appendix j nus data reduction, validation and reporting · describing each revision. the note is...

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APPENDIX J

NUS

DATA REDUCTION, VALIDATION AND REPORTING

flR300657

OATA REDUCTION, VALIDATION, AND REPORTING

The following procedures summarize practices routinely used by

laboratory and office, staffs for data reduction, validation, and reporting.

Numerical analyses including manual calculations, mapping, and conputeri

modeling, are documented and subjected to quality control review. Records

of numerical analyses are legible and ...complete enough to permit

reconstruction of the work by a qualified individual other than the

originator. . . . ._._. , .'.

: _ . _ ' . .laboratory Data Validation

Data validation begins with data reduction and continues through to

reporting of data. Data processing and data processing review are

performed by the .analysts and group leaders. After the draft

report is prepared, Laboratory Supervisors review the draft report.

The NUS Laboratory Manager reviews the report and approves it for

issue. The procedure is outlined in Figure 1.

Data processing is performed by the analyst in one of the following

ways:

o ffenual computation of the results directly in the benchbookor on calculation sheets , :

o Direct acquisition of reduced computer data

o Input of raw data for computer processing.

If" data are manually ccmputated, all steps performed are provided

including equations..used and the source of input information (response

constants, etc.) . Ttie analyst initials and dates each page of

calculations.

J3R30Q658

ACTIVITY RESPONSIBILITY

DataProcessing

v

VCheckingof Draft

Data Jteport

Final Review

Approval forIssue

Analysts

Reviewof Group DsadersData

Processing

Preparationof laboratory SupervisorsDraftReports

laboratory Supervisors

laboratory Onager

Laboratory Manager

FIGURE 1

LABORATORY DATA VALIDATION PROCESS

AR3QQ659

If data are computer processed, the input data is recorded in the

benchbook (if entered directly form .the benchbook) or with the raw data

file. Ttie analyst initials and dates all data input pages.

If reduced data are directly acquired from a computer, the analyst

verifies the sample numbers, calibration constants, response factors

and output parameters. The analyst initials and dates the resulting

output.

Data processing is checked by the group leader or by an analyst other

than the anayst who performed the data processing. The checker reviews

the data for the following:

o Utilization of the proper equations-

o Correctness of numerical input -

o Correctness of computationsi

o Correct interpretation of raw data (chronatographs, stripcharts, etc.) .

The checking process is thorough enough to verify the results. If the

checker disagrees with any part of the computations, the checker marks

through the number with a single line and places the revised number

above it. The originator reviews all changes made by the checker. If

the originator agrees with the change, no action is necessary. If

there is a disagreement between checker and originator, the differences

are resolved and the result is agreed upon. The checker initials and

dates all pages of the computations to indicate his agreement with the

calculation and the originator's agreement with any changes.

When data conputations are performed with a conputer, the checker

reviews all input entries. If the checker disagrees with any entry,fiR300660

the checker marks through the number with a single, line and places the

revised number above it. The originator reviews all changes as

discussed previously. The revised input entries are reprocessed. The

checker initials and dates all entry input sheets, original and

revised, to indicate agreement.

Review of data reports is performed to verify that reported information

corresponds with processed analytical results. A draft report is

prepared. After validation of processed data, steps taken to prepare

the draft report do not need to be validated.

Reported results contained in the draft report are checked against the

validated process data to verify transcription errors are not present.

The checker does not have to be independent of the work. Incorrect

entries are marked through with a single line and the correct entry

placed above it. The checker initials and dates all~'pages of the draft

report. The draft report is maintained to document the review.

After the draft report is typed, Laboratory Supervisors review the

report to verify typographical errors are not present. All errors are

marked through with a single line and the correct entry placed above.5laboratory Supervisors review the corrected report and jaends the report

to the Laboratory Itenager for final review. The Laboratory Manager

approves the report for issuance.

AR3Q066

i» 2.0 Office Data Validation

Analytical activities are performed" in a planned and controlled manner.

Performance" responsibility rests with _t_he Project Onager. Prior to

initiating activities, the Project £fenger discusses scope of work,-•-, |contractual and regulatory requirements, and applicable QA/QC

procedures with project personnel. At the request of the Project

Manager, this will be done by the QA Officer..

To provide evidence of satisfactory work performance and the basis for• t

information transmitted, external analyses and their results are

completely ..documented. Documentation may include calculations,

computer programs/ logs, drawings, and tables.

2.1 Calculations . .,_.„.._ „„. „_....,.„,,. .. ..... - - •> •

Calculations, as appropriate, include a statement of calculation

intent, description of methodology used, assumptions and their

justification, input data and equation references, numerical

calculations including units, and results. Input data may include:

o Regulatory requirements

o Bsrformance and operational requirements under variousconditions

o teterial, geological, environmental, and geotechnicalrequirements

o Results of field and laboratory testing or calculations

o Information obtained from external personnel or literatureand site data surveys.

Computer printout that become an integral part of calculations are

referenced in the calculations by run number or other unique means of

identi fication.

ftR300662

At the end of calculations, results are summarized to provide clarity.

Assignments for checking are made or approved by the Project Manger.

Verification is performed by an individual(s) other than the person(s)

who performed the original work or (specified the method or input

parameters to be used.) The individual (s) selected will have technical

expertise in the calculation subj ect. It is enphasi zed that a

numerical check is not sufficient. The checker is responsible for

every item on every sheet.

When calculations are performed utilizing a computer program, the input

data is checked as described in Section 13.1.

2-2 Logs, Drawings, and Tables __

The results may be presented in logs, drawings, and tables of various

forms. The format of logs and tables is governed by information to be

presented. Drawings are uniquely identified by drawing or figure

number and appropriate title. Standardized symbols and nationally

accepted drafting standards are used. References to 'other drawings and

sources of information are provided, as necessary.

Drawings signed and dated by the draftsperson performing the work and

the responsible member of the project group who has checked the

drawing.

flR300663

Revisions are noted on the original , drawing with a brief note* I

describing each revision. The note is signed and dated by the

draftsperson performing the wsrk and the repsonsible member of the

project group who has checked the revision.

Final subsurface logs are. verified by a responsible member of thet• iproject group. Verification provides that changes from original field

representative's logs to final log sheets are consistent with results

of laboratory testing or other investigations. Final log sheets are

checked and the checker initials and dates each sheets.

Indication of final drawing and revision approval is through signing

and dating of drawings by the Project Manager or a member of project

staff delegated this responsibility by the Project ffenager. Drawings

are not issued without completion of the checking cycle as evidenced by

the checker's signature.1 ....--.. h

2.3 Field Data Validation .. , -

Field data generated in accordance with the project work plan will

be validated by review of project documentation to check that all formsfspecified in the sampling plan and QAPP have been completely and

icorrectly filled out and that documentation exists for required

instrument calibration. This documentation will be considered

sufficient to provide proper procedures have been followed during the

field investigation.

Software Verification

Computer software used to acquire, process, or report data is verified

to demonstrate its intended functions are performed correctly.

Externally prepared prograns are accepted as valid. Verification by

NUS is not necessary.

Programs developed within NUS and externally prepared prograns modified

by NUS undergo a complete verification before being used. The

verification procedure is dependent upon the function of the software.

For software that only performs numerical manipulation, sample sets of

numbers are processed. Results are compared to results from hand

manipulation of the sample sets. The sample set is chosen so that all

program options are tested. Ability of the software to store and

manage files is also tested.

Software operational performance . for an instrument is tested by

processing standard materials through the system. Instrument response

is compared to the known result of standard materials.

The individual performing verification signs and dates computer outputs

and manual computations. The verifier's signature indicates acceptable

comparison of output and manual computations. When standard materials

are used for verification, the know values are included. All

documentation is maintained.

AR3QQ665

2.5 Recorded Entries . ::— ...:..-, n_ .;/t.-.. r - .; "

All entries made in benchbooks, data sheets, computation sheets, input

sheets, etc. are made in ink. No entry will be rendered illegible.

2-6 Hounding of Numbers , : .. .

Whenever a value needs to be rounded, the following procedures are

used:

o If the digit "following the digit to be rounded is greaterthan five, the digit to be rounded is raised to the nexthigher digit.

o If the digit following the digit to be rounded is less thanfive, the digit to be rounded remains as is.

o If the digit following the digit to be rounded is a five andno digits follow the five, and if the digit to be rounded isodd, the digit to be rounded is raised to the next higherdigit. If the digit to be rounded is even, the digit remainsas is.

o If- the digit following the digit to be rounded is a five,followed by other digits, the digit to be rounded is raisedto the next higher digit.

2.7 Analytical Reports

Analytical data will be reported as specified in CLP protocol. The

following information will be included in the data package:

o Efcraneters analysed, report units, values, and qualifiers.

o Sample number; laboratory name and code; contract number;case, SAS and SDG number; and corresponding lab sanple ID.

o Date of sample receipt and analysis./i

o Sanple matrix and level.

o Tentatively identified organic compounds and estimated values.

o Surrogate, matrix spike, matrix spike duplicate, and duplicaterecover ies.

o tethod blank results.

o GC/MS tuning and mass calibration.

o Initial calibration and continuing calibration check data

o GQ/MS internal standard areas*

o Pesticide evaluation standards summary.

o Efesticide/PCB confirmation data*

o AA and ICP CRDL standard data.

o ICP interference check data.

o Inorganic laboratory control sample data.

o Standard addition results.

o ICP serial dilutions data.

o Inorganics holding times.

o Inorganics instrument detection limits.

o ICP interelament correction factors.

o ICP linear ranges.

The following figures contain the reporting forms:

IIfIIIIIIIIIIIII

N,

APPENDIX K

DATA SUMMARY FORMS

DATA VALIDATION SUMMARY FORMS

DATA PACKAGE REPORTING FORMS

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9IX&AXIC IATA ¥AL1UT10K SUWWtY HP 1 if

ftate tevltw CompleteC«e No. m SSfte IUH-Xai^lt ftos.

4AS lo. IMIIII contract Lab

Contract w.Labt*tfif'

eOHCEPCTJUTIONIUTR1X "low Mtoil/solidaoueousether

0 MflW -K/U1II KUTEB

»Dever*• Keoion n

f COWEKTS

r pnonePT* •

ICPHoTSTng T1neCalibration Blanks.Initial CalibrationContinuing CalibrationPreparation BlankInterference Check SanpleLab Control SanpleLab Duplicateftatri* SpikeSerial Dilution

OK m ACTION COWEMTS

•

FU*NACEHolding TimeCalibration BlanksInitial CalibrationContinuing CalibrationPreparation Blanktab Control SancieLab DuplicatePatrii SpikeDuplicate InjectionsAnalytical Seifce

•

HERCUftY t CYM1DEHolding Tl»eCalibration Blankinitial CalibrationContinuing Calibrationpreparation BlankLab DuplicatePatrlx Spike

- —'s comrrrs:

•OOCUHENTAT10K ATTACHED (Set following P•»*»). MR30067U

ORGANIC DATA VALIDATION SUMMARY page 1 of•- '-'•• y*1 ^ T *

Date Review ConpletedCase No. SA5~Rb. Contract LabSite Name Contract Ho.Sancle Nos. Lab DPO

Reviewerfrom Region Phone

FTSV •»

CONCENTRATIONMATRIX 1soil/solidaqueousother

low med hi 9*1 MATRIX RELATED COMMENTS

VOLATILESGC/MS tuning--BFBInitial CalibrationContinuing CalibrationSurrogate RecoveryMatrix SpikesReagent BlanksHolding times

OK FYI ACTION COMMENTS

*

SEMI-VOLATILESGC/MS tuning— OFTPPInitial CalibrationContinuing CalibrationSurrogate RecoveryMatrix SpikesReagent BlanksHolding times

PESTICIDESInstrument PerformanceInitial CalibrationContinuing CalibrationSurrogate RecoveryMatrix SpikesReagent BlanksHolding times

OVERALL CASECoroound IdentificationData Concleteness

REVIEWER'S COMMENTS:

"DOCUMENTATION ATTACHED (see following pages)

3H3Q0675

U.S. EPA - CLPf1 COVER PAGE - INORGANIC ANALYSES DATA PACKAGEj

4 Lab Name: ______" ______ Contract: _____

I Lab Cods: _____ Case No.: ____ SAS No.: _____ SDG No.

