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PRELIMINARY FACHJTIESCHARACTERIZATION SUMMARY

OLEAN WELL FIELD SUPPLEMENTAL RI/FS

VOLUME HIUSEPA Region 2

Inorganic Data Validation Checklists

May 1992

Prepared for

Clean Cooperating IndustriesC/O Nixon, Hargrave, Devans & Doyle

Clinton SquareP.O. Box 1051

Rochester, New York 14603

Prepared by

Geraghty & Miller, Inc.24 Madison Avenue Extension

Albany, New York 12203(518) 452-7826

300888

Evaluation of Ketala Data for the Contract Laboratory Program (CLP)

based on

SOW. 3/90

(SOP Revision XI)

PREPARED BY: TTliv.-'l ^Vvn-L^______________ DATE; } — 3 ^ —Assurance Chemist

Waste Section

: H'l J r- VLq/vHahif SheJJth, Quality AsToxic and Hazardous Wasi

APPROVED BY; y -j- >\ v)y • C.u \\-\L__________ DATE:Kevin Kubik, ChiefToxic and Hazardous Waste Section

APPROVED BY; .--><>--^ ________ DATE:Robeft Runyon, & tMonitoring Management Branch

300889

STANDARD TX?>:-'ZS& HCCEEURE Page 1 of 34

Title: Evaluation of Metals Data'-itor iw Date: Jan. 1992Contract Laboratory Program Number: HW-2

Revision: 11 •'

1.0

1.1 This procedure is applicable to inorganic data obtained front contractorlaboratories working for Hazardous Waste Site Contract LaboratoryProgram (CLP).

1.2 The data validation is based upon analytical and quality assurancerequirements specified in Statement of Work (SOW) 3/90 .

2 . 0 Responsibilities - Data reviewers will complete the following tasks as assigned by theData Review Coordinator:

2.1. For a total review;

The reviewer must answer every question on the checklist.

2.1.2 Data Assessment - Data XssesTit Narrative (Accept x A. 2)The answer on the checklist must natch the action in the narrative(appendix A.2) and on Form I's. Do not use pencil to write the narrative.

2.1.3 Contract Non-Oonolianoe - SMO Report (Appendix A. 3)This report is to be completed only when a serious contract violation isencountered, or upon the request of the Data Validation Task Monitor, or TechnicalProject Officer (TPO) . Forward 5 copies: one each for internal files,appropriate Regional TPO, Sample Management Office (SMO) and last two addresses ofMailing List for Data Reviewers (Appendix A. 4). In other cases, all contractviolations should be appended to the end of the Data Assessment Narrative (Sec.A.2. 2).

2.1.4 CT-P Pat'1

2.1.4.1 Appendix. fttgFill in the total number of analytes analyzed by different analyses andthe number of analytes rejected or flagged as estimated due to correspondingquality control criteria. Place an "X" in boxes where analyses were notperformed, or criteria do not apply.

2.1.4.2 Appendix A. 6Data reviewer is also required to fill cut Inorganic Regional Data Assessmentform (Appendix A. 7) provided by EPA Headquarters. Codes listed on the formwill be used to describe the Data Assessment Summary.

900890

STANDARD OPERATING PROCEDURE Page 2 of 34

Title: Evaluation of Metals Data for the Data: Jan. 1992Contract laboratory Program Number: HW-2

Revision: 11

2.1.5 Data Review Logi It is xw.niinHinried that each data reviewer should maintain a log ofthe reviews completed to include: a. date of start of case review

b. date of completion of case reviewc. sited. case numbere. contract laboratory

„ f. number of samples* g. matrixh. hours workedi. -reviewer's initials

2.1.6 Telephone Record Log - the data reviewer should enter the bare facts ofinquiry, before initiating any phone conversation with CLP laboratory.After the case review has been completed, mail white copy of TelephoneRecord Log to the laboratory and pink copy to SMD. File yellow copy inthe Telephone Record Lag folder, and attach a xerox copy of the TelephoneRecord Log to the completed Data Assessment Narrative (Appendix A.2).

2.1.7 Forwarded Paperwork4

2.1.7.1 Upon completion of review, the following are to be forwarded to the RegionalSample Control Center (RSOC) located in the Surveillance and Monitoring Branch:a. data packageb. completed data assessment checklist (Appendix A.I,original)c. SMO Contract Compliance Screening (CCS)d. Record of Communication (copy)e. CLP Reanalysis Request/Approval Record (original + 3 copies)f. Appendix A.6 (original).

2.1.7.2 Forward 2 copies of completed Data Assessment Narrative (Appendix A.2)along with 2. copies of the Inorganic Data Assessment Form (Appendix A. 6) andTelephone Record Log , if any,: one each for appropriate Regional TFO,and the other one to EPA EMSL office in las Vegas. The addresses of TPOs and EPAoffice in Las Vegas are given in Appendix A-4. •"

2.1.8 Filed Paperwork - Upon completion of review, the following are to be filedwithin MMB files:a. Two copies of completed Data Assessment Narrative (Appendix A.2) each carrying

Appendix A.6.b. Telephone Record Log (copy)c. SMD Report (copy Appendix A-3)d. CLP Reanalysis Request/Approval Record (copy)

300891

STANDARD OPERATING PROCEDURE Page 3 of 34i

Title: Evaluation of Metals Data for the Data: Jan. 1992Contract Laboratory Program Number: HW-2

Revision: 11

3.0 DataEach data package is checked by a Regional Sample Control Coordinator (RSSC) forcompleteness. A data package is assaimed to be complete when all the deliverablesrequired under the contract are present. If a data package is incomplete, the RSSCwould call the laboratory for missing document (s) . If the laboratory does not respondwithin a week, SMD and MMB coordinator of Region II will be notified.

4.0 Rejection of Data - All values determined to be unacceptable on the Inorganic AnalysisData Sheet (Form I) must be lined over with a red pencil. As soon as any reviewcriteria causes data to be rejected, that data can be eliminated from any further reviewor consideration.

5.0 Acceptance Criteria - In order that reviews be consistent among reviewers, acceptancecriteria as stated in Appendix A.I (pages 4-25) should be used. Additional guidancecan be found in the National Inorganic Functional Guidelines of October 1, 1989.

6.0 SMD Contract Compliance Screening (PCS) - This is intended to aid reviewer in locatingany problems, both corrected and unconnected . However, the validation should be carriedout even if CCS is not present. Resubmittals received from laboratory in response toCCS mist be used by the reviewer.

7.0 Request for ReaT jv f - Data reviewers must note all items of contract non-compliancewithin Data Assessment Narrative. If holding tiroes and sample storage times have not beenexceeded, TPO may request reana lysis if items of non-compliance are critical to dataassessment. Requests are to be made on "CLP Re-Analysis Request/Approval Record".

8.0 Record «f "pr"?1Pi "fltJTn ~ Provided by the Regional Sample Control Center (RSCC) toindicate which data packages have been received and are ready to be reviewed.

9.0 Roundina off numbers - The data reviewer will follow the standard practice.

300892

STANDARD OPERATING PROCEDURE 4 of 34

Title: Evaluation of Metals Data for theContract laboratory ProgramAppendix A.I: Data Assessment - ContractCompliance (Total Review)

Date: Jan. 1992Number: HW?2Revision: 11

A.I.I (CCS) - Present?

ACTION; If no, contact RSOC.

A. 1.2 Record of Oemnunication (from RSCC) - Present?

ACTION: If no, request from RSOC.

YES

C __ ]

NO N/A

X

A. 1.3 Trip Report - Present and conplete?

ACTION; If no, contact RSOC for trip report.

A. 1.4 Sample Traffic Rqx>rL — Present?

Legible?

ACTION; If no, request from Regional Sanple ControlCenter (RSCC) .

A. 1.5 Cover Page - Present?

Is cover page properly filled in and signed by the labmanager or the manager's designee?

ACTION: If no, prepare Telephone Record Lag, andcontact laboratory.

Do numbers of sanples correspond to numbers on Recordof Communication?

Do sanple numbers on cover page agree with sanplenumbers on:

(a) Traffic Report Sheet?

(b) Form I's?

ACTION: If no for any of the above, contact RSCC forclarification.

c_]

\

300893

STANDARD OPERATING PROCEDURE

Title: Evaluation of Metals Data for theContract Laboratory FrograaAppendix A. 1.! Data AssofUjiumt ~ Contract

Page 5 of 34

Date: Jan. 1992Number: Hy-2Revision: li

Compliance (Total Review)

A.1.6 Font I to

A. 1.6.1 Are all the Porn I through Form DC labeled with:

Laboratory name?

Case/SAS number?

EPA sample No.?

SDG No.?

Contract No.?

Correct units?

Matrix?

ACTION; If no for any of the above, note underContract Prcblenv/Non-Ccnpliance sectionof the "Data Assessment Narrative".

A. 1.6.2 Do any conputation/transcription errors exceed 10% ofreported values on Forms I-IX for:

(NOTE: Check all forms against raw data.)

(a) all analytes analyzed by ICF?

(b) all analytes analyzed by GFAA?

(c) all analytes analyzed by AA Flame?

(d) Mercury?

(e) Cyanide?

ACTION; If yes, prepare Telephone Leg, contactlaboratory for corrected data andcorrect errors with red pencil and initial.

N/A

[__] __ A.

<_. V

t_3 _ A.t_] *L _

V

300894


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Piujtan Number:Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

YES j£~A.I.7 Raw Data

A. 1.7.1 Digestion Log* for flame AA/ICP (Porn XHI) present? r}( 1 __ __

Digestion Log for furnace AA Porn XIII present? [X 1 __ __

Distillation Log for mercury Porn XIII present? [ ] __ __

Distillation Log for cyanides Form XIII present? [ /> ] __ __

Are pH values (pH<2 for all metals, ptt>12 for cyanide) \/present? [ f\ 1 __ __

*Weights, dilutions and volumes .used to obtain values.

Percent solids calculation present for soils/sediments? [__] __ X

Are preparation dates present on sample preparation \ylogs/bench sheets? [_1_] '. __ __

A. 1.7.2 Measurement read out record present? ICP [JiL] __ __

Flame AA [__] __ A

Furnace AA [ 1 __ __

Mercury [_ _] __ __

cyanides [Vj __ __

A.1.7.3 Are all raw data to support all sample analyses and \QC operations present? [ / ] __ __

Legible? f 1 __ __

Properly Labeled? [_V_] __ __

ACTION; If no for any of the above questionsin sections A.I.7.1 through A.I.7.3,write Telephone Record Log and contactlaboratory for resubmittals.

300895


Title: Evaluation of Metals for the Contract Date: Jan. 1992laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: !!••

Conpliance (Total Review)

YES N£ N/AA. 1.8 Holding TirtT - (aqueous and soil samples )

(Examine sample traffic reports and digestion/distillation logs.)

Mercury analysis (28 days) ....... exceeded? __ [/* ] __

Cyanide distillation (14 days) ..... exceeded? __ [ X ] __

Other Metals, analysis (6 months) . . . . exceeded? __

NOTE; Prepare a list of all samples and analytes forwhich holding times have been exceeded. Specifythe number of days from date of collection to the dateof preparation (from raw data) . Attach to checklist.

ACTION; If yes, reject (red-line) values less thanInstrument Detection Limit (IDL) and flagas estimated (J) the values above IDL eventhough sample (s) was preserved properly.

A. 1.8. 2 Is pH of aqueous samples for: WMetals Analysis >2? __ [_/J __

Cyanides Analysis <12? __ f A ] ___

Action; If yes, flag the associated metals and cyanidess estimated.

A. 1.9

A. 1.9.1 Are all Form I's present and complete? [X 1 __ __

ACTION; If no, prepare telephone record log and contactlaboratory for submittal.

A. 1.9. 2 Are correct units (ug/1 for waters and ing/Kg for soils) \/indicated on Form I's? [_Aj __ __

Are soil sample results for each parameter corrected for \,percent solids? [ __ ] __ *

VAre all "less than IDL" values properly coded with "U"? [ A ] __ __

300896

STANDARD OPERATING PROCEDURE Page 8 Of 34

Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

__ _ N/A

Are the correct concentration qualifiers used withfinal data?

ACTION; If no for any of the above, prepare TelephoneRecord Log, and contact laboratory for correcteddata.

A. 1.9.3 Are EPA sample I s and corresponding laboratory sampleID # s the same as on the Cover Page, Form I's and -yin the raw data? [__] __

Was a brief physical description of samples given \/on Form I's? f ft 1 __

Was the dilution of any sample diluted beyond therequirements of the contract noted on Form I or \/Form XIV? __ f * 1

ACTION; If no for any of the above, note underContract-Problem/Non-Compl ianceof the"Data Assessment Narrative".

A. 1.10 Calibration

A. 1.10.1 Is record of at least 2 point calibration \present for ICP analysis? [___]

Is record of 5 point calibration present for VHg analysis? r A 1

Is record of 4 point calibration present for: -

Flame AA? [__]

Furnace AA? r X 1

r>,Cyanides?

Is one calibration standard at the CRDL level for \tall AA (except Hg) and cyanides analyses? r X 1 __ __

ACTION; If no for any of the above, write in theContract Problem/Non-Compliance section ofthe "Data Assessment Narrative".

300897


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11.Compliance (Total Review)

IE i s N / AA. 1.10.2 Is correlation coefficient less than 0.995 for:

Mercury Analysis? __ f )* 1 __

Cyanide Analysis? __ C_lL] __V

Atomic Absorption Analysis? __ [__L1 __

ACTION; If yes, flag the associated data as estimated.

NOTE: The data validator shall calculate the correlationcoefficient using concentrations of the standardsand the corresponding instrument response( e.g. absorbance, peak area, peak height, etc.).

A. 1.10.3 In the instance where less than 4 standards aremeasured in absorbance (or peak area, peak height,etc.)mode, are the remaining standards analyzed inconcentration mode immediately after calibration \/within ±10% of the true values? [ __ ]

ACTION; If no, flag the associated data as estimatedif standards are not within ±10% of true values.Do not flag the data as estimated in linear rangeindicated by good recovery of standard(s) .

A. l.ll Form II A {Initial and Continuing <"*»' *"'»tion Verification)-

A. l.ll.l Present and complete for every metal and cyanide? [A ] __ __

Present and complete for AA and ICP when both areused for the same analyte?

ACTION; If no for any of the above, prepare TelephoneRecord Log and contact laboratory.

A. l.ll. 2 Circle on each Form IIA all percent recoveries thatare outside the contract windows.Are all calibration standards (initial and continuing)within control limits: y

Metals- 90-110%R? f A 1

Bg - 80-120%R? f / ] __ __

Cyanides- 85-115%R? f^ 1 __ __

300898


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Cornpliance (Total Review)

MO N/AACTION; Flag as estimated (J) all positive data (not

flagged with a "IP*) analyzed between acalibration standard with %R between 75-89%(65-79% for Hg; 70-84% for CN) or 111-125%(121-135% for Hg; 116-130% for Of) recovery andnearest good calibration standard. Qualify results<IDL as estimated (U7) if the ICV or OCV %R is75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line)as unacceptable data if recovery of the ICV orOCV is outside the range 75-125% (CN, 70-130%; Hg,65-135%) . Qualify five sanples on either side ofverification standard out of control limits.

A. 1.11. 3 Was continuing calibration performed every 10 sanples \/or every 2 hours? [ X ] __ __

Was ICV for cyanides distilled? [Xj __ __

ACTION: If no for any of the above, write in theContract-ProblaVNon-Ccnpliance section of the"Data Assessment Narrative".

A. 1.12 Fo™1 II B (CRDL BteiTv rds for AA and ICP) -

A. 1.12.1 Was a CRDL standard (CRA) analyzed after initialcalibration for all AA metals (except Ha)?

Was a mid-range calib. verification standard distilled \.and analyzed for cyanide analysis? f X ]

Was a 2xCRDL ( or 2x1711. when IDLXSDL) analyzed (CRI) \,for each ICP run? r X(Note: CRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.)

ACTION; If no for any of the above, flag as estimatedall data falling within the affected ranges.The affected ranges are:AA Analysis - **True Value ± CRDLICP Analysis - **True Value ± 2CRDLCN Analysis - **True Value ± 0.5 x True Value.

**True value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL.Compute the concentration of the missing mid-range standard from the calibration range.

30089$


Title: Evaluation of Metals Data for the Data: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

YES M2 N/AA.l. 12. 2 Was CRI analyzed after ICV/ICB and before the final \,

OCV/CCB, and twice every eight hours of ICP run? r /X l __ __

ACTIOM: If no, write in Contract Problem/Non-ComplianceSection of the "Data Assessment Narrative11.

A. 1.12. 3 Circle on each Form IIB all the percent recoveries thatare outside the acceptance windows.

Are CRA and CRI standards within control limits:

Metals 80 - 120%R? [ __ ] / __

Is mid-range standard within control limits:

Cyanide 80 - 120%R? f A 1 __ __

ACTION; Flag as estimated all sample results withinthe affected range if the recovery of thestandard is between 50-79%; flag only positivedata within the affected range if the recoveryis between 121-150%; reject all data within theaffected range if the recovery is less than 50%;reject only positive data within the affected rangeif the recovery is greater than 150%. Qualify 50% ofthe sanples on either side of CRI standard outsidethe control limits.

Note: Flag or reject the final results only when sanpleraw data are within the affected ranges and the CRDLstandards are outside the acceptance windows.

A. 1.13 yterm TII (Initi»i and Qpn*"*"" 7*r C Ttfrr tion Blanks)

A. 1.13.1 Present and complete? f/\ 1 __ __

For both AA and ICP when both are used for the Vsame analyte? [ __ ] __ *

yWas an initial calibration blank analyzed? [___] __ __

Was a continuing calibration blank analyzed afterevery 10 sanples or every 2 hours (which ever is more \^T-eriMorrM'? T /\

300900


Title: Evaluation of .Witals Data for the Date: Jan. 1992Contract Lakoraixo./ i-rtgram Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

vis ^ N/AACTION; If no, prepare Telephone Record Log, contact

laboratory and write in the Contract-Problems/Non-Compliance section of the "Data Assessment Narrative".

A. 1.13.2 Circle on each Form III all calibration blank valuesthat are above CRDL (or 2 x IDL when IDL > CRDL).

Are all calibration blanks (when IDLcCRDL) less than or \.equal to the Contract Required Detection Limits (CRDLs)? [j(_] __ __

Are all calibration blanks less than two times \Instrument Detection Limit (when IDI CRDL)? [£__] __ __

ACTION: If no for any of the above, flag as estimated(J) positive sample results when raw samplevalue is less than or equal to calibrationblank value analyzed between calibration blankwith value over CRDL (or 2xIDL) and nearest good,calibration blank.Flag five samples on either side of thecalibration blank outside the control limits.

4

A.1.14 FORM III (Preparation Blank) -(Note: The preparation blank for mercury is the saneas the calibration blank.)

A. 1.14.1 Was one prep, blank analyzed for:

each Sample Delivery Group (SDG)?

each batch of digested samples?

each matrix type?

both AA and ICP when both are used for Vthe same analyte?

ACTION; If no for any of the above, flag asestimated (J) all the associated positivedata <10 x IDLs for which prep, blankwas not analyzed.

NOTE: If only one blank was analyzed for morethan 20 samples, then first 20 samples analyzeddo not have to be flagged as estimated (J).

