecordsHazardous Waste Management Plan
J-26
EM 200-1-11 Jul 94
CHART J-10 Government QA Functions (Applicable to government
1.
2.
3.
4.
QA labs only.)
Project Coordinationa. Designated coordinatorb. Review CDAPSc. DQO clarification
QA Activitiesa. Review/comment on project documentsb. Attend project meetingc. Perform site visitsd. Receive/review government QA samplese. Analyze government QA samplesf. Evaluate contractor QC datag. Prepare CQARSh. Other activities
CQAR Preparationa. Evaluation Parameters
(1) Precision (RPD based on MD, MSD, and BSD/LCSD if. .not enough samples.)
(2) Accuracy (Spike recovery based on LCS, MS/MSD,surrogates, and BS/BSD if not enough samples.)
(3) Representativeness (Holding time, MB, and MQ/MSD.)(4) Comparability (Analytical method, MDL, precision,
accuracy, and reporting unit.)(5) Completeness (COC, holding times, MDL, MB, LCS, MS,
MD/MSD, and surrogates.)(6) Others
b. Evaluation Criteriac. Agreement between contractor and government datad. Timely release (Within 20 working days after receipt of
contractor’s final QC data, but before the completion ofcontractor’s final engineering report.)
Contract Management (Appendix L)a. Prepare SOW for new contractb. Evaluate and select contractorc. Assess contractor’s data qualityd. Request corrective actionse. Suspend/terminate contract
J-27
EM 200-1-11 Jul 94
APPENDIX K
SAMPLE RECORD
OF
THE LABORATORY VALIDATION DATABASE
K-1
EM 200-1-11 Jul 94
Window 1LABORATORY FILE
VIEW SCREEN: 1/10UPDATING DATE: 02/25/92GENERAL
Record No: 222 ___Lab Name: ABC alytical Laboratory ____________POC Name: Joe Frank, Mary George ________________Address: 123 Main Street _____________
Suite 4 _______________City: Anytown _____________State: MD
Zip: 56789Phone: (111) 222-3333
FAX: (111) 222-4444
Window 1[ABC A.MD]
Project 1
Request Date:Project Name:
Type:A-E/Contractor:
USACE TM:Phone:
HTW Analyses:
LABORATORY FILE
FUNDS 1VIEW SCREEN: 2/10
06/04/91Elmwood County Landfill______________ State: NJSF ____ Phase: _____________ Contract No: DACW01-91-C-2345DEF, Inc. ______________________________ State: PA
John Dow _____________ Office: CEMRO-ED-EZ ___________(222) 333-4444 Sampling Date: 09/01/91
VOA, BNA, PCB, PEST, TAL METALS, TRPH, CN.__________________
PE Sample Cost:Funds Billed:
Funds Received:Funds Remarks:
$1100.00 Travel Cost: $275.00_ Labor Cost: $420.00_$300.00_ Date: 06/10/91$300.00_ Date: 07/01/91Billed ABC Lab $300 for non-project PEs.___
Figure K-1 Sample Record of the Laboratory ValidationDatabase
K-2
EM 200-1-11 Jul 94
Window 1[ABC A.MD]
Project 2
Request Date:Project Name:
Type:A-E/Contractor:
USACE TM:Phone:
HTW Analyses:
PE Sample Cost:Funds Billed:
Funds Received:Funds Remarks:
LABORATORY FILE
FUNDS 2VIEW SCREEN: 3/10
01/20/92Any AFB; Fire Fighting Training 2A_ State: AZACC _ Phase: PA/SI_______ Contract No:DACAO1-91-B-1234Any Environmental Services, Inc.______ State: CA
Paula Smith __________ Office: CEMRK-ED-EZ __________(333) 444-5555 Sampling Date: 04/15/92
RCRA METALS, TRPH, AVO, TPH (Mod. 8015)._________________________
$400.00_ Travel Cost: $0.00 Labor Cost: $0.00___$0.00___ Date: 00/00/00$0.00___ Date: 00/00/00
Window 1[ABC A.MD] LABORATORY FILE
LQMMVIEW SCREEN: 4/10
Request Date: 06/05/91 Receiving Date: 06/07/91Title: Laboratory Quality Management Manual_______________ Date: 05/01/91Reviewer: S. Smith_______ Date: 07/16/91
EPA-CLP VOA: _ Exp.Date: 00/00/00 Organics: x Exp.Date: 05/01/92Inorganics: x Exp.Date: 03/01/91 Dioxin: _ Exp.Date: 00/00/00