SOW No. :

EPA Sample No. " T t? Sample ID.

Were ICP interelement corrections applied? Yes/No

Were ICP background corrections applied? Yes/NoIf yes-were raw data generated beforeapplication of background corrections? Yes/No

Comments:

Release of the data contained in this hardcopy data package and in thecomputer-readable data submitted on floppy diskette has been authorizedthe Laboratory Manager or the Manager's designee, as verified by thefollowing signature.

Lab Manager:

——— — «-_• r- rr-COVER PAGE - IN A K 3 U 0 6 7 6 7/3?

U.S. EPA - CLP

1 EPA SAMPLE NO,INORGANIC ANALYSIS'DATA SHEET ___________

Lab Name: _______ ________ Contract:

Lab Code: ____ Case No.: ____ SAS No.:____ SDG No.:

Matrix (soil/water): ____ - Lab Sample ID: __

Level (low/med): ____ . Date Received: __

% Solids: ____

Concentration Units (ug/L or mg/kg dry weight): ___

- 1CAS No. | Analyte

17429-90-5 I Aluminum7440-36-0 (Antimony7440-38-2 | Arsenic7440-39-3 | Barium7440-41-7 | Beryllium7440-43-9 | Cadmium7440-70-2 (Calcium7440-47-3 | Chromium7440-48-4 | Cobalt7440-50-8 (Copper7439-89-6 I Iron7439-92-1 1 Lead7439-95-4 (Magnesium7439-96-5 (Manganese7439-97-6 (Mercury7440-02-0 (Nickel7440-09-7 I Potassium7782-49-2 (Selenium7440-22-4 1 Silver7440-23-5 1 Sodium7440-28-0 [Thallium7440-62-2 (Vanadium7440-66-6 I Zinc

1 Cyanide1

1Concentration | C

Ii1iI11

' 111iI!1S1iii11i;!!11t

I

M Q

Color Before: ______ Clarity Before: ____ Texture:

Color After: ______ Clarity After: ____ Artifacts:

Comments:

FORM i - ik flR300677 7/37

U.S. EPA - CLP

! . 2AINITIAL AND CONTINUING CALIBRATION VERIFICATION

Lab Name: _______ ____ Contract:

Lab Code: ____ Case No.: ____ SAS No.: ,__ SDG No.:

Initial Calibration Source: _________

Continuing Calibration Source: _________

Concentration Units: ug/L :

' ' i MInitial Calibration | Continuing Calibration I \

I (Analyte | True Found %R(1)True Found %R(1) Found %R(1) i i M

1 I Aluminum 1 ij 1 Antimony I 1

1 Arsenic [ jf (Barium i 1i (Beryllium! I1 (Cadmium I [

1 Calcium j j| {Chromium j j1 (Cobalt 1 !

I Copper _ | |I llron 1 11 I Lead 1 1(Magnesium) i

j (Manganese] f(Mercury 1 I(Nickel I 1

. I Potassium 1 11 Selenium ] t

* (Silver i 1I Sodium | !

t (Thallium f 1I (Vanadium I 1IZinc | |

f 1 cyanide 1 I1 1 1 1

-

™

(1) control Limits: Mercury 80-120; Other Metals 90-110; cyanide 85-115,

7/87

• U.S. EPA - CLP

J ! . 2§CRDL STANDARD FOR AA AND ICP

Lab Name: _______________ ___ Contract::

Lab Code: ____ Case No,: ____ SAS No.;; . SDG No.: __

AA CRDL Standard Source: _________•

ICP CRDL Standard Source: -______i . • . _ - < - - . -

Concentration Units: ug/L ri———j n————————| | CRDL Standard for AA | | CRDL Standard for ICP( I I I Initial " Finalj Analyte | True Found %R j j True Found %R Found %R

.11.1 Aluminum 11 Antimony 1(Arsenic I1 Barium 1| erylliumj

.dmium j! Calcium j(Chromium I1 Cobalt 11 Copper |I Iron |(Lead 1I Magnesium jI Manganese I1 Mercury 1(Nickel 1I Potassium 11 Selenium |1 Silver 1(Sodium |(thallium 1(Vanadium |IZinc 11 = 1

f I I 1 I I1 I I 1 I I1 I I I I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 1 11 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 II 1 1 11 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I1 I I 1 I I

n ««,„-^

I U.S. EPA - CLP

{ ' BLANKS

iLab Name: __________ Contract:

Case No.: "__ SAS No.: . SDG No.

Preparation Blank Matrix (soil/water): ____

Preparation Blank Concentration Units (ug/L or ag/kg):

1 1 I '| I Initial |( | Calib. | Cont.1 | Blank 1(Analyte | (ug/L) C| lI " 1 I1 Aluminum | 1 |I Antimony I i _|_1 Arsenic I I II Barium j 1 j .1 Beryllium! 1 J(Cadmium I 1 I1 Calcium I ( I[Chromium j j j(Cobalt 1 I (1 Copper 1 ( (I Iron 1 ( 1(Lead 1 1 I.Magnesium! 1 I'Manganese) 1 I1 Mercury 1 1 1' Nickel | I |Potassium! 1 j

i Selenium I I j(Silver 1 1 |Sodium I I 1.Thallium I 1 i(Vanadium I 1 |Zinc I I |.cyanide 1 1 !1 1 (I

LmB:cling Calib.Lank (ug/L

2

raiIC

tion3 C

Prepa-rationBlank C

1

M

•_

FORM in-IN flR300680 7/87

U.S. EPA - CLP

4ICP INTERFERENCE CHECK SAMPLE

Lab Name: Contract:

Lab Code: _____ Case No: ____ " SAS No.: _____ SDG No.

ICP ID Number: ICS Source: __

Concentration Unit$:_ug/iL

1| True| Sol. Sol.

Analyte | A AB1

Aluminum I IAntimony 1 1Arsenic 1 jBarium j jBeryllium! jCadmium I jCalcium I jChromium j jCobalt | |Copper. I |iron I !Lead I [Magnesium! jManganese | iMercury 1 1Nickel 1 IPotassium! 1Selenium 1 1Silver 1 1Sodium | 1Thallium j IVanadium j IZinc | I

I 1

Initial Foun<Sol. Sol.A AB

(I111i!11111iI11I1II1h11

i

%R

i

iF

: 3Sol.A

Final FouneSol.AB

1

%R

FORM IV - IN fl R $ 0 0 fi R I V87

U.S. EPA - CLP

EPA SAMPLE

Lab Name: ._____________ Contract:

Lab Code: _____ Case No.: ____ SAS No.: ____ SDG No.:

Matrix (soil/water): ____ - Level (low/med):•

Concentration Units (ug/L or mg/kg dry weight):

111 -| Analyte1| Aluminum| Antimony_1 Arsenic1 Barium1 BerylliumI Cadmiumj Calcium1 Chromium1 Cobalt| Copperllron(Lead1 Magnesium| Manganese1 Mercury1 Nickel1 Potassium| Selenium(Silver(Sodium|Thalliu«_j Vanadium(ZincI Cyanide1

Comments :

1Control |Limit j Spiked Sample%R | Result (SSR)

1111111I111111111111111111

C

"

. sampleResult (SR)•

C. spikeAdded (SA) %R Q

>•»

<

M

r

FORM V (PART 1)-IN flRJ00682 7/87

. U.S. EPA - CLP

SB , EPA SAMPLE NOPOST DIGEST SPIKE SAMPLE RECOVERY .———________

! Lab Name: ___________________ Contract:

Lab Code: ____. Case No.: ____ SAS No.: ____ SDG No.:

Matrix (soil/water): ____ - Level (low/med):

Concentration Units: ug/L

! i I Control1 L Limit|Analyte |~ %R

' {Aluminum 11 Antimony \

! 1 Arsenic 1J 1 Barium 1

f Beryllium 1i I cadmium I\ l Calcium j| Chromium |

•' Cobalt I-pper 1 _

i— .on... I1 Lead 1

I (Magnesium!' ! Manganese I

i Mercury I\ ( Nickel (i (Potassium I

1 Selenium Ij {Silver Ij (Sodium _.. i

(Thallium 1. (Vanadium I

1 Zinc 11 1 Cyanide (' 1

1 I !

Comments :

j

Spiked SampleResult (SSR)

4

CSample

Result (SR)

.

•

i

cSpike

Added (SA) %R

_

Q M

„

FORM V (PART 2) - IN 7/87

U.S. EPA - CLP

6 EPA SAMPLE NO,DUPLICATES

Lab Name: ________________ Contract:

Lab Code: _____ Case No.: ____ SAS No.: _____ SDG No.:

Matrix (soil/water): ____ - Level (low/med) :

% Solids for Sample: _____ % Solids for Duplicate:

Concentration Units (ug/L or mg/kg dry weight): ___

1 1 iI - I control || Analyte | Limit (1 ! 1{ Aluminum f 11 Antimony 1 1(Arsenic 1 1j Barium i I1 Beryllium I (1 Cadmium 1 11 Calcium i I1 Chromium 1 jI Cobalt | [I Copper 1 1( Iron I 11 Lead i 1(Magnesium! I| Manganese | |1 Mercury 1 11 Nickel i 1(Potassium! j(Selenium 1 j1 Silver 1 f1 Sodium ( I(Thallium ( I(Vanadium I I1 Zinc I |1 Cyanide i i1 i 1

Sample (S)

_

c.\Duplicate (D) C RPD Q M

1

4

FORM VI- i* SR30068U 7/87

^U.S. EPA - CLP

7LABORATORY CONTROL SAMPLE

Lab Name: _________ ___ Contract:

Lab Code: _____ Case No.: ____ SAS No.: _____ SDG No,•

Solid LCS Source: _________

Aqueous LCS Source: _________

AnalyteAqueous (ug/L) | Solid (mg/kg)

True Found %R j True Found C Limits %R

( Aluminum_|Antimony_I ArsenicI Barium(Berylliumt <?admium

IciumI -aromium1 CobaltI Copper _.,.(Iron(Lead(Magnesium| Manganese1 Mercury1 Nickelj Potassium| Selenium1 Silverj Sodium| Thalliumj VanadiumIZincI Cyanide1

11111111111111111111111I1

1111111111111111111111111

1|

-I._l.-I.J.-I.-I._l._lJ.-I,

FORM VII -IN flR300S85

U.S. EPA - CLP

8STANDARD ADDITION RESULTS

1 Lab Name: _______________ Contract:

Code: ____ Case No.: ____ SAS No.: _____ SDG No.:


1 11 EPA |j Sample |"| ' No. (An1 11 11 11 11 11 11 11 11 1^V i1 11 1M 1

1 11 1! 11 11 11 11 11 1! 1! 11 1> I

Dil0 ADDABS CON

,

1 ADDABS

2CON

ADDABS

3CON

ADDABS

FinalCone.

