semspub.epa.gov · i standard chlorine bdg #clp253 data reviewer: douglas godfrey data supervisor:...

QUALITY ASSURANCE REVIEWGROUNDWATER ANALYTICAL DATAROY F. WESTON, INC. LABORATORY

(SAMPLES COLLECTED IN JULY, AUGUST, AND OCTOBER 1990)

"9 *

JANUARY 1991

REMEDIAL INVESTIGATION/FEASIBILITY STUDYSTANDARD CHLORINE OF DELAWARE, INC.

DELAWARE CITY, DELAWARE

flB302383

rri

VOLATILE, SEMIVOLATILE, PESTICIDE/PCBAND METALS ANALYSES

STAR ENTERPRISEWELL OR-6A

(PRE-PUMP TEST SAMPLING)

flR30238ii

iSTANDARD CHLORINE

BDG #CLP253

Data Reviewer: Douglas GodfreyData Supervisor: Zohreh Hamid, Ph.D.

The laboratory's portion of SDG ICLP253 consisted of three watersamples analyzed for TAL metals by Roy F. Weston, Inc.

The laboratory reported no problems with the receipt and analysisof the samples received on 08/01/90,

The laboratory performed the analyses according to the proceduresset forth in the USEPA CLP method. Analyses of the preparationblank indicated no contamination problems. Initial and continuingcalibration verification samples were within acceptable controllimits. The most significant problems affecting the data usabilityare associated with the QC performance requirements and areaddressed in the following sections.

Minor Issues

The matrix spike percent recovery for Pb was below the CLP controllimits. All associated sample results are qualified as estimatedand are considered to be biased low.

The duplicate digestion relative percent difference (RPD) for Znwas outside the CLP control limits. All associated sample resultsare qualified as estimated.

The serial dilution percent difference for Ca was outside the CLPcontrol limits. All associated sample results are qualified asestimated.

The post-digestion spike percent recoveries for Tl were below theCLP control limits. All associated sample results are qualified asestimated and are considered to be biased low.

TABLE I

Sample # Analvte +DL -QL Comments

All samples Pb J UJ lAll samples Zn J — 2All samples Ca J — 3GW4-0-1-ORGAGW4-0-1-ORGA Tl UJ 4

1. Due to a low matrix spike percent recovery indicating alaboratory or matrix spike problem, all associated sampleresults are qualified as estimated and considered to be biasedlow,

2. Due to a duplicate digestion outside of the CLP controllimits, all associated sample results are qualified asestimated.

3. Due to a high serial dilution percent difference, allassociated sample results are qualified as estimated.

4. Due to a low post-digestion percent difference, all associatedsample results are qualified as estimated and are consideredto be biased low.

Notes

The reported IDL and linear range data were from the wrong quarter.Although this is contractually non-compliant, the data should beconsidered to be acceptable.

IInformation Regarding Report Content

All data have been validated with regard to usability according toUSEPA CLP Functional Guidelines for Evaluating Inorganic Analyses.If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215) 524-6100.

Inorganic Attachments

1. Glossary of Data Qualifier Codes.

2. Data Summary. This includes:All positive results with qualifier codes if applicable;all estimated detection limits qualified with "UJ".

3. Appendix A - Data Validation Form for Inorganics

4. Appendix B - DPO Report - This addresses laboratory complianceissues with respect to the statement of work.

5. Appendix C - Support Documentation.

4f?302387

ATTACHMENT IGLOSSARY OF DATA QUALIFIERS

flR302388

GLOSSARY OF DATA QUALIFIERS

CODES RELATING TO IDENTIFICATION

(confidence concerning presence or absence of compounds)

U = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.

R = UNRELIABLE RESULT, ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.

N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.

(NO CODE) = CONFIRMED IDENTIFICATION

CODES RELATING TO OUANTITATION . —— -

(can be used for both positive results and sample guantitation|£4 (can r>e{•• limits) :

J = ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.

L = ANALYTE PRESENT. REPORTED VALUE MAY BEBIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.

UJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.

0L = NOT DETECTED. QUANTITATION LIMIT MAY BEHIGHER.

OTHER CODES

NO ANALYTICAL RESULT,

ATTACHMENT IIDATA SUMMARY

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ATTACHMENT IIICLP DATA REVIEW FORM

/5R302392

OPERATING JfcOOIXlRE Page 4 01 35

Title; Evaluation of Metals Data for tne Date: Feb. 1990Contract laboratory Program Number: HA- 2Appendix A.I: Data Assessnent - Contract Revision: 10Conpliance (Itotal Review - Inorganics)

ACTICK: If no, request iron RSCC.

A, 1,5 cover Page - Present?

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

if no, prepare Itelephone Record Log, andcontact laboratory.

/5R302393

A. 1.3 TYJP Resort - Present and complete? [ _ ]

: If no, contact RSCC for trip report.

A. 1.4 Sample Traffic Report - Present or en file? [ \ 3

Legible? [ V ]

: If no, request from Regional Sanple controlCenter (RSCC).

v ,_X]

ID

: If no, contact RSCC.