300901

.STANTARD 'VPERATBIG PROCEDURE Page 13 of 34Title: Evaluation of Metals Data for the Date: Jan. 1992

Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

__ _- N/A

A.1.14.2 Is concentration of prep, blank value greater \,than the CRDL when IDL is less than or equal to CRDL? __ [ /> 1 __

If yes, is the concentration of the sample withthe least concentrated analyte less than 10 timesthe prep.blank? __ [__]

ACTION; If yes, reject (red-line) all associateddata greater than CRDL concentration butless than ten times the prep, blank value.

A. 1.14.3 Is concentration of prep, blank value (Form III) less \/than two tiines IDL, when IDL is greater than CRDL? [ 1

ACTION; if no, reject (red-line) all positive sampleresults when sample raw data are less than 10tiines the prep, blank value.

A. 1.14.4 Is concentration of prep, blank below Vthe negative CRDL? __ [_A

ACTION: If yes, reject (red-line) all associated sampleresults less than lOxCRDL.

A.i.is Fo1" IV (ICP In+ rf rence Check ____ vA.1.15.1 Present and complete? C A J __ __

(NOTE: Not required for furnace AA, flame AA, mercury,cyanide and Ca, Mg, K and Na.)

Was ICS analyzed at beginning and end of run \i(or at least twice every 8 hours)? [_LJ __ _

ACTION; If no, flag as estimated (J) all the samples forwhich AL, Ca, Fe, or Mg is higher than in ICS.

A. 1.15.2 Circle all values on each Form IV that are morethan + 20% of true or established mean value.

Are all Interference Check Sample results insidethe control limits (± 20%)?

If no, is concentration of Al, Ca, Fe, or Mg lower Vthan the respective concentration in ICS? [__] __ /*

300902

STANDARD OPERATING HOCmiRE Page 14 of 34

Title: Evaluation of Metals Data lor the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract , Revision: 11Compliance (Total Review)

If no, flag as estimated (J) those positiveresults for which ICS recovery is between 121-150%;flag all sanple results as estimated if ICSrecovery falls within 50-79%; reject (red-line)those sanple results for which ICS recovery is lessthan 50%; if ICS recovery is above 150%, rejectpositive results only (not flagged with a "U") .

A. 1.16 FOTTI y A (SpiXed P*T|T»le Recovery — Pre— Digestion/Pre— Distillation) —( Note: Not required for Ca, Mg, K, and Na (both matrices) , Al, and Fe(soil only.)

XA. 1.16.1 Present and complete for: each SDG?

each matrix type? f * 1 __ __

each cone, range (i.e. low, med., high)? r X_] __ __

For both AA and ICP when both are used for V/the same analyte? [__] __ A

ACTION: If no for any of the above, flag asestimated (J) all the positive data lessthan four times the spiking levels specifiedin SOW for which spiked sanple was not analyzed.

NOTE; If one spiked sample was analyzed for morethan 20 samples, then first 20 samplesanalyzed do not have to be flagged asestimated (J).

A. 1.16.2 Was field blank used for spiked sanple?

ACTION: If yes, flag all positive data less than4 x spike added as estimated (J) for whichfield blank was used as spiked sanple.

A. 1.16.3 Circle on each Form VA all spike recoveries thatare outside control limits (75% to 125%).

Are all recoveries within control limits? [__] X

If no, is sample concentration greater than or equal yto four times spiJce concentration? [__]

300903

STANDARD OPERATING PWDCECDRE Page 15 of 34

Title: Evaluation of Metals Data for theContract. laboratory ProgramAppendix A.I: Data Assessment - ContractCompliance (Total Review)

Date: Jan. 1992Number: HW-2Revision: 11

A. 1.16. 4

sACTIOM; If yes, disregard spike recoveries for analytes

whose concentrations are greater than or equalto four times spike added. If no, circle thoseanalytes on Fora V for which sample concentrationis less than four tines the spike concentration.

Are results outside the control limits (75-125%)flagged with "N" on Form I's and Form VA?

ACTION: If no, write in the Contract - Problem/Non -Carpi ianoe section of "Data Assessment Narrative".

AqueousAre any spike recoveries:

(a) less than 30%?

(b) between 30-74%?

(c) between 126-150%?

X

(d) greater than 150%? __

ACTION; If less than 30%, reject all associated aqueousdata; if between 30-74%, flag all associatedaqueous data as estimated (J) ; if between126-150%, flag as estimated (J) all associatedaqueous data not flagged with a "U"; ifgreater than 150%, reject (red-line) allassociated aqueous data not flagged with a "U".

V[__]

[ __ ]

f X 1

f )( 1

N/A

V/[A 1 __ __

A.1.16.5Are any spiXe recoveries:

(a) less than 10%?

(b) between 10-74%?

(c) between 126-200%?

(d) greater than 200%?

_ L_] X_ [_] X_ L_J 2L_ !_. i.

300904



fi N/AACTION: If less than 10%, reject all associated data; if

between 10-74%, flag all associated data as estimated;if between 126-200%, nag as estimated all associateddata was not flagged with a "U"; if greater than 200%,reject all associated data not flagged with a "IT*.

A 1 17 Form VT (T^ Duplicates)V

A. 1.17.1 Present and conplete for: each SDG? [ 1 __ __

each matrix type? f V 1 __ __

each concentration range (i.e. low, med. , high)? [ X 1 __ __

both AA and ICP when both are used for the same Vanalyte? [ __ ] __ __

ACTION; If no for any the above, flag as estimated(J) all the data >CRDL* for which duplicatesample was not analyzed.

Note: 1. If one duplicate sample was analyzed formore than 20 samples, then first 20 samples do nothave to be flagged as estimated.

2. If percent solids for soil sample and its duplicatediffer by more than 1%, prepare a Form VI for eachduplicate pair, report concentrations in ug/Lon wet weight basis and calculate RFD or Differencefor each analyte. x

VA. 1.17.2 Was field blank used for duplicate analysis? __ [ A 1 __

ACTION; If yes, nag all data >CRDL* as estimated(J) for which field blank was used as duplicate.

A. 1.17.3 Are all values within control limits (RPD 20% or \difference < 4CRDL)? r A 1 __ __

If no, are all results outside the control limits \/flagged with an * on Form I's and VI? [__] __ X

ACTION; If no, write in the Contract - Problems/Non-Compliance section of "Data Assessment Narrative".

* Substitute IDL for CRDL when IDL > CRDL.

300905


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.1: Data Assessment - Contract Revision: 11Compliance {Total Review) f

__ _. __.NOTE; l. KPD is not calculable for an analyte of the

sample - duplicate p»<r- when both values areless than IDL.

2. If the result of lab duplicate analyzedby GFAA is rejectable due to coefficient ofcorrelation of MSA, analytical spike recovery,or duplicate injections criteria, do not applyprecision criteria to metals analyzed by GFAA.

A.1.17.4 Aqueous

Circle on each Form VI all values that are:

RPD > 50%, orDifference > CRDL*

Is any RFD greater than 50% vhere sanple and duplicate Vare both greater than or equal to 5 times *CRDL? __ [_L_3 __

Is any difference** between sanple and duplicate greater \than *CRDL where sanple and/or duplicate is less than V5 times *CRDL? __ f" 1 __

ACTION: If yes, flag the associated data as estimated.

A.1.17.5


RPD > 100%, or

Difference > 2 x CRDL*

Is any RFD (vhere sanple and duplicate are bothgreater than or equal to 5 times *CRDL) :

> 100%? __ [__] r

Is any **difference between sanple and duplicate ,(where sanple and/or duplicate is less than 5x*CRDL) : V

> 2x*CRDL? __ [__] _

* Substitute IDL for CRDL when IDL > CRDL.** Use absolute values of sanple and duplicate to calculate the difference.

30090S


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Conpliance (Total Review)

N£ N/A

ACTIOM: If yes, flag the associated data as estimated.

A.1.18 Field Duplicates .

A.1.18.1 Were field duplicates analyzed? [2_J __ __

ACTION; If yes, prepare a Form VI for each aqueous fieldduplicate pair. Prepare a Fora VI for each soilduplicate pair, if percent solids for sample andits duplicate differ by more than 1%; reportconcentrations of soils in ug/1 on wet weightbasis and calculate RPDs or Difference for eachanalyte.

NOTE; 1. Do not calculate RPD when both values areless than IDL.

2. Flag all associated data only for fieldduplicate pair.

A.1.18.2 Aqueous

Circle all values on self prepared Form VI forfield duplicates that are:


Is any RPD greater than 50% where sample and duplicateare both greater than or equal to 5 times *CRDL? __

Is any **difference between sample and duplicate greaterthan *CRDL where sample and/or duplicate is less than5 times *CRDL? . __

If yes, flag the associated data as estimated.>

* Substitute IDL for CRDL when IDL > CRDL.** Use absolute values of sample and duplicate to calculate the difference.

300907

STANDARD OPERATING PROCEDURE Pag* 19 of 34

Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data Aniin.i iffrth - ContnCompliance (Total Review)


A.1.18.3

Y££ NJ2


RPD >100%, or


Is any RPD (where sample and duplicate are bothgreater than 5 times *CRDL) :

Is any **dif ference between sample and duplicate(where sample and/or duplicate is less than 5x *CRDL )

>2x *CRDL?

ACTICH: If yes, flag the associated data as estimated.

N/A

_ [_] _LL

A. 1.19 Forn VH (Laboratory Control P*Tlt) (Note: LCS - notrequired for aqueous Hg and cyanide analyses.)

A. 1.19.1 Was one LCS prepared and analyzed for:

each SDG?

each batch samples digested/distilled?

both AA and ICP when both are used for the sameanalyte?

If no for any of the above, prepare TelephoneRecord Log and contact laboratory for submittalof results of I£S. Flag as estimated (J) allthe data for which LCS was not analyzed.

If only one LCS was analyzed for more than 20samples, then first 20 samples close to LCSdo not have to be flagged as estimated.

t_) _ .2.

* Substitute IDL for CRDL when IDL > CRDL.** Use absolute values of saitple and duplicate to calculate the difference.

300908


Title: Evaluation of Metals Data for theContract laboratory ProgramAppendix A.I: Data Assessment - ContractCoitpliance (Total Review)


JESA.I.19.2

Circle on each Fora VII the US percent recoveriesoutside control limits (80 - 120%) except for aqueousAg and Sb.

Is any LCS recovery: less than 50%?

between 50% and 79%?


_ [>J_ (V,_ tXj

greater than 150%? __

ACTION; TPSS than 50%, reject (red-line) all data;between 50% and 79%, flag all associated dataas estimated (J); between 121% and 150%, flagall positive (not flagged with a "U") resultsas estimated; greater than 150%, reject allpositive results.

N/A

A.I.19.3 Solid LCS

ACTION;

ACTION;

If "Found" value of DCS is rejectable due to duplicateinjections or r lYtl" ] spike recovery criteria,regardless of LCS recovery, flag the associated dataas estimated (J).If IDL of an analyte is equal to or greater thantrue value of LCS, disregard the "Action" below eventhough LCS is out of control limits.

Is LCS "Found" value higher than the controllimits on Form VII?

iated positive dataIf yes, qualify all asas estimated.

Is LCS "Found" value lower than the Controllimits on Form VTI?

If yes, qualify all associated data asestimated.

__ [_] 11.

300909


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

__ _- __.

A.1.20 F?m ff (ICP Serial Dilution) -

NOTE; Serial dilution analysis is required onlyfor initial concentrations equal to orgreater than 10 x IDL.

A. 1.20.1 Was Serial Dilution analysis performed for: Veach SDG? f /* 1 __ __

Veach matrix type? [ A ] __ __

each concentration range (i.e. low, mad.)? [ /> ] __ __

ACTION; If no for any of the above, flag as estimatedall the positive data > lOxIDLs or > CRDL whenlOxIDL < CRDL for which Serial Dilution Analysiswas not performed.

vA. 1.20.2 Was field blank(s) used for Serial Dilution Analysis? __ [

ACTION; If yes, flag all associated data > 10 x IDLas estimated (J). If lOxIDL < CRDL, flag alldata >. CRDL.

A.1.20.3 Are results outside control limit flagged with an "E"on Form I's and Form DC when initial concentration onForm IX is equal to 50 times IDL or greater.

ACTION; If no, write in the Contract-Problero/Non-Compliance section of the "Data AssessmentNarrative".

A. 1.20.4 Circle on each Form DC all percent differencethat are outside the control limits for initialconcentrations equal to or greater than 10 x IDLs only.

Are any % difference values:

3

> 100%? A [__] __

300910



__ _ _ACTION; Flag as estimated (J) all the associated sample

data > lOxIDLs (or > CRDL when lOxIDL < CRDL)for which percent difference is greater than 10%but less than 100%. Reject (red-line) all theassociated sample results equal to or greaterthan lOxIDLs (or > CRDL when lOxIDL < CRDL) forwhich PD is greater than or equal to 100%.

Note; Flag or reject on Form I's only the sample resultswhose associated raw data are > lOxIDL (or > CRDLwhen lOxIDix CRDL)

A.1.21 Furnace Atomic Absorbtion (AA) QC

A. 1.21.1 Are duplicate injections present in furnace raw data(except during full Method of Standard Addition) for yeach sample analyzed by GFAA? [__]

ACTION; If no, reject the data on Form I's for whichduplicate injections were not performed.

A. 1.21.2 Do the duplicate injection readings agree within 20%Relative Standard Deviation (RSD) or Coefficient of VVariation (CV) for concentration greater than CRDL? [___]

Was a dilution analyzed for sample with analyticalspike recovery less than 40%? [__]

ACTION; If no for any of the above, flag all theassociated data as estimated.

A. 1.21.3 Is *analytical spike recovery outside the control \Vlimits (85-115%) for any sample? A [__] __

ACTION; If yes, flag as estimated the affected sample resultsif the recovery is between 10-84%; if the recovery isbetween 115-200%, flag the associated positive sampleresults as estimated; reject the associated sampleresults if the recovery is less than 10%; rejectpositive sample results if the recovery is greaterthan 200%.

* Analytical spike is not required on the pre-digestion spiked sample.

300911

STANDARD CHEATING PROCEDURE Page 23 of 34

Title: Evaluation of Metals Data for the Data: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11


s N/ANOTE; Reject or flag the data only when the affected

sample (s) was not subsequently analyzed by Methodof Standard Addition.

A. 1.22 FOr" VIII (Method of

{X 1A. 1.22.1 Present? f-^ 1 __ _

If no, is any Form I result coded with "SH or a "+"? __ [__] V

ACTION; If yes, write request on Telephone Record Logand contact laboratory for submittal of Form VIII.

A. 1.22.2 Is coefficient of correlation for MSA less than 0.990 for \,any saitple? __ [__] *

ACTION; If yes, reject (red-line) the affected data.

VA. 1.22.3 Was *MSA required for any sample but not performed? __ • [__] _

Is coefficient of correlation for MSA less than 0.995? __ [__]

Are MSA calculations outside the linear range of thecalibration curve generated at the beginning of the \/analytical run? __ [__] *

ACTION; If yes for any of the above, flag allthe associated data as estimated (J).

A. 1.22.4 Was proper quantitation procedure followed correctly yas outlined in the SOW on page E-23? [__] __ "

ACTION; If no, note exception under Contract Problem/Non-Compliance section of the "Data AssessmentNarrative", and prepare a separate list.

* MSA is not required on LCS and prep, blank.

300912

STANDARD OPERATING PROCEDURE Pag* 24 Of 34

Title: Evaluation n_ totals Data for the Date: Jan. 1992Contract Lc-lwraSxiry Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

ifi N/A

A. 1.23.1 Were any analyses performed for dissolved as well as Wtotal analytes on the sane sample(s). __ t_i_] __

Were any analyses performed for inorganic as well as total \,(organic + inorganic) analytes on the same sample (s)? __ L±_l __

NOTE; 1. If yes, prepare a list comparing differencesbetween all dissolved (or inorganic) andtotal analytes. Compute the differences asa percent of the total analyte only whendissolved concentration is greater than ORDLas well as total concentration.

2. Apply the following questions only if in-organic (or dissolved ) results are (i) aboveCRDL, and (ii) greater than total constituents.

3. At least one preparation blank, ICS, and LCSshould be analyzed in each analytical run.

A. 1.23. 2 Is the concentration of any dissolved (or inorganic) -. xanalyte greater than its total concentration by ynore than 10%? __ [ __ ] __

A. 1.23. 3 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration bymore than 50%?

ACTION: If more than 10%, flag both dissolved (orinorganic) and total values as estimated (J) ;if more than 50%, reject (red-line) the datafor both values.

A. 1.24 Fora I (Field Blank! -

(jtote.* Pftffimate |fField Blany* ff y

A. 1.24.1 Circle all field blank values on Form I that aregreater than CRDL, (or 2 x IDL .when H3L > CRDL) .

Is field blank concentration less than CRDL(or 2 x IDL when IDL > CRDL) for all parametersof associated aqueous and soil samples?

300913


Title: Evaluation of Metals' Zata for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContractCcrnpliance (Total Review)


If no, was field blank value already rejecteddue to other QC criteria?

If no, reject (except field blank results)all associated positive sample data lessthan or equal to five tines the field blankvalue. Reject on Form I's the soil sampleresults that when converted to ug/L on wetbasis are less than or equal to five timesthe field blank value in ug/L.

YES N/A

A.1.25 porm x. n. 3PI {Verification of

A. 1.25.1 Is verification report present for:

Instrument Detection Limits (quarterly)?

ICP Interelement Correction Factors (annually)?

ICP Linear Ranges (quarterly)?

ACTION; If no, contact TPO of the lab.

A.I. 25. 2 Form X (Instnrognt Detection Trequired for Cyanide.)

~ (Note: IDL is not

A.1.25.2.1 Are IDLs present for: all the analytes?

all the instruments used?

For both AA and ICP when both are used for the sameanalyte?

ACTION; If no for any of the above, prepareTelephone Record Log and contactlaboratory.

A. 1.25.2.2 Is IDL greater than CRDL for any analyte?

If yes, is the concentration on Fora I of the sampleanalyzed on the instrument whose IDL exceeds CRDL,greater than 5 x IDL.

•y

[__] __ _1_\

t_i _ _

300914

STANDARD OWRATE'S FROCTXURE Page 26 of 34

Title: Evaluation of Metals Data *ry- va Date: Jan. 1992Contract laboratory Frogr<ci Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

YJS i g j i K / A

Action : If no, flag as estimated all values Icthan five times IDL of the instrument whoseIDL exceeds GRDL.

A.1.25.3A. 1.25.3.1 Was any sample result higher than high linear range

of ICP.

Was any sample result higher than the highestcalibration standard for non-ICP parameters?

If yes for any of the above, was thesample diluted to obtain the result on Form I? [__] __

ACTION; If no, flag the result reported on Form Ias estimated (J).

A.1.26 Percent Solids of S** ™nt3

A. 1.26.1 Are percent solids in sediment(s): V/< 50%? __ [__] *

< io%? _ACTION; If yes, qualify as estimated all the

results of a sample that has per centsolids between 10%-50% (i.e. moisturecontent between 50%-90%). Reject allthe results of a sample that has per centsolids less than 10% (i.e. moisture contentgreater than 90%).