-

" r

1

iQlJJ

1J

1JJ.1J

i

JJ

1111

,11111I

,11

FORMVTII-INJ J5R300686 7/87

1 ICP SERIAL DILUTIONS

1 me: ______M____ Contract:

U.S. EPA - CLP

SPA SAMPLE NO.

-ode: ____ Case No.: ____ SAS No.: ____ SDG No.:

Lx (soil/water): ____ - Level (low/med) :


1 1 II! | (I Initial Sample

lAnalyte || Result (I) Ci '1 II! (Aluminum 1 1 1

(Antimony 1 1 j1 Arsenic 1 1 1

{ 1 Barium i 1 11 1 Beryllium 1! I

1 Cadmium I I 11 calcium 1 1 11 Chromium I I 11 Cobalt 1 1 I

! 1 Copper I I 1i 1 Iron 1 1 1

1 Lead II - 1I Magnesium! 1 1I Manganese I j I(Mercury 1 I 11 Nickel I 1 1I Potassium I 1 1I Selenium I I 1(Silver II 1I Sodium 1 1 1(Thallium 1 1 1(Vanadium 1 1 1

' (Zinc II 1i 1 II 1

SerialDilutionResult (S) C

Differ-ence Q :M

300687

U.S. EPA - CLP

I 10* HOLDING TIMES

Contract:

Lab Code: ____ Case No.: ____ SAS No.: _____ SDG No.:

1 1 11 1 1| • EPA • | |. Date[Sample No. j Matrix (Received1 1 11 1 1

1 11 1 1

1 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 »1 11 11 1

1 1I Mercury (MercuryI Prep (Holding1 Date j Time1 11 11 11 11 11 11 !1 11 f1 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 1

CyanidePrepDate

Cyanide(-Holding)

Titte |11!

111111I111f1111111

FORM X-IH fiRHH

U.S. EPA - CLP

11INSTRUMENT DETECTION LIMITS (QUARTERLY)

3 Name:

3 Code: Ca:

? ID Number:

ime AA ID Number:

rnace AA ID Number:

-

1!I(AnalyteiI Aluminum^1 Antimony^I Arsenic _j Bariumj BerylliumI Cadmium _[ Calcium _j Chromiumi Cobalt _1 Copper _miillronILeadj Magnesium![ Manganese |I Mercury ]1 Nickel ~|j Potassium![Selenium |(Silver 1I Sodium 1IT&alliumJ[Vanadium jfZinc |I i

ments :

•e No. :

Wave-length(nm)

...

i

Back-ground

, ,

ContraSAS No

Date:

'

CRDL(ug/L)

200601020055

5000105025100S

5000150.240

5000510

5000105020

ct:.. .

•

r

IDL(ug/L) M

SDG No.:

-

-

«

————— |——————————

FORM XI -IN flR3Q0689 7/87

JJ.S. EPA - CLP

12AICP INTERELEMENT CORRECTION FACTORS (QUARTERLY)

! Lab Name: __________________. Contract:

Lab Code: ; Case No.: ____ SAS No.: ____ SDG No.:

ICP ID Number: _________ Date:

IiI(Analyte1I Aluminum| Antimony^(Arsenic _j Bariumj Beryllium[Cadmium _1 Calcium _j Chromium•bait

pper __(IroniLead(MagnesiumI Manganesei MercuryNickel

f Potassiumj SeleniumSilver. Sodium|Thallium_'VanadiumZinc[

Wave-length(nm)

ii - iji1 Al1111111111111111111111111

iterelement Correction

Ca Fe

111111111——— 1 ———1111111111111

Factors for: |

Mg ]1

1 11 11 11 11 11 11 11 111 11 11 11 11 11 11 11 11 11 11 11 11 11 11 1

osiments:

FORM XII (PART 1) - IN flR300690 V87

U.S. EPA - CLP

12BICP INTERELEMENT CORRECTION FACTORS (QUARTERLY)

Lab Name:

Lab Code: Case No

ICP ID Number:•

1 i M1 ( Wave-- | ( UI " 1 length 1 |(Analyte I (nm) i I1 f I!(Aluminum 1 1 (1 Antimony 1 1 (1 Arsenic f ( !1 Barium I I 1! Beryllium! I 1! cadmium I I 1I Calcium ( | I! Chromium 1 I I1 -»balt i I (

pper I 1 (1 iron 1 1 !1 Lead 1 1 !| Magnesium! ! ((Manganese! I I1 Mercury I 1 1(Nickel 1 ||(Potassium! I 11 Selenium I 1 11 Silver ! - III Sodium | | I(Thallium I 1 1(Vanadium 1 1 11 Zinc 1 1 11 I II

.. .

at er element

Contract :SAS No. :

Date:

Correction

SD<•

Factors fo:

I I I N I

3 No. :

r:

^Bpr

Comments:

FORM XII (PART 2) - IN 7/87

flR30069I

Comments:

U.S. EPA - CLP

13ICP LINEAR RANGES (QUARTERLY?

! Lab Name: __________ • Contract:

j Lab Code: • Case No.: ____ SAS No.: _____ SDG No.

* ICP ID Number: - Date:

I I Integ. | |! . . | Time J Concentration j(Analyte | (Sec.) ( (ug/L) | M1 , I ______ I __________ f_I Aluminum |

_I Barium IBeryllium!

; Cadmium_ _ |Calcium _ |Chromium_ |Cobalt __ |Copper __ |Iron ___ (Lead i(Magnesium)(Manganese!|Mercury_J(Nickel f|Potassium|{Selenium |

_ISodium __ |IThallium || Vanadium"!

!

; flR300692I FORM XIII - IK 7/87

1A EPA SAMPLE NO,VOLATILE ORGANICS ANALYSIS DATA SHEET ____________

II

Lab Name: _____ Contract:________ |____

Lat> Code: _____ Case No.: . SAS No.: ______ SDG No.:•"' "' —— — -— _ . " .Matrix: (soil/water)____ Lab Sample ID: __

Sample wt/vol: _____(g/fflL)___ Lab. File ID: __

Level: (low/med) ____ Date Received: __

% Moisture: not dec.____ Date Analyzed: __

i Column: (pack/cap) ____ Dilution Factor:

CONCENTRATION UNITS:CAS NO. COMPOUND (ug/L or ug/Kg)_____

I74-87-3———————Chloromethane__74-33-9———————Bromomethane__75-01-4——————Vinyl Chloride^75-00-3——————Chloroethane75-09-2——————Methylene Chloride,67-64-1——————Acetone75-15-0——————-Carbon Disulfide_________75-35-4———————1,1-Dichloroethene________75-34-3———————1,1-Dichloroethane________540-59-0——————1,2-Dichloroethene (total)_67-66-3———————Chloroform107-06-2—————l,2-Dichloroethane_78-93-3———————2-Butanone71-55-6———————1,1 r l-Trichloroethane_56-23-5——————-Carbon Tetrachloride_^108-05-4—————-Vinyl Acetate75-27-4——————Bromodichloromethane78-87-5———————1,2-Dichloropropane10061-01-5————cis-l,3-Dichloropropene_79-01-6——————-Trichloroethene124-48-1—————-Dibromochloromethane_79-00-5—————l,l,2-Trichloroethane_71-43-2———-——Benzene10061-02-6———~trans-l,3-Dichloropropene_75-25-2——————Bromoform108-10-1——————4-Methyl-2-Pentanone____591-78-6—————2-Hexanone____________127-18-4——————Tetrachloroethene______79-34-5———————l,l/2/2-Tetrachloroethane-108-88-3—————Toluene108-90-7——————Chlorobenzene_100-41-4—————'Ethylbenzene_J100-42-5—————styrene1330-20-7—————Xylene (total)

FORM I VOA 1/87 Rev,

flR300693

"IB EPA SAMPLE NO.SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET

_ La

Ra

Lab Name: Contract:

Code: Case No.: SAS No.: SDG No.:

» Matrix: (soil/water)____ Lab Sample ID:

f Sample wt/vol: _____(g/n»L)___ Lab File ID:

Level: (low/med) ___ Date Received:

» % Moisture: not dec.____ dec.____ Date Extracted:I ———— ————Extraction: (SepF/Cont/Sonc) ___ Date Analyzed:

GPC Cleanup: (Y/N)__ pH:___ Dilution Factor:

CONCENTRATION UNITS:CAS NO. COMPOUND (ug/L or ug/Kg)______

108-95-2——————Phenol_______________111-44-4——————bis(2-Chloroethyl)ether_95-57-8————————2-Chlorophenol541-73-1——————l,3-Dichlorobenzene_106-46-7——————1,4-Dichlorobenzene"100-51-6——————Benzyl alcohol95-50-1———————1,2-Dichlorobenzene95-48-7———————2-Methylphenol108-60-1——————bis(2-Chloroisopropyl)ether106-44-5——————4-Methylphenol621-64-7——————N-Nitroso-di-n-propylamzne_j67-72-1———————Hexachl or oe thane_________|98-95-3——————Nitrobenzene____________|78-59-1———————Isophorone88-75-5———————2-Nitrophenol____105-67-9——————2,4-Dimethylphenol_65-85-0——————-Benzoic acid111-91-1—————bis (2-Chloroethoxy) methane^120-83-2——-—~2,4-Dichlorophenol_120-82-1—————1,2 f 4-Trichlorobenzene91-20-3——————Naphthalene,106-47-8——-——4-Chloroaniline87-68-3—————-Hexachlorobutadiene___59-50-7—————4-Chloro-3-nethylphenol91-57-6———————2-Methylnaphthalene77-47-4——————Hexachlorocyclopentadiene_ga-06-2—————-2 f 4,6-Trichlorophenol__"95-95-4——————2,4,5-Trichlorophenol___91-58-7——————2-Chloronaphthalene____88-74-4——————2-Nitroaniline131-11-3——————Dimethylphthalate,208-96-8—————-Acenaphthylene606-20-2——————2,6-Dinitrotoluene

FORM I SV-1 1/87 Rev,

1C EPA SAMPLE NO.SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET _________

II

Lab Name: Contract: . I

Lab Code: _______ Case No.: _____ SAS No.: ... SDG No.:

Matrix: (soil/water)____ Lab Sample ID: __

Sample wt/vol: _____(g/*L)___ Lab File ID: __


% Moisture: not dec. dec. Date Extracted:

Extraction: (SepF/Cont/Sonc) ____ Date Analyzed:


CONCENTRATION UNITS:CAS NO. COMPOUND (ug/L or ug/Kg)_____

99-09-2 ——————— 3-Nitroaniline83-3 2-9 —————— Acenaphthene51-28-5 ——————— 2 , 4-Dinitrophenol100-02-7 —————— 4-Nitrophenol132-64-9 —————— Dibenzofuran121-14-2 —————— 2,4-Dinitrotoluene84-66-2 —————— -Piethylphthalate7005-72-3 ————— 4-Chlorophenyl-phenylether _

100-01-6 —————— 4-Hitroaniline534-52-1 —————— 4 , 6-Dinitro-2-methylphenol86-30-6 ——————— N-Nitro»odiphenylamine (1) _101-55-3 —————— 4-Bromophenyl-phenylether118-74-1 —————— Hexachlorobenzene87-86-5 —————— Pentachlorophenol

120-12-7 —————— Anthracene84-74-2 —————— Di-n-butylphthalate206-44-0 —— • — —— Fluoranthene129-00-0 ————— Fyrene85-68-7 ——— — —— Butylbenzylphthalate91-94-l——f- — -S.S'-Dichlorobenzidine56-55-3 — • ———— Benzo (a) anthracene218-01-9 —————— Chrysene117-81-7 —————— bis (2-Ethyih.xyl) phthalat.117-84-0 —————— Di-n-octylphthalate205-99-2 ————— Benzo (b)fluoranthene207-08-9 —————— Benzo (k) f luoranthene50-32-8 —————— Benzo(a)pyrene193-39-5 —————— Indeno (1,2, 3-cd) pyrene53-70-3 ——————— Dibenz (a,h) anthracene191-24-2 —————— Benzo (g,h,i)perylene

111111111111111111111111I1

' 1111111i

(1) - Cannot be separated from Diphenylamine

FORM I SV-2 1/87 Rev,

UR300695

, ID . . . „ , _.._,..-=. EPA SAMPLEPESTICIDE ORGANICS ANALYSIS DATA SHEET

kLab Name: __ _____ Contract

Lab Code: ______ Case No.: _____ SAS No.: ______ SDG No.:


Sample wt/vol: _____(g/mL)___ Lab File ID: __


% Moisture: not dec.____ dec.____ Date Extracted:

Extraction: (SepF/Cont/Sonc) ____ Date Analyzed:


CONCENTRATION UNITS:CAS NO. COMPOUND (ug/L or ug/Kg)______

319-84-6———————alpha-BHC_________319-85-7———————beta-BHC_______319-86-8———————delta-BHC _____58-89-9———-———gamma-BHC (Lindane)76-44-8——————Heptachlor_______'309-00-2——————Aldrin1024-57-3—————Heptachlor epoxide959-98-8—————Endosulfan I____~60-57-1——————Dieldrin_____72-55-9————————4,4 '-DDE__________72-20-8——————Endrin33213-65-9————Endosulfan II72-54-8————————4,4'-ODD1031-07-8—————Endosulfan sulfate50-29-3————————4 , 4 ' -DOT________"72-43-5——————Methoxychlor__53494-70-5————Endrin ketone_5103-71-9——»——alpha-Chlordane_5103-74-2—————gamma-Chlordane~8001-35-2————Toxaphene12674-11-2————Aroclor-101611104-28-2—————Aroclor-122l"11141-16-5—————Aroclor-1232"53469-21-9—————Aroclor-1242"12672-29-6—————Aroclor-1248~11097-69-1—————Aroclor-125411096-82-5—————Aroclor-1260"

FORM I PEST 1/87 Rev.'. /1R300S96

IE EPA SAMPLE NO.VOLATILE ORGANICS ANALYSIS DATA SHEET _______________TENTATIVELY IDENTIFIED COMPOUNDS |"

ILab Name: _______________ Contract:__________ |_____

Lab Code: ____._ Case No.: ____ SAS No,: _____ SDG No.:


Sample wt/vol: _____(g/fflL)___ Lab File ID: __


% Moisture: not dec.____ Date Analyzed: __

Column: (pack/cap) ____ Dilution Factor:

CONCENTRATION UNITS:Number TICs found: _____ (ug/L or ug/Kg)____

!GAS NUMBER | COMPOUND NAME

1. 12. 13. 14. 15. 16. 17. 18. 19. 110. |11. 112. I13. 114. 115. 116. |17. 113. I19. 120. 121. I22. I23. |24. I25. |26. I27. |28. |29. |30. |

1

RT EST. CONC.•»»•••;— -B» -— = 3B*»»—B — -m

,

Q

W—41

_ mFORM I VOA-TIC 1/87 Rev.

BR30Q697

PLa

1 IF EPA SAMP!_£ NOSEMXVOIATILE ORGANICS ANALYSIS DATA SHEET ______________

TENTATIVELY IDENTIFIED COMPOUNDS | '< I

Lab Name: __ ______ Contract:___._____ |_____

b Code: Case No.: _____ SAS No.: ____ SDG No.:! —————————" ' ——————— ' I ————————

' Matrix: (soil/water)____ Lab Sample ID: __

j Sample wt/vol: _____(g/mL)___ Lab File ID: __


I % Moisture: not dec.____ dec.____ Date Extracted:__s •• —— - - - — _ "Extraction: (SepF/Cont/Sonc) ____ Date Analyzed: __

' GPC Cleanup: (Y/N)__ pH:___ Dilution Factor:

1 CONCENTRATION UNITS:Number TICs found: ____ (ug/L or ug/Kg)_____

CAS NUMBER

1.2.3.

f 5:6.7.8.9.10.11.12.13.14.15.16.17.18.19.20.21.22.23.24.25.26.27.28.

|30.'

1COMPOUND NAME | RT

1111111111111111111111111111111

EST. CONC.

'

Q

FORM I SV-TIC 1/87 Rev.i AR3Q0698

2AWATER VOLATILE SURROGATE RECOVERY

Lab Name: ... ;______________ Contract:iLab Code: _____ Case No.: _____ SAS No.: ______ SDG No.:

| 010203!

I 04]* 05|

06|07|

? 08109 |10|

f "I-f 12|

131! "iI 15|

16|17 |

f 18119120 |

i 21|1 22|

23|] 24!f 25|

26|77 iI *' I28|,

1 29'301

EPASAMPLE NO.

SI(TOL) #

S2(BFB) 1

S3(DCE) *

OTHER TOTOUT

QC LIMITSSl'(TOL) « Toluene-d8 (88-110)S2 (BFB) - Bromofluorobenzene (86-115)S3 (DCS) « l,2-Dichloroethane-d4 (76-114)

I Column to be used to flag recovery values *

* Values outside of contract required QC limits

D Surrogates diluted out

page _ of _FORM II VOA-1 1/87 Rev.

flR30Q699

Lab Name: _______________ Contract,:

fLab Code: ______ Case No.: ____ SAS No.: _____ SDG No.:

Level:(low/med) ____

Oil02 |03|04|05 |06 |07 |08 |09 i10|HI12 |

17 |18|19120|21|22|23|24 i25126|27j28!29j30

EPA | SISAMPLE NO. | (TOL)#

aB-S-Bac gatag-gss-s -s j ae»=:z=«

111111111111111111111111111

- 111

S2 | S3(BFB)#| (DCE)#

1111|11111111111111I1111111111

OTHER

3SSSS=3S_3

TOTOUT

' QC LIMITSSI (TOL) » Toluene-d8 (81-117)S2 (BFB) - Bromofluorobenzene (74-121)S3 (DCE) « l,2-Dichloroethane-d4 (70-121)

# Column to be used to flag recovery values '

* Values outside of contract required QC limits


page ofFORM II VOA-2 1/87 Rev,

AR3007QQ

2CWATER SEMIVOLATILE SURROGATE RECOVERY

Lab Name: ___ _______ Contract:

Lab Code: ______ Case No.: ____ SAS No.: _____ SDG No.:

i

| EPA | SI| SAMPLE NO. | (NBZ)#

Oil 1021 103! 1041 1051 !061 1071 I081 !091 I101 |111 1121 I131 1141 I151 I16| |17! I181 |191 1201 |211 I22| |23| I241 I251 I261 I271 I281 I291 I301 I

S2(FBP) *

S3(TPH) |

S4(PHL)#

S5(2FP)#

S6(TBP) f

OTHER TOTOUT

1

111

^

QC LIMITSSI (NBZ) * Nitrobenzene-d5 (35-114)S2 (FBP) - 2-Fluorobiphenyl (43-116)S3 (TPH) » Terphenyl-dl4 (33-141)S4 (PHL) « Phenol-d5 (10-94) .S5 (2FP) * 2-Fluorophenol (21-100) '36 (TBP) * 2,4,6-Tribromophenol (10-123)

# Column to be used to. flag recovery values* Values outside of contract required QC limitsD Surrogates diluted out

pag© _ of _FORM II SV-1 1/87 Rev.

flR30Q7Qj

*2ff * 'SOIL SEMIVOLATILE SURROGATE RECOVERY"

Lab Name: __ ____ Contract:

FLab Code: _______ Case No.: _____ SAS No.: ______ SDG NoI , ' ; '1 Level:(low/med)____

1I-

oil

EPA | SI | S2 | S3 | S4 | S5SAMPLE NO. | (NBZ)f | (FBP)#| (TPH)f | (PHL)#| (2FP) *

1 I 1 1 1

1 1 1 1 1021 1 1 1 1 1031 1 1 1 1 1041 1 1 1 1 10 5 1 I I I I . I061 1 1 1 1 1071 1 1 1 1 1081 1 1 1 1 1091 1 1 1 1 1101 1 1 1 1 1HI 1 1 1 1 1121 1 I 1 1 1131 1 1 1 1 1141 1 1 1 1 1151 1 1 1 1 1161 1 1 1 I 1171 1 1 1 1 1181 1 1 1 1 1191 1 1 1 1 120| 1 1 1 1 1211 1 1 1 1 1221 1 1 1 1 123|_ 1 1 1 1 1241 1 1 1 1 125f -1- 1 1 1 12 6 1 . 1 1 1 127 L 1 1 1 1 1281 1 1 1 1 12 9 1 I I 1 1 130|_ 1 1 1 1 1

S6 | OTHER |TOT(TBP) # j | OUT==- — | ==____ | _ —

1 11 11 11 11 11 11 11 11 1

1 11 11 11 11 11 11 11 11 11 11 11 1! 11 11 11 11 11 11 11 1

QC LIMITSSI (NBZ) Nitrobenzene-d5 (23-120)S3 (FBP) 2-Fluorobiphenyl (30-115)S3 (TPH) Terphenyl-dl4 (18-137)S4 (PHL) Phenol-d5 (24-113) ,S5 (2FP) 2-Fluorophenol (25-121) 'S6 (TBP) 2,4,6-Tribromophenol (19-122)

f Column to be used to. flag recovery values* Values outside of contract required QC limitsD Surrogates diluted out

page _ of _ _ _ _ _ _ . .FORM II SV-2 1/87 Rev.

flR300702

2EWATER PESTICIDE SURROGATE RECOVERY

Lab Name: _________________ Contract:

Lab Code: ___ Case No.: ____ SAS No.: .. .._.. SDG No,

| EPA| SAMPLE NO.)______»»

Oil02103104!05|06|07|OS!09|10111112113114|15|16|17118119120|21122123|24125126127|28129|301

SI(DBC) *

.