Dioxin: _ Radiochemical: x TCLP: xEPA Compendium Air: x AIHA/NIOSH Air: x
# of Chemist: 35_, GC: 10, GC/MS: 4_, ICP: 2, AA: 2_, IR: 2,UV/VIS: 2, HPLC: 2, Ion Chromatography: 2.
Remarks: TCLP w/ZHE; AIHA accredited for analysis of organic solvents and metals; EPA Compendium method T01 only._______________________
Figure K-1 Sample Record of the Laboratory ValidationDatabase (continued)
K-3
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Window 1[ABC A.MD]
VIEW SCREEN: 5/10
PARAMETER_ _ _ _ _ _ _ _ _ _
MATRIX_ _ _ _ _ _ _
METHOD_ _ _ _ _ _
12345678910
VOA__BNA__BNA__PEST_PCB__PCB__META3META3TRPH_TRPH_
H2O_H2O_SED_H2O_H2O_SED_H2O_SED_H2O_SOIL
8240__8270__8270__8080__8080__8080__SW846_SW846_418.l_418.1_
DATESUPPLIED--------06/10/9106/10/9107/15/9106/10/9106/10/9106/10/9106/10/9106/10/9106/10/9106/10/91
DATERECEIVED--------07/03/9107/03/9107/27/9107/15/9107/03/9107/03/9107/03/9107/15/9107/03/9107/03/91
PASS----GOODGOODPASSPASSGOODGOODGOODPASSGOODGOOD
12345678910
Window 1[ABC A.MD] LABORATORY FILE
VIEW SCREEN: 6/10PE SAMPLE 2
11121314151617181920
PARAMETER---------
HVO__AVO__HERB_TOC__CN___ANIONTPH__TPH______________
MATRIX------H2O_H2O_H2O_H2O_H2O_H2O_H2O_SOIL
DATEMETHOD SUPPLIED------ --------8010__ 00/00/008020__ 01/26/928150__ 07/15/919060__ 06/10/919010__ 06/10/91300s__ 06/10/918015M_ 01/26/928015M_ 01/26/92
_______ _______ 00/00/00_______ _______ 00/00/00
DATERECEIVED--------00/00/0002/19/9207/27/9107/03/9107/03/9107/03/9102/19/9202/25/9200/00/0000/00/00
PASS----________GOODFAILGOODGOODGOODGOODPASS
11121314151617181920
Figure K-1 Sample Record of the Laboratory ValidationDatabase (continued)
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Window 1[ABC A.MD] LABORATORY FILE
VIEW SCREEN: 7/10PE SAMPLE 3
PE Sample Remarks:
07/11/91: BNA/s: Several compunds were diluted out and not detected, PEST: Degradation products were too high and reported as false positives, METAL/s: Due to interelement interferences, Sb and Cd were high outside 3σ , Se was not detected. Failed to identify and quantify HERB. 07/15/91: Revised data for PEST and METAL/s acceptable; BNA/s and HERB notacceptable. Order 2nd BNA/s and HERB. 07/27/92: Pass 2nd BNA/s but fail 2ndHERB. 02/25/92: TPH/s low outside 2ó. Revised results acceptable.______
Window 1[ABC A.MD) LABORATORY FILE
VIEW SCREEN: 8/10INSPECTION
Inspector: S. Smith _______________________ Inspection Date: 07/25/91
Date Inspection Report To TM 1: 08/02/91 TM 2: 00/00/00 Lab: 08/02/91
Inspection Remarks:An excellent lab. No major deficiency except for failed HERB PE. Twoinor deficiencies: Needs segregated storage area for volatile standardsand improved documentation for standard preparation in metal section.__
Lab Responses: Response Date: 07/30/91Satisfactory. Will have segregated storage for volatile stadards and inproved logbook for metal standard.______________________________________
Figure K-1 Sample Record of the Laboratory ValidationDatabase (continued)
K-5
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Window 1[ABC A.MD]
VIEW SCREEN: 9/10
Reviewers: S. Smith, R. Anderson, C. Jones____ Date: 08/01/91Approval: x Not Approval:__ Conditional Approval: __
Review Remarks:Full approval for all parameters except for HERB. The lab has to waitfor six months before another try for HERB PE sample again. _________