NOTE; Reject or flag(J) only the sample resultsthat were not previously rejected or flageddue to other QC criteria.

300915

U.S. EPA - CLP

DUPLICATESEPA SAMPLE NO

Lab Name:

Lab Code:

JL Contract:

Case No.: *-"71 SAS Ho.: SDG No. :

Matrix (soil/water) :

* Solids for Sample:

Level (low/med): i-o '

\ Solids for Duplicate:

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

11I Analyte1i AluminumI AntimonyI Arsenic ~~I BariumI BerylliumI CadmiumI CalciumI Chromium1 CobaltI CopperI Iron(Lead1 Magnesium| ManganeseI Mercury1 Nickel| PotassiumI Selenium1 Silver! SodiumI ThalliumI VanadiumIZincI Cyanide1

ControlLimit

1111

.,

11

Sample (S) C|

/•/* IBI3. i.o \(A\3.<z iei

3 ^ . 3 | fr |/. <-> I<A|• X O I t f l

/yc-po 1 1*.^ IP,!V.& IUI</. o IUI

>^^ 1 1/.o Ml

-30^0 fBIV0.6 I I0.1& \(*\-3.0 IUI

\-=><*o 1BIa.o IMIZ - O i f / I

/ I f c 0 c > I Ir .O IM!?.o l ( / l

/V-^ ISI'*•<> \U\

\ \

\\

Duplicate (D) C|1

is& IS!y-f.o \(A\t.^ l /^ l

36.? • |/SIAO IM*.Q \<A\

(£-/crv \ \•=>.* \£\<-/. 0 \t*\o.v \*\^v</ i r/.o \l*\

t/S-0 1 &\*/T.V \ 10.20 IM.I•?-6 UA!

/ f / ^ I /SI5L./ 1/51-?.& 1^1

//-9^^ | |/.& \IA\

•&.G \(A/> -^7 1-7*1/o.o \IA\

1 1

RPD

7-y

S,"5--VO. o

-L.O/I. 0

2-5^

/#A 9

io.<?T^-0

^.o

//, <?

Q

•

M :

|

iI1

!iiiii!

i

!1Ii!!111i!I!!

FORM VI - IN 3/90


Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.2: Data Assessment Narrative

Page 27 of 34


Case*

SDG#

Contractor

2299

Z2299

Geraehtv & Miller. Inc.

Site Qlean Well Field

LablEA

Reviewer L. Siogren

Matrix: Soil

Water X

Other

A.2.1 Validation Flags-

J-

Red- Line-

Fullv Usable Data-

Contractual Oualifiers-

The following flags have been applied in red by thedata validator and must be considered by the datauser.

This flag indicates the result qualified as estimated.

A red-line drawn through a sample result indicatesunusable value. The red-lined data are known tocontain significant errors based on documentedinformation and must not be used by the data user.

The results that do not carry *J* or "red-line" arefitlfy usable.

The legend of contractual qualifiers applied by the labon Form I's is found on page B-20 of SOW 1IM01.0.

A. 2.2 The data assessment is given below and on the attached sheets.

GERAGHTY & MILLER, INC. DATA ASSESSMENT

The following CRDL standard spike recoveries were outside the control limits of 80-120%:

Analyte

Copper - InitialCopper - FinalAntimony - Final

% Recovery

77.367.179.7

300917

STANDARD OPERATING PROCEDUREPage 28 of 34

Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.2: Data Assessment Narrative Revision: 11

The following sample results were qualified based on the associated CRDL standardresults listed above:

Sample I.D. Analyte Concentration (ug/L)MGGWEW3 Copper 4.0 UJMGGWDP1 Copper 4.0 UJFB-1 Copper 4.0 UJ

The spike sample recovery of selenium was 69.0% which is below the control limitsof 75-125%. As a result, selenium non-detects were qualified as estimated (UJ) andselenium hits were qualified as estimated (J).

The percent difference values of calcium and magnesium reported for the ICP serialdilution analysis were 67.5% and 255.3% respectively. Both these percent difference valuesare above the control limit of 10%. Since calcium was detected in the samples withconcentrations > CRDL, these results were qualified as estimated (J). Since magnesium wasdetected in the samples with concentrations < CRDL, no qualification of the magnesiumresults was necessary.

The arsenic post-digestion spike recovery for sample MGGWEW3 was 82.5% whichis outside the control limits of 85-115%. As a result, the arsenic detected in this sample wasqualified as estimated (J).

Selenium post-digestion spike recoveries were 84.0%, 124.0% and 75.0% for samplesMGGWDP1, FB-1 and MGGWEW3, respectively. These spike recoveries are outside thecontrol limits of 85-115%. As a result, the selenium detected in sample MGGWDP1 wasqualified as estimated (J) and the non-detect selenium result for sample MGGWEW3 wasqualified as estimated (UJ). No qualification of the non-detect selenium result for FB-1 wasnecessary since the post-digestion spike recovery was found to be above control limits.

The quality of the data is acceptable with the qualifications discussed above.

300918



A.2.3 Contract-Problem/Non-Compliance


No contract problems were found.

MMB Reviewer: _________________________ Date:Signature

Contractor Reviewer: e^9^~ c*>>*<.^-^ Date:Signature

Verified by: _____________________________ Date:

OL2799ZI.doc

300919

Evaluation of Metals Data for tha Contract Laboratory Program (CLP)

based on

SOW. 3/90

(SOP Revision XI)

PREPARED BY; Tfl'i ^-'l ^-VU.^(/\________________ DATE; | — 3 <*Quality Assurance Chemist

•izardous Waste Section

APPROVED BY; fy .«-..'TV V.) '• >.vj\>- VKevin Kubi, ChiefToxic and Hazardous Waste Section

APPROVED BY!\ e x P . / y y - / < ^ ^ " __________ DAIE:Runyon, hi

Monitoring Management Branch

3Q0920-

STANDARD f?;--™.? KW2EURE Page 1 of 34

Title: Evaluation of Metals Data'-i r c ia Date: Jan. 1992Contract laboratory Program Number: HW-2

Revision: 11 '

1.0

1 . 1 This procedure is applicable to inorganic data obtained from contractorlaboratories working for Hazardous Waste Site Contract LaboratoryProgram (CLP).


2.0 Responsibilities - Data reviewers will complete the following tasks as assigned by theData Review Coordinator:

2.1. For a total review;

2.1.1 Data Assessment - "Total Review-Inorganics*1 Checklist App** ** (A.IKThe reviewer must answer every question on the checklist.

2.1.2 Da a Ass atrynt •• Pfitat As3/*s°'TW>nt y*rrat'iv< (Acrfrviiix A. 2)The answer on the checklist must match the action in the narrative(appendix A. 2} and on Form I's. Do not use pencil to write the narrative.

2.1.3 Contract Non-compliance - BMP Report (Appendix A. 3)This report is to be completed only when a serious contract violation isencountered, or upon the request of the Data Validation Task Monitor, or TechnicalProject Officer (TPO) . Forward 5 copies: one each for internal files,appropriate Regional TPO, Sample Management Office (SMO) and last two addresses ofMailing List for Data Reviewers (Appendix A. 4). In other cases, all contractviolations should be appended to the end of the Data Assessment Narrative (Sec.A.2.2).

2.1.4

2.1.4.1 Appendix A. 5Fill in the total number of analytes analyzed by different analyses andthe number of analytes rejected or flagged as estimated due to correspondingquality control criteria. Place an "X" in boxes where analyses were notperformed, or criteria do not apply.

2.1.4.2 Appendix A. 6Data reviewer is also required to fill cut Inorganic Regional Data Assessmentform (Appendix A.7) provided by EPA Headquarters. Codes listed on the formwill be used to describe the Data Assessment Summary.

300921


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2

Revision: 11

2.1.5 Data Review Log: It is iwyiiiumtert that each data reviewer should maintain a log ofthe reviews completed to include: a. date of start of case revie//

b. date of completion of case reviewc. sited. case numbere. contract laboratory. f. number of samples" g. matrixh. hours workedi. reviewer initials

2.1.6 Telephone Record Log - the data reviewer should enter the bare facts ofinquiry, before initiating any phone conversation with CLP laboratory.After the case review has been completed, mail white copy of TelephoneRecord Log to the laboratory and pink copy to SMD. File yellow copy inthe Telephone Record Log folder, and attach a xerox copy of the TelephoneRecord Log to the completed Data Assessment Narrative (Appendix A.2).

2.1.7 Forwarded Paperwork«

2.1.7.1 Upon completion of review, the following are to be forwarded to the RegionalSample Control Center (RSOC) located in the Surveillance and Monitoring Branch:a. data packageb. completed data assessment checklist (Appendix A.I,original)c. SMO Contract Compliance Screening (CCS)d. Record of Communication (copy)e. CLP Reanalysis Request/Approval Record (original + 3 copies)f. Appendix A.6 (original).

2.1.7.2 Forward 2 copies of completed Data Assessment Narrative (Appendix A.2)along with 2. copies of the Inorganic Data Assessment Form (Appendix A. 6) andTelephone Record Log , if any,: one each for appropriate Regional TPO,and the other one to EPA EMSL office in Las Vegas. The addresses of TPOs and EPAoffice in Las Vegas are given in Appendix A-4. ;


Appendix A.6.b. Telephone Record Log (copy)c. SMD Report (copy Appendix A-3)d. CLP Reanalysis Request/Approval Record (copy)

300922

STANDARD OPERATING PROCEDURE Page 3 Of 34r

Title: Evaluation of Metals Data for the Data: Jan. 1992Contract Laboratory Program Number: HW-2

Revision: 11

3.0 _________ __Each data package is checked by a Regional Sample Control Coordinator (RSSC) forcorpleteness. A data package is M»imad to be complete when all the deliverablesrequired under the contract are present. If a data package is inccnplete,the RSSCwould call the laboratory for missing document (s) . If the laboratory does not respondwithin a week, SMD and Mffi coordinator of Region II will be notified.



6.0 SMD Contract OT iT"** Scr lin (PCS) - This is intended to aid reviewer in locatingany problems, both corrected and uncorrected. However, the validation should be carriedout even if CCS is not present. Resubmittals received from laboratory in response toCCS must be used by the reviewer.

7.0 Request for Reanalysis - Data reviewers must note all items of contract non-compliancewithin Data Assessment Narrative. If holding tines and sample storage times have not beenexceeded, TPO may request reanalysis if items of non-compliance are critical to dataassessment. Requests are to be made on "CLP Re-Analysis Readiest/Approval Record".

8.0 Record of Comafiini7 i7n - Provided by the Regional Sample Control Center (RSCC) toindicate which data packages have been received and are ready to be reviewed.

9.0 Pounding off nn if»»rj - The data reviewer will follow the standard practice.

300923

STANDARD OPERATING PROCEDURE 4 Of 34

Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContractCompliance (Total Review)

Oate: Jan. 1992Number: HWT2Revision: 11

A.1.1 Contrwt

ACTION: If no, contact RSCC.

(CCS) - Present?

A. 1.2 Record of Oonnmnication (from RSCC) - Present?

ACTION; If no, request from RSCC.

A. 1.3 Trip Report - Present and complete?

ACTION; If no, contact RSCC for trip report.

A. 1.4 Sample Traffic Report - Present?

Legible?

ACTION; If no, request from Regional Sample ControlCenter (RSCC).



ACTION: If no, prepare Telephone Record Log, andcontact laboratory.

Do numbers of samples correspond to numbers on Recordof Communication?

Do sample numbers on cover page agree with samplenumbers on:


(b) Form I's?

ACTION; If no for any of the above, contact RSCC forclarification.

YES Up,

[__1 __

N/A

[__] __

300924


Title: Evaluation of Hetala Data for theContract Irthnaratoy ProgramAppendix A.I: Data Asaeuumt - ContractCompliance (Tbtal Review)

Date: Jan. 1992Number: Htf-2Revision: 11

A.l.6.1 Are all the Form I through Form IX labeled with:

Laboratory name?

Case/SAS number?

ERA sample No.?

SDG No.?

Contract No.?

Correct units?

Matrix?

ACTION; If no for any of the above, note underContract Prtiblenv Non-Compliance sectionof the "Data Assessment Narrative".

A. 1.6.2 Do any computation/transcription errors exceed 10% ofreported values on Forms I-IX for:

(NOTE: check all forms against raw data.)

(a) all analytes analyzed by ICP? [__]

(b) all analytes analyzed by GFAA? [__]

(c) all analytes analyzed by AA Flame? [__]

(d) Mercury? [__]

(e) cyanide? [__]

ACTION; If yes, prepare Telephone Log, contactlaboratory for corrected data andcorrect errors with red pencil and initial.

N/A

C__] _

X _

300925

STANDARD OPERATING FRDCZZXJRE Page 6 of 34

Title: Evaluation of Hetals Data for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContnCompliance (Total Review)

Data: Jan. 1992Number:Revision: 11

A.I.7 Raw Data

A. 1.7.1 Digestion Log* for flame AA/ICP (Form XIII) present?

Digestion Log for furnace AA Form xm present?

Distillation Log for mercury Form xm present?

Distillation log for cyanides Form XIII present?

Are pH values (pH<2 for all metals, pH>12 for cyanide)present?

*Weights, dilutions and volumes .used to obtain values.

Percent solids calculation present for soils/sediments?

Are preparation dates present on sample preparationlogs/bench sheets?

A. 1.7.2 Measurement read out record present? ICP

Flame AA

Furnace AA

Mercury

cyanides

A. 1.7.3 Are all raw data to support all sample analyses andQC operations present?

Legible?

Properly labeled?

Acnctl; If no for any of the above questionsin sections A.I.7.1 through A.I.7.3,write Telephone Record Log and contactlaboratory for resubmittals.

Hfi MB N/A

I _ ) _ A.

300926


Title: Evaluation of Metals for the Contract Date: Jan. 1992laboratory Program Number: HW-2Appendix A.I: Data Assessment - Oontract Revision: !!••


YES NJ2 N/AA.1.8 Hftl inq Tin** - (aqueous and soil samples )


Mercury analysis (28 days)....... exceeded? __

Cyanide distillation (14 days)..... exceeded? __

Other Metals analysis (6 months).... exceeded? __

NOTE; Prepare a list of all samples and analytes forwhich holding times have been exceeded. Specifythe number of days from date of collection to the dateof preparation (from raw data). Attach to checklist.

ACTION; If yes, reject (red-line) values less thanInstrument Detection Limit (IDL) and flagas estimated (J) the values above IDL eventhough sample(s) was preserved properly.

A. 1.8.2 Is pH of aqueous samples for: VMetals Analysis >2? __ f A 1

Cyanides Analysis <12? __ f^A ]

Action; If yes, flag the associated metals and cyanidesdata as estimated.

A.1.9 FOrnl I (Fir*!

A. 1.9.1 Are all Form I's present and complete? r x\l __ __


A. 1.9.2 Are correct units (ug/1 for waters and mg/kg for soils) Vindicated on Form I's? [_Aj __ __

Are soil sample results for each parameter corrected forpercent solids? fxA 1 __

Are all "less than IDL" values properly oodpd with "U"? [X 1 __ __

300927



IBS Ifi N/A~Are the correct concentration qualifiers used with v,final data? [A"\ __ _

2CH3i: If no for any of the above, prepare TelephoneRecord log, and contact laboratory for correcteddata.

A. 1.9.3 Are EPA sample I s and corresponding laboratory sampleID f s the same as on the Cover Page, Form I's and i/in the raw data? [ X 1 __ __

Was a brief physical description of samples given \/on Form I«s? r A 1 __

Was the dilution of any sample diluted beyond therequirements of the contract noted on Form I or WForm XIV? __ f A 1

ACTION; If no for any of the above, note underOontract-Problem/Non-Compl ianceof the"Data Assessment Narrative".

4

A.1.10 Calibration

A.l.io.l Is record of at least 2 point calibration \/present for ICP analysis? [' ] __

Is record of 5 point calibration present forHg analysis?


Flame AA? [__]

Furnace AA? [X 1

cyanides?

Is one calibration standard at the CRDL level forall AA (except Hg) and cyanides analyses? [ A, 1 __ __

ACTION: If no for any of the above, write in theContract Problem/Non-Oompl iance section ofthe "Data Assessment Narrative".

300928



A. 1.10. 2 Is correlation coefficient less than 0.995 for:

Mercury Analysis?

Cyanide Analysis?

Atomic Absorption Analysis?

HS

1

M2 w.

tXi _t*J _t _ ] _


NOTE: The data validator shall calculate the correlationcoefficient using concentrations of the standardsand the coiT'uspuntling instrument response( e.g. absorbance, peak area, peak height, etc.).

A.1.10.3 In the instance where less than 4 standards aremeasured in absorbance (or peak area, peak height,etc.)mode, are the remaining standards analyzed inconcentration mode immediately after calibrationwithin ±10% of the true values? [__]

ACTION; If no, flag the associated data as estimatedif standards are not within ±10% of true values.Do not flag the data as estimated in linear rangeindicated by good recovery of standard (s).

A.l.ll Form II A (ini *i and Ooirt-i.w * < * *>T tion verification) —

A.l.il.i Present and complete for every metal and cyanide? [A ] __

Present and complete for AA and ICP when both are \/used for the same analyte? [/\ 1 __


A.l.ll.2 Circle on each Form HA all percent recoveries thatare outside the contract windows.Are all calibration standards (initial and continuing)within control limits:

Metals- 90-110%R? .__. __

Vq - 80-120%R? LA 1 __

Cyanides- 85-115%R? f \1 __

300929



as is"*N/A~ACTION; Flag as estimated (J) an positive data (not

flagged with a "U") analyzed between acalibration standard with %R between 75-89%(65-79% for Hg; 70-84% for CN) or lU-125%(121-135% for Hg; 116-130% for CN) recovery andnearest good calibration standard. Qualify results<IDL as estimated (UJ) if the ICV or CCV %R is75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line)as unacceptable data if recovery of the ICV orCCV is outside the range 75-125% (CN, 70-130%; Hg,65-135%). Qualify five samples on either side ofverification standard out of control limits.

A. 1.11.3 Was continuing calibration performed every 10 samples \,or every 2 hours? [)( ] __ __

Was ICV for cyanides distilled?

ACTION; If no for any of the above, write in theContrart-Prctolem/Non-Compliance section of the"Data Assessment Narrative".

«

A. 1.12 FO"" II B (CRDL 8t*"A>rTte for AA and ICP) -

A.1.12.1 Was a CRDL standard (CRA) analyzed after initial vcalibration for all AA metals (except Ha) ? \X 1 __ __

Was a mid-range calib. verification standard distilledand analyzed for cyanide analysis?

Was a 2xCRDL ( or 2xIDT. when IDL>CRDL) analyzed (CRI)for each ICP run?(Note: CRI for AL,Ba,Ca,Fe,Hg,Na,or K is not required.)


**True value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL.Conpute the concentration of the missing mid-range standard from the calibration range.

300930

A.1.13 FO TH IH (Initial and OOP ^ T*? calibration Blanks)

A. 1.13.1 Present and complete? [X1

For both AA and ICP when both are used for the wsame analyte? f A ]

Was an initial calibration blank analyzed? f X 1

Was a continuing calibration blank analyzed after \every 10 samples or every 2 hours (which ever is more yfrequent)? \n 1


Title: Evaluation of Metals Data for the Data: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

_

A.I.12.2 Was CRI analyzed after ICV/ICB and before the finalCCV/CCB, and twice every eight hours of ICP run?

