u - p2s€¦ · web view13.0 method performance 5.0 standards and reference materials 14.0...

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U. S. Department of Energy

Consolidated Audit Program

Checklist 2

Data Quality for Organic Analyses

DoD/DOE QSM - Revision 4.3October 2015

Use of this DOECAP checklist is authorized only if the user has satisfied the copyright restrictions associated with TNI-EL-V1-2009 and ISO 17025:2005. DOECAP does not control or restrict the use of copyrighted standards that have been incorporated into this checklist; however, TNI and ISO do restrict use of their standards.

OFFICIAL USE ONLYMay be exempt from public release under the Freedom of Information Act(5 U.S.C 552), exemption number and category: Exemption #4: Commercial Proprietary Department of Energy review required before public releaseName/Org: TBD Date: TBD Guidance (if applicable) Memo dated October 30, 2008 from Charles B. Lewis III to Larry Kelly, DM No 419069

Audit ID: Date:

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OFFICIAL USE ONLYU.S. Department of Energy Consolidated Audit Program

Data Quality Organic Analyses

DOECAP Audit Checklist: 2 Rev. 4.3

Revision Date: October 2015 Page 1 of 1

Audit ID: ___________________________Laboratory: ______________________________Auditor:

Areas of Review During Audit

1.0 Standard Operating Procedures (SOPs) 10.0 Carryover Minimization

2.0 Sample Preparation/Extraction 11.0 Spike Recovery Requirements

3.0 Cleanup Methods 12.0 Second-Column Confirmation

4.0 Initial and Continuing Calibration 13.0 Method Performance

5.0 Standards and Reference Materials 14.0 Analytical Worksheets

6.0 Method Proficiency 15.0 Instrument Operation

7.0 Limit of Detection (LOD) and Limit of Quantitation (LOQ) 16.0 Contamination Control

8.0 Precision and Accuracy 17.0 Data Review

9.0 Instrument Run Logs

A=Acceptable U=Unacceptable NA=Not ApplicableF=Finding NO=Not Observed O=Observation

Referenced regulations are accessible at the following URLs: http://www.p2s.com/?page_ id=1526 http://www.epa.gov/epaoswer/hazwaste/test/main.htm

NOTE: When audit findings are written against site-specific documents (i.e., SOPs, QA Plans, licenses, permits, etc.), a copy of the

pertinent requirement text from that document must be attached to this checklist for retention in DOECAP files. Fully document any deviation from the LOI or the requirements of QSM Version 5.0, ISO 17025:2005, and TNI ELV1 For method specific quality control criteria, please refer to Appendix B of the DoD/DOE QSM Refer to Page 39 for the record of revision. For method specific quality control requirements, refer to QSM Rev. 5.0, Appendix A, Pages 77 – 109.

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http://www.epa.gov/epaoswer/hazwaste/test/main.htm

http://www.p2s.com/?page_%20id=1526




Revision Date: March 2014 Page 2 of 39

Audit ID: ___________________________Laboratory: ______________________________Auditor:_________________________________________

Item Number Line of Inquiry Status Summary of Observations/Objective Evidence

Reviewed Audit Notes1.0 Standard Operating Procedures (SOPs)1.1 Does the laboratory have and maintain an in-house methods manual(s) for each

accredited analyte or test method. The manual consists of copies of published or referenced test methods or SOPs that have been written by the laboratory. Each method contains:

identification of the test method; applicable matrix or matrices; detection limit; scope and application, including components to be analyzed; summary of the test method; definitions; interferences; safety; equipment and supplies; reagents and standards; sample collection, preservation, shipment, and storage; QC; calibration and standardization; procedure; calculations; method performance; pollution prevention; data assessments and acceptance criteria for QC measures; corrective actions for out-of-control data; contingencies for handling out-of-control or unacceptable data; waste management; references; and any tables, diagrams, flowcharts, and validation data.

QSM Rev. 5.0, Module 2, Section 4.2.8.5; TNI Standard, EL-V1-2009, Sections 4.2.8.5 a) through f)

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Reviewed Audit Notes1.2 When utilized, are permanent, bound laboratory notebooks (logbooks) or

notebooks with measures in place to prevent the removal or addition of pages are required, if utilized?

Electronic logbooks are acceptable. For permanent, bound logbooks are the following applied:a) Are laboratory notebook pages pre-numbered, all entries are signed or

initialed and dated by the person responsible for performing the activity at the time the activity is performed, and all entries are recorded in chronological order?;

b) Are all notebook pages closed when the activities recorded are completed or carried over to another page?

c) Is the person responsible for performing the closure t h e s a m e person who performed the last activity recorded?

d) Did closure occur at the end of the last activity recorded on a page, as soon as practicable thereafter?

e) Did documentation of the closure include analyst initials and date?; andf) Does each laboratory notebook have a unique serial number clearly

displayed?