Validation Expiration Date: 02/06/93
Window 1[ABC A.MD] LABORATORY FILE
PERFORMANCE EVALUATIONVIEW SCREEN: 10/10
Project A Name:Comments:
Responses:
Project B Name:Comments:
Responses:
Project C Name:Comments:
Responses:
Elm County Landfill_________________ Phase: RI/FS_______Missed the holding time for 10 VOA samples due to workload.
Date: 12/02/91Resample and reanalysis of all 10 samples at lab’s cost. The lab makes sure not happen again.________ Date: 12/12/91
Phase: _____________
Date: 00/00/00
Date: 00/00/00Phase: _______________
Date: 00/00/00
Date: 00/00/00
Figure K-1 Sample Record of the Laboratory ValidationDatabase (continued)
K-6
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APPENDIX L
SUPPLEMENTAL QUESTIONNAIRE
FOR
VALIDATION OF USACE DIVISION LABORATORIES
L-1
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SUPPLEMENTAL QUESTIONNAIRE FORVALIDATION OF USACE DIVISION LABORATORIES
This supplemental questionnaire is designed to elicitadditional information from USACE division laboratories thatserve as government Quality Assurance (QA) laboratories for theUSACE HTRW programs. Please make a concerted effort to furnishthe information as accurately and concisely as possible.
The preliminary questionnaire (Appendix E) is divided intoseven sections. This supplemental questionnaire adds the eighthsection to address the QA role of the government QA laboratories.
L-2
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SECTION 8. QUALITY ASSURANCE CONTROLS
1. Are procedures documented for performing all of the requiredQA activities per ER 1110-2-263? Yes [ ] No [ ] If yes,please attach copies of any available SOPs to thisquestionnaire.
[ ][ ][ ][ ]
[ ][ ][ ][ ]
2. What kinds of QA activities does your laboratory engage in?
Review and Comment on Project DocumentsAttend Project MeetingsPerform Site VisitsReceive/Review Incoming QA Samples
Analyze QA Samples In-HouseEvaluate Contractor’s DataWrite Chemical QA ReportsOther Activities (specify)
3. Summary of QA Staff. The primary duties of the QA staffshould be the performanceabove.
Name Title
of QA duties as
YrsEducation Exp
described in Item 2
QA & OtherDuties Performed
4. For the complete last fiscal year, how much chemistry work(in dollars) has your lab completed?
In-House Contracted Out
HTRW Testing HTRW TestingOther Testing Other Testing
L-3
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5. For the HTRW workanalyses that arelaboratory at theconducted at your
Method
824080108020
8250/8270808080808150
60107000s7000s7470/7471
418.18015M8100/83108330
9010/90129060300s1311
described above, please check the chemicalroutinely conducted in-house at yourpresent time and those that will belaboratory within the next couple years:
Parameters
Volatile OrganicsHalogenated Volatile OrganicsAromatic Volatile Organics
Semivolatile OrganicsOrganochlorine PesticidesPolychlorinated BiphenylsChlorinated Herbicides
Trace Metals (ICP)Trace Metals (Flame AA)Trace Metals (GFAA)Trace Metals (Hg by CVAA)
Petroleum HydrocarbonsPetroleum HydrocarbonsPolynuclear Aromatic HydrocarbonsNitroaromatics and Nitramines
CyanideTotal Organic CarbonCommon AnionsTCLP
Other analyses (Please list.)