OTHER

W, "f BBia*! ^

ADVISORYQC LIMITS

SI (DBC) - Dibutylchlorendate (24-154)

# Column used to flag recovery values

* Values outside of QC limitsD Surrogates diluted out

page _ of _FORM II PEST-1 1/87 Rev.

flR30Q7Q3

2FSOIL PESTICIDE SURROGATE RECOVERY

Lab Name: ________________ Contract:__

ib Code: ______ Case No.: _____ SAS .Mp..:....,_____ SDG No,

Level:(low/med)____

| EPA| SAMPLE NO.»«a3 ========

on02103104105|06|07|08|09|10|11112113114115|16|17118119120|21122)23124125126127|28|291301

SI(DBC)#K3S3B:-5S

OTHER

JK B Bgj J,. Ji

ADVISORYQC LIMITS

SI (DBC) - Dibutylchlorendate (20-150)

I Column to be used to flag recovery values,i* Values outside of QC limits


page _ of _FORM II PEST-2 1/87 Rev.

1 flR30Q7Qtf

, 3BSOIL VOLATILE MATRIX .SPIKE/MATRIX SPIKE DUPLICATE RECOVERY

Lab Name: ___ _____ Contract; _,... .-

FLab Code: ____ Case No.: _____ SAS No.: ______ SDG No,. —•'•' -—-— i "Matrix Spike - EPA Sample No.: _________ Level:(low/med)

COMPOUND

1, 1-DichloroetheneTr i chl or oe theneBenzeneTolueneChlorobenzene

1 SPIKE| ADDED1 (ug/Kg)

« _ii!111

| SAMPLE| CONCENTRATION1 (ug/Kg)

111111

MSCONCENTRATION

(ug/Kg).-.« ——— _^____

MS | QC% i LIMITS

REC #| REC.

159-172162-137166-142159-139160-1331

| SPIKE | MSD 1 MSD | || ADDED | CONCENTRATION | % | % | QC L:

COMPOUND | (ug/Kg) | (ug/Kg) | REC #| RPD #| RPDS— =___= 3 — -* ——— ==« | =S_

1, 1-Dichloroethene |Trichloroethene jBenzene |Toluene |Chlorobenzene |

1 1 | | 221 i | | 241 | | | 21( I i ! 211 I i I 21

1 1 i l l

CMITSREC.

59-17262-13766-142:59-139160-133!

i


* Values outside of QC limits


COMMENTS:

FORM III VOA-2 1/87 Rev,

. ! 5R3007Q6

3CWATER SEMIVOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY

Lab Name: _______________ Contract:_________

Lab Code: _______ Case No.: _____ SAS No.: ______ SDG No.:

Matrix Spike - EPA Sample No.:

COMPOUNDaimm-K-BxacK mac m a:»3B3E=35ss = .Essssssm

Phenol2-Chlorophenol1 , 4-DichlorobenzeneN-Nitroso-di-n-prop. (1)1,2, 4-Trichlorobenzene4-Chloro-3-methylphenolAcenaphthene4-Nitrophenol2 , 4-DinitrotoluenePentachlorophenolPyrene

SPIKE | SAMPLEADDED | CONCENTRATION(ug/L) | (ug/L)

i1111!!111I1

MS | MS | QCCONCENTRATION | % | LIMITS

(ug/L) | REC #| REC.

1 112- 89;! 127-12311 136- 97!1 141-116'I [39- 98!I 123- 97;I 146-1181I 110- 801I 124- 96I | 9-103I 126-1271 I

COMPOUND

Phenol2-Chlorophenol1 , 4-DichlorobenzeneN-Nitroso-di-n-prop. (1)1,2, 4-Trichlorobenzene4-Chloro-3-methylphenolAcenaphthene4-Nitrophenol2 , 4-DinitrotoluenePentachlorophenolPyrene

SPIKEADDED(ug/L)

MSDCONCENTRATION

(ug/L)

MSD |* 1 %

REC #| RPD #

111111111111

QC LRPD

4240233828423150385031

IMI_y i| REC. 1i|12- 89127-123-|36- 97!| 41-116139- 98!|23- 97(146-1181|10- 80)|24- 96|| 9-103||26-127|1 1

(1)' N-Nitroso-di-n-propylaaine

# Column to be used to flag recovery and RPD values with an* asterisk* Values outside of QC limits

RPD:____ out of _____ outside limitsSpike Recovery:____ out of ____ outside limits

COMMENTS:

FORM III SV-1 1/87 Rev,

fiR300707

3DSOIL SEMIVOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY

Lab Name: ____ Contract:

FLab Code: ______ Case No.: ____ SAS No.: _____ SDG No.:

Matrix Spike - EPA Sample No.: _________ Level:(low/med) _

COMPOUND

Phenol2 -Chlorophenol1 , 4-DichlorobenzeneN-Nitroso-di-n-prop. (1)1,2, 4-Trichlorobenzene4-Chloro-3-methylphenolAcenaphthene4-Nitrophenol2 , 4-DinitrotoluenePentachlorophenolPyrene

SPIKEADDED(ug/Kg)

SAMPLECONCENTRATION

(ug/Kg)MS | MS | QC

CONCENTRATION | % | LIMITS(ug/Kg) | REC ft REC.

! 126- 9C1 [25-1021 [28-104i [41-1261 138-107I 126-1031 131-1371 t 11-1141 128- 89I 117-109I 135-142i !

1 SPIKEj ADDED

COMPOUND | (ug/Kg)

Phenol j2 -Chl orophenol I1 , 4-Dichlorobenzene |N-Nitroso-di-n-prop. (i) I1,2, 4-Trichlorobenzene 14-Chloro-3-methylphenol jAcenaphthene I4-Nitrophenol 12 , 4-Dinitrotoluene IPentachlorophenol jPyrene I

i

MSD | MSDCONCENTRATION | *

(ug/Kg) | REC *

111111111111

1% 1 QC

RPD #| RPD_ j

1 35I 501 27i 381 23I 331 19! 501 47i 471 36i

LIMITS| REC.

-I——— -|26- 90125-102128-104141-126138-107126-103131-137111-114|28- 89117-109[35-142!

(1) N-Nitroso-di-n-propylamineI Column to be used to flag recovery and RPD values with an. asterisk* Values outside of QC limits

RPD:_____ out of _____ outside limitsSpike Recovery:____ out of ____ outside limits

COMMENTS:

FORM III SV-2 1/87 Rev.

' fl~R3Q07Q8

3EWATER PESTICIDE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY

Lab Name: _______________ Contract:________


Matrix Spike - EPA Sample No.: _________

COMPOUND

Lindane

I SPIKE| ADDED

- 1 (ug/L)

1

| SAMPLE| CONCENTRATION1 (ug/L)

1Heptachlor 1 |Aldrin i |Dieldrin 1 1Endrin 1 I4,4' DDT ( |

i 1

MSCONCENTRATION

(ug/L)

MS |% 1

REC #|

i111111

QCLIMITSREC.

56-12340-13140-12052-12656-12138-127

11| COMPOUND

I Lindanej HeptachlorI Aldrinj DieldrinI EndrinI 4,4' DDT

-

SPIKEADDED(ug/L)

mmssssaESSEm

MSDCONCENTRATION

(ug/L)X-xm-KSasssss-KataBS

MSD%

REC i

i ^% | QC LIMITS

RPD #| RPD 1 REC.

i 15 156-123I 20 140-131| 22 140-120i 18 152-126I 21 156-121| 27 |38-1271 1


* Values outside of QC Units

RPD:_____ out of ____ outside limitsSpike Recovery:____ out of ____ outside limits

COMMENTS:

FORM III PEST-1 1/87 Rev,

4R300709

3F . , .-. .=SOIL PESTICIDE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY

Lab Name: Contract:

,b Code: _______ Case No.: _____ SAS No.: ______ SDG No.:

Matrix Spike - EPA Sample No.: _________ Level:(low/med) _

COMPOUND

LindaneHeptachlorAldrinDieldrinEndrin4,4' DDT

SPIKEADDED(ug/Kg)

| SAMPLE1 CONCENTRATION1 (ug/Kg)j :B=SS==SS-5=.:===:3==5S

1111111

i MS| CONCENTRATION1 (ug/Kg)

1111111

MS | QC% | LIMITS

REC #| REC.—————————— 1 ——— - —————

[46-127135-130134-132131-134142-139123-134I

\COMPOUND

LindaneHeptachlorAldrinDieldrinEndrin4,4' DDT

I SPIKE| ADDEDt (ug/Kg)

iiiiiii

MSDCONCENTRATION

(ug/Kg)

MSD | |% 1 % 1

REC f| RPD If-.•-.•-at | ==_3 —— [ =

I 1I 11 11 1I 11 !1 1

QCRPD

503143384550

LIMITS| REC.

146-127135-130134-132131-134142-139123-134!

f Column to be used to flag recovery and RPD values with an asterisk

* Values outside of QC liaits


i

COMMENTS:

FORM III PEST-2 1/87 Rev.

4AVOLATILE METHOD BLANK SUMMARY

Lab Name: ______________ Contract:


Lab File ID: ___________ Lab Sample ID: __

Date Analyzed: ________ Time Analyzed:

Matrix: (soil/water) ____ Level:(low/med)

Instrument ID:

THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD;

| EPA | LAB| SAMPLE NO. | SAMPLE ID

Oil I021 !031 |04| |051 |06| |07| |081 |091 |10! |HI 112| |131 |141 |15 1 |16 j ' - 1171 |18! 1191 I20! I211 |221 I231 |241 |25| |26| }271 |28| |29 1 130| |

LABFILE ID

'

TIMEANALYZED

.

,

•

- - ....... ^COMMENTS:

page _ of _FORM IV VOA 1/87 Rev.

4R30071 i

4BSEMIVOLATILE. .METHOD BLANK SUMMARY

Lab Name: Contract.:

>Lab Code: _______ Case No. : ; SAS No. ; SDG No.:

Lab File ID: ___________ _ . _„ Lab Sample ID: __

Date Extracted: _______ Extraction:(SepF/Cont/Sonc)

1 Date Analyzed: ________ Time Analyzed: __

Matrix: (soil/water) ____ Level:(low/med) __

Instrument ID: _______, - iTHIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD:

I EPA j LAB j LAB j DATE |I SAMPLE NO. I SAMPLE ID I FILE ID | ANALYZED I

01!02|03|04|05|.06|07|.08|09 |'101;111.12113|.14115|."I.17 I.18|."I.20|211.'22 |231;24|.25|.26|.27|.28 |29 |30|.