QSM Rev. 5.0, Module 2, Section 4.13.41.3 Is a system in place to ensure that quality records are legible, accurate, and

complete, e.g., independent review of records, logbooks, etc.?

ISO/IEC 17025 Clause 4.13.1.21.4 When mistakes occur in records, are they crossed out with a single line,

corrected, and initialed and dated? Are all such alterations to records initialed by the person making the correction?

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Reviewed Audit NotesIn the case of records stored electronically, are equivalent measures taken to avoid loss or change of original data?

ISO/IEC 17025 Clause 4.13.2.32.0 Sample Preparation/Extraction2.1 In order to minimize instrument contamination and downtime, does the

laboratory employ a sample screening procedure prior to extraction and analysis?

EPA SW-846, Method 8000B, Section 3.22.2 Does the laboratory have a documented procedure for the determination of

extraction level?

EPA SW-846, Chapter One, Section 4.3.42.3 Are glassware and containers designated as disposable or cleaned according to

an SOP?

EPA SW-846, Chapter One, Section 4.3.32.4 General Facility:

Is the laboratory clean and organized? Is sample preparation performed on a clean tabletop? Are hoods clutter free; and Is workspace adequate?

EPA SW-846, Chapter One, Section 4.12.5 Is check weighing performed daily using NIST-traceable weights?

Do the balance checks bracket the range of use?

Are daily balance checks documented?

QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table and TNI 5.5.13.1 b)

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Reviewed Audit Notes2.6 Are Class 1 (formerly referred to as Class S) certified check weights calibrated

every five years using recognized National Metrology Institute, such as NIST, traceable references, when available?

NOTE: The date for recalibration of the check weights is stated on the certificate of calibration supplied by the accredited calibration firm.Are all support equipment, including balances, calibrated or verified at least annually, using a recognized National Metrology Institute, such as NIST, traceable references when available, bracketing the range of use?Does the laboratory maintain a copy of the Certificate of Calibration from an ISO/IEC accredited calibration laboratory?

QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table and TNI EL-V1-2009, Section 5.5.13.1 b) and d)

2.7 Prior to use, are balances checked on a daily basis using two standards weights that bracket the expected mass?

QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table2.8 Are the acceptance criteria for a top-loading balance ±2% or ±0.02 grams

whichever is greater?Are the acceptance criteria for an analytical balance ±0.1% or ±0.5 mg. whichever is greater?

QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table2.9 Are liquid in-glass thermometers calibrated against a NIST-traceable standard

before the first use and annually?Are electronic thermometers checked before use and on a quarterly basis?

QSM Rev. 5.0, Module 2, Section 5.5.13.1 and TNI EL-V1-2009, Section 5.5.13.1 d)

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Reviewed Audit Notes2.10 Are mechanical volumetric pipettes checked daily before use and is the bias

within ± 2% of the nominal volume?

NOTE: For variable volume pipettes, the nominal value is the volume of use.

QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table

2.11 Are samples stored according to the conditions specified by the preservation protocol?For samples that require thermal preservation stored under refrigeration that is ±2°C of the specified preservation temperature unless regulatory or method specific criteria exist?NOTE: For samples with a specified storage temperature of 4°C, storage at a temperature above the freezing point of water to 6°C shall acceptable.

Note: EPA has recently promulgated temperature conditions of 0°Cto 6°C, with a footnote “above freezing” and the QSM Rev. 5.0, Section 5.5.13.1 f) Table also requires the same temperature ranges. The existing LOI can be used or the revision may be applied.

TNI-EL-V1M2, Section 5.8.9 a) and i)2.12 Are refrigerator temperatures are monitored daily and recorded in a logbook or

via electronic media such as a data logger?NOTE: Daily temperature monitoring of refrigerators and freezers is required for all samples that require temperature preservation. Daily monitoring for rad samples other than Tritium will not be required.

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Reviewed Audit NotesThe requirement for daily monitoring for sample storage refrigerators and freezers will not apply in the event that samples are not being stored from a DOE site.

QSM Rev. 5.0, Module 2, Section 5.5.13.1 f)2.13 Does the laboratory have procedures for recording catastrophic failure of

support equipment (e.g., refrigerators, freezers) and that addresses identification of affected samples and customer notification?