RunNow
RunLater
6. For the above HTRW work, how much work (in dollars) isconventional analytical work (or QC(in dollars) is used to perform the
In-House
QC WorkQA Work
work) and how muchQA duties?
Contracted Out
work
QC WorkQA Work
L-4
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7. Does your laboratory write Chemical Quality AssuranceReports? Yes [ ] N o [ ] If yes, how many reports has yourlaboratory completed during last fiscal year? ________Please attach copies of some representative reports to thisquestionnaire.
8. Please complete CHART L-1 (Page L-6) for all HTRW projectsperformed by your laboratory during last fiscal year. Makeadditional copies of CHART L-1 if needed.
9. Please complete the following chart for all commercialanalytical chemistry laboratories that are under currentcontracts to support your laboratory. For each laboratory,please list the size and duration of the contract and thetype of work each laboratory is performing for you.
ContractLab Name/State Size/Duration Type of Work
L-5
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Please circleproject performed
CHART L-1
all applicable QA functions for each HTRWby your laboratory during last fiscal year.
Project Name and Phase
Type of QA Functions:
QA Activities
(1) Document Review, (2) Attend Project Meetings, (3) Perform
1
1
1
1
1
1
1
1
1
1
1
1
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6
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7
8
8
8
8
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8
8
8
8
8
8
8
8
8
Site Visits, (4) Receive/Review Incoming QA Samples, (5) Analyze
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
QA Samples In-House, (6) Evaluate Contractor’s Data, (7) WriteChemical QA Reports, (8) Other Activities as listed on Page L-3,(9) All of the above.
L-6
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APPENDIX M
LIST OF ABBREVIATIONS, ACRONYMS,
FORMULAS, SYMBOLS, NUMBERS, AND TERMS
M-1
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LIST OF ABBREVIATIONS, ACRONYMS,FORMULAS, SYMBOLS, NUMBERS, AND TERMS
The following list defines the abbreviations, acronyms,formulas, symbols, numbers, and terms used in this manual. Someof these entries are common throughout the environmental industryand government offices; many are unique to the U.S. Army Corps ofEngineers. They are listed here as an aid to the reader of thismanual.
Term
AARAA
ACCACSAFAgAlALKALANIONAPHAAPIARCSAsASTASTMAVO
AWWABaBDBFBBeBNA
BRACBSBSDCaCCCCCSCCVCdCDAPCEMRD
Definition
Atomic absorption spectrophotometerAsbestos Analyst RegistryAir Combat CommandAmerican Chemical SocietyAir ForceSilverAluminumAlkalinity (Methods 310s)Common anions (Methods 300.0/300s)American Public Health AssociationAmerican Petroleum InstituteAlternative Remedial Contracts StrategyArsenicAboveground storage tankAmerican Society for Testing and MaterialsAromatic volatile organic compounds(Method 8020)American Water Works AssociationBariumBlank duplicate4-BromofluorobenzeneBerylliumBase neutral, and acid extractable organiccompoundBase Realignment and ClosureBlank spikeBlank spike duplicateCalciumCalibration check compoundContinual calibration standardContinual calibration verificationCadmiumChemical Data Acquisition PlanCorps of Engineers, Missouri River Division
M-2
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Term
CFRCLPCMSCNCoCOCCODCORCQARCrCr (VI)CuCVAADalaponDCBPDDDDDTDERPDFTPPDOEDOTDQODROECDELCDEMEMSLEndrinENGEPEQLERERDEC
EXPLO
FAXFeFIDFLAAFOAFPDFRFUDSFSGC
Definition