COMMENTS:

page _ of _FORM IV SV 1/87 Rev.

flR3007i2

4CPESTICIDE METHOD BLANK SUMMARY


Lab Code: _______ Case No.: _____ SAS No.: ,......._ SDG No.:

Lab Sample ID: ___________ Lab File ID: _____

Matrix:(soil/water) ____ Level:(low/med) ____

Date Extracted: _______ Extraction: (SepF/Cont/Sonc)

Date Analyzed (1): _______ Date Analyzed (2): ___

Time Analyzed (1): ________ Time Analyzed (2): ____

Instrument ID (1): ________ Instrument ID (2): ____

GC Column ID (1): ________ GC Column ID (2): ____

THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD:

| EPA I LAB| SAMPLE NO. | SAMPLE ID

Oil 1021 1031 1041 |05| |061 107| 108| |091 1101 I111 1121 I131 I14! I151 I161 I171 I181 I191 1201 I211 I221 I23| |24! I25! 126! 1

DATEANALYZED 1

DATEANALYZED 2n sss-aesssKac:

COMMENTS:

of _ /FORM IV PEST 1/87 Rev,

flR300713

5AVOIATILE ORGANIC GC/MS TUNING AND MASSCALIBRATION - BROMOFLUOROBENZENE (BFB)

Lab Name: ___ _______ Contract: ...

,b Code: ______ Case No.: ____ SAS No.; SDG No.:

Lab File ID: ___________ BFB Injection Date:_

Instrument ID: ______• BFB .Injection Time:

Matrix:(soil/water) ____ Level:(low/med) ____ Column:(pack/cap) ___

| j j % RELATIVE| m/e I ION ABUNDANCE CRITERIA I ABUNDANCE

50 | 15.0 - 40.0% of mass 95________75 I 30.0 - 60,0% of mass 95__________95 j Base peak, 100% relative abundance96 I 5.0 - 9.0% of mass 95173 | Less than 2.0% of mass 174_____________________|____( )ij174 | Greater than 50.0% of mass 95________________________I___________I175 I 5.0 - 9.0% of mass 174________________________|____( )l|176 | Greater than 95.0%, but less than 101.0% of mass 174|____( )1|177 | 5.0-9.0% Of mass 176__________________________I_____( }2|___I_______,___________________________________I___________I

1-Value is % mass 174 2-Value is % mass 176

IS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:

| E P A j L A B j L A B j D A T E j T I M E || SAMPLE NO. | SAMPLE ID | FILE ID | ANALYZED | ANALYZED |

Oil__________I____________I____________i_________|________I02|__________|_________I____________I________I________I03|__________|__________I__________I_________I________I04|__________|_________I__________I_________I________I05|__________|____________|____________|_________|________|06|__________|__________|___________I ________I________I07|________I____________I____________I.________I_______I08|__________|________I________I______\_______I09|__________|____________|__________I ________\_________I10|__________I_________I________I.________I________IHI_______I__________I____________I.________I________I12)__________I_________I____________I.________I_______\13|__________|____________|___________I.______I________\14|__________|_________I____________I._______I________I15|__________|____________I___________l_________I________I16|_________I____________I____________I_________I_______\17|__________|__________I________I_________I________I18|__________|____________|___________I_________I________I191________I_________I____________I_________I________I20|________I____________I____________I_________I________I211__________|____________|____________I_________I______I22|_________I____________|__________I_________I________I

page _ of _FORM V VOA 1/87 Rev.

flR3007lt.

5BSEMIVOLATILE ORGANIC GC/MS TUNING AND MASS

CALIBRATION - DECAFLUOROTRIPHENYLPHOSPHINE (DFTPP)

Lab Name: _______ ________ Contract:______


Lab File ID: ___________ DFTPP Injection Date:

Instrument ID: _______ DFTPP Injection Time:

m/emaca=.=K

5168697012719719819927536544144*2443

ION ABUNDANCE CRITERIA

30.0 - 60.0% of mass 198Less than 2.0% of mass 69Mass 69 relative abundanceLess than 2.0% of mass 6940.0 - 60.0% of mass 198Less than 1.0% of mass 198Base Peak, 100% relative abundance5*0 to 9*0% of mass 19810.0 - 30.0% of mass 198Greater than 1.00% of mass 198Present , but less than mass 443Greater than 40.0% of mass 19817.0 - 23.0% of mass 442

% RELATIVEABUNDANCE

( )1

( )1

( )2

1-Value is % mass 69 2-Value is % mass 442

THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARD?

| EPA | LAB| SAMPLE NO. | SAMPLE ID

Oil I021 I031 1041 |051 106| |071 |081 I09! 1101 111! 1121 |131 I141 I151 |161 |171 |181 I191 1201 |211 !221 |

LABFILE ID

DATEANALYZED

TIMEANALYZED

page _ ofFORM V SV 1/87 Rev

6R300715

6AVOLATILE ORGANICS INITIAL CALIBRATION DATA


b Code: ______ Case No.: ____ SAS No.: _____ SDG No.:

Instrument ID: _______ Calibration Date(s):_______

Matrix:(soil/water) ____ Level:(low/med) ___ Column:(pack/cap)

Min RRF for SPCC(#) - 0.300 (0.250 for Bromoform) Max %RSD for CCC(*) » 30.0%

|LAB FILE I D : R R F 2 0 » R R F 5 0 « |JRRF100- RRF150- RRF200- I11 1| COMPOUND IRRF20

! Chloromethane #i Bromomethane 1! Vinyl Chloride *! Chloroethane 1IMethylene Chloride Ij Acetone 1| Carbon Disulfide j| 1 , 1-Dichloroethene *1 1 , 1-Dichloroethane I| 1,2-Dichloroethene (total) |jChloroform *•1,2-Dichloroethane IT2-Butanone Ij 1 , 1 , 1-Trichloroethane |I Carbon Tetrachloride j1 Vinyl Acetate i1 Bromodichloromethane fi 1, 2-Dichloropropane *1 cis-1, 3-Dichloropropene i[ Trichloroethene II Dibromochloromethane j1 1, l, 2-Trichloroethane Ii Benzene 1j trans-l , 3-Dichloropropene !j Bromoform ff 4-Methyl-2-Pentanone 11 2-Hexanone Ii Tetrachloroethene f11,1,2, 2-Tetrachloroethane f! Toluene *i Chlorobenzene f[ Ethylbenzene *I Styrene |IXylene (total) I

IToluene-dS Iteromofluorobenzene 1ifl , 2 -Dichloroethane-d4 |1 1

RRF50 RRF100 RRF150 RRF200

'

RRF% 1

RSD |

#|*It

1**1*iiiiii*i!II11f11I#*f*11

111!

FORM VI VOA 1/87 Rev.

flR3007i6

6BSEMIVOLATILE ORGANICS INITIAL CALIBRATION DATA

Lab Name: _____ Contract:

Lab Code: ______ Case No,: ____ SAS No,: _____ SDG No.:

Instrument ID: ________ Calibration Date(s):________

Min 5SF for SPCC(f) » 0,050 " Max %RSD for CCC(*) = 30.0.

ILAB FILE ID: RRF20 -[RRF80 - RRF120-11 1| COMPOUND IRRF20| «_isss-S-«-«»M.3«JBsae:a::saB=3.«aB3a3B:s=3£==:e65£ 1 ssss=:===

1 Phenol *i bis (2-Chloroethyl) ether 11 2-Chlorophenol 11 1,3-Dichlorobenzene . j| 1 , 4-Dichlorobenzene *1 Benzyl alcohol !1,2-Dichlorobenzene j|2-Methylphenol i| bis (2-Chloroisopropyl) ether ||4-Methylph«nol I| N-Nitroso-di-n-propylamine #1 Hexachloroethane INitrobenzene I

! Isophorone I1 2-Nitrophenol *2 , 4-Dimethylphenol 1Benzole acid jbis (2-Chloroethoxy) methane 1

1 2 , 4-Dichlorophenol *[1,2, 4-Trichlorobenzene I1 Naphthalene I4-Chloroaniline 1

l Hexachlorobutadiene *4-Chloro-3-methylphenol *2-Methylnaphthalene IHexachlorocyclopentadiene t2,4, 6-Trichlorophenol *2,4, 5-Trichlorophenol 1

I 2 -Chloronaphthalene 1[2-Nitroaniline I[ Dimethylphthalate 1I Acenaphthylene I1 2 , 6-Dinitrotoluene 1|3-Nitroaniline 1! Acenaphthene *2 , 4-Dinitrophenol f

I 4-Nitrophenol I1 1

RRF50

RRF5(RRFK

RRF80

) »50-

RRF120 RRF160J3-«-S-3SS==

"

RRF=-SS = 3= =

%

RSDss: = == j

*

1

!1*iiiii*i*iii*iii**If*iiiiiii**#

FORM VI SV-1 1/87 Rev,

flR300717

6CSEMIVOLATILE ORGANICS INITIAL CALIBRATION DATA

Lab Name: ____ ______ Contract:________

Lab Code: ______'m Case No.: _. SAS No, : ______ SDG No.:

Instrument ID: _____ Calibration Date(s):_______

Min RRF for SPCC(i) » 0.050 . . . . . . Max %RSD for CCC(*) « 30.0'-

LAB FILE ID: RRF20RRF80 « RRF12C

COMPOUND

Dibenzofuran2 , 4-DinitrotolueneDiethylphthalate4-Chlorophenyl-phenyletherFluorene4-Nitroaniline4 , 6-Dinitro-2-methylphenol_N-Nitrosodiphenylamine ( 1 ) *4-Bromophenyl-phenyletherHexachlorobenzenePentachlorophenol 'PhenanthreneAnthraceneDi-n-butylphthalateFluoranthene 'PyreneButylbenzylphthalate3,3' -DichlorobenzidineBenzo (a) anthraceneChrysenebis ( 2 -Ethylhexyl ) phthalateDi-n-octylphthalate ^Benzo (b) f luorantheneBenzo (k) f luorantheneBenzo (a) pyrene <Indeno (1,2, 3-cd) pyreneDibenz .a,h) anthraceneBenzo (a, h . i) perylene

Nitrobenzene-dS2-FluorobiphenylTerphenyl-dl4Phenol-d52 -Fluorophenol2,4, 6-Tribromophenol

-)«

RRF20SSS== -=

fe

k

k

k

1

RRF50;xs:ssss-3

EaBsacaauM

RRF5CRRFK

RRF80SB-B3K-S-«=«

) -50-

I.RF120 RRF1603ES=:s::-==

«.e:=:=:s:ss:s

RRF%RSD

i

.