QSM Rev. 5.0, Module 2, Section 5.5.13.12.14 Are refrigerator storage blanks present for the storage of all volatile organic

samples and include the following:

Is a refrigerator storage blank present for the storage of all volatile organic samples?

Are specific procedures for assessing the adequacy of storage blank data and taking action for nonconforming conditions established?

When samples are stored in refrigerators, are associated storage blanks analyzed every 14 days?

Are the storage blanks stored in the same manner as the client samples? Is the data from the analysis of the refrigerator storage blank available

for review?

QSM Rev. 5.0, Module 2, Section 5.3.3 a) b) and c)

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Reviewed Audit Notes2.15 Does the sample preparation documents indicate the following:

extraction procedure, matrix, identification number of standards and spikes added, spike composition, blanks, volume/concentration of standards/spikes added, name of analyst, volume/weight of sample used, final concentrated volume, dilution information, cleanup steps, reagent log numbers, start/stop dates/time for soxhlet and continuous liquid/liquid extraction,

and observations?

EPA SW-846, Chapter One, Sections 4.3.4, 4.3.10, and 4.6

2.16 Do sample preparation practices assure homogenization so that a representative aliquot is obtained for analysis?

EPA SW-846, Method 3550 B, Section 7.12.17 Sonication equipment is tuned prior to use to ensure optimum performance.

EPA SW-846, Method 3550B, Section 7.0 2.18 For solids extraction using ultrasonic extraction are surrogate and spiking

solutions added prior to solid prior to adding extraction solvent.

EPA SW-846, Method 3550, Section 7.3

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Reviewed Audit Notes2.19 Does the Chain of Custody contain all signatures of all personnel that handled

the sample(s)?

QSM Rev. 5.0, Module 2, Section 5.8.8 b)3.0 Cleanup Methods3.1 Does the laboratory maintain and follow SOPs for all cleanup methods

performed at their facility including, but not limited to: Gel-Permeation Chromatography (GPC), florisil, silica gel, alumina, and sulfur cleanup?

EPA SW-846, Chapter One, Section 4.33.2 Is the laboratory’s selection of cleanup methods appropriate for the matrix of

concern and for the potential interference?

EPA SW-846, Method 8000B, Section 3.4; EPA SW-846, Method 3600C, Sections 1.0 and 7.3

3.3 When sample extracts are subjected to cleanup procedures, is the associated quality control samples (e.g. spikes, blanks, replicates, and duplicates processed through the same cleanup procedure?

EPA SW-846, Method 3600C, Section 8.3.23.4 Is the GPC calibrated at least once per week during operation?

EPA SW-846, Method 3640A, Section 7.53.5 When GPC is used, does the final sample concentration calculations account for

the volume of sample lost in the dump of the instrument?

EPA SW-846, Method 3640A, Section 7.7

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Reviewed Audit Notes3.6 Are instrument and maintenance logs maintained for the GPC?

TNI-ELV1M2, Section 5.5.53.7 Are florisil lot checks performed to ensure adequate recovery of target analytes

and adequate exclusion of interferences (e.g., trichlorophenol)?

EPA SW-846, Method 3620B, Section 8.03.8 Are biological matrices cleaned using a method that effectively excludes fats

and lipids (e.g., sulfuric acid and cleanup)?

EPA SW-846, Method 8290, Section 2.43.9 Is sulfuric acid cleanup not used for analytes that are destroyed by acids (e.g.,

some pesticides and herbicides)?

EPA SW-846, Method 3665A, Section 1.14.0 Initial and Continuing Calibration4.1 Are controlled procedures present at the workstation and do they that list

requirements for instrument calibration and tuning?

ISO/IEC 17025:2005 Clause 5.4.1 (General Requirement), EPA SW-846, Chapter One, Section 4.3.5

4.2 Is out-of-calibration equipment tagged or segregated and not used until it has been re-calibrated?

QSM Rev. 5.0, Section 5.5.13.1 f)4.3 Is equipment consistently found to be out-of-calibration repaired or replaced?

QSM Rev. 5.0, Module 2, Section 5.5.13.1 f)

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Reviewed Audit Notes4.4 If a linear calibration is to be used:

does the relative standard deviation for calibration standard responses meet defined acceptance criteria or does the linear calibration least squares regression meet defined acceptance criteria, and

the curve is not forced through zero?

EPA SW-846, Method 8000B, Section 7.54.5 Does the laboratory follow a documented procedure for the determination and

verification of retention time windows for Gas Chromatography (GC) and High Performance Liquid Chromatography (HPLC) methods that do not employ internal standard calibration?