Code of Federal RegulationsContract Laboratory ProgramCorrective measures studyTotal and amenable cyanide (Methods 9010A/9012)CobaltChain-of-custodyChemical oxygen demand (Methods 410s)Contracting officer representativeChemical Quality Assurance ReportChromiumHexavalent chromiumCopperCold vapor atomic absorptionA trade name for a herbicideDecachlorobiphenylDichlorodiphenyl-dichloroethaneDichlorodiphenyl-trichloroethaneDefense Environmental Restoration ProgramDecafluorotriphenylphosphineDepartment of EnergyDepartment of TransportationData quality objectiveDiesel range organicsElectron capture detectorElectrolytic conductivity detectorEngineering manualEnvironmental Monitoring Systems LaboratoryA trade name for an insecticideEngineeringExtraction procedureEstimated quantitation limitEngineering regulationEdgewood Research, Development and EngineeringCenterNitroaromatics and nitramines explosives(draft Method 8330)FacsimileIronFlame ionization detectorFlame atomic absorptionField operating activitiesFlame photometric detectorFederal RegisterFormerly Used Defense SiteFeasibility studyGas chromatography
M-3
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Term
GC/MSGFAAGHAAGPCGROHARDHAZWRAPHClHERBHgHNO3
HPLCH 3P O4
HRGC/LRMS
HRGC/HRMS
HQUSACE/OCE
H 2SO4
HTRWHTRW MCXHVOICICP
ICP/MSICSICVIDIDLIRIRPJP-4KKCNLC/MSLCSLCSDLIMSLVCLQMMMBMCXMDMDL
Definition
Gas chromatograph/mass spectrometerGraphite furnace atomic absorptionGaseous hydride atomic absorptionGel permeation chromatographyGasoline range organicsTotal hardness (Methods 130s)Hazardous waste remedial action programHydrochloric acidChlorinated herbicides (Method 8150A)MercuryNitric acidHigh performance liquid chromatographyortho-Phosphoric acidHigh resolution gas chromatograph/lowresolution mass spectrometerHigh resolution gas chromatograph/highresolution mass spectrometerHeadquarters, U.S. Army Corps of Engineers/Office of the Chief of EngineersSulfuric acidHazardous, toxic, and radioactive wasteHTRW Mandatory Center of ExpertiseHalogenated volatile organic compoundIon chromatographyInductively coupled plasma-atomic emissionspectrometerInductively coupled plasma/mass spectrometerInterference check standardInitial calibration verificationInside diameter; or identificationInstrument detection limitInfraredInstallation Restoration ProgramAn engine fuel for jet-propelled aircraftPotassiumPotassium cyanideLiquid chromatograph/mass spectrometerLaboratory control samplesLaboratory control sample duplicateLaboratory information management systemLaboratory validation coordinatorLaboratory quality management manualMethod blankMandatory Center of ExpertiseMatrix duplicateMethod detection limit
M-4
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Term
METALMgMnMoMRDMRDLMSMSAMSDNaNaOHNa2 S2 O3
NACIP
NEESA
NiNIOSH
NISTNPDESNRCNVLAP
O&GOSHAOSWPAPAH
PARCCS
PATPbPCBPCDDPCDFPEPESPESTPFBpHPHENOPHENLPIDPOC
Definition
Trace metals (Methods 6010A/7000s)MagnesiumManganeseMolybdenumMissouri River DivisionMissouri River Division LaboratoryMatrix spike; or mass spectrometerMethod of standard additionsMatrix spike duplicateSodiumSodium hydroxideSodium thiosulfateNaval Assessment and Control of InstallationPollutantsU.S. Navy Energy and Environmental SupportActivityNickelNational InstituteHealthNational InstituteNational PollutionNuclear RegulatoryNational VoluntaryProgramOil and grease
for occupational Safety and
of Standards and TechnologyDischarge Elimination SystemCommissionLaboratory Accreditation