ACTION; If no, write in Contract Problem/Non-ComplianceSection of the "Data Assessment Narrative11.

A. 1.12.3 Circle on each Form ILB all the percent recoveries thatare outside the acceptance windows.


Metals 80 - 120%R?


Cyanide 80 - 120%R? [X ] __ __

ACTION; Flag as estimated all sample results withinthe affected range if the recovery of thestandard is between 50-79%; flag only positivedata within the affected range if the recoveryis between 121-150%; reject all data within theaffected range if the recovery is less than 50%;reject only positive data within the affected rangeif the recovery is greater than 150%. Qualify 50% ofthe samples on either side of CRI standard outsidethe control limits.

Note: Flag or reject the final results only when sampleraw data are within the affected ranges and the CRDLstandards are outside the acceptance windows.

300931


Title: Evaluation of >!*tals Data for the Date: Jan. 1992Contract Laboratory i-zcgram Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review) *

M2 N/AACTION; If no, prepare Telephone Record Log, contact

laboratory and write in the Contract-Problems/Non-Compliance section of the "Data Assessment Narrative".


Are all calibration blanks (when IDKCRDL) less than orequal to the Contract Required Detection Limits (CRDLs)? [

Are all calibration blanks less than two times \>Instrument Detection Limit (when IDLX303L)? [/J_J __ __

ACTION: If no for any of the above, flag as estimated(J) positive sample results when raw samplevalue is less than or equal to calibrationblank value analyzed between calibration blankwith value over CRDL (or 2xIDL) and nearest goodcalibration blank.Flag five samples on either side of thecalibration blank outside the control limits.

A.1.14 FORM III (Preparation Blank) -(Note: The preparation blank for mercury is the sameas the calibration blank.)


each Sample Delivery Group (SDG)? f /(1 __ __

each batch of digested samples? r X1 __ __

each matrix type?

both AA and ICP when both are used forthe same analyte? f Xl __

ACTION; If no for any of the above, flag asestimated (J) all the associated positivedata <10 x IDLs for which prep, blankwas not analyzed.

NOTE; If only one blank was analyzed for morethan 20 sanples, then first 20 sanples analyzeddo not have to be flagged as estimated (J).

300932

.STANDARD OPERATING PROCEDURE Page 13 Of 34Title: Evaluation of Metals Data for the Data: Jan. 1992

Contract laboratory Procjyam Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

A.I. 14. 2YES

Is concentration of prep, blank value greaterthan the CRDL when IDL is less than or equal to CRDL? __

If yes, ia the concentration of the sample withthe least concentrated analyte less than 10 timaBthe prep. blank?

£t _ ] y.

If yes, reject (red-line) all associateddata greater than CRDL concentration butless than ten times the prep, blank value.

A. 1.14.3 Is concentration of prep, blank value (Form III) less \,than two tiines IDL, when IDL is greater than CRDL? [A ]

ACTION: If no, reject (red-line) all positive sampleresults when sample raw data are less than 10tiines the prep, blank value.

A. 1.14.4 Is concentration of prep, blank belowthe negative CRDL? __

ACTION; If yes, reject (red-line) all associated sampleresults less than lOxCRDL.

A.1.15 Fo"n IV (ICP Interference Check

A.1.15.1 Present and complete? [ A 1 __ __


Was ICS analyzed at beginning and end of run y(or at least twice every 8 hours)? f/>] __ __

ACTIOM; If no, flag as estimated (J) all the samples forwhich AL, Ca, Fe, or Mg is higher than in ICS.


Are all Interference Check Sample results inside \st/Ll __ __the control limits (± 20%)?

If no, is concentration of Al, Ca, Fe, or Mg lower V,than the respective concentration in ICS? [__] __ A

300933

STANDARD OPERATING FROCEniRE Page 14 of 34

Title: Evaluation of Mbtals Data fof the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract . Revision: 11Compliance (Total Review)

ACnOM; If no, flag as estimated (J) those positiveresults for which ICS recovery is between 121-150%;flag all sample results as estimated if ICSrecovery falls within 50-79%; reject (red-line)those sample results for which ICS recovery is lessthan 50%; if ICS recovery is above 150%, rejectpositive results only (not flagged with a "U").

A. 1.16 Form V A (?pJV*1 Pamole Recovery - Pre-Diaestion/Pre-Distillation)-( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe(soil only.)

A. 1.16.1 Present and complete for: each SDG? [X] __

each matrix type? [ Al __

each cone, range (i.e. low, roed., high)? C A\ __

For both AA and ICP when both are used forthe same analyte?

ACTION: If no for any of the above, flag asestimated (J) all the positive data lessthan four times the spiking levels specifiedin SOW for which spiked sample was not analyzed.


A. 1.16.2 Was field blank used for spiked sample? , __

ACTION: If yes, flag all positive data less than4 x spike added as estimated (J) for whichfield blank was used as spiked sample.

A.1.16.3 Circle on each Form VA all spike recoveries thatare outside control limits (75% to 125%).

Are all recoveries within control limits? [__]

If no, is sample concentration greater than or equalto four times spike concentration? [__]

300934

STANDARD OPERATING PKXmiRE Page 15 of 34


IS N/A

If yes, disregard spike recoveries for analyteswhose concentrations are greater than or equalto four times spike added. If no, circle thoseanalytes on Form V for which sample concentrationis less than four times the spike concentration.

Are results outside the control limits (75-125%)flagged with "N*1 on Form I's and Form VA?

ACTION; If no, write in the Contract - Problem/Non -Compliance section of "Data Assessment Narrative".

A.1.16.4 AqueousAre any spike recoveries:

(a) less than 30%? _

(b) between 30-74%? __ [__] /\

(c) between 126-150%?

(d) greater than 150%?

ACTION; If less than 30%, reject all associated aqueousdata; if between 30-74%, flag all associatedaqueous data as estimated (J); if between126-150%, flag as estimated (J) all associatedaqueous data not flagged with a "U11; ifgreater than 150%, reject (red-line) allassociated aqueous data not flagged with a "U".

A.1.16.5 SoiAre any spike recoveries:

(a) less than 10%?

(b) between 10-74%? X [__] __

(c) between 126-200%? __ f^V] __

(d) greater than 200%? __ r X1 __

300935


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: UConpliance (Total Review)

YES tfi N/AACTION: If less than 10%, reject all associated data; if

between 10-74%, flag an associated data as estimated;if between 126-200%, flag as estimated all associateddata was not flagged with a "U"; if greater than 200%,reject all associated data not flagged with a "U11.

A.1.17 Form v\ ft-Q Duplicates)

A. 1.17.1 Present and complete for: each SDG?

each matrix type?

each concentration range (i.e. low, med., high)?

both AA and ICP when both are used for the same V/analyte? [_A_] __ __

ACTION; If no for any the above, flag as estimated(J) all the data >CRDL* for which duplicatesanple was not analyzed.

Note; 1. If one duplicate sample was analyzed formore than 20 samples, then first 20 samples do nothave to be flagged as estimated.

2. If percent solids for soil sanple and its duplicatediffer by more than 1%, prepare a Form VI for eachduplicate pair, report concentrations in ug/Lon wet weight basis and calculate RPD or Differencefor each analyte. \

V/A. 1.17.2 Was field blank used for duplicate analysis? __ [/\_] __

ACTION; If yes, flag all data >CRDL* as estimated(J) for which field blank was used as duplicate.

A. 1.17.3 Are all values within control limits (RPD 20% or ,difference <±CRDL)? [__] X __

If no, are all results outside the control limitsflagged with an * on Form I's and VI?

ACTION; If no, write in the contract - Problems/Non-Compliance section of "Data Assessment Narrative".


300936


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.1: Data Annonnnrnt. - Contract Revision: 11Compliance (Total Review) *

^g———jgMOTE; 1. RPD is not calculable for an analyte of the

sample - duplicate r*tr when both values areless than IDL.


A.1.17.4 Aqueous



Is any RPD greater than 50% where sample and duplicate \are both greater than or equal to 5 times *CRDL? __ [__] /\

Is any difference** between sample and duplicate greater Ithan *CRDL where sample and/or duplicate is less than y5 times *CRDL?


A. 1.17.5

Circle on each Form VT all values that are:

RFD > 100%, or


Is any RPD (where sample and duplicate are bothgreater than or equal to 5 times *CRDL) : .

> 100%? __ [X1 __

Is any "difference between sample and duplicate(where sample and/or duplicate is less than 5x*CRDL) :

> 2x*CRDL? __ \X 1 __


300937

STANDARD OPERATING PROOEURE Page 18 of 34



A.I. 18 Field Duplicates

A. 1.18.1 Were field duplicates analyzed? [ __ ] / __

ACTION; If yes, prepare a Form VI for each aqueous fieldduplicate pair. Prepare a Fora VI for each soilduplicate pair, if percent solids for sample andits duplicate differ by more than 1%; reportconcentrations of soils in ug/1 on wet weightbasis and calculate RPDs or Difference for eachanalyte.



A. 1.18. 2 Aqueous



Is any RPD greater than 50% where sample and duplicate V/Aare both greater than or equal to 5 times *CRDL?

Is any **difference between sample and duplicate greaterthan *CRDL where sample and/or duplicate is less than V/5 times *CRDL? .. __ [ __ ] X



300938

STANDARD OPERATING PROCEDURE Peg* 19 Of 34

Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data ftnnn mm lit - CentoCompliance (Total Review)

Dot*: Jan. 1992NuDber: HW-2Revision: 11

A.1.18.3

Circle all values on self prepared Porn VI forfield duplicates that are:

RPD >100%, or


Is any RPD (where sample and duplicate are bothgreater than 5 times *CRDL) :

YES

Is any "difference between sample and duplicate(where sample and/or duplicate is less than 5x *CRDL ):

>2x *CRDL?


M2 N/A

C__]

A. 1.19 POTT* VII (Laboratory Control Pji"!T'10) (Note: LC? ~ notrequired for aqueous Hg and cyanide analyses.)

A.1.19.1 Was one LCS prepared and analyzed for:

each SDG?


both AA and ICP when both are used for the sameanalyte? [_

ACTION: If no for any of the above, prepare TelephoneRecord Log and contact laboratory for submittalof results of LCS. Flag as estimated (J) allthe data for which LCS was not analyzed.

NOTE; If only one LCS was analyzed for more than 20samples, then first 20 samples close to LCSdo not have to be flagged as estimated.

C/J _


300939

STANDARD OPERATING PROCEDURE 20 of 34

Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContractCcrpliance (Total Review)


A. 1.19. 2 Aqueous LCB

Circle on each Foot VII the LCS percent recoveriesoutside control limits (80 - 120%) except for aqueousAg and Sb.




greater than 150%?

ACTION; TPSS than 50%, reject (red-line) all data;between 50% and 79%, flag all associated dataas estimated (J) ; between 121% and 150%, flagall positive (not flagged with a "U") resultsas estimated; greater than 150%, reject allpositive results.

N/A

A.I.19.3 Solid LCS

ACTION;

ACTION;

If "Found" value of LCS is rejectable due to duplicateinjections or analytical spike recovery criteria,regardless of LCS recovery, flag the associated dataas estimated (J).If IDL of an analyte is equal to or greater thantrue value of LCS, disregard the "Action" below eventhough LCS is out of control limits.

Is LCS "Found" value higher than the controllimits on Form VII?

If yes, qualify all associated positive dataas

Is LCS "Found" value lower than the Controllimits on Form VII?

If yes, qualify all associated data asestimated.

300940


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review) ••

YES ie N/A"A. 1.20 pprm ix (TCP Serial Dilution) -


A. 1.20.1 Was Serial Dilution analysis performed for:each SDG? t*.

each matrix type? [A ]

each concentration range (i.e. low, med.)? f X 1


A. 1.20.2 Was field blank(s) used for Serial Dilution Analysis? __ F/^1 __4

ACTION: If yes, flag all associated data > 10 x IDLas estimated (J). If lOxIDL < CRDL, flag alldata > CRDL.

A.1.20.3 Are results outside control limit flagged with an "E" \on Form I's and Form IX when initial concentration on YForm IX is equal to 50 times IDL or greater. [__] __ '

ACTION; if no, write in the Oontract-Problem/Non-Compliance section of the "Data AssessmentNarrative11.

A. 1.20.4 Circle on each Form IX all percent differencethat are outside the control limits for initialconcentrations equal to or greater than 10 x IDLs only.


> 10%? __

> 100%?

300941



B N/AACTION; Flag as estimated (J) all the associated sample

data > lOxIDIfi (or > CRDL when lOxIDL < CRDL)for which percent difference is greater than 10%but less than 100%. Reject (red-line) all theassociated sample results equal to or greaterthan lOxIDlB (or > CRDL when lOxIDL < CRDL) forwhich PD is greater than or equal to 100%.

Note; Flag or reject on Form I's only the sample resultswhose associated raw data are >. lOxIDL (or > CRDLwhen 10xIDL< CRDL)

A. 1.21

A.1.21.1 Are duplicate injections present in furnace raw data(except during full Method of Standard Addition) foreach sample analyzed by GFAA?

ACTION: If no, reject the data on Form I's for whichduplicate injections were not performed.

A.1.21.2 Do the duplicate injection readings agree within 20%Relative Standard Deviation (RSD) or Coefficient ofVariation (CV) for concentration greater than CRDL?

Was a dilution analyzed for sample with analytical \,spite recovery less than 40%? [__] __ jk_


A.1.21.3 Is analytical spite recovery outside the controllimits (85-115%) for any sample?


* Analytical spite is not required on the pre-digestion spited sample.

300942


Title: Evaluation of Matals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11


A. 1.22.2 Is coefficient of correlation for MSA less than 0.990 forany sanple? _


calibration curve generated at the beginning of the V__ L/JJ

ACTION; If yes for any of the above, flag allthe nffffocia **"! data as estimated (J) .

A . l . 22 . 4 Was proper quantitation procedure followed correctlyas outlined in the SOW on page E-23?

ACTION; If no, note exception under Contract Problem/Non-Compliance section of the "Data AssessmentNarrative11, and prepare a separate list.

* MSA is not required on LC5 and prep, blank.

MOTE; Reject or flag the data only when the affectedsample (s) was not subsequently analyzed by Methodof Standard Addition.

A. 1.22.1 Present? [X 1 __

If no, is any Form I result coded with "S" or a "+"? __ [ __ ] j(_

ACTION: If yes, write request on Telephone Record Logand contact laboratory for submitted of Form VIII.

A.1.22.3 Was *MSA required for any sanple but not performed? __ - [/X ] __

Is coefficient of correlation for MSA less than 0.995? __ L__] __

Are MSA calculations outside the linear range of thecalibration curvanalytical run?

300943

STANDARD CHEATING PROCEZURE Page 24 of 34

Title: Evaluation oJ Katals Data for the Date: Jan. 1992Contract U-ba.-aSjory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

M2 N/A

A. 1.23.1 Were any analyses performed for dissolved as well as Y/total analytes on the same sample(s). __ [__] />

Were any analyses performed for inorganic as well as total y(organic + inorganic) analytes on the sane sample (s)? __ [__] A\

NOTE; 1. If yes, prepare a list comparing differencesbetween all dissolved (or inorganic) andtotal analytes. Compute the differences asa percent of the total analyte only whendissolved concentration is greater than CRDLas well as total concentration.



A. 1.23.2 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration bymore than 10%? __ [__] j2_

d (or inorganic) < \ntration by y

r i A

A. 1.23.3 Is the concentration of any dissolved (or inorganic) \analyte greater than its total concentration by yraore than 50%? __ [__] A

ACTION; If more than 10%, flag both dissolved (orinorganic) and total values as estimated (J);if more than 50%, reject (red-line) the datafor both values.

A.1.24 FQT™ I (Field Blank) - ;

(Notes r icrrm + "PiVld Blank" M ych OH Po* It)

A. 1.24.1 Circle all field blank values on Form I that aregreater than CRDL, (or 2 x IDL .when IDL > CRDL).


300944


Title: Evaluation of Metals -Data for theContract laboratory ProgramAppendix A.I: Data Assessment - ContractCarpi iance (Total Review)

Data: Jan. 1992Number: HW-2Revision: 11


if no, reject (except field blank results)all associated positive sample data lessthan or equal to five times the field blankvalue. Reject on Form I's the soil sampleresults that when converted to ug/L on wetbasis are less than or equal to five timesthe field blank value in ug/L.

A. 1.25

A. 1.2 5.1

V c a o n o f

Is verification report present for:




ACTION: If no, contact TPO of the lab.

A. 1.25. 2 For" X (Instrument Detecti'*required for Cyanide.)

A. 1.25. 2.1 Are IDLs present for:

~ (Note: IDL is not

all the analytes?



ACTION: If no for any of the above, prepareTelephone Record Log and contactlaboratory.


If yes, is the concentration on Form I of the sampleanalyzed on the instrument whose IDL exceeds CRDL,greater than 5 x IDL.

f /\ ]

i[_] _

& _

300945

STANDARD OPffEATf G FRDCFUJRE Page 26 of 34

Title: Evaluation of Metals Data frr- va Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Conpliance (Total Review)

N/'A

Action t If no, flag as estimated all values lessthan five times IDL of the instrument whoseTUL exceeds CRDL.

A.1.25.3

A.1.25.3.1 Was any sanple result higher than high linear rangeof ICP. ' __

Was any sanple result higher than the highest vcalibration standard for non-ICP parameters? X

If yes for any of the above, was thesanple diluted to obtain the result on Form I?

ACTION; If no, flag the result reported on Form Ias estimated (J).

A.1.26

A.1.26.1 Are percent solids in sediment(s):< 50%?

< 10%?

ACTION; If yes, qualify as estimated all theresults of a sanple that has per centsolids between 10%-50% (i.e. moisturecontent between 50*-90%). Reject allthe results of a sanple that has per centsolids less than 10% (i.e. moisture contentgreater than 90%).

NOTE; Reject or flag(J) only the sanple resultsthat were not previously rejected or flageddue to other QC criteria.

300946



Page 27 of 34


Case* 2137

SDG# A2137

Contractor Geraehtv & Miller. Inc.

Site Olean Well Field

LabffiA

Reviewer L. Sioeren

Matrix: Soil _

Water

Other

A.2.1 Validation Flags-

J-

Red- Line-

Fullv Usable Data-

Contractual Oualifiers-

The following flags have been applied in red by thedata validator and must be considered by the datauser.

This flag indicates the result qualified as estimated.

A red-line drawn through a sample result indicatesunusable value. The red-lined data are known tocontain significant errors based on documentedinformation and must not be used by the data user.

The results that do not carry *J" or "red-line' arefully usable.

The legend of contractual qualifiers applied by the labon Form I's is found on page B-20 of SOW IIM01.0.

A.2.2 The data assessment is given below and on the attached sheets.


For the initial calibration of lead performed on December 5, 1991, the correlationcoefficient calculated is < 0.995. Therefore, the lead results for the water preparation blankand water laboratory control sample associated with this initial calibration were qualified asestimated.