QSM Rev. 5.0, Module 2, Organic QC Tables, EPA SW-846, Method 8000B, Section 7.6

4.6 For GC analysis, are retention time windows established for each analyte of concern and each column?

NOTE: In some cases pattern recognition can be used in lieu of retention time identification.

EPA SW-846, Method 8000B, Section 7.6.64.7 Are retention time windows established so as to minimize false positive or false

negative results?

EPA SW-846, Method 8000B, Section 7.64.8 Are the details of the initial and continuing instrument calibration procedures

including calculations, integrations, acceptance criteria and associated statistics included or referenced in the method SOP and retained for the laboratory for review?

TNI-EL-V1M4, 2009, Section 1.7.1.1 a); Section 1.7.2 a)

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Reviewed Audit Notes4.9 Are acceptance criteria defined and documented for all initial calibration and

continuing calibration requirements?

TNI-EL-V1M4, 2009, Section 1.7.1.1 e); Section 1.7.2 e)4.10 If the initial calibration is not performed on the day of analysis, is the validity of

the initial calibration verified by continuing calibration verification with each analytical batch?

TNI EL-V1M4-2009, Section 1.7.2 4.11 Is instrument calibration verification performed:

i. once after each instrument calibration (ICAL)

ii. after the analysis of a second source standard prior to sample analysis

QSM Rev. 5.0, Table 1 Organic Analysis by GC and Table 4 Organic Analysis by GC/MS

4.12 Is the lowest calibration standard for the initial calibration at or below the limit of quantitation?Are data reported below the LOQ reported using defined qualifiers?

TNI EL-V1M4-2009, Section 1.7.1.11 f)4.13 Is the highest calibration standard at or above the highest concentration for

which quantitative data are to be reported?

Is data reported above the calibration range reported using defined qualifiers or explained in the narrative?

QSM Rev. 5.0, Module 4, Section 1.7.1.1.g)4.14 If the initial calibration data are outside established acceptance criteria are

corrective actions performed and associated sample reanalyzed?

TNI-EL-V1M4-2009, Section 1.7.1.1 i)

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Reviewed Audit Notes4.15 If the continuing calibration verification (CCV) results are outside the

established acceptance criteria and analysis of two additional consecutive (immediate) CCVs fails to produce results within acceptance criteria, are corrective actions performed?

NOTE: Immediately is defined as starting a consecutive pair within one hour; no samples can be analyzed between the failed CCV and the two additional CCVs.

QSM Rev. 5.0, Module 4, Section 1.7.2 i)4.16 Are initial calibrations verified with a standard obtained from a second

manufacturer or from a different lot number?

QSM Rev. 5.0, Module 4, Section 1.7.1.1 d)

5.0 Standards and Reference Material5.1 Does the laboratory ensure that purchased supplies and reagents and

consumable materials that affect the quality of tests and/or calibrations are not used until they have been inspected or otherwise verified as complying with standard specifications or requirements defined in the methods for the tests and/or calibrations concerned? Do the purchased supplies and reagents comply with specified requirements? Are records of actions taken to check compliance maintained?

ISO/IEC 17025, Clause 4.6.25.2 Does the laboratory maintain documentation for reagents and solvents and are

they checked to ensure that the stated purity meets the intended use? Are records of purity checks filed in a manner that is retrievable?

QSM Rev, 5.0, Module 2, Section 5.6.4.25.3 Do purchasing documents for items affecting the quality of laboratory output

contain data describing services and supplies?

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Reviewed Audit Notes

Are the purchasing documents reviewed and approved for technical content prior to release?NOTE: The description may include type, class, precise identification, specifications, drawings, inspection instructions, and other technical data including approval of test results, the quality required and the management system standard under which they were made.

ISO/IEC 17025, Clause 4.6.35.4 Do records for services and supplies that may affect the quality of

environmental tests include the following, where applicable:a) Date of receipt;b) Expiration date;c) Source;d) Lot or serial number;e) Calibration and verification records; andf) Accreditation or certification scopes/certificates

QSM Rev. 5.0, Module 2, Section 4.6.15.5 Are calibration standards assigned a unique identification number traceable to

the original standards, lot number and an expiration date?Are these numbers and dates placed on the standards container?

TNI EL-V1M2-2009, Section 5.6.4.25.6 Are standards and reference materials traceable to NIST or other certified

standards, including: initial calibration standards, continuing calibration standards, spiking standards, and surrogates.

TNI-EL-V1M2-2009 Section 5.6.3.2

.

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Reviewed Audit Notes5.7 Are calibration standards prepared using certified standards traceable to a

nationally recognized or consensus source, and are the certificates of authenticity are kept on file?