Occupational Safety and Health AdministrationOffice of Solid WastePreliminary assessmentPolynuclear aromatic hydrocarbons(Methods 8100/8310)Precision, accuracy, representativeness,comparability, completeness, and sensitivityProficiency Analytical Testing ProgramLeadPolychlorinated biphenyls (Method 8080)Polychlorinated dibenzo-p-dioxinsPolychlorinated dibenzofuransPerformance evaluationPE sample supplierOrganochlorine pesticides (Method 8080)PentafluorobenzylbromidePotential of hydrogenPhenols (Method 8040A)Phenolics (Methods 9065/9066/9067)Photoionization detectorPoint of contact
M-5
EM 200-1-11 Jul 94
Term
POLPPppbppmPQLQAQC%RRCRARFARFIRARADCHEMRASRDREMRFRIRPDRRTSAESASSbSBASDWASeSEMSFSISIMSOPSOWSPCC
SQGSSSW-846
TALTBATCLTCDTCDDTCLPTCMXTDS
Definition
Petroleum, oils, or lubricantPriority pollutantPart per billionPart per millionPractical quantitation limitQuality assuranceQuality controlPercent recoveryResource Conservation and Recovery ActRCRA facility assessmentRCRA facility investigationRemedial actionRadiochemistryRoutine Analytical ServiceRemedial designRemedial Engineering ManagementResponse factorRemedial investigationRelative percent differenceRelative retention timeSociety of Automotive EngineersSpecial Analytical ServiceAntimonySmall Business AdministrationSafe Drinking Water ActSeleniumScanning electron microscopeSuperfundSite investigationSelected ion monitoringStandard operating procedureScope of workSystem performance check compound; or spillprevention control and countermeasureSmall quality generatorStainless steelThe USEPA document, "Test Method for EvaluatingSolid Waste"Target Analyte ListTetrabutylammoniumTarget Compound ListThermal conductivity detectorTetrachlorodibenzo-p-dioxinsToxicity characteristic leaching procedure2,4,5,6-Tetrachloro-m-xyleneTotal dissolved solids (Method 160.1)
M-6
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Term
TICTlTOTOCTOXTMTM/COR
TPH
TRPH
TSSUSACEUSAECUSAFOEHL
USDAUSEPAUSGSUSTUV/VISVVOAVOCv/vWESWPWPCFWSZHEZn130s300s300.0
310s410s413.1
413.2418.1
601602
Definition
Tentatively identified compoundThalliumToxic organicsTotal organic carbon (Method 9060)Total organic halides (Methods 9020A/9022)Technical managerTechnical manager/contracting officerrepresentativeTotal petroleum hydrocarbons (modifiedMethod 8015)Total recoverable petroleum hydrocarbons(Method 418.1)Total suspended solids (Method 160.2)U.S. Army Corps of EngineersU.S. Army Environmental CenterU.S. Army Force Occupational and EnvironmentalHealth LaboratoryU.S. Department of AgricultureU.S. Environmental Protection AgencyUnited States Geological SurveyUnderground storage tankUltraviolet/VisibleVanadiumVolatile organic analyte (Method 8240A)Volatile organic compoundVolume to volumeWaterways Experiment StationWater pollutionWater Pollution Control FederationWater supplyZero-headspace extractorZincUSEPA methods for total hardnessUSEPA methods for common anionsUSEPA method for common anions by ionchromatographyUSEPA methods for alkalinityUSEPA methods for chemical oxygen demandUSEPA method for oil and grease by gravimetricmethodUSEPA method for oil and grease by IRUSEPA method for total recoverable petroleumhydrocarbons by IRUSEPA method for purgeable halocarbons by GCUSEPA method for purgeable aromatics by GC
M-7
EM 200-1-11 Jul 94
Term
603
604606607608
609
610
611612624625
1010
1020A
11101310A
1311
3005A
3010A
3020A
3040
3050A
3060
3510A
3520A
3540A3550
Definition
USEPA methodGCUSEPA methodUSEPA methodUSEPA methodUSEPA methodPCBS by GCUSEPA methodby GCUSEPA methodhydrocarbonsUSEPA methodUSEPA methodUSEPA methodUSEPA methodGC/MSUSEPA method
for
forforforfor
for
for
acrolein and acrylonitrile by