300947



_____Appendix A.2: Data Assessment Narrative_________Revision: 11____

The following CRDL standard spike recoveries were outside the control limits of80 -120%:

Run AnaMe % Recovery2 Lead 73.32-Final Copper 157.02-Final Lead 62.74 Lead 53.3

The following sample results were qualified based on the associated CRDL standardresults listed above:

Sample I.D. Anatyte Concentration (mg/kg^)ALSB050406 Copper 80.6 JMGSB050406 Copper 25.0 JMGSB050406 Lead 35.7 JMGSB050608 Copper 23.0 JMGSB050810 Copper 30.2 JMGSB050810 Lead 26.2 J

The following spike sample recoveries were outside the control limits of 75-125%:

Analyte % Recovery

Antimony 67.1Arsenic 74.9Selenium 71.9

For the samples in this SDG, all positive antimony, arsenic and selenium sampleresults were qualified as estimated (J) and all antimony, arsenic and selenium non-detectswere qualified as estimated (UJ).

300948



The thallium post-digestion spike recovery for field blank FB-4 was 192.0%. Sincethallium was not detected in FB-4, no qualification of this result was necessary. The seleniumpost-digestion spike recovery for sample MGSB050810 was 84.0%. The non-detect seleniumwas qualified as estimated (J).

The quality of the data is acceptable with the qualifications discussed above.




MMB Reviewer:________________________ Date:Signature

Contractor Reviewer: ^^L_- JX-a-~^_______Date:Signatvufe /

Verified by:_________________________ Date:

OL2137AI.doc

300949

Evaluation of Metals Data for the Contract Laboratory Program (CLP)

based on

SOW. 3/90

(SOP Revision XI)

PREPARED BY -v Vvi <- L l\Quality Assurance Chemist

zardous Waste Section

DATE:

''APPROVED BY: V o N. A-> \ >- V

APPROVED BYRobeA Runyon,Monitoring Memagement Branch

DATE: \ ~Kevin Kubik, ChiefToxic and Hazardous Waste Section

DATE:

"

300950

STANDARD :?r*°: 'ITA- HKXEDURE Page I of 34

Title: Evaluation of Metals Data xor wki Date: Jan. 1992Contract Laboratory Program Number: HW-2

Revision: 11 ••

l.o1.1 This procedure is applicable to inorganic data obtained from contractor

laboratories working for Hazardous Waste Site Contract LaboratoryProgram (CLP).


2.0 Responsibilities - Data reviewers will complete the following tasks as assigned by theData Review Coordinator:

2.1. For

2.1.1 Data Assessment - "Total Review-Inorganics" Checklist Appendix (A.IKThe reviewer must answer every question on the checklist.

" 2.1.2 Data Assessment - Data Assessment Narrative (Append* *-?)The answer on the checklist must match the action in the narrative(appendix A.2) and on Form I's. Do not use pencil to write the narrative.

2.1.3 Contract Non-Compliance - SMO Report (Appendix A.3)This report is to be completed only when a serious contract violation isencountered, or upon the request of the Data Validation Task Monitor, or TechnicalProject Officer (TPO). Forward 5 copies: one each for internal files,appropriate Regional TPO, Sample Management Office (SMD) and last two addresses ofMailing List for Data Reviewers (Appendix A.4). In other cases, all contractviolations should be appended to the end of the Data Assessment Narrative (Sec.A.2.2).

2.1.4 CLP Data Assessment Summary Forma

2.1.4.1 Appendix A.5Fill in the total number of analytes analyzed by different analyses andthe number of analytes rejected or flagged as estimated due to correspondingquality control criteria. Place an "X" in boxes where analyses were notperformed, or criteria do not apply.

2.1.4.2 Appendix A.6Data reviewer is also required to fill out Inorganic Regional Data Assessmentform (Appendix A.7) provided by EPA Headquarters. Codes listed on the formwill be used to describe the Data Assessment Summary.

300951


'Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2

Revision: 11

2.1.5 Data Review Log; It is recommended that each data reviewer should maintain a log ofthe reviews completed to include: a. date of start of case review

b. date of completion of case reviewc. sited. case numbere. contract laboratory

_ f. number of samplesg. matrixh. hours workedi. reviewer's initials

2.1.6 Telephone Record Log - the data reviewer should enter the bare facts ofinquiry, before initiating any phone conversation with CLP laboratory.After the case review has been completed, mail white copy of TelephoneRecord Log to the laboratory and pink copy to SMO. File yellow copy inthe Telephone Record Log folder, and attach a xerox copy of the TelephoneRecord Log to the completed Data Assessment Narrative (Appendix A. 2).

2.1.7 Forwarded Paperwork

2.1.7.1 Upon completion of review, the following are to be forwarded to the RegionalSample Control Center (RSCC) located in the Surveillance and Monitoring Branch:a. data packageb. completed data assessment checklist (Appendix A.I,original)c. SMO Contract Compliance Screening (CCS)d. Record of Communication (copy)e. CLP Reanalysis Request/Approval Record (original + 3 copies)f. Appendix A.6 (original).

2.1.7.2 Forward 2 copies of completed Data Assessment Narrative (Appendix A.2)along with 2. copies of the Inorganic Data Assessment Form (Appendix A. 6) andTelephone Record Log , if any,: one each for appropriate Regional TPO,and the other one to EPA EMSL office in Las Vegas. The addresses of TFOs and EPAoffice in Las Vegas are given in Appendix A-4.


Appendix A.6.b. Telephone Record Log (copy)c. SMO Report (copy Appendix A-3)d. CLP Reanalysis Request/Approval Record (copy)

300952

STANDARD OPERATING PROCEDURE Page 3 of 34•* r


Revision: 11

3.0 DataEach data package is checked by a Regional Sample Control Coordinator (RSSC) forcompleteness. A data package is assanned to be complete when all the deliverablesrequired under the contract are present. If a data package is incomplete, the RSSCwould call the laboratory for missing document (s) . If the laboratory does not respondwithin a week, SMD and MMB coordinator of Region II will be notified.



6.0 SM3 Contract Cccyl lance Screening (CCS) - This is intended to aid reviewer in locatingany problems, both corrected and uncorrected. However, the validation should be carriedout even if CCS is not present. Resubmittals received from laboratory in response toCCS must be used by the reviewer.

7.0 Request for Reanalysis - Data reviewers must note all items of contract non-conpliancewithin Data Assessment Narrative. If holding times and sample storage times have not beenexceeded, TPO may request reanalysis if items of non-compliance are critical to dataassessment. Requests are to be made on "CLP Re-Analysis Request/Approval Record".

8.0 Record of Corammication - Provided by the Regional Sample Control Center (RSCC) toindicate which data packages have been received and are ready to be reviewed.

9.0 Hounding off numbers - The data reviewer will follow the standard practice.

300953



Oate: Jan. 1992Number: HWT2Revision: 11

A.1.1 Contract Oraty>lii

ACTION; If no, contact RSCC.

(CCS) - Present?

A. 1.2 Record of Communication (from RSCC) - Present?

ACTION; If no, request from RSCC.

A. 1.3 Trip Report - Present and complete?

ACTION; If no, contact RSCC for trip report.

IBS M2

C _ 1 _ _X_

[_] _

A. 1.4 Sample Traffic Report - Present?

Legible?

ACTION: If no, request from Regional Sample ControlCenter (RSCC).



ACTION; If no, prepare Telephone Record Log, andcontact laboratory.




(b) Form I's?

ACTION; If no for any of the above, contact RSCC forclarification.

LAl _

300954


Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContractCompliance ("total Review)

Date: Jan. 1992Number: Htf-2Revision: li

A.1.6

A.1.6.1

Form I

v.1.6.2

Are all the Form I through Form DC labeled with:

Laboratory name?

Case/SAS number?

EPA sample No.?

SDG No.?

Contract No.?

Correct units?

Matrix?

ACTION: If no for any of the above, note underContract Prxfclem/Non-Oompliance sectionof the "Data Assessment Narrative".

Do any computation/transcription errors exceed 10% ofreported values on Forms I-LX for:


(a) all analytes analyzed by ICP?



(d) Mercury?

(e) Cyanide?

ACTION: If yes, prepare Telephone Log, contactlaboratory for corrected data andcorrect errors with red pencil and initial.

N/A

X

X _- XX

300955


Title:

A. 1.7

A. 1.7.1

Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContractCompliance (Total Review)

Raw Data

Digestion Log* for flame AA/ICP (Form XIII) pre

Date: Jan. 1992Number: HW- 2Revision: 11

YES NjQ

sent? [\ 1 __

N/A

Digestion Log for furnace AA Form XIII present?

Distillation Log for mercury Form XIII present?

Distillation Log for cyanides Form XIH present?

Are pH values (pH<2 for all metals, pit>12 for cyanide)present?

* Weights, dilutions and volumes used to obtain values.



A.1.7.2 Measurement read out record present? ICP

Flame AA

Furnace AA

Mercury

Cyanides


Legible?

Properly Labeled?

ACTION; If no for any of the above questionsin sections A.1.7.1 through A.1.7.3,write Telephone Record Log and contactlaboratory for resubmittals.

X

Qii _ _

300956


Title: Evaluation of Metals for the Contract Date: Jan. 1992laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: in-

compliance (Total Review)

YES NO N/AA. 1.8 TteitMng Times - (aqueous and soil samples )

(Examine sanple traffic reports and digestion/distillation logs.)

Mercury analysis (28 days)....... exceeded? __ [ A 1 __

Cyanide distillation (14 days)..... exceeded? __ [ Aj __

Other Metals analysis (6 months).... exceeded? __ [ X ] __

NOTE; Prepare a list of all sanples and analytes forwhich holding times have been exceeded. Specifythe number of days from date of collection to the dateof preparation (from raw data). Attach to checklist.

ACTION; If yes, reject (red-line) values less thanInstrument Detection Limit (IDL) and flagas estimated (J) the values above IDL eventhough sanple(s) was preserved properly.

A. 1.8.2 Is pH of aqueous saitples for: \ +Metals Analysis >2? __ r X 1 __

Cyanides Analysis <12? __ [ A ] __


A.1.9 ppTm I (PJjuO Dat^i)

A. 1.9.1 Are all Form I's present and ccrplete?


A. 1.9.2 Are correct units (ug/1 for waters and mg/kg for soils) ,,indicated on Form I's? [ X 1

Are soil sanple results for each parameter corrected for Vpercent solids? f A 1 __

Are all "less than IDL" values properly coded with "U"? [X 1 __

300957



YES I£ N/A"Are the correct concentration qualifiers vised with \,final data? . f A 1 __ _


A. 1.9. 3 Are EPA sample # s and corresponding laboratory sampleID # s the same as on the Cover Page, Form I's and ^in the raw data? [X ] __ __

Was a brief physical description of samples given \,on Form I's? [ /\1 __ __

Was the dilution of any sample diluted beyond therequirements of the contract noted on Form I or \ ,Form XIV? __ r\ 1 __

ACTION: if no for any of the above, note underContrart-ProbleiVllon-Conplianceof the"Data Assessment Narrative".

A. 1.10 calibration

A. l.io.l Is record of at least 2 point calibration

Is one calibration standard at the CRDL level forall AA (except Hg) and cyanides analyses?

ACTION: if no for any of the above, write in theContract Problem/Non-Compliance section ofthe "Data Assessment Narrative".

\.A 1present for ICP analysis? [ 1

Is record of 5 point calibration present for \,Hg analysis? C J __


Flame AA? [ __ ] __ A

Furnace AA? [ X 1 __ __

Cyanides? [ X 1 __ __

.1,

300958

XPresent and conplete for AA and ICP when both areused for the same analyte?

ACTION; if no for any of the above, prepare TelephoneRecord Log and contact laboratory.

A. 1.11. 2 Circle on each Form IIA all percent recoveries thatare outside the contract windows.Are all calibration standards (initial and continuing)within control limits: \7

Metals- 90-110%R? r A 1

Hg - 80-120%R? rX 1

Cyanides- 85-115%R?



_ i sA. 1.10.2 Is correlation coefficient less than 0.995 for:

Mercury Analysis? __ [ A 1 __

Cyanide Analysis? __ [_>_] __

Atomic Absorption Analysis? X [__] __


NOTE; The data validator shall calculate the correlationcoefficient using concentrations of the standardsand the corresponding instrument response( e.g. absorbance, peak area, peak height, etc.)*

A.1.10.3 In the instance where less than 4 standards aremeasured in absorbance (or peak area, peak height,etc.)mode, are the remaining standards analyzed inconcentration mode immediately after calibration \,within ±10% of the true values? [__] __ X

ACTION; If no, flag the associated data as estimatedif standards are not within ±10% of true values.Do not flag the data as estimated in linear rangeindicated by good recovery of standard (s).

A.1.11 Form II A (Initial and Continu'''ngf fl*n ration verification)~

A. 1.11.1 Present and complete for every metal and cyanide? [A 1 __ __

300959


;itle: Evaluation of Metals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

__ __, __.ACTION; Flag as estimated (J) all positive data (not

flagged with a "U") analyzed between acalibration standard with %R between 75-89%(65-79% for Hg; 70-84% for CN) or 111-125%(121-135% for Hg; 116-130% for CN) recovery andnearest good calibration standard. Qualify results<IDL as estimated (UJ) if the ICV or CCV %R is75-89% (CN, 70-84% ; H3, 65-79%). Reject (red-line)as unacceptable data if recovery of the ICV orCCV is outside the range 75-125% (CN, 70-130%; Bg,65-135%). Qualify five samples on either side ofverification standard out of control limits.

A. 1.11. 3 Was continuing calibration performed every 10 samples ,or every 2 hours? [X 1 __ __

Was ICV for cyanides distilled? fX 1 __ __

ACTION: If no for any of the above, write in theContract-Pnablem/Non-Compliance section of the"Data Assessment Narrative11.

A. 1.12 Font II B (CRDL Standards for AA

A. 1.12.1 Was a CRDL standard (CRA) analyzed after initial \/[ A ]calibration for all AA metals (except Ha)? [ A ]

Was a mid-range calib. verification standard distilledand analyzed for cyanide analysis? f A ]

Was a 2xCRDL ( or 2xIDL when IDL>CRDL) analyzed (CRI)for each ICP run? f A ](Note: CRI for AL,Ba,Ca,Fe,J r,Na,or K is not required.)

ACTION; If no for any of the above, flag as estimatedall data falling within the affected ranges.The affected ranges are:AA Analysis - **True Value + CRDLICP Analysis - **True Value ± 2CRDLCN Analysis - **True Value + 0.5 x True Value.

**True value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL.Corpute the concentration of the missing mid-range standard from the calibration range.

300960

"""•• STANDARD OPERATING PROCEDURE Page 11 of 34

Title: Evaluation of Matals Data for the Date: Jan. 1992Contract laboratory Program Number: FjW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

__ _ __A.I.12.2 Was CRI analyzed after ICV/ICB and before the final \>

CCV/CCB, and twice every eight hours of ICP run? [X 1 __ __

ACTION; If no, write in Contract Prtijlem/Non-OonplianceSection of the "Data Assessment Narrative".

A. 1.12.3 Circle on each Form IIB all the percent recoveries thatare outside the acceptance windows.


Metals 80 - 120%R? [__] A __


Cyanide 80 - 120%R? [\ 1 __ __


Note: Flag or reject the final results only when sampleraw data are within the affected ranges and the CRDLstandards are outside the acceptance windows.

A.I.13 Form III (Initial and Continuing Calibration Blanks)

A. 1.13.1 Present and complete?

For both AA and ICP when both are used for the ysame analyte? [/A. 1 __ __

Was an initial calibration blank analyzed? r X 1 __ __

Was a continuing calibration blank analyzed afterevery 10 samples or every 2 hours (which ever is more \/frequent)? [A 1 __ __

300961


Title: Evaluation of .I->.tii.s Data for the Date: Jan. 1992Contract Laboraiciy ircgram Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

NjQ N/AACTION: If no, prepare Telephone Record Log, contact

laboratory and write in the Contract-Problems/Non-Compliance section of the "Data Assessment Narrative11.


Are all calibration blanks (when IDIXCRDL) less than or wequal to the Contract Required Detection Limits (CRDLs)? [\ ] __ __

Are all calibration blanks less than two timesInstrument Detection Limit (when IDLXKDL)? [^ ] __ __

ACTION: If no for any of the above, flag as estimated(J) positive sample results when raw samplevalue is less than or « j i to calibrationblank value analyzed between calibration blankwith value over CRDL (or 2xIDL) and nearest goodcalibration blank.Flag five samples on either side of thecalibration blank outside the control limits.

«

A.1.14 FORM III (Preparation Blank) -(Note: The preparation blank for mercury is the sameas the calibration blank.)


each Sample Delivery Group (SDG)? [X 1 __ __

each batch of digested samples? t_Xj __ __

each matrix type? [ A 1 __ __

both AA and ICP when both are used for \>the same analyte? [ X 1 __ __

ACTION; If no for any of the above, flag asestimated (J) all the associated positivedata <10 x IDLs for which prep, blankwas not analyzed.If only one blank was analyzed for morethan 20 samples, then first 20 samples analyzeddo not have to be flagged as estimated (J).

300962

STANDARD OPERATING PROCEDURE Page 13 Of 34Title: Evaluation of Metals Hat* for the Date: Jan. 1992


V i s I S T N / A ~A. 1.14.2 Is concentration of prep, blank value greater \.

than the CRDL when IDL is less than or equal to CRDL? __ [X 1 __

If yes, is the concentration of the sample withthe least concentrated analyte less than 10 times /the prep.blank? __ [__] X,

acnoN; If yes, reject (red-line) all associateddata greater than CRDL concentration butless than ten times the prep, blank value.

A. 1.14.3 Is concentration of prep, blank value (Form III) less \,than two times IDL, when IDL is greater than CRDL? [__] __ X

ACTION; If no, reject (red-line) all positive sanpleresults when sanple raw data are less than 10times the prep, blank value.

A. 1.14.4 Is concentration of prep, blank below \ythe negative CRDL? __ fX 1 __

ACTICM; If yes, reject (red-line) all associated sanpleresults less than lOxCRDL.

A. 1.15 Fonn IV (ICP Interference Check Sample)

A. 1.15.1 Present and complete? [A ] __ __

than the respective concentration in ICS? [__]


Was ICS analyzed at beginning and end of run(or at least twice every 8 hours)?


A. 1.15.2 Circle all values on each Form IV that are morethan ± 20% of true or established mean value.

Are all Interference Check Sanple results inside \,the control limits (± 20%)? [Xj __ __

If no, is concentration of Al, Ca, Fe, or Mg lower V

300963

STANDARD CFE9ATING FHXmjRE Page 14 of 34

Title: Evaluation of Metals Data ior t*>e Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

MQ N/AACTION: If no, flag as estimated (J) those positive

results for which ICS recovery is between 121-150%;flag all sample results as estimated if ICSrecovery falls within 50-79%; reject (red-line)those sample results for which ICS recovery is lessthan 50%; if ICS recovery is above 150%, rejectpositive results only (not flagged with a "U").

A. 1.16 Form V A (SpiXed Sample Recovery - Pre-Digestion/Pre-Distillationl-( Note: Not required for Ca, Vq, K, and Na (both matrices), Al, and Fe(soil only.)

A. 1.16.1 Present and complete for: each SDG? [\ ] __ __

each matrix type? [ A ] __ __

each cone, range (i.e. low, med., high)? f X1 __ __

For both AA and ICP when both are used for \/the same analyte? t^J __ __

ACTION: If no for any of the above, flag asestimated (J) all the positive data lessthan four times the spiking levels specifiedin SOW for which spited sample was not analyzed.