TNI-EL-V1M2-2009 Section 5.6.3.25.8 Do procedures exist for the storage of reagents and laboratory consumable

materials?

TNI-EL-V1M2-2009, Section 4.6.15.9 Do the procedures require organic standards be properly refrigerated and stored

as required by the specific EPA method?

TNI-EL-V1M2-2009, Section 4.6.15.10 Are the following calibration criteria met:

appropriate number, type and range of calibration standards are used as required by the EPA method;

for each analyte and surrogate of interest, initial calibration standards are prepared at a minimum of 5 different concentrations.

EPA SW-846, Method 8000B, Sections 7.4.1.1 and 7.4.1.4

6.0 Method Proficiency6.1 Has the laboratory performed and documented the results of a method validation

study for each method.

TNI EL-V1M4-2009, Section 1.5.1a)6.2 Has the laboratory validated all non-reference methods or laboratory developed

methods?

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Reviewed Audit NotesAre the results of the method validation documented and readily available for review?

TNI EL-V1M4-2009, Section 1.5.1b)6.3 Are samples that were initially diluted and had no identified compounds

reanalyzed at a lower dilution, if required by client specific instructions? QSM Rev. 5.0, Module 4, Section 1.7.1.1 g)

7.0 Limit of Detection (LOD) and Limit of Quantitation (LOQ)Note: If the laboratory is not reporting a value below the Limit of Quantitation, a Limit of Detection study is not required.7.1 Does the laboratory maintain procedures for determining limits of detection and

the frequency of verification?

TNI-ELV1M4-2009, Section 1.5.27.2 Does the laboratory document how LODs were derived from the method

determinations?

TNI-ELV1M4-2009, Section 1.5.2.17.3 Are all sample-processing and analysis steps of the analytical method included

in the determination or validation of the LOD?

TNI-ELV1M4-2009, Section 1.5.2.17.4 Is the validity of the LOD verified by detection (a value above zero) of the

analyte(s) in QC sample in each quality system matrix and the does the QC sample contain the analyte at no more than 3 times the LOD for single analytes and 4 times the LOD for multiple analyte tests?

QSM Rev. 5.0, Module 4, Section 1.5.2.1 b)

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Reviewed Audit Notes7.5 Has the laboratory performed a LOD on every instrument this to be used for

analysis of samples and reporting of data?

QSM Rev. 5.0, Module 4, Section 1.5.2.1 b)7.6 Is the validity of the LOD verified as part of the LOD determination process and

is the verification of the LOD completed prior to the use of the LOD for sample analysis?

QSM Rev. 5.0, Module 4, Section 1.5.2.1 b)NOTE: A LOD study is not required for any component for which spiking solutions or quality control samples are not available such as temperature.

7.7 Is a LOD performed each time there is a change in the method that affects how the test is performed or when a change in instrumentation occurs that affect the sensitivity of the analysis?

TNI-ELV1M4-2009, Section 1.5.2.1 e)7.8 Are LODs verified quarterly for each quality system matrix, technology, and

analyte?

QSM Rev. 5.0, Module 4, Section 1.5.2.1 f)7.9 Are all sample-processing and analysis steps of each applicable analytical

method included in the determination of the limit of quantitation (LOQ)?

TNI-ELV1M4-2009, Section 1.5.2.2 a)7.10 Is the validity of the LOQ verified by successful analysis of a QC sample

containing the analytes of concern in each quality system matrix at 1 to 2 times the claimed LOQ?

QSM Rev. 5.0, Module 4, Section 1.5.2.2 c)

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Reviewed Audit Notes7.11 Is the criteria for analysis of the LOQ based on the recovery of each analyte is

within the laboratory established method acceptance criteria or client data quality objectives for accuracy?

QSM Rev. 5.0, Module 4, Section 1.5.2.2 c)7.12 Is the LOQ above the LOD, if the LOD is determined by the laboratory (See

Note below LOI 7.0)?

TNI-ELV1M4-2009, Section 1.5.2.2 d)7.13 Is the LOQ verified quarterly for each quality system matrix, technology, and

analyte?

QSM Rev. 5.0, Module 4, Section 1.5.2.1 f)

8.0 Precision and Accuracy8.1 Has the he laboratory evaluated the precision and bias of a reference method for

each analyte of concern for each quality system matrix or alternate documented procedure when the analyte cannot be spiked into the sample matrix and where QC samples are not commercially available?

TNI-ELV1M4-2009, Section 1.5.3 a)8.2 For laboratory-developed methods or non-reference methods that were not in

use by the laboratory before July 2003, has the laboratory developed and documented a procedure to evaluate precision and bias?Has the laboratory also compared results of the precision and bias measurements with criteria established by the client, by criteria given in the reference method or criteria established by the laboratory?