1

ll

1

i

*

it

-ST-EJS-SSS

11

1 (1) Cannot be separated from Diphenylamine

FORM VI SV-2 1/87 Rev.

flR3007J8

Lab Name: _ _____ Contract:


Instrument ID: ___ Calibration Date: Time:

Lab File ID: ___________ Init. Calib. Date(s):

Matrix:(soil/water) ____Level:(low/med) ___Column:(pack/cap)

Min RRF50 for SPCC(jf) - 0.300 (0.250 for Bromoform) Max %D for CCC(*) » 25.0%

I1 COMPOUND

j Chloromethane :] Bromomethane1 Vinyl Chloride .j ChloroethaneIMethylene Chloridej Acetone(Carbon Disulfide1 1 , 1-Dichloroethene *j 1 , 1-Dichloroethane =jl,2-Dichloroethene (total)[ Chloroform -j 1, 2-Dichloroethane|2-Butanone| 1 , 1 , 1-Trichloroethanej Carbon Tetrachloride] Vinyl AcetateI Bromodichloromethanej 1, 2-Dichloropropane *i cis-1, 3-Dichloropropene[ Trichloroethenej Dibromochloromethanejl,l, 2-Trichloroethane1 Benzene| trans-1, 3-DichloropropeneI Bromof orm •I 4-Methyi-2-Pentanone12-Hexanone1 Tetrachloroethene[1,1,2, 2-Tetrachloroethane .j Toluene *I Chlorobenzene •| Ethylbenzene i\ StyreneIXylene (total)

| Toluene-d8j Bromof luorobenzenej l,2-Dichloroethane-d4I

RRF

t

k

k'

k

r

••

•k

't

==_SB3t»=a

RRF501

%D |*^ 1

*

!*iiii*ii*iiiiii*iiiiii§iii£

*

#*

1

1SKK3S=S 1

1111

FORM VII VOA 1/87 Rev.

flR3007i9

7BSEMIVOLATILE CONTINUING CALIBRATION CHECK

Lab Name: Contract;

ib Code: ______ Case No.: ____ SAS No,: _____ SDG No.:

Instrument ID: ____ Calibration Date: Time:

Lab File ID: __________ Init. Calib. Date(s):

Min RRF50 for SPCC(#) • 0.050 Max %D for CCC(*) * 25.0%

COMPOUND

Phenolbis (2-Chloroethyl) ether2 -Chl orophenol1, 3-Dichlorobenzene1, 4-DichlorobenzeneBenzyl alcohol1,2-Dichlorobenzene2-Methylphenolbis(2-Chloroisopropyl)ether4 -Methy IphenolN-Nitroso-di-n-propylamineHexachloroe thaneNitrobenzeneIsophorone2-Nitrophenol *2 , 4 -Dime thy IphenolBenzoic acidbis (2-Chloroethoxy) methane2 , 4-Dichlorophenol ^1,2, 4-TrichlorobenzeheNaphthalene4-ChloroanilineHexachlorobutadiene4-Chloro-3-methylphenol2 -Me thy InaphthaleneHexachlorocyclopentadiene2,4, 6-Trichlorophenol2,4, 5-Trichloroph«nol2-Chloronaphthalene2-HitroanilineDiaethylphthalateAcenaphthylene2 , 6-Dinitrotoluene3-NitroanilineAcenaphthene ^2 , 4-Dinitrophenol4-Nitrophenol

RRF:xz3eaB.B:5

f

t

'•'

k

fc

kk

>* _

ir\\ '

RRF503B3S-BC3--m3E

%D

*

4

*

4

*

*

*

f*

<

.

\

FORM VII SV-1 1/87 Rev,

AR300720 '

7CSEMIVOLATILE CONTINUING CALIBRATION CHECK

Lab Name: __ Contract:

Lab Code: ______. Case No.: ____ SAS No.: _____ SDG No,:

Instrument ID: ____ Calibration Date:___ Time:

Lab File ID: _______.___ Init. Calib. Date(s):

Min RRF50 for SPCC(#) - 0.050 Max %D for CCC(*) - 25.0*

COMPOUND

Dibenzofuran2 , 4-DinitrotolueneDiethylphthalate4-Chlorophenyl-phenylether_Fluorene4-Nitroaniline4 , 6-Dinitro-2-methy IphenolN-Nitrosodiphenylamine (1) t4-Bromophenyl-phenyletherHexachlorobenzenePentachlorophenol *PhenanthreneAnthraceneDi-n-butylphthalateFluoranthene *PyreneButylbenzylphthalate3,3' -Dichlorobenz idineBenzo (a) anthraceneChrysenebis ( 2-Ethylhexyl ) phthalateDi-n-octylphthalate *Benzo (b) f luorantheneBenzo (k) f luorantheneBenzo (a) pyrene *Indeno (1,2, 3-cd) pyreneDibenz (a,h) anthraceneBenzo (g,h,i)perylene

Nitrobenz«ne-d52-FluorobiphenylTerphenyl-dl4Phenol-d52-Fluorophenol2,4, 6-Tribromophenol

RRF

>*

»

»k

B5aCS3B3£K£

RRF50-t -ES-S

S—S2£3=ZS a

%D

4

4

i

•*

4

(1) Cannot be separated from Diphenylamine

FORM VII SV-2 1/87 Rev.

AR30072!

8AVOLATILE INTERNAL STANDARD AREA SUMMARY

Lab Name: Contract:

Lab Code: Case No.: * SAS No.: SDG No.:

Lab File ID (Standard) : , Date Analyzed:

Instrument ID: Time Analyzed:

Matrix: (soil/water) Level: (low/med) Column: (pack/cap)

| | ISl(BCM) | | IS2(DFB) || | AREA #| RT | AREA #| RT

I 12 HOUR STD| I | |

1 UPPER LIMIT | I | |

I LOWER LIMIT! I | f

| EPA SAMPLE | || |1 NO. | || |

O i l 1 I I I02| ] || |031 i || |

^04| I || || 05| | || |F 06| | || |

07| | || |08 | | || f09| | || |1 0 j j j j jH I 1 I I 11 2 1 1 I I I1 3 | I I I I1 4 | I I I I1 5 ! 1 I I 11 6 1 . 1 I I 11 7 ! t i l l1 8 ! 1 I I 1191 1 1 I 12 0 1 I I I !211 1 1 1 I221 I j 1 1

IS3(CBZ) |AREA || RT

1s__.;s _ . .g j __

i— , ——— _ t __- —— _ — i ____==iiiiiiiiiiiiiiiiiiiiiiiii

IS1 (BCM) =• Bromochloromethane UPPER LIMIT *' + 100%IS2 (DFB) « 1,4-Difluorobenzene of internal standard area.IS3 (CBZ) » Chlorobenzene LOWER LIMIT » - 50%

of internal standard area,. f.# Column used to flag internal standard area values with an asterisk

f g e _ o f _ - - - . - - •

1 FORM VIII VGA ' 1/87 Rev,

1 Lab Name: _______________ Contract:

Lab Code: ______ Case No.: ____ SAS No.: _____ SDG No,!

j Lab File ID (Standard): ___________ Date Analyzed:_

Instrument ID: _______ Time Analyzed:_

01020304050607080910111213141516171819202122

| ISl(DCB)| AREA 1

12 HOUR STDImmE«3-BaEsasa-E--«~'2-S5ss3 1 —— ——— _B=—:a

UPPER LIMIT!

LOWER LIMIT!

EPA SAMPLE |NO. |

1111111111111111111111

RT

-____

IS2(NPT)AREA |

—

____

| IS3(ANT)RT | AREA *

1""

1

1_•_-_ m_ | SS — _

11

1111111111111111111111

RT

=====

IS1 (DCB) - l,4-Dichlorobenzene-d4 UPPER LIMIT - + 100%IS2 (NPT) » Naphthalene-dS of internal standard area.IS3 (ANT) * Acenaphthene-d8 LOWER LIMIT - - 50%

of internal standard area.

I Column used to flag internal standard area values with an asterisk

page _ of _

FORM VIII SV-1 1/87 Rev,

SR300723

8CSEMIVOLATILE INTERNAL STANDARD AREA SUMMARY

Lab Name: ________ Contract:

Lab Code: ______ Case No.: ____ SAS No.: _____ SDG No.

Lab File ID (Standard) : _____________ Date Analyzed:__

Instrument ID: _______ . Time Analyzed:

| | IS4(PHN)I I AREA #

I 12 HOUR STD|

1 UPPER LIMIT!

I LOWER LIMIT |

| EPA SAMPLE 11 NO. |

Oil 1021 I031 I04| |05| |06| |071 |081 I09| |10! I111 1121 I131 |141 I151 I161 |17| |181 I191 1201 I211 I221 |

RT

aesesxaEX

ISS(CRY)AREA * RT

s==53Z-=:s

•KSSISESX

IS6(PRY) |AREA #| RT

1

Is* — •=•_• _ r — «.= ———————— =_ | = —— __s

1

11

•BMX3K33SSS ] JB-K-Z -«SS

111111111111I11i111111

IS4 (PHN) « Phenanthrene-dlO UPPER LIMIT - + 100%IS5 (CRY) * Chrysene-dl2 of internal standard area.IS6 (PRY) - Perylene-dl2 LOWER LIMIT - - 50%

of internal standard area.

# Column used to flag internal standard area values with an asterisk

>age _ of _

FORM VIII SV-2 1/87 Rev.

8DPESTICIDE EVALUATION STANDARDS SUMMARY

Lab Name: ________ Contract:

Lab Code: ______ Case No.: ____ SAS No.: _____ SDG No.

Instrument ID:________ GC Column ID: ________

Dates of Analyses:________ to _______

Evaluation Check for Linearity

PESTICIDE

ALDRINENDRIN4,4' -DDTDBC

I CALIBRATIONI FACTOR1 EVAL MIX A

111Ii

CALIBRATIONFACTOREVAL MIX B

•»————— «———

CALIBRATIONFACTOREVAL MIX C

i1

%RSD(</-10.0%)

11(1) If > 10.0% RSD, plot a standard curve and determine the ng

for each sample in that set from the curve.

Evaluation Check for 4,4'-DDT/Endrin Breakdown(percent breakdown expressed as total degradation)

Oil02103 i04|05 |06 |07]08|09 |10|HI1211314

| DATEI ANALYZED

INITIAL 1EVAL MIX B 1EVAL MIX B |EVAL MIX B |EVAL MIX B 1EVAL MIX B IEVAL MIX B iEVAL MIX B iEVAL MIX B 1EVAL MIX B iEVAL MIX B IEVAL MIX B |EVAL MIX B |EVAL MIX B !EVAL MIX B |

1

TIMEANALYZED

ENDRIN 4, 4 '-DDT

.

.'

COMBINED(2)

(2) See Form instructions.

FORM VIII PEST-1 1/87 Rev.

AR3QG725

8EPESTICIDE EVALUATION STANDARDS SUMMARY

Evaluation of Retention Time Shift for Dibutylchlorendate

Lab Name: Contract:__

'Lab Code: ______ Case No.: ____ SAS No.: _____ SDG No.:

Instrument ID: ___ GC Column ID:

Dates of Analyses:________ to

| EPA | LAB SAMPLE| SAMPLE NO. | ID

Oil 1021 1031 1041 1051 1061 I07| |081 1091 I101 |111 1121 |131 I141 I15| |161 |171 |181 |191 !201 |211 |221 |23| |24| I251 I26| |27| |28| |291 I301 |311 |321 |331 |341 |351 |36| |37| |381 |

DATEANALYZED

TIMEANALYZED

Jl M Ji M J. fc t _- 1 Jl

...