Do numbers of sanples correspond to nutters en Record Wof Ccmnunication? LiL,J — - 1Do sarrple nutters on cover page agree with sanplenurters en:

(a) Traffic Report Sheet?

(b) Form I's?

f: If no for any of the above, contact RSOC forclarification.

iiii!

SINCftto OPERATING PROCEDURE Page 5 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 10Certpliance (Ttital Review - Inorganics)

NO

A.1.6 TOTTR i f Final Dfrta) - Are all Form I's present and conplete? [ K\

2CII33: If no, prepare telepiione record log and contactlaboratory for sutmittal.

Are correct units (ug/1 for waters and mg/*g for soils)indicated en Fonn I's?

Are soil sanpie results for each parameter corrected for ,percent solids? [ V 3

Are UA sanple f s and correspcsrding laboratory sanpleID # s the same as on the Cover Page, Fonn I fs andin the raw data? r*w

Are compulation/transcription errors less than 10%of reported values?

Are all "less than HJL" values properly coded with "U"?

Was a brief physical description of sanples given on A .Form I's? \X 1 _

Were the result qualifiers used correctly with final .,data? I S _

aCIIffi: If no for any of the above, prepare TelephoneRecord Log, and contract laboratory forcorrected data.

Were any sanples diluted beyond requiranents of contract? __

If yes, vere dilutions noted on Form I's? I__]

jCIiaik If »» note under Ccntract-Problari on-CaTplianceof theTata Assessnent Narrative".

X.1.7 Tfeldim Tiffffi - (aqueous and soil sarples )( camine sanple traffic reports and digestion/distillation logs.)

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

Cyanide distillation (14 d ysK .... exceeded? __

^302394

IOFEBATOC fSOCEIXHE Page 6 o: 35

Title: Evaluation of Metals for the Contract Date: Feb. 1990Laboratory Program Number: H/.r-2Appendix A.1: Data Assessment - Contract Revision: 10Ccrrpliance (total Review - Inorganics)

If yeSr reject (red-line) values less thanInstrument Detection Lijnit (H3L) and flagas estojrated (J) the values above H3L eventhough sample (s) was preserved properly.

A. 1.8 Rau

A. 1,8.1 Digestion Log* for flame AA/ICF (Form XIII) present? [

Digestion Log for furnace AA Form XIII present? [fi\ ]

Distillation Log for mercury Form XIII present? t

Distillation Log for cyanides Form XIII present? [

Are pH values (pH<2 for all m&tals, pH>12 for cyanide)present? f (X. I

"R302395

Other Metals analysis (6 months). . . . exceeded? __ [_V }

Prepare a list of all samples and analytesfor which holding times have teen exceeded. Specifythe number of days fron date of collection to the dateof preparation (fron raw data). Attach to cheOtlist.

, dilutions and volvxnes used to obtain values*

Percent solids calculation present for soils/sedijnents? [ _ ]

Are preparation dates present on Digestion Log? { __ ] _ __

XI. 8.2 Measurement read out record present? IO* [A 1 _ _

Flame AA [ _ ) _ A.Furnace AA [

Mercury

Irii

OPERATING PROCEDURE Page 7 of 35Title: Evaluation of Metals Data for the Date: Feb. 1990

Contract Laboratory Program Number: HW-2Appendix A.I: Data Assessrerrt - Contract Revision: 10Compliance (Sbtal Review - Inorganics)

—— —— - _ __ _ __

A. 1.8. 3 Are all raw data to support all sample analyses anaQC operations present? f £< ] _

Legible? - [

Properly Labeled? [

If no for any of the above, write TelephoneRecord Log and contact laboratory. Flag metaldata as estimated if pH of sarrple is greaterthan 2. Flag cyanide data as estimated if pHsample is less than 12.

A. 1.9 jy a Vfli llflfltion and

A.I. 9.1

A.l.9.1.1 Is record of at least 2 point calibrationpresent for 2CP analysis?

Is record of 5 point calibration present forHg analysis?

If no for any of the above, write in theContract Problan/Ncn-Conpliance section ofthe "Data Assessment Narrative91.

A.I.9.1.2 Is record of 4 point calibration present for:Flane AA? [_JFurnace AA?Cyanides?

t£2E£: 1. If less than 4 standards are measured in absorbancerode, then the retaining standards in concentrationmode most be run immediately after calibration andbe within ±10% of true value.

2. For all AA (except Hg) and Cyanide analyses, onecalibration standard is at OCL level. If not,write in the Contract-PrbblaVNon-ccnpliance sectionof the "Data Assessment Narrative11.

flR302396

CFE*ACTC PROCEDURE Page 8 01 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program * Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 10Carpiiance (3tJtal Review - Inorganics)

__

ACTiCM: Flag associated data as estinated if standardsare not within +10% of true values (except CJttcalibration standard). Do not flag the data asestimated in linear range indicated by goodrecovery of standard.