TNI-ELV1M4-2009, Section 1.5.3 b)

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Reviewed Audit Notes8.3 Do precision and bias measurements evaluate the method across the analytical

calibration range of the method? Has the laboratory also evaluated precision and bias in the relevant quality system matrices and processed the samples through the entire measurement system for each analyte of interest?

TNI-ELV1M4-2009, Section 1.5.3 b)8.4 Does the systematic approach to the evaluation of precision and bias include the

following approach:

Are QC samples analyzed in triplicate containing the analytes of concern at or near the limit of quantitation, at the upper-range of the calibration (upper 20%) and at a mid-range concentration? Are these samples processed on different days as three (3) sets of samples through the entire measurement system for each analyte of interest? On each day, is one (1) QC sample at each concentration analyzed?Is a separate method blank subjected to the analytical method along with the QC samples on each of the three (3) days?NOTE: The three (3) samples at the LOQ concentration can demonstrate sensitivity as well.For each analyte, does the laboratory calculate the mean recovery for each day, for each level over each day, and for all nine (9) samples?Does the laboratory calculate the relative standard deviation for each of the separate means obtained? Are the standard deviations compared for the different days and the standard deviations for the different concentrations?

TNI-ELV1M4-2009, Section 1.5.3 b) i)

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Reviewed Audit Notes8.5 Has the laboratory evaluated selectivity by following the checks established

within the method, which may include mass spectral tuning, second column confirmation, chromatography retention time windows, and sample blanks?.TNI-ELV1M4-2009, Section 1.5.4

9.0 Instrument Run Logs9.1 Do GC and GC/MS instrument run logs include:

data file names and address; notation for any failure where the sample is to be re-run at a later time; pH of sample for VOAs; notation for reanalysis that references the original run when any failure

occurred; reference to the original run for diluted samples when the calibration

range was exceeded; reference to the sample purge manifold port used for Volatile Organic

Compounds (VOCs); and documentation of decontamination activities?

EPA SW-846, Chapter One, Section 4.610.0 Carryover Minimization10.1 Is an instrument (solvent) blank analyzed when the previous sample showed the

presence of an analyte at a high concentration?

EPA SW-846, Method 8000B, Section 3.111.0 Spike Recovery Requirements11.1 Are the methods for establishing acceptable ranges for spike recoveries and

calibration check samples defined and documented by the laboratory?

EPA SW-846, Chapter 1, Section 4.4

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Reviewed Audit Notes11.2 Are the analysts following the steps specified in the SOP when spike recoveries

and calibration check samples fall outside control limits?

EPA SW-846, Chapter 1, Section 4.411.3 Are statistical Control Charts :

Maintained and used to detect trends and prevent out-of-control conditions?

Monitored on an on-going basis (at least quarterly) for shifts in mean recovery, changes in standard deviation, and development of trends?

Has the laboratory chosen representative compounds for control charts for the purpose of trend analysis?

NOTE: Data analysis software may also be used for the statistical evaluation of data for trends and biases.

QSM Rev. 5.0, Module 4, Section 1.7.3.2.3 d)11.4 Does the QA Officer of designee review control charts are a specified frequency

and are appropriate corrective actions initiated for out-of-control conditions?

QSM, Rev. 5.0, Module 4, Section 1.7.3.2.3 e)11.5 Does the laboratory use its in house statistically established LCS control limits

for the purpose of trend analysis?

QSM, Rev. 5.0, Module 4, Section 1.7.3.2.3 f)11.6 In the absence of client specified LCS reporting criteria, are the LCS control

limits outline in the DoD/DOE QSM Appendix C tables used in reporting data?

QSM, Rev. 5.0, Module 4, Section 1.7.3.2.3 g)

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Reviewed Audit Notes11.7 Are the LCS limits specified in the DoD/DOE QSM Appendix C tables used for

batch control unless project specific criteria exist?

QSM, Rev. 5.0, Module 4, Section 1.7.3.2.3 h)12.0 Second-Column Confirmation12.1 Has the laboratory documented procedures and possesses equipment to perform

second-column confirmation verification of results when required by the method or the laboratory SOP for a given method?

EPA SW-846, Chapter 1, Section 4.312.2 Are columns uniquely identified in such a manner that facilitates differentiation

between results obtained from the primary column and those obtained from a secondary column?Does the confirmatory column contain a different stationary phase from the primary column?