NOTE: If one spited sample was analyzed for morethan 20 samples, then first 20 samplesanalyzed do not have to be flagged asestimated (J).

A. 1.16.2 Was field blank used for spited sample? __ [_A_] __

ACTION: If yes, flag all positive data less than4 x spite added as estimated (J) for whichfield blank was used as spited sample.

A. 1.16.3 Circle on each Form VA all spite recoveries thatare outside control limits (75% to 125%).

Are all recoveries within control limits? [__]

If no, is sample concentration greater than or equalto four times spite concentration? [__] A

300964

STANDARD OPERATING PHOCEaiRE Page 15 of 34


YES NO

ACTION: If yes, disregard spike recoveries for analyteswhose concentrations are greater than or equalto four times spike added. If no, circle thoseanalytes on Form V for which sanple concentrationis less than four times the spike concentration.

Are results outside the control limits (75-125%) V,flagged with "N" on Form I's and Form VA? [ J\ 1 __

ACTION; If no, write in the Contract - Problem/Non -Compliance section of "Data Assessment Narrative".

A.1.16.4 AqueousAre any spike recoveries:

(a) less than 30%? __ [__] S\

(b) between 30-74%? __ [__] A

(c) between 126-150%? __ [__] X

(d) greater than 150%? __ [__] X

ACTION; If less than 30%, reject all associated aqueousdata; if between 30-74%, flag all associatedaqueous data as estimated (J); if between126-150%, flag as estimated (J) all associatedaqueous data not flagged with a "U"; ifgreater than 150%, reject (red-line) allassociated aqueous data not flagged with a "U".

A.1.16.5 Soil/SedimentAre any spike recoveries: ^ .

(a) less than 10%? X [__]

(b) between 10-74%? X [__]

(c) between 126-200%? __ f Xl

(d) greater than 200%? __

300965


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: "HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

S I S 1 * 2 N/A"ACTION: If less than 10%, reject an associated data; if

between 10-74%, flag all associated data as estimated;if between 126-200%, flag as estimated all associateddata was not flagged with a "IT; if greater than 200%,reject all associated data not flagged with a "U".

A.1.17.1 Present and complete for: each SDG?

each matrix type?

each concentration range (i.e. low, med., high)?


ACTION; If no for any the above, flag as estimated(J) all the data >GRDL* for which duplicatesample was not analyzed.

Note; l. If one duplicate sample was analyzed formore than 20 samples, then first 20 samples do nothave to be flagged as estimated.

2. If percent solids for soil sample and its duplicatediffer by more than 1%, prepare a Form VI for eachduplicate pair, report concentrations in ug/Lon wet weight basis and calculate RPD or Differencefor each analyte.

A.1.17.2 Was field blank used for duplicate analysis? __

ACTION: If yes, flag all data >CRDL* as estimated(J) for which field blank was used as duplicate.

A. 1.17.3 Are all values within control limits (RPD 20% ordifference < +CRDL)? [__]

If no, are all results outside the control limits v>flagged with an * on Form I's and VT? [\ ] __ _



300966


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.1: Data Assessment - Contract Revision: 11Conpliance (Ttfcal Review) <•

Njp. N/ANOTE: 1. RPD is not calculable for an analyte of the

sanple - duplicate r*iy when both values areless than IDL.


A. 1.17.4 Aqueous



Is any RPD greater than 50% where sanple and duplicate \,are both greater than or equal to 5 tunes *CRDL? __ [__] yS

Is any difference** between sanple and duplicate greater vthan *CRDL where sanple and/or duplicate is less than V5 tijnes *CRDL? __ [__] <\


A.1.17.5


RPD > 100%, or


Is any RPD (where sanple and duplicate are bothgreater than or equal to 5 times *CRDL) :

> 100%? __ [ X ]

Is any **difference between sanple and duplicate(where sanple and/or duplicate is less than 5x*CRDL) :

> 2x*CRDL? __ [ A]


300967



j£ N/


A. 1.18 Field DuplicatesV

A. 1.18.1 Were field duplicates analyzed? [ /\ ] __ __

ACTION; If yes, prepare a Form VI for each aqueous fieldduplicate pair. Prepare a Form VI for each soilduplicate pair, if percent solids for sanple andits duplicate differ by more than 1%; reportconcentrations of soils in ug/1 on wet weightbasis and calculate RPDs or Difference for eachanalyte.

NOTE: 1. Do not calculate RPD when both values areless than IDL.


A. 1.18. 2 Aqueous



Is any RPD greater than 50% where sample and duplicate x/are both greater than or equal to 5 times *CRDL? __ [ _ _] A

Is any difference between sample and duplicate greaterthan *GRDL where sample and/or duplicate is less than \S5 times *CRDL? . __ [ __ ] A



300968




A.I.18.3 8oil/8edi mt


RPD >100%, or


Is any RPD (where sanple and duplicate are bothgreater than 5 times *CRDL) :

YES

Is any **difference between sanple and duplicate(where sanple and/or duplicate is less than 5x *CRDL ) :

>2x *CRDL?

If yes, flag the associated data as estimated.

N/A

A. 1.19 Porm VTI (Laboratory Control Sanple) (Note: LCSrequired for aqueous Hg and cyanide analyses.)

- not


each SDG?

each batch samples digested/distilled? [ A


ACTION; If no for any of the above, prepare TelephoneRecord Log and contact laboratory for submittalof results of LCS. Flag as estimated (J) allthe data for which LCS was not analyzed.

NOTE; If only one LCS was analyzed for more than 20sanples, then first 20 sanples close to LCSdo not have to be flagged as estimated.


300969


Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContractCortpl lance (Total Review)


A.1.19.2

YES N/A

Circle on each Form VII the LCS percent recoveriesoutside control limits (80 - 120%) except for aqueousAg and Sb.




greater than 150%?

ACTION: Less than 50%, reject (red-line) all data;between 50% and 79%, flag all associated dataas estimated (J); between 121% and 150%, flagall positive (not flagged with a "U") resultsas estimated; greater than 150%, reject allpositive results.

_ tXi _

A.1.19.3 Solid LCS

NOTE: 1. If "Found" value of LCS is rejectable due to duplicateinjections or analytical spiJce recovery criteria,regardless of LCS recovery, flag the associated dataas estimated (J).

2. If IDL of an analyte is equal to or greater thantrue value of LCS, disregard the "Action" below eventhough LCS is cut of control limits.

Is LCS "Found" value higher than the controllimits on Form VII? __

ACTION: If yes, qualify all associated positive dataas estimated.

Is LCS "Found" value lower than the Controllimits on Form VII? __

ACTION; If yes, qualify all associated data asestimated.

300970


'Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

__ _ __

A.1.20 form jj{ (ICP Serial Dilution) —

NOTE: Serial dilution analysis is required onlyfor initial concentrations equal to orgreater than 10 x IDL.

A. 1.20.1 Was Serial Dilution analysis performed for: \,each SDG? [\ 1 __ _

each matrix type? [\ 1 __ _

each concentration range (i.e. low, med.)? [ V] __ __


A. 1.20.2 Was field blank(s) used for Serial Dilution Analysis? __

ACTION; If yes, flag all associated data > 10 x IDLas estimated (J). If lOxIDL < CRDL, flag alldata > CRDL.

A. 1.20.3 Are results outside control limit flagged with an "E"on Form I's and Form IX when initial concentForm IX is equal to 50 times IDL or greater.

ACTION: If no, write in the Contract-Problem/Non-Compliance section of the "Data AssessmentNarrative".



> 10%?

> 100%?

on Form I's and Form IX when initial concentration on V[Aj __ __

300971




ACTION;YES

Flag as estimated (J) all the associated sanpledata > lOxIDLs (or > CRDL when lOxIDL < CRDL)for which percent difference is greater than 10%but less than 100%. Reject (red-line) all theassociated sanple results equal to or greaterthan lOxIDLs (or > CRDL when lOxIDL < CRDL) forwhich PD is greater than or equal to 100%.

Flag or reject on Form I's only the sanple resultswhose associated raw data are >. lOxIDL (or >. CRDLwhen lOxIDix CRDL)

N/A

A.I.21 Furnace Atonic Absorbtion (AA) PC Analysis

A. 1.21.1 Are duplicate injections present in furnace raw data(except during full Method of Standard Addition) foreach sample analyzed by GFAA?


A.1.21.2 Do the duplicate injection readings agree within 20%Relative Standard Deviation (RSD) or Coefficient ofVariation (CV) for concentration greater than CRDL?

Was a dilution analyzed for sample with analyticalspike recovery less than 40%?

ACTION: If no for any of the above, flag all theassociated data as estimated.

A. 1.21.3 Is *analytical spike recovery outside the controllimits (85-115%) for any sanple?


<_, _

* Analytical spike is not required on the pre-digestion spiked sanple.

300972


"Title: Evaluation of Metals Data for theCouLract laboratory ProgramAppendix A.I: Data Assessment - Contract



Reject or flag the data only when the affectedsample (s) was not subsequently analyzed by Methodof Standard Addition.

N/A

A.1.22

A.1.22.1

A.I.22.2

Fora VIII (Method of

Present?

If no, is any Form I result coded with "S" or a "+"?

ACTION: If yes, write request on Telephone Record Logand contact laboratory for submittal of Form VIII.

Is coefficient of correlation for MSA less than 0.990 forany sample?


C__3 >cir V_ tJLJ _

A.1.22.3 Was *MSA required for any sample but not performed?

Is coefficient of correlation for MSA less than 0.995?

Are MSA calculations outside the linear range of thecalibration curve generated at the beginning of theanalytical run?


A.1.22.4 Was proper quantitation procedure followed correctlyas outlined in the SOW on page E-23?

ACTION: If no, note exception under Contract Problem/Non-Ccrpliance section of the "Data AssessmentNarrative", and prepare a separate list.

[A] __ __

* MSA is not required on LCS and prep, blank.

300973

STANDARD OPERATING PKXHJURE Page 24 of 34

Title: Evaluation o:.~ Kstals Data for the Date: Jan. 1992Contract Li-oora-oory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

ios Ee N/A~A. 1.23 D

A. 1.23.1 Were any analyses performed for dissolved as well as \,total analytes on the same sample(s) . __ [ __ ] />

Were any analyses performed for inorganic as well as total V(organic + inorganic) analytes on the same sample (s)? __ [ __ ) /\

NOTE: l. If yes, prepare a list comparing differencesbetween all dissolved (or inorganic) andtotal analytes. Compute the differences asa percent of the total analyte only whendissolved concentration is greater than CRDLas well as total concentration.



A. 1.23. 2 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration by Ymore than 10%? __ [ __ ] / 1

A. 1.2 3. 3 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration by ymore than 50%? __ [ __ ] A

ACTION; If more than 10%, flag both dissolved (orinorganic) and total values as estimated (J);if more than 50%, reject (red-line) the datafor both values.

A.1.24 Form I (Field BlanlO -

(Note; Designate "Field BlanX"

A.1.24.1 Circle all field blank values on Form I that aregreater than CRDL, (or 2 x IDL when IDL > CRDL).


300974

STANDARD OPERATING PRXHJURE Page 25 of 34




If no, reject (except field blank results)all associated positive sample data lessthan or equal to five times the field blankvalue. Reject on Form I's the soil sanpleresults that when converted to ug/L on wetbasis are less than or equal to five timesthe field blank value in ug/L.

N/A

[_] _

A.1.25 Form X, XI. XII (Verificatior

A. 1.25.1 Is verification report present for:





cl) _ _

A.1.25.2 Form X (Instrument Detecti<required for Cyanide.)

- (Note: IDL is not

A. 1.25.2.1 Are IDLs present for: all the analytes?



acTION; If no for any of the above, prepareTelephone Record Log and contactlaboratory.



A t_] _

300975

STANDARD Oc/1'RAri£>"G FROCFUURE

"Title: Valuation of Metals Data frr- • -<2Contract Laboratory FrogroMAppendix A.I: Data Assessment - ContractConpliance (Total Review)

Page 26 of 34


Action : If no, flag as estimated all values lessthan five tines IDL of the instrument whoseIDL exceeds CPDL.

YES N/A

A.1.25.3 Ranges)

A. 1.25.3.1 Was any sanple result higher than high linear rangeof ICP.

Was any sanple result higher than the highestcalibration standard for non-ICP parameters?

If yes for any of the above, was thesanple diluted to obtain the result on Fora I?

X

acnoN: If no, flag the result reported on Form Ias estimated (J).

A. 1.26

A. 1.26.1

percent Soli * of

Are percent solids in sediment ( s) :< 50%?

< 10%?

ACTION; If yes, qualify as estimated all theresults of a sanple that has per centsolids between 10%-50% (i.e. moisturecontent between 50%-90%) . Reject allthe results of a sanple that has per centsolids less than 10% (i.e. moisture contentgreater than 90%) .

Reject or flag(J) only the sanple resultsthat were not previously rejected or flageddue to other QC criteria.

300976

IIIIIIii

U.S. EPA - CLP

EPA SAMPLE NO

II1i11

Lab Name: cT/? Contract: |/1'X~ & ~ |

Lab Code: Case No. : • 3-/3 '

Matrix (soil/water) :

% Solids for :

Co

11I Analyte1I Aluminura_I Antimony_[ArsenicI Barium __I BerylliumI Cadmium(CalciumI Chromium(CobaltI Copper1 Iron[Lead1 MagnesiumI Manganese1 Mercury(Nickel^ _I Potassium1 Selenium(Silver1 Sodium|Thallium_1 Vanadium"[Zinc ~1 Cyanide1

Sample: S'J.P-

SAS No . :

Level

% Solids for

ncentration Units (ug/L or rag/kg dry weight) :

ControlLimit

1

Sample (S)

/<S-crc»

?•>D-3-?0-3(~). *> ?d-7 727*, : 0Z-/-3-il.l£o . I

*? / \j £y^^24^- j i (5?"? S"0

__- ^>—

0.03/3>.:>3_Y\-O0 V/0.5-3-/ 1? fo. y/

?-/ . 9?*?. oJ.CJ

1C

1\~

I

yMl

tfl

11

ui1

Duplicate (D) C

i ^ r-O^ %^

1*3- t»

"0. 9-7O. "?

/5 %-T/• ./ .lA?.-

?ut? >-e>5". «/

T / o*c -y6. / 0

2. i. y3-/ 6 6fD-Y^-5./ 5~

- * ~o. y Vy*. /??. 7 1A--? 1

1to

B§

I

<4

5

I<z

SDG No. :

(low/med)

Duplicate

.

1111

*

RPD

T-O

•5-? .3t, "/. >/ ?"W'*/5P--*• V1C?/6>i C-

S'-c?oL

3^07 .icr*/S~3.1

ZP/^7

»

••

Q

—

—

i*,~tr.f

M

iii

1FORM VI - IN 3/90

300977



Case # 2137 Site Olean Well Field Matrix: Soil X_

SDG# Z2137 LabffiA_____ Water__

Contractor Geraehtv & Miller. Inc. Reviewer L. Sioeren Other

A.2.1 Validation Flags - The following flags have been applied in red by the datavalidator and must be considered by the data user.

J - This flag indicates the result qualified as estimated.

Red- Line- A red-line drawn through a sample result indicates unus-able value. The red-lined data are known to containsignificant errors based on documented information andmust not be used by the data user.

Fully Usable Data - The results that do not carry "J" or "red-line" are fullyusable.

Contractual Qualifiers - The legend of contractual qualifiers applied by the lab onForm I's is found on page B-20 of SOW IIM01.0.



Correlation coefficients for the initial calibration of lead performed on December 4, 1991 usinginstrument 5100 and December 5, 1991 using instrument 3030 were < 0.995. The two field blanks inthis SDG, the water preparation blank and the water laboratory control sample were associated with thesecalibrations. Lead results for these blanks and laboratory control sample were qualified as estimated (J)if detected and estimated (UJ) if not detected.

For the CRDL standards analyzed, the following % recoveries were found to be outside thecontrol limits of 80-120%:

ICP Analysis

Analyte % Recoveries

Chromium 121.6Lead 165.3, 144.4

300978



GFAA Analysis

Run*

2478

The following sample

Sample ID

AL-SB01-0204AL-SB02-0002AL-SB03-0002AL-SB03-0204AL-SB05-0002AL-SB05-0204

Analvte

LeadThalliumLeadLead

results were qualified

Analvte

LeadLeadLeadLeadLeadLead

% Recovery

733131.053.353.3

based on the associated CRDL results:

Concentrations fmg/kgl

R16.4J13.7J20.7J36.6J87.9J

In addition, all samples that have chromium reported as detected were qualified as estimated(J).

The following spiked sample recoveries were found to be outside the control limits of 75-125%:

Analvte %Recoverv

Antimony 68.2Arsenic -31.6

All arsenic results were qualiGed as unusable (R). All antimony results were qualiGed asestimated (J) if detected and estimated (UJ) if not detected.

For the ICP several dilution analysis, the following analyte initial concentrations were >. 10times the IDL and had % difference values between the initial and serial dilution concentrations of> 10%:

300979



Page 29 of 34


Analyte % Difference

CobaltPotassiumSodiumVanadiumZinc

18.117.010.615.832.5

The following sample results were qualified as estimated (J) since the concentrations were >_ 10times the IDL or >, the CRDL when 10 times the IDL is <, CRDL:

Concentration fmg/kgl

11.9J2880J21.9J79.0J2160J18.U

97.9J14.4J

2770J21.6J

86.8J1220J15. U73.2J

1400J28.6J

61.9J1390J

Sample IDAX-SB01-002

AX-SB01-D1

AX-SBO 1-0204

AX-SB03-0002

AX-SB03-0204

AL-SBOl-0204

AnalyteCobaltPotassiumVanadiumZincPotassium

VanadiumZincCobaltPotassiumVanadiumZincPotassiumVanadiumZinc

PotassiumVanadiumZincPotassium

300980



Page 30 of 34


Sample IDAL-SB01-0204

AL-SB01-0406AL-SB01-0608

AL-SB02-0002

AL-SB03-0002

AL-SB04-0002

AL-SB03-0204

AL-SB04-0204

AnalyteVanadiumZincZincPotassiumVanadiumZincPotassiumVanadiumZincPotassiumVanadiumZincCobalt

PotassiumVanadiumZincCobaltPotassium

VanadiumZincCobaltPotassiumVanadiumZinc

Concentration (mg/kg)27. 1J109J

64.0J

1550J18.6J

68. U1770J12.5J29.4J

1500J

15.5J

77. U

10.5J

1290J22.2J

82.2J

9.8J

1590J16.2J67. U9.6J1130J

15.5J45.3J

300981



Sample ID Analyte Concentration (mg/kg)AL-SB05-0002 Cobalt 11.6J

Potassium 2090JVanadium 31.1JZinc %.9J

AL-SB05-0204 Potassium 1340JVanadium 21.2J

AL-SB05-0204 Zinc 111J

Arsenic post-digestion spike recoveries for FB-1 and FB-2 were both 82%. As a result, the non-detect arsenic result for FB-1 was qualified as estimated (UJ) and the arsenic detected in FB-2 wasqualified as estimated (J). All other arsenic post-digestion recoveries were within the control limits of85-115%. All lead and selenium post-digestion spike recoveries were within the controllimits of 85-115%. Thallium post-digestion spike recoveries were > 115% and < 200% for severalsamples and both field blanks. However, since thallium was not detected in any of these samples andfield blanks, no qualification of the data was necessary.