* 1D | *

iiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiii!1111 '

* Values outside of QC limits (2.0% for packed columns,0.3% for capillary columns)

page _ of _ .FORM VIII PEST-2 1/87 Rev.

flR300726

9PESTICIDE/PCB STANDARDS SUMMARY

Lab Name: __ _______ Contract:


Instrument ID:________ GC Column ID: '_____

| DATE (3) OF FROM:1 ANALYSIS TO:| TIME(S) OF FROM:1 ANALYSIS TO:1l i RT

COMPOUND | RT | WINDOW| | FROM TO

alpha-BHC i 1beta-BHC 1 1delta-BHC I Igamma-BHC I iHeptaclor 1 1Aldrin 1 1Hept. epoxidel IEndosulfan I 1 1Dieldrin 1 I4,4' -DDE I 1Endrin 1 IEndosulfan III 14,4' -DDD I 1Endo.sulfate j i4, 4 '-DDT 1 1Methoxychlor i 1Indrin ketone) 1a. Chlordane I ig. Chlordane 1 1Toxaphene 1 1Aroclor-1016 I IAroclor-1221 | IAroclor-1232 1 1Aroclor-1242 1 1Aroclor-1248 1 1Aroclor-1254 1 1Aroclor-1260 | 1

i t

CALIBRATIONFACTOR

DATE OF ANALYSIS |TIME OF ANALYSIS jEPA SAMPLE NO. |(STANDARD) j

RT

1t

CALIBRATIONFACTOR

1QNT|Y/NI

iI11

i%D

t

=*j

——————————

Under QNT Y/N: enter Y if quantitation was performed, N if not performed,%D must be less than or equal to 15.0% for quant it at ion, and less thanor equal to 20.0% for confirmation.

Note: Determining that no compounds were found above the CRQL is a form ofquantitation, and therefore at least one column must meet the 15.0% criteria,

For multicomponent analytes, the single largest peak that is characteristicof the component should be used to establish retention time and %D.Identification of such analytes is based primarily on pattern recognition

page _ of _FORM IX PEST 1/87 Rev.

AR30Q727

10 EPA SAMPLE NO.PESTICIDE/PCB IDENTIFICATION

Lab Name: Contract:

b Code: Case No.: SAS No.: SDG No.:

GC Column ID (1): ________ GC Column ID (2):

Instrument ID (1): ________ Instrument ID (2):

Lab Sample ID: ___________

Lab File ID: ___________ (only if confirmed by GC/MS)

PESTICIDE/PCB RETENTION TIME RT WINDOW QUANT? GC/MS?OF STANDARD (Y/N) (Y/N)FROM TO

01 Column 1 ......... - .--,- —

02 Column 2

03___________ Column 1

04 Column 2

05___________ Column 1

06 Column 2

07___________ Column 1

08 Column 2

09__________ Column l10 Column 2

ll__________ Column 112 Column 2

Comments:

page _ of _FORM X PEST 1/87 Rev,

AR3GQ728

I^IIIIIIi

IIII

APPENDIX L

LANCY'S PROGRAM

FOR

CORRECTIVE ACTION

AR300729

14.0 CORRECTIVE

Corrective action is taken vfcenever a nonconformance occurs. A

nonconformace is defined as an event which is beyond the limits established

for a particular operation by the QAPP. tfonconfoomances can occur in a

nunber of activities. Such activities include sampling procedures, sample

receipt, sample storage, sanple analysis, data reporting, and computations.

The following personnel are responsible for detecting and reporting

noncon fbnnances :

o Project Staff - during the performance of fieldinvestigations and testing, supervision of subcontractors,and preparation and verification of numerical analyses.

o Laboratory Staff - during the preparation for analyses,performance of analytical procedures, calibration ofequipment and quality control activities.

o Quality Assurance Ooordinator-during performance audits.

14.1 Corrective Action

Nonconformances are documented by the person originating or identifying

it. Nonconformance fonns are used for this purpose. The

laboratory nonconformance fonns consist of individual forms for each of

the following areas:

o Bctractiorv'Sanple Preparation

o Sample Receiving

o General Chemistry

o Metals/Soils

o (E-OC/MS (Figure 14-1)

flR3007

Docunentation includes the following:

o Identification of the individual (s) originating oridentifying the nonconformance.

o Description of the nonconformance.

o Any required approval signatures (initials) .

o Corrective action taken*

o Corrective action completion date.

Within the laboratory organization, a completed nonconfonuance form is• r.routed through the Qroup Leader to the Laboratory Supervisor. The

Laboratory Supervisor reviews and approves the docunentation and then

routes the form to the QA Coordinator. Ihe nonconformance is entered

into the Nonconformance tog by the QA Coordinator. If M & E needs to

be notified of the nonconformance, the nonconformance form is routed to

the Project Manager. M & E is notified of the nonconformance and the

corrective action taken by a letter of transnittal that is issued with

the Analysis Rsport.

Within the laboratory, a nonconformance that can be corrected during

the course of analysis is corrected by the analyst and/or the Group

Leader. All other nonconformances are corrected by the Laboratory

Supervisor in conjunction with the QA Coordinator.

If the QA Coordinator and the Project fanager or Laboratory Supervisor

disagree on the necessary corrective action, the ffenager-Technical

Operations makes the final decision as to the corrective action that is

to be taken.

AR30073I

M & E is notified of the nonconformance and corrective action if one of

the following is true:-

o A nonconformance causes a delay in work beyond the schedulecompletion date.

o A nonconformance affects information already reported to M & E.

o A nonconformance affects the validity of the data._ • , . 1 .

Ihe QA Coordinator verifies the conpletion of all corrective actions.

Verification of completion is documentated on a nonconformance form and

in the Nonconformance Log*

14-2 Limits of Operation

The limits of operation that are used to identify nonconfocmances are

established by the contents of the QAPP and by control charts produced

by statistical analyses.

SR300732

I

lIl1Ill

APPENDIX M

BIOASSAY QUALITY CONTROL PROGRAM

BR300733

QUALITY CONTROL PROGRAM , . . . .

A. An acceptable degree of precision for definitive bioassays shall be

that the 95 percent confidence or fiducial intervals be within less

than +30 percent of the 96^hour or Incipient LC50 valve.

B. The laboratory shall develop and have on file and available for

inspection a written description of the current laboratory quality

control program. The written description shall outline the procedures

which the laboratory will use In meeting the quality control

requirements. A record.of analytical control tests and quality control

checks on equipment and materials shall be.prepared by the laboratory

and retained for at least five years."

1. The-laboratory shall perform the following analytical quality

control tests to ensure that general laboratory practices and

methodology are in compliance with the requirements.

a. Laboratory pure water shall be analyzed for and meet the

following requirements:

pH ,. 5.5 - 7.5

Conductivity Greater, than 0.2 mehohm-cm asresistivity or less than 5.0micromhos-cm as conductance at 25 C

Trace Metals:

- A single metal - Not greater than 0.05 mg/L

- Total metals Equal to or less than 1.0 mg

- Test for bactericidalproperties of distilledwater (Standard Methods,14 Edition, orMicrobiological Methods - 0.8-3.0EPA, Free chlorine residual 0.0

b. Laboratory pure water checks for pH, conductivity, and free

chlorine residual shall be performed monthly and documented.

flR30073i*

I c. Laboratory pure water checks for trace metals, bactericidal

properties, and standard plate count shall be performed

« annually and documented.t

d. Laboratory grade water shall be analyzed monthly for pH, D.O.,

I chlorine residual, and specific conductance,

e. Laboratory grade fresh water shall be analyzed at least twice

J annually.

I. Each ph meter shall be cleaned Immediately after each use

I period and calibrated prior to usage using two pH buffer

standards and records of each calibration shall be

i maintained; buffer allquots shall not be used more than

once; and commercial buffer solutions shall be dated at

the time of initial use; it .Is recommended that the

, buffer standards bracket the value to be measured;

* II. Top loader or pan balances shall be calibrated annually,

i calibration shall be checked monthly against class "s"i

weights, and a record shall be made of each calibration

? check;

ill. The accuracy of all thermometers used to monitor

~t temperature shall be verified by comparing the readings

of such thermometers with the readings of a certifiedi

f thermometer. A record shall be made containing the

identification number of each thermometer, thef * . . . .I '* temperature displayed on the certified thermometer and

the thermometer being verified, correction factors when

applicable, dates on which quality control checks were

i performed, and the name of the analyst performing such

checks. Glass thermometers shall be verified yearly and

metal thermometers shall.be verified quarterly.

iv. The temperature of air or water-jacketed incubators,

aluminum block incubators, water baths and Incubator

rooms shall be either recorded continuously or recorded

daily from in-place thermometers immersed in liquid and

placed on at least one of the shelves in use.

v. Date, time and temperature shall be either recorded

continuously, or recorded individually during each

sterilization cycle of the autoclave;

vi. Each hot air oven shall be equipped with a thermometer,

the bulb of which shall be placed in sand, or with a

temperature recording device, and records shall be

maintained showing the date, time and temperature of each

sterilization cycle;

vii. The temperature of each refrigerator shall be either

recorded continuously or recorded daily from an in-place

thermometer immersed in liquid and placed on at least onei

of the shelves in use.

vili. Materials of substandard reactivity and deteriorate

materials shall not be used; and

tx. All outdated material shall be discarded immediately.

C. The temperature In and flow rate through the exposure chambers and the

maintenance of effluent concentrations, shall be checked initially,

daily during the duration of the test, and upon completion of the test,

adjusted as necessary, and documentation of these adjustments and

measurements shall be made.

RR300736

APPENDIX N

BIOASSAY RECORDS AND DATA REPORTING

HR300737

I•

M

•

B

•

m

*

i1

RECORDS AND DATA REPORTING

A. Each laboratory shall maintain records and report data in accordance

with the requirements set out in this section.

B. Records of bioassay analysis shall be kept by the laboratory for not

less than five years. This requirement Is equally applicable to all

raw data, quality control data, chain of custody forms and laboratory

reports.

C. The following information shall be kept by the laboratory as part of

the daily log of feeding, behavioral observations, and mortality of

organisms during holding and acclimation:

1. Water temperature of holding tanks;

2. Air temperature in culturing/holdlng room;

3. Mortalities of organisms per holding tank;

4. Analysis of laboratory grade water;

5. Food and feeding schedule; and

6. General observations of behavior and condition.

D. A sample report form shall be completed immediately after collection of

either dilution water or effluent composite or grab samples and shall

state the sampling location, date and time of collection, chlorine

residual, collectors name, and any remarks.

E. The bioassay experimental results shall be reported in accordance with

Methods for Measuring Acute Toxicity - EPA, and;

1. The incipient LC50 shall be reported If applicable.

2. A figure showing the toxtcity curve shall be included.

F. The original or true duplicate of the results of the bioassay shall be

sent promptly to the person who requested such test and shall be signed

by the laboratory manager or a designee.

300738

IIfII

APPENDIX O

CLP PRESERVATIVES AND HOLDING TIMES

AND

COMPARISON OF QC PROTOCOLS FOR GC AND GC/MS ANALYSES

AR3Q0739

EPA CONTRACT LABORATORY PROGRAM (CLP)/PRESERVATIVES AND HOLDING TIMES

10/86 Statement of Work

Parameter

Volatiles(Purgeabies)

Semivolati.es(Including Bases, Neutrals Acids,Pesticides, and PCBs)

Preservative

4°C(±2°C)Store in Dark

4°C(±2°C)Until Extraction andAnalysis

Holding Time

Water: 10 DaysSoil/Sediment: 10 Days

Separatorv Tunnel ExtractionWater: 5 DaysSoil/Sediment: 10 Days

Continuous Liquid-LiquidExtractionWater: 5 DaysSoil/Sediment: 10 Days

3-14 NUS CORPORATION

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IIIIIIIIIIIIII AR30071.9

appendix j nus data reduction, validation and reporting · describing each revision. the note is...

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