EPA SW-846, Method 8000B, Section 7.912.3 Do analyses performed on a secondary (confirmatory) column meet all required

QC criteria?

EPA SW-846, Method 8000B, Section 7.913.0 Method PerformanceNegative Controls – Method Blank13.1 Is a method blank processed along with and under the same conditions as the

associated samples including all steps of the analytical procedure? Are procedures in place to determine if a method blank is contaminated?

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Reviewed Audit NotesAre any affected samples associated with a contaminated method blank reprocessed for analysis or the results reported with appropriate data qualifiers?

TNI-ELV1M4-2009, Section 1.7.3.1 a)

13.2 Is a method blank analyzed at a minimum of one (1) per preparation batch?

In those instances for which no separate preparation method are used (for example, volatiles in water), is the batch defined as environmental samples that are analyzed together with the same method and personnel, using the same lots of reagents, not to exceed the analysis of twenty (20) environmental samples, not including method blanks, LCS, matrix spikes and matrix duplicates?

TNI-ELV1M4-2009, Section 1.7.3.1b)13.3 Does the method blank consist of a quality system matrix that is similar to the

associated samples and is known to be free of the analytes of interest?

TNI-ELV1M4-2009, Section 1.7.3..1.c)13.4 Is the concentration of a targeted analyte in the blank at or above the

reporting limit as established by the method or regulation, and is the concentration greater than 1/10 of the amount measured in the sample?If a blank is determined to be contaminated, is the cause investigated and measures taken to minimize or eliminate the problem?Are samples associated with a contaminated blank evaluated as to the best corrective action for the samples (e.g., reprocessing or data qualifying codes)?

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Reviewed Audit NotesIn all cases the corrective action shall be documented.

TNI-ELV1M4-2009, Section 1.7.4.1 a) c)Positive Controls – Laboratory Control Samples13.5 Are any affected samples associated with an out of control LCS reprocessed for

re-analysis or the results reported with appropriate data qualifier?

TNI-ELV1M4-2009, Section 1.7.3.2.1)13.6 Are LCS analyzed a minimum of one per preparation batch?

TNI-ELV1M4-2009, Section 1.7.3.2.213.7 Are all reported analytes spiked in the LCS (with the exception of Aroclor

analysis which is spiked per the method)?

QSM, Rev. 5.0, Module 4, Section 1.7.3.2.3 b)13.8 Where there are no established criteria, has the laboratory determined internal

criteria and document the method used to establish the limits or utilize client specified assessment criteria?

TNI-ELV1M4-2009, Section 1.7.4.2 a)13.9 Is the concentration of the spiked compounds at or below the midpoint of the

calibration if project specific concentrations are not specified?

QSM Rev. 5.0, Module 4, Section 1.7.4.2 b)Sample Specific Controls

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Reviewed Audit Notes13.10 Does the laboratory have procedures in place for tracking, managing, and

handling matrix-specific QC criteria, including spiking appropriate components at appropriate concentrations, calculating recoveries and relative percent difference, and evaluating and reporting results based on performance of the QC samples?

Note: Examples of matrix-specific QC include: Matrix Spike (MS), Matrix Spike Duplicate (MSD), sample duplicates, and surrogate spikes.

TNI-ELV1M4-2009, Section 1.7.3.313.11 Does the laboratory have a procedure for the frequency for the matrix spike and

matrix spike duplicates?

TNI-ELV1M4-2009, Section 1.7.3.3 b)13.12 Are the MS and MSD spiked with all reported analytes (with the exception of

Aroclor analysis which is spiked per the method)?

QSM, Rev. 5.0, Section 1.7.3.3.1 c)13.13 For matrix spikes and matrix spike duplicates, does the laboratory document the

calculation for %R, RPD or other statistical treatment used?Are the results are compared to the acceptance criteria as published in the mandated method?Where there are no established criteria, does the laboratory determine internal criteria and document the method used to establish the limits?For matrix spike results outside established criteria, corrective action shall be documented or the data for that sample reported with appropriate data qualifying codes.

TNI-ELV1M4-2009, Section 1.7.4.3 a)

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Reviewed Audit Notes13.14 Does the laboratory have an established frequency for the matrix duplicates and

is the results reported with the client data?

TNI-ELV1M4-2009, Section 1.7.3.3 213.15 For matrix duplicates, does the laboratory document the calculation for relative

percent difference or other statistical treatments?

TNI-ELV1M4-2009, Section 1.7.4.3 b)13.16 Are matrix duplicates results compared to the acceptance criteria as published in

the mandated method?Where there are no established criteria, does the laboratory determine internal criteria and document the method used to establish the limits?For matrix duplicates results outside established criteria, are corrective action documented or the data for that sample reported with appropriate data qualifiers?