phenols by GCphthalate esters by GCnitrosamines by GCorganochlorine pesticides and
nitroaromatics and isophorone
polynuclear aromaticby GCfor haloethers by GCfor chlorinated hydrocarbons by GCfor purgeables by GC/MSfor base/neutrals and acids by
for ignitability by Pensky-Martensclosed-cup methodUSEPA method for ignitability by Setaflashclosed-cup methodUSEPA method for corrosivity toward steelUSEPA method for extraction procedure toxicitytest method and structural integrity testUSEPA method for toxicity characteristicleaching procedureUSEPA method for acid digestion of water fortotal recoverable or dissolved metals foranalysis by FLAA or ICPUSEPA method for acid digestion of aqueoussamples and extracts for total metals foranalysis by FLAA or ICPUSEPA method for acid digestion of aqueoussamples and extracts for total metals foranalysis by GFAAUSEPA method of dissolution products for oils,greases, or waxesUSEPA method for acid digestion of sediments,sludges, and soilsUSEPA method for alkaline digestion ofhexavalent chromium in solid wasteUSEPA method for separator funnelliquid-liquid extractionUSEPA method for continuous liquid-liquidextractionUSEPA method for Soxhlet extractionUSEPA method for sonication extraction
M-8
Term
3580A3610A3620A3630A36403650A3660A3810
5030A6010A7000s
7060
7061A
7470
7471
7740
7741
8010A
8015A
8015M
8020
8040A8080
8100
8140
8150A8240A8250
8270A
EM 200-1-11 Jul 94
Definition
USEPA method for waste dilutionUSEPA method for alumina column cleanupUSEPA method for Florisil column cleanupUSEPA method for silica gel cleanupUSEPA method for gel-permeation cleanupUSEPA method for acid-base partition cleanupUSEPA method for sulfur cleanupUSEPA method for headspace extraction andscreening of purgeable organicsUSEPA method for purge-and-trapUSEPA method for metal analysis by ICPUSEPA methods for metal analysis by FLAA, GFAA,or CVAAUSEPA method for analysis of aqueous arsenicsamples by GFAAUSEPA method for analysis of aqueous arsenicsamples by GHAAUSEPA method for analysis of mercury in liquidwaste by CVAAUSEPA method for analysis of mercury in solidor semisolid waste by CVAAUSEPA method for analysis of aqueous seleniumsamples by GFAAUSEPA method for analysis of aqueous seleniumsamples by GHAAUSEPA method for halogenated volatile organicsby GCUSEPA method for nonhalogenated volatileorganics by GCModified USEPA Method 8015 for total petroleumhydrocarbons by GCUSEPA method forGCUSEPA method forUSEPA method forPCBs by GCUSEPA method for
aromatic volatile organics by
phenols by GCorganochlorine pesticides and
polynuclear aromatichydrocarbons by GCUSEPA method for organophosphorus pesticides byGCUSEPA method for chlorinated herbicides by GCUSEPA method for volatile organics by GC/MSUSEPA method for semivolatile organics bypacked column GC/MSUSEPA method for semivolatile organics bycapillary GC/MS
M-9
EM 200-1-11 Jul 94
Term
82808310
8330
9010A
9012
90609065
9066
9067
9071
Definition
USEPA method for PCDD and PCDF by GC/MSUSEPA method for polynuclear aromatichydrocarbons by HPLCDraft USEPA method for nitroaromatics andnitramines by HPLCUSEPA method for total and amenable cyanide bymanual calorimetric methodUSEPA method for total and amenable cyanide byautomated calorimetric methodUSEPA method for total organic carbonUSEPA method for phenolics by manualspectrophotometric methodUSEPA method for phenolics by automatedcalorimetric methodUSEPA method for phenolics byspectrophotometric methodUSEPA method for oil and grease extraction ofsludge samples
M-10 U.S. GOVERNMENT PRINTING OFFICE: 1994 - 521- 101/81133