MMB Reviewer: _______________________ Date:Signature

Contractor Reviewer: -*~~~~^ f-*^>^~- DateSignature (J o

Verified by: _______________________ Date:OL2137ZI.DOC

: *•// / s

300982

Evaluation of Matals Data for th« Oontract Laboratory Program (Of)

based on

SOW. 3/90

(SOP Revision XI)

PREPARED BY \_Assurance Chemist

Waste Section

APPROVED BY '• rV -«-.'TV \»- v

APPROVED BY:Robeft. Ruinyon,Monitoring Mana Branch

DATE: | - 3 <* -

DATE: \ "Kevin Kubik, ChiefToxic and Hazardous Waste Section

DATE:

~\ 2.

300983

STANDARD TKP.V2M5 HTCCEDURE Page 1 of 34

Title: Evaluation of Metals Data'-ixsr a» Date: Jan. 1992Contract Laboratory Program Number: HW-2

Revision: 11"

1.0

1.1 This procedure is applicable to inorganic data obtained fron contractorlaboratories working for Hazardous Waste Site Contract LaboratoryProgram (CLP).


2 . 0 Responsibilities - Data reviewers will ooiplete the following tasks as assigned by theData Review Coordinator:

2.1. For a total review:

2.1.1 Data Assessment - "Total Review-Inorganics" Checklist Appendix (A.I).The reviewer must answer every question on the checklist.

The answer on the checklist must match the action in the narrative(appendix A. 2) and on Form I's. Do not use pencil to write the narrative.

2.1.3 Contract Non-Carol iance - SMO Report (Appendix A. 3)This report is to be cccpleted only when a serious contract violation isencountered, or upon the request of the Data Validation Task Monitor, or TechnicalProject Officer (TPO) . Forward 5 copies: one each for internal files,appropriate Regional TPO, Sample Management Office (SMO) and last two addresses ofMailing List for Data Reviewers (Appendix A.4). In other cases, all contractviolations should be appended to the end of the Data Assessment Narrative (Sec.A.2.2).

2.1.4 CT-P Datfr Ass w*"* Pyamary FoTT"ff

2.1.4.1 Appendix A. 5Fill in the total number of analytes analyzed by different analyses andthe number of analytes rejected or flagged as estimated due to correspondingquality control criteria. Place an "X" in boxes where analyses were notperformed, or criteria do not apply.

2.1.4.2 Appendix A. 6Data reviewer is also required to fill cut Inorganic Regional Data Assessmentform (Appendix A. 7) provided by EPA Headquarters. Codes listed on the formwill be used to describe the Data Assessment Summary.

300984


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Nunber: HW-2

Revision: 11

2.1.5 Data Review Loai It is mxninenrted that each data reviewer should maintain a log ofthe reviews completed to include; a. date of start of case review

b. date of completion of case reviewc. sited. case numbere. contract laboratory. f. number of samplesg. matrixh. hours workedi. reviewer's initials

2.1.6 Telephone Record Log - the data reviewer should enter the bare facts ofinquiry, before initiating any phone conversation with CLP laboratory.After the case review has been completed, mail white copy of TelephoneRecord Log to the laboratory and pink copy to SMD. File yellow copy inthe Telephone Record Log folder, and attach a xerox copy of the TelephoneRecord Log to the completed Data Assessment Narrative (Appendix A.2).

2.1.7 Forwarded Paperwork

2.1.7.1 Upon completion of review, the following are to be forwarded to the RegionalSample Control Center (RSCC) located in the Surveillance and Monitoring Branch:a. data packageb. completed data assessment checklist (Appendix A.I,original)c. SMO Contract Compliance Screening (CCS)d. Record of Communication (copy)e. CLP Reanalysis Request/Approval Record (original + 3 copies)f. Appendix A.6 (original).

2.1.7.2 Forward 2 copies of completed Data Assessment Narrative (Appendix A.2)along with 2. copies of the Inorganic Data Assessment Form (Appendix A. 6) andTelephone Record Log , if any,: one each for appropriate Regional TPO,and the other one to EPA EMSL office in Las Vegas. The addresses of TPOs and EPAoffice in Las Vegas are given in Appendix A-4. ;


Appendix A.6.b. Telephone Record Log (copy)c. SMO Report (copy Appendix A-3)d. CLP Reanalysis Request/Approval Record (copy)

300985

STANDARD OPERATING PROCEDURE Page 3 of 34t

Title: Evaluation of Metals Data for the Data: Jan. 1992Contract Laboratory Program Hunter: HW-2

Revision: 11

3.0 __Each data package is checked by a Regional Sample Control Coordinator (RSSC) forcompleteness. A data package is assumed to be complete when all the deliverablesrequired under the contract are present. If a data package is incomplete, the RSSCwould call the laboratory for missing document (s) . If the laboratory does not respondwithin a week, SMD and M-ffi coordinator of Region II will be notified.

4 . 0 Rejection of Data - All values determined to be unacceptable on the Inorganic AnalysisData Sheet (Form I) must be lined over with a red pencil. As soon as any reviewcriteria causes data to be rejected, that data can be eliminated from any further reviewor consideration.


6.0 SHD Contract Compliance Screenj.pq f si - This is intended to aid reviewer in locatingany problems, both corrected and uncorrected. However, the validation should be carriedcut even if CCS is not present. Resubmittals received from laboratory in response toCCS must be used by the reviewer.

7.0 Request for Reanalvais - Data reviewers must note all items of contract non-compliancewithin Data Assessment Narrative. If holding times and sample storage times have not beenexceeded, TPO may request reanalysis if items of non-compliance are critical to dataassessment. Requests are to be made on "CLP Re-Analysis Request/Approval Record".

8.0 Record ?f """TTCBiT ti?!! - Provided by the Regional Sample Control Center (RSCC) toindicate which data packages have been received and are ready to be reviewed.

9.0 Bounding off numbers - The data reviewer will follow the standard practice.

300986



Date: Jan. 1992Number: HWr2Revision: 11

A.1.1 Contmn"!t

ACTION; If no, contact RSOC.

A. 1.2 Record of Ornunication Itxrn RflOC) — Present?

ACTION; If no, request from RSOC.

A. 1.3 Trip Report - Present and oonplete?

ACTION; If no, contact RSOC for trip report.

A.1.4 Sample Traffic Report - Present?

Legible?

ACTION; If no, request from Regional Sairple OontrolCenter (RSOC).



AcnoM: If no, prepare Telephone Record Log, andcontact laboratory.




(b) Form I's?

ACTION; If no for any of the above, contact RSOC forclarification.

1X1X

N/AYES

(CCS) - Present? [__] __ A_

t__] __

t_]

1X1 _

[_] _ _L1X

300987

STANDARD OPERATING PRXHXJRE Page 5 of 34

Title: Evaluation of Metals Data for theContract laboratory ProgramAppendix A.1: Data A'lin'iuiaiit - ContractCompliance (Total Review)


A.I.6 Fom I to TT

A.I.6.1 Are all the Form I through Form IX labeled with:

Laboratory name?

Case/SAS number?

EPA sample No.?

SDG NO.?

Contract No.?

Correct units?

Matrix?ACTION; If no for any of the above, note under

Contract Problenv/Non-Compliance sectionof the "Data Assessment Narrative".

A. 1.6.2 Do any computation/transcription errors exceed 10% ofreported values on Forms I-IX for:


(a) all analytes analyzed by ICF?



(d) Mercury?

(e) Cyanide?

ACTION; If yes, prepare Telephone Log, contactlaboratory for corrected data andcorrect errors with red pencil and initial.

Xfifi K2 N/A

x. _

[__]

300988


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

Y E S E Q N/A"A.I.7 Raw Data

A. 1.7.1 Digestion Log* for flame AA/ICP (Fora XIII) present?

Digestion Log for furnace AA Form XIII present? r X ] __ __

Distillation Log for mercury Form XHI present?

Distillation Log for cyanides Form XIII present?

Are pH values (pH<2 for all metals, pH>12 for cyanide)present?

Weights, dilutions and volumes .used to obtain values.



A. 1.7.2 Measurement read out record present? ICP

Flame AA [__] __ X

Furnace AA f Xl __ __Mercury

cyanides


Legible?

Properly Labeled?

ACTION; If no for any of the above questionsin sections A.I.7.1 through A.I.7.3,write Telephone Record Log and contactlaboratory for resubmittals.

300989

STANDARD CHEATING PROCEDURE Page 7 of 34

Title: Evaluation of Metals for the Contract Date: Jan. 1992laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: In-

compliance (Total Review)

YES NO N/AA. 1.8 raisin? TJTT - (aqueous and soil samples )


Mercury analysis (28 days) ....... exceeded? __ [ Xl __

Cyanide distillation (14 days) ..... exceeded? __ r r 1 __

Other Metals analysis (6 months) .... exceeded? __ [_£J __

NOTE; Prepare a list of all samples and analytes forwhich holding times have been exceeded. Specifythe number of days from date of collection to the dateof preparation (from raw data) . Attach to checklist.

ACTION; If yes, reject (red-line) values less thanInstrument Detection Limit (IDL) and flagas estimated (J) the values above IDL eventhough sample (s) was preserved properly.

A. 1.8. 2 Is pH of aqueous samples for: \/Metals Analysis >2? __ [A 1 __

cyanides Analysis <12? __ r Xl __


A. 1.9 FQTW T (rir*J Data)

A. 1.9.1 Are all Form I's present and complete? [X 1 __ __


A. 1.9. 2 Are correct units (ug/1 for waters and mg/kg for soils) Vindicated on Form I's? [A 1 __ __

Are soil sample results for each parameter corrected for v,percent solids? [A ] __ __

Are all "less than IDL" values properly coded with "U"? rX 1 __ __

300990


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Carpiiance (Total Review)

Y E S J aAre the correct concentration qualifiers used with \/final data? f X 1 __


A. 1.9.3 Are EPA sample I s and corresponding laboratory sampleID f s the same as on the Cover Page, Form I's and yin the raw data? f/\ ] __

Was a brief physical description of samples given Von Form I's? [A ] __

A.1.10 Calibration

A. 1.10.1 Is record of at least 2 point calibrationpresent for ICP analysis?

Is record of 5 point calibration present for

present for ICP analysis? [A 1

JLS r coru ot 3 point r?i 1 1 nrat-Lon present tor \ ,•Hg analysis? ' [ X 1


Flame AA? [ __ ]

Furnace AA? fX 1

Cyanides? f X ]*

Is one calibration standard at the CRDL level forall AA (except Hg) and cyanides analyses?

ACTION; If no for any of the above, write in theContract Prctolem/Nan-Oonpliance section ofthe "Data Assessment Narrative11.

Was the dilution of any sanple diluted beyond therequirements of the contract noted on Form I or \yForm XIV? __ r A 1 __

ACTION; If no for any of the above, note underOontract-Problem/Non-Oomplianceof the"Data Assessment Narrative".

300991



Date: Jan. 1992Number: HW-2Revision: 11.

A. 1.10.2 Is correlation coefficient less than 0.995 for:

Mercury Analysis?

Cyanide Analysis?

Atomic Absorption Analysis?


YES tfi N/A

X [__] __

NOTE; The data validator shall calculate the correlationcoefficient using concentrations of the standardsand the corresponding instrument response( e.g. absorbance, peak area, peak height, etc.).

A. 1.10.3 In the instance vhere less than 4 standards aremeasured in absorbance (or peak area, peak height,etc.)mode, are the remaining standards analyzed inconcentration mode immediately after calibrationwithin ±10% of the true values? [__]

ACTION; If no, flag the associated data as estimatedif standards are not within ±10% of true values.Do not flag the data as estimated in linear rangeindicated by good recovery of standard(s).

A.1.11 Form II A (Initial and Continuing Calibration verificat

A.l.ll.l Present and complete for every metal and cyanide?

Present and complete for AA and TCP when both areused for the same analyte?


A. 1.11.2 Circle on each Form HA all percent recoveries thatare outside the contract windows.Are all calibration standards (initial and continuing)within control limits:

Metals- 90-110%R?

Vq - 80-120%R?

Cyanides- 85-115%R?

300992


Title: Evaluation of Metals Data for the Dot*: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

as SaT N/A~ACTION; Flag as estimated (J) an positive data (not

flagged with a "U") analyzed between acalibration standard with %R between 75-89%(65-79% for Hg; 70-84% for CN) or 111-125%(121-135% for Hg; 116-130% for CN) recovery andnearest good calibration standard. Qualify results<IDL as estimated (UJ) if the ICV or CCV %R is75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line)as unacceptable data if recovery of the ICV orCCV is outside the range 75-125% (CN, 70-130%; Hg,65-135%). Qualify five samples on either side ofverification standard cut of control limits.

A. 1.11.3 Was continuing calibration performed every 10 samples \/uLor every 2 hours? [ A 1

Was ICV for cyanides distilled? fY 1

ACTION; If no for any of the above, write in theContract-Prx±>lenv/Non-Ccrpliance section of the"Data Assessment Narrative".

A.1.12

A.1.12.1 Was a CRDL standard (CRA) analyzed after initial wcalibration for all AA metals (except Hal? f \ 1

Was a mid-range calib. verification standard distilled yand analyzed for cyanide analysis? f A 1

Was a 2xCRDL ( or 2xIDL when IOLXSDL) analyzed (CRT) \,for each ICP run? f <\ 1(Note: CRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.)


**True value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL.Conpute the concentration of the missing mid-range standard from the calibration range.

300993


Title: Evaluation of Mrtals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review) ,

A. 1.12. 2 Was CRI analyzed after ICV/ICB and before the final yCCV/CCB, and twice every eight hours of ICP run? f A 1 __ __

ACTION; If no, write in Contract Problem/Non-ComplianceSection of the "Data Assessment Harrative".

A. 1.12. 3 Circle on each Form IIB all the percent recoveries thatare outside the acceptance windows.


Metals 80 - 120%R? [ __ ] A __


Cyanide 80 - 120%R? [Al __ __


Note; Flag or reject the final results only when sampleraw data are within the affected ranges and the CRDLstandards are outside the acceptance windows.

A. 1.13 porm in fTriitifll and O ntl mil TXT 1 i rytion Blanks)

A.I. 13.1 Present and complete? [A 1 __ __

For both AA and ICP when both are used for the vsame analyte? f A 1 __ _

Was an initial calibration blank analyzed? (s 1 __

Was a continuing calibration blank analyzed afterevery 10 samples or every 2 hours (which ever is morefrequent)?

300994


Title: Evaluation of i tals Data for the Date: Jan. 1992Contract Lafcorair/i/ rcgram Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review) ••

ACnOM; If no, prepare Telephone Record Log, contactlaboratory and write in the Contract-Problems/Ncn-Gompliance section of the "Data Assessment Narrative


Are all calibration blanks (when IDLcCRDL) less than or x,equal to the Contract Required Detection Limits (CRDLs)? r Al

"

Are all calibration blanks less than two times v,Instrument Detection Limit (when IDL>CRDL)? r A ] __ __

ACTTOM; If no for any of the above, flag as estimated(J) positive sanple results when raw samplevalue is less than or equal to calibrationblank value analyzed between calibration blankwith value over CRDL (or 2xIDL) and nearest goodcalibration blank.Flag five samples on either side of thecalibration blank outside the control limits.

4

A.I.14 FORM III (Preparation Blank) -(Note: The preparation blank for mercury is the sameas the calibration blank.)


each Sample Delivery Group (SDG)? r A 1 __ __

each batch of digested samples? f V 1 __ __

each matrix type? f V1 __ __

both AA and ICP when both are used forthe same analyte? f /^l __

ACTION; If no for any of the above, flag asestimated (J) all the associated positivedata <10 x IDLs for which prep, blank

__ was not analyzed.NOTE; If only one blank was analyzed for more

than 20 samples, then first 20 samples analyzeddo not have to be flagged as estimated (J).

300995

STANDARD 'VPERATING PRXEDURE Page 13 of 34Title: Evaluation of Metals Data for the Date: Jan. 1992


A.I. 14. 2YJfi

Is concentration of prep, blank value greaterthan the CRDL when IDL is less than or equal to CRDL? __

If yes, is the concentration of the sample withthe least concentrated analyte less than 10 timesthe prep. blank?

t£[ __ 3

N/A

XACTION; If yes, reject (red-line) all associated

data greater than CRDL concentration butless than ten times the prep, blank value.

A. 1.14.3 Is concentration of prep, blank value (Form III) less ythan two times IDL, when IDL is greater than CRDL? C A 1 __ _

ACTION; If no, reject (red-line) all positive sampleresults when sample raw data are less than 10times the prep, blank value.

A. 1.14.4 Is concentration of prep, blank below \/the negative CRDL? __ r A1 __

ACTION; If yes, reject (red-line) all associated sampleresults less than lOxCRDL.

A. 1.15 FOT1*! IV (ICP In rf rcnoe Chock Sirle)

A. 1.15.1 Present and complete? [ A 1 __ __


Was ICS analyzed at beginning and end of run \.(or at least twice every 8 hours)? [ A 1 __ __



Are all Interference Check Sample results inside Wthe control limits (± 20%)? l/\1 __ __

If no, is concentration of Al, Ca, Fe, or Mg lower Wthan the respective concentration in ICS? [

30099K

STANDARD CHP.VTING PnXUZJRE Page 14 of 34

Title: Evaluation of Metals Data tat the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract . Revision: 11Carpi iance (Total Review)

__ _ __IdKK: If no, flag as estimated (J) those positive

results for which ICS recovery is between 121-150%;flag all sanple results as estimated if ICSrecovery falls within 50-79%; reject (red-line)those sanple results for which ICS recovery is lessthan 50%; if ICS recovery is above 150%, rejectpositive results only (not flagged with a "If1).

A. 1.16 pprm y A (Spiked Sample Reoovory — Pre—Diq stion/Pre—Distillation)—( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe(soil only.)

A. 1.16.1 Present and complete for: each SDG? [)\ ] __ __

each matrix type? [X.l __ __

each cone, range (i.e. low, med., high)? C X 1 __ __

For both AA and ICP when both are used for Vthe same analyte? [/\ ]

ACTION: If no for any of the above, flag asestimated (J) all the positive data lessthan four times the spiking levels specifiedin SOW for which spiked sample was not analyzed.


A. 1.16.2 Was field blank used for spiked sample? __

ACTION: If yes, flag all positive data less than4 x spike added as estimated (J) for whichfield blank was used as spiked sample.

A.1.16.3 Circle on each Form VA all spike recoveries thatare outside control limits (75% to 125%).

Are all recoveries within control limits? [__] /\

ater than or equal \ /to four times spike concentration?If no, is sample concentration greater than or equal \ /

[AJ — _

300997

STANDARD OPERATING PHDCECtmE Page 15 Of 34


sis Eo N/A~acncM; If yes, disregard spite recoveries for analytes

whose concentrations are greater than or equalto four tines spike added. If no, circle thoseanalytes on Form V for which sample concentrationis less than four times the spite concentration.

Are results outside the control limits (75-125%) \/flagged with "N" on Form I's and Form VA? rA 1 __ __

ACTION: If no, write in the Contract - Problem/Non -Compliance section of "Data Assessment Narrative".