TNI-ELV1M4-2009, Section 1.7.4.3 b)13.17 For surrogate standards:

a) Are Surrogates, when required, chosen to reflect the chemistries of the targeted components of the method and are added prior to sample preparation/extraction?

b) Except where the matrix precludes its use or when not commercially available, a r e surrogate compounds added to all samples, standards, and blanks for all appropriate methods?

TNI-EL-V1M4-2009, Section 1.7.3.3.313.18 Are the results for the surrogate standards compared to the acceptance criteria as

published in the mandated method?Where there are no established criteria, has the laboratory determined internal criteria and documented the method used to establish the limits?

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Reviewed Audit NotesAre surrogates that fall outside the acceptance criteria evaluated for the effect indicated for the individual sample results?

Do results reported from analyses with surrogate recoveries outside the acceptance criteria include appropriate data qualifiers?

TNI-EL-V1M4-2009, Section 1.7.4.3 c)14.0 Analytical Worksheets14.1 Do analytical worksheets include, at a minimum:

name of the person performing the analysis; instrument used in the analysis (If the subcontract laboratory has more than

one instrument of a particular model, a unique designation is given to each.); name or initials of the peer, supervisory, or QA reviewer; calibration information for all analytical work information on standards used

during the analysis; analytical procedure used; equations for calculations used to obtain results (If instrument readouts give

results, without the need for further mathematical manipulation, the worksheets include the statement “result = instrument readout”; and

date and time that the analysis was performed.

EPA SW-846, Chapter 1, Section 4.615.0 Instrument Operations15.1 Are analysts familiar with chromatographic anomalies and the instrument

conditions that cause them?

EPA SW-846, Method 8000B, Section 8.215.2 Is maintenance performed on analytical instrumentation recorded in a logbook?

TNI-EL-V1M2-2009, Section 5.5.5

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Reviewed Audit Notes15.3 Are instrument modifications documented in a permanent record?

TNI-EL-V1M2-2009, Section 5.5.515.4 Are instruments connected to a source of stable power or surge protection

devices are used?

EPA SW-846, Chapter 1, Section 4.116.0 Contamination Control16.1 Is there effective separation between neighboring areas in which there are

incompatible activities?Has the laboratory taken measures to prevent cross-contamination?Is access to and use of areas affecting the quality of the tests and/or calibrations controlled?Have measures been taken to ensure good housekeeping in the laboratory? TNI-ELV1M2-2009, Section 5.3.3 and 5.3.4

17.0 Data Review17.1 Is data review inclusive of all quality related steps in the analytical

process, including sample preparation, dilution calculations, chromatography, and spectral interpretations?

QSM Rev. 5.0, Module 2, Section 4.2.8.4 x)17.2 Is data review documented and are records maintained?

QSM Rev. 5.0, Module 2, Section 4.2.8.4 x)17.3 Spreadsheets used for calculations are verified before use and

documentation is readily available for review.

QSM Rev. 5.0, Module 2, Section 5.4.7.2 h)

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Notes:

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Record of Revision for Checklist 2Data Quality for Organic Analyses

Revision Number

EffectiveDate Reason for Revision Line of

Inquiry3.5 11/2009 Changed reference for laboratory notebooks from Section 4.12 DOE-5 to DOE-6 1.23.5 11/2009 Changed reference for closure of laboratory notebooks from Section 4.12 DOE-5 to DOE-6 1.5

3.5 11/2009 Verification of Class 1 check weights must be performed with weights that are traceable to the National Metrology Institute (such as NIST). 2.6

3.5 11/2009 Deleted the requirement for daily refrigerator and freezer monitoring in the event that samples are not being stored from a DOE site. 2.9

3.5 11/2009 Add requirement for solvent screening (QSAS Section 5.6 DOE-1) 5.13.6 11/2010 No Changes or Revisions3.7 11/2011 Added to the note; Fully document any deviation from the LOI or the requirements of QSAS 2.7 Page 13.8 1/2012 Added to the note; Fully document any deviation from the LOI or the requirements of QSAS 2.8 Page 14.0 11/2013 Complete revision to incorporate DoD/DOE QSM Rev. 5.0, ISO 17025:2005, and TNI ELV1-2009 All4.1 2/2014 Minor revision after first audit All4.2 3/2014 Deletion of quarterly accuracy checks for mechanical pipettes 2.104.2 10/2015 Add note for EPA promulgated requirement for temperature ranges 2.114.3 10/2015 Add hyperlink for DOECAP website for external access 1

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