A.1.16.4 AqueousAre any spite recoveries:

(a) less than 30%? __ [_ J X

(b) between 30-74%? __ (__] A

(c) between 126-150%? __ [__] /

(d) greater than 150%? __ £__]

ACTION; If less than 30%, reject all associated aqueousdata; if between 30-74%, flag all associatedaqueous data as estimated (J); if between126-150%, nag as estimated (J) all associatedaqueous data not flagged with a "U"; ifgreater than 150%, reject (red-line) allassociated aqueous data not flagged with a "U".

A. 1.16. 5Are any spite recoveries:

(a) less than 10%?

(b) between 10-74%? X

(c) between 126-200%? __ f Xl

(d) greater than 200%? __ [_Xj

300998


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Ccctpliance (Total Review)

as EQ HZFACTIOM: If less than 10%, reject all associated data; if

between 10-74%, flag all associated data as estimated;if between 126-200%, nag as estimated all associateddata was not flagged with a "IF; if greater than 200%,reject all associated data not flagged with a "U".

A. 1.17 Form VI (TJI

A. 1.17.1 Present and complete for: each SD3? [A_]

each matrix type? [ X 1

each concentration range (i.e. low, med., high)? [£_J

both AA and ICP when both are used for the same \janalyte? r/( 1

ACTION; If no for any the above, flag as estimated(J) all the data >CRDL* for which duplicatesample was not analyzed.

Note; 1. If one duplicate sample was analyzed formore than 20 samples, then first 20 samples do nothave to be flagged as estimated.

2. If percent solids for soil sample and its duplicatediffer by more than 1%, prepare a Form VI for eachduplicate pair, report concentrations in ug/Lon wet weight basis and calculate RPD or Differencefor each analyte.

A. 1.17.2 Was field blank used for duplicate analysis? __

ACTION; If yes, flag all data X3RDL* as estimated(J) for which field blank was used as duplicate.

A. 1.17.3 Are all values within control limits (RFD 20% or Vdifference < +CRDL)? [__] A

If no, are all results outside the control limitsflagged with an * on Form I's and VI?



300999


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.1: Data Assessment - Contract Revision: 11Compliance (Total Review) *

YJS 1£ N/A~NOTE: 1. RPD is not calculable for an analyte of the

saaple - delicate pair when both values areless than IDL.

2. If the result of lab duplicate analyzedby GFAA is rejectable due to coefficient ofcorrelation of MSA, analytical spite recovery,or duplicate injections criteria, do not applyprecision criteria to metals analyzed by GFAA.

A.1.17.4 Aqueous



Is any RPD greater than 50% where sanple and duplicate \.are both greater than or equal to 5 tiroes *CRDL? __ [__] X

Is any difference** between sanple and duplicate greater ,than *CRDL where sanple and/or duplicate is less than V5 times *CRDL? __ f._] '


A. 1.17.5 Soil/Be** "**"it


RPD > 100%, or


Is any RPD (where sample and duplicate are bothgreater than or equal to 5 times *CRDL) :

> 100%? __ f A] __

Is any "difference between sample and duplicate(where sanple and/or duplicate is less than 5x*CRDL) :

> 2x*CRDL? __ f Al __


301000

STANDARD OPERATING PROCEDURE Pag* 18 of 34



A. 1.18 Field Duplicates

A. 1.18.1 Were field duplicates analyzed? r/M __ __

ACTION; If yes, prepare a Form VI for each aqueous fieldduplicate pair. Prepare a Fora VI for each soilduplicate pair, if percent solids for sanple andits duplicate differ by more than 1%; report

ntrations of soils in ug/1 on wet weightbasis and calculate RFDs or Difference for eachanalyte.



A.1.18.2 Aqueous



Is any RPD greater than 50% where sanple and duplicate Vare both greater than or equal to 5 times *CRDL? __ [__] /\

Is any **difference between sample and duplicate greaterthan *CRDL where sample and/or duplicate is less than y5 times *CRDL? [ ] /\



301001

STANDARD OPERATING PROCEDURE Fag* 19 Of 34

Title: Evaluation of Metals Data for theContract Laboratory ProgramAppendix A.I: Data AJIIKI:i •• lit - Contract



A.I.18.3

Circle all values on self prepared Form VT forfield duplicates that are:

RPD >100%, or


Is any RPD (where sanple and duplicate are bothgreater than 5 tunes *CRDL) :

Is any **difference between sample and duplicate(where sanple and/or duplicate is less than 5x *CRDL ):

>2x *CRDL?


N/A

A. 1.19 PoT1^ vxi (Laboratory Control P 'Tfle) (Note: I.CS ~ notrequired for aqueous Hg and cyanide analyses.)


each SDG?



ACTION; If no for any of the above, prepare TelephoneRecord Log and contact laboratory for submittalof results of LCS. Flag as estimated (J) allthe data for which LCS was not analyzed.

NOTE; If only one LCS was analyzed for more than 20samples, then first 20 samples close to LCSdo not have to be flagged as estimated.


301003


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Coirpliance (Total Review)

YJS J£ N/A

A.1.19.2

Circle on each Form VII the LCS percent recoveriesoutside control limits (80 - 120%) except for aqueousAg and Sb.

Is any LCS recovery: • less than 50%?



greater than 150%?

ACTION; LPSS than 50%, reject (red-line) all data;between 50% and 79%, flag all associated dataas estimated (J); between 121% and 150%, flagall positive (not flagged with a "U") resultsas estimated; greater than 150%, reject allpositive results.

A.I.19.3 Solid LCS

NOTE; 1. If "Found" value of LCS is rejectable due to duplicateinjections or iv lYaffil spike recovery criteria,regardless of LCS recovery, flag the associated dataas estimated (J).

2. If IDL of an analyte is equal to or greater thantrue value of LCS, disregard the "Action" below eventhough LCS is out of control limits.

Is LCS "Found" value higher than the control \/limits on Form VII? __ r AJ __

ACTION: If yes, qualify all associated positive dataas estimated.

Is LCS "Found" value lower than the Controllimits on Form VII? __

ACTION; If yes, qualify all associated data asestimated.

301003


Title: Evaluation of Metals Data for the Data: Jan. 1992Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review) ••

YES Ifi N/A

A.1.20 F?rn p (ICP Serial Dilution) -


A. 1.20.1 Was Serial Dilution analysis performed for: /each SDG? rX 1 __ _

each matrix type? [_ljj __ _

each concentration range (i.e. low, mad.)?


A. 1.20.2 Was field blank(s) used for Serial Dilution Analysis? __

ACTION; If yes, flag all associated data > 10 x IDLas estimated (J). If lOxIDL < CRDL, flag alldata >. CRDL.

A. 1.20.3 Are results outside control limit flagged with an "E"on Form I's and Form IX when initial concentration on \.Form IX is equal to 50 times IDL or greater. rX 1 __ __

ACTION; If no, write in the Contract-Problem/Non-Complianoe section of the "Data AssessmentNarrative11.


Are any % difference values: v

> 10%? A [__] _

> 100%? __ fV 1 __

301004

STANDARD OPERATING FRXXZURE Page 22 of 34


ACTION; Flag as estimated (J) all the associated sampledata > lOxIDLs (or > CRDL when lOxIDL < CRDL)for which percent difference is greater than 10%but less than 100%. Reject (red-line) all theassociated sample results equal to or greaterthan lOxIDLs (or > CRDL when IQxIDL < CRDL) forwhich PD is greater than or equal to 100%.

Note; Flag or reject on Form I's only the sample resultswhose associated raw data are > lOxIDL (or > CRDLwhen 10xIDL< CRDL)

A. 1.21 Furnace Atonic Absorbtion (AA) QC

A. 1.21.1 Are duplicate injections present in furnace raw data(except during full Method of Standard Addition) for Veach sample analyzed by GFAA? [/\ 1 __ __


A. 1.21.2 Do the duplicate injection readings agree within 20%Relative Standard Deviation (RSD) or Coefficient of \JVariation (CV) for concentration greater than CRDL? [/S ] __ __

Was a dilution analyzed for sample with analytical Vspike recovery less than 40%? [__] __ A


A.1.21.3 Is analytical spike recovery outside the control )(limits (85-115%) for any sample? A [__] __

ACTION: If yes, flag as estimated the affected sample resultsif the recovery is between 10-84%; if the recovery isbetween 115-200%, flag the associated positive sampleresults as estimated; reject the associated sampleresults if the recovery is less than 10%; rejectpositive sample results if the recovery is greaterthan 200%.

* Analytical spike is not required on the pre-digestion spiked sample.

301005


Title: Evaluation of Metals Data for the Date: Jan. 1992Coi'itract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11


NOTE; Reject or flag the data only when the affectedsample(s) was not subsequently analyzed by Methodof Standard Addition.

A. 1.22 To^m VTH (Method of

/A

A. 1.22.1 Present? r A1 __ __

If no, is any Form I result coded with "S" or a "+"? __ (__] X

ACTION; If yes, write request on Telephone Record Logand contact laboratory for submittal of Form VIII.

A. 1.22.2 Is coefficient of correlation for MSA less than 0.990 for yany sample? __ [ \ 1 __

ACTION: If yes, reject (red-line) the affected data.

A. 1.22.3 Was *MSA required for any sample but not performed? __ -.[ X ] __

Is coefficient of correlation for MSA less than 0.995? __ [ X 1 __

Are MSA calculations outside the linear range of thecalibration curve generated at the beginning of theanalytical run? __


A. 1.22.4 Was proper quantitation procedure followed correctly \/as outlined in the SOW on page E-23? [A 1 __ __

ACTION; If no, note exception under Contract Problem/Non-Compliance section of the "Data AssessmentNarrative11, and prepare a separate list.

MSA is not required on LCS and prep, blank.

30100B

STANDARD OPESATDC PROCEDURE Page 24 of 34

Title: Evaluation «: Ffetals Data for the Date: Jan. 1992Contract L>i»raSjory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Compliance (Total Review)

__ _ __

A.1.23 Disaoiwyprtttl ?r imTTA.I.23.1 Were any analyses performed for dissolved as wall as

total analytes on the same sample (s). __ [__] ^

Were any analyses performed for inorganic as well as total y(organic + inorganic) analytes on the same sample (s)? __ [__] ft

NOTE; 1. If yes, prepare a list comparing differencesbetween all dissolved (or inorganic) andtotal analytes. Compute the differences asa percent of the total analyte only whendissolved concentration is greater than CRDLas well as total concentration.



A. 1.23.2 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration by \more than 10%? __ [__] __

A. 1.23.3 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration by \,more than 50%? __ [__] X

ACTION; If more than 10%, flag both dissolved (orinorganic) and total values as estimated (J) ;if more than 50%, reject (red-line) the datafor both values.

A.1.24 T -

A. 1.24.1 Circle all field blank values on Form I that aregreater than CRDL, (or 2 x IDL .when IDL > CRDL) .

Is field blank concentration less than CRDL(or 2 x IDL when IDL > CRDL) for all parameters \Sof associated aqueous and soil samples? tX 1 __ __

301007


Title: Evaluation of Metals' Ifeta for theContract Laboratory ProgramAppendix A.I: Data Assessment - ContractCarpi iance (Total Review)



ACTION: If no, reject (except field blank results)all associated positive sample data lessthan or equal to five times the field blankvalue. Reject on Form I's the soil sampleresults that when converted to ug/L on wetbasis are less than or equal to five timesthe field blank value in ug/L.

[__1

MB N/A

- X

A. 1.25 Fora X. XI. XII (Verifii

A.1.25.1 Is verification report present for:



ICP T.-JTWO- Ranges (quarterly)?


A.1.25.2 form fl (instrument Detection T-<»1ta) - (Note: IDL is notrequired for Cyanide.)

A. 1.25.2.1 Are IDLs present for: all the analytes?



ACTION; If no for any of the above, prepareTelephone Record Log and contactlaboratory.

A.1.25.2.2 Is IDL greater than CRDL for any analyte?


c_, _

301008

STANDARD OWRATE'iG PROCEDURE Page 26 of 34

Title: Evaluation of Metals Data frr- *i%* Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 11Conpliance (Total Review)

Action i If no, flag as estimated all values Itthan five times IDL of the instrument whoseIDL exceeds CRDL.

A.1.25.3

A.1.25.3.1 Was any sample result higher than high linear rangeof ICP.

Was any sample result higher than the highestcalibration standard for non-ICP parameters?

If yes for any of the above, was thesanple diluted to obtain the result on Form I?

ACTION; If no, flag the result reported on Form Ias estimated(J).

^

A.1.26 percent Boli* * of SfxHmnntff

A. 1.26.1 Are percent solids in sediment(s): . .< 50%? A [__] __

< 10%?

ACTION; If yes, qualify as estimated all theresults of a sanple that has per centsolids between 10%-50% (i.e. moisturecontent between 50%-90%). Reject allthe results of a sample that has per centsolids less than 10% (i.e. moisture contentgreater than 90%).

NOTE; Reject or flag(J) only the sample resultsthat were not previously rejected or flageddue to other QC criteria.

301009

U.S. EPA - CLP

EPA SAMPLE NO.u

Lab Name: J, £. '1

Lab Code : Case No . :

Matrix (soil/water) : S-<" /

% Solids for Sample: £> ' • r

u£-u.iv_nx c,

Contract:

SAS No. :

Level

% Solids for

|/!X-5-T?

SDG No. : Z.

(low/med) :

Duplicate:

1\ ,? ' "' *

L- o i^-7 -> U

Concentration Units (ug/L or rag/kg dry weight): JL-

11I Analyte1I AluminumI Antimonyj ArsenicI BariumI Beryllium[ Cadmium[CalciumI Chromium(Cobalt •••••-1 Copper1 Iron[Lead[MagnesiumI ManganeseI Mercury[NickelI Potassium[Selenium[Silver1 Sodium[Thallium1 Vanadium1 Zincj Cyanide1

ControlLimit

p

Sample (S)

f-Ty <^^

<ry. )<r<~/ Q-

<;- ,- -^^.33 . ' • ?. ?

! "? Z> £> <? &/v<r-^-^-o =•<-<v _. 1

c. '<: .?^2"T t^

ff. 1i -~r. &./*-£> • 2--z •>: 9. -y

c1

1111

Duplicate (D)

4/?/?>

•r-?. z.v5<"

-- 3 - C ? 6.i<r. 9-S-i.^

/o S- 9 •*-»/•y?

frfo ^^>

t/i- 0s)0.^9

T . L3^V-^ S"'<r<~,??.'<'

1°\ •>a0? • V

c RPD

^V

/.<*'^."-f-

/9Z-/2? s.^/. //^/?•a -WL. &T--0~l~f->

(.'!>.}•%

^3x«

Q M

FORM VI - IN 3/90

301010



_____Appendix A.2: Data Assessment Narrative____Revision: 11___________

Case # 2152 Site Olean Well Field Matrix: Soil X_

SDG# Z2152 LabffiA______ Water__

Contractor Geraehtv & Miller. Inc. Reviewer L. Sioeren Other

A.2.J Validation Flags- The following flags have been applied in red by the datavalidator and must be considered by the data user.

J- This flag indicates the result qualified as estimated.

Red- Line- A red-line drawn through a sample result indicates unus-able value. The red-lined data are known to containsignificant errors based on documented information andmust not be used by the data user.

Fullv Usable Data- The results that do not carry "J" or "red-line" are fullyusable.

Contractual Qualifiers- The legend of contractual qualifiers applied by the lab onForm I's is found on page B-20 ofSOWIIMOl.O.



The correlation coefficients for the initial calibration of thallium performed on December 10, 1991was < 0.995. The only sample associated with this calibration was AX-SD01D with the non-detectthallium result qualified as estimated (UJ). For the CRDL standards analyzed, the following %recoveries were found to be outside the control limits of 80-120%:

ICP Analysis

Analyte % Recovery

Copper 157.0Lead 62.7

301011


Title: Evaluation of Metals Data for the Date: Jan. 1992Contract Laboratory Program Number: HW-2Appendix A.2: Data Assessment Narrative____________Revision: 11_____

The following sample results were qualified as estimated (J) based on the associated CRDLresults:

Sample ID Analyte Concentration Units

AX-SD03-0001 Lead 371J mg/kgMG-SB03-0406 Copper 23.2J mg/kgMG-SB03-1012 Copper 35.2J mg/kgMG-SB03-1214 Copper 31.8J mg/kgFB-6 Copper 8.3BJ ug/LAX-SD01-0001 Copper 26.9J mg/kgAX-SD01-0203 Copper 16.9J mg/kgAX-SD02-0001 Copper 22.9J mg/kgAX-SD02-0203 Copper 15.8J mg/kgAX-SD03-0001 Copper 2890J mg/kgAX-SD03-0203 Copper 39.0J mg/kgAX-SD01-D Copper 22.2J mg/kg

The "B" qualifier indicates that the sample concentration is between the instrument detectionlimit (IDL) and the contract required detection limit (CRDL).

The following spiked sample recoveries were found to be outside the control limits of 75-125%:

Analvte %Recovery

Antimony 67.1Arsenic 74.9Selenium 71.9

All antimony, arsenic, and selenium results were qualified as estimated (J) if detected andqualified as estimated (UJ) if not detected.

For the ICP serial dilution analysis, the following analyte initial concentrations were >. 10times the IDL and had % difference values between the initial and serial dilution concentrations of> 10%:

Anarvte % Difference

Copper 50.9Vanadium 10.1

301012



The copper detected in the samples contained in this SDG were already qualified as estimated (J)based on the CRDL standard results. The following vanadium sample results were qualified as estimated(J) since the concentrations were >_ 10 times the IDL:

Sample ID Concentration (mg/kg)

MG-SB03-0406 15.3JMG-SB03-1214 15. UAX-SDOl-0001 22.9JAX-SD01-0203 23.2JAX-SD02-0203 16.4JAX-SD03-0203 32.3JAX-SD01-D 21.3J

Selenium post-digestion spike recoveries were 78.0%, 76.0%, 74.0%, and 84.0% for samplesMG-SB03-0406, MG-SB03-1012, MG-SB03-1214, and AX-SD01-0203, respectively. All non-detectselenium results for these samples were qualified as estimated (UJ).

Thallium post-digestion spike recoveries were 81.5%, 84.5%, 83.0%, and 78.5% for samplesMG-SB03-1012, MG-SB03-1214, AX-SD01-0203, and FB-6, respectively. The thallium detected in FB-6was qualified as estimated (J) and the thallium non-detects for samples MG-SB03-1021, MG-SB03-1214,and AX-SDO1-0203 were qualified as estimated (UJ). All lead and arsenic post-digestion spike recoverieswere within the control limits of 85-115%.

The percent solids measured for sample AX-SD03-0001 was 20.9%. Therefore, all results forthis sample were qualified as estimated (J) if detected and estimated (UJ) if not detected.

301013




GERAGHTY & MILLLER, INC. DATA ASSESSMENT


MMB Reviewer: _______________________ Date: ________Signature

Contractor Reviewer: ~*-^ ^^v^— ____ Date: ////"> //Signature ~/T / '

Verified by: ________________________ Date:

OL2132H.1*

301014

t ,-.v w *m^ife · standard operating procedure 4 of. 34. title: evaluation of metals data for the...

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