A.I.9.1.3 Is correlation *coefficient less than 0.995 for:

Mercury Analysis? _Cyanide Analysis? _ [,

Atonic Absorption Analysis? __ [£X 3

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

. 1.9. 2

.1.9.2.1 Present and ccrrpiete for every metal and cyanide? [ V 3

Present and ccrplete for AA and ICP when both areused fof same analyte? [ _ ]

Acnm: If no for any of the above, prepare TelephoneRecord Log and contact laboratory.

A.I. 9. 2. 2 Circle all values on data simnary sheet that areoutside contract windows. Are all calibrationstarriards (initial and continuing) within controllimits? ,

90-110* f A]

She reviewer will calculate correlation coefficient.

Hg - 80-120* ttf 3 __

Cyanides fi5-115% f 3 __

5R302397

IIiII

OFEKATiN3 PROCEDURE Page 9 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: *Hiv-2Appendix A.I: Data Assessnent - Contract Revision: 10Ccrpliance (ItJtal Review - Inorganics)

Flag as estimated (J> all positive data (notflagged with a "U") analyzed between acalibration standard with %R between 75-89%(€5-79% for Hg; 70-34* for CN) or 111-125%{121*135% for Hg; 116-130% for CN) recovery andnearest good calibration standard. Qualify results<HS, 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.

Was continuing calibration performed every 10 samplesor every 2 hours? [jX ] _

Sdlffl: If no, flag the excess samples (eleventh andup) data as estimated (J).

Was ICV for cyanides distilled? [ _ ]

If nof write in the Contract-PrctolerTvtton-Ccrrpiiancesection of the "Data Assessnent Narrative" .

A.I. 9. 3 fbrm II f? fggyf StaTT " f°r AA arc3 1O?) -

A. 1.9. 3.1 Was a CKDL standard (CRA) analyzed after initialcalibration for all AA metals (except Hoi?

*Was a mid-range calib. verification standard distilledand analyzed for cyanide analysis? [ __ ]

Was a 2XCT3X ( or 2xIXZ. when ICLXKX) analyzed (CRI)for *ac ICP run? [ ](Note: Oil for ALfBa,Ca,Fe,Mg,Na,or K is not required.)2£H£B: If no for any of the above, flag as estimated

all data falling within the affected ranges*Ote affected ranges are: __AA Analysis - **True Value ± OTLICP Analysis - **Ttue Value ± 2OTX,Oi Analysis - "True Value ± 0.5 x True Value.

* Find the results of mid-range standard in the raw data.**True value of CRA, O*I or mid-range standard. Substitute IEL for CREL when IDL > CRDU

flR302398

ICPESAJTOG 5BQOZXJRE Page 10 of

.Title: Evaluation of Metals Data for the Date: Feb.Contract laboratory Program Number: 'HWAppendix A.1: Data Assessment - Contract Revision: 10Ccnpliance (Ttotal Revi - Inorganics)

JES ffiA.l.9.3.2 Was era analyzed after ICV/ICB and before the final

. CCV/CCB, and for every four hours of ICP run? [/\ ] _

JOaaj: If no, write in Contract Problan/Non-OciT?>lianceI Section of the "Data Assessnent Narrative".

A. 1.9.3.3 Circle all values on sunrary sheet that are outsidet acceptance windows. V^ £ 5 tC

Are ORA and O*I standards within control limits:Metals 80 - 120%R? (__] __

* Is mid-range standard within control lijnits:Cyanide 80 - 120%R? [__] _

Flag as estimated all data within the affectedranges if the recovery of the standard isbetween 50-79%; flag only positive data ifthe recovery is between 121-150%; reject<red line) all data if the recovery is lessthan 50%; reject only positive data if therecovery is greater than 150%.

A. 1.9,4.1 Present and complete? itX* ] _

For both AA and ICP vff>en both are used for same analyte? [_Aj __

Was an initial calibration blank analyzed? I ft ] __

Was a continuing calibration blank analyzed afterevery 10 sarples or every 2 tours (whichever is morefrequent)?

If no, prepare Telephone Record Log, contactlaboratory and write in the contract-problens/non-carpiiarce section of the Data AssessnentNarrative.

SR302399

III

SIANEftHD OFEBATOC fKXmjRE Page 11 Of 35

Titlt: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: *HW-2Appendix A.I: Data Assessment - Contract Revision: 10compliance (Sfctal Review - Inorganics)

NO N/A

A.l.9.4.2 Circle all calibration blank values en Data Sumary Sheetthat are above O£L (or 2 x IDL when H3L > CRDL) . Areall calibration blanks (when HXxCHJL) less than or equalto contract Required Detection Limits <CRDL)?

Are all calibration blanks less than two timesInstrument Detection Limit (when H3LKKOL)? [ __ ] _

SCCnM-" If no for any of the above, flag as estiirated (J)all positive data less than or equal tocalibration blank values analyzed betweencalibration blank with value over CRDL (or 2xIDL)and nearest good calibration blank- Flag fivesairples on either side of the calibration blank.

(Note: The preparation blank for mercury is the sameas the calibration blank. )

A.I. 9. 5.1 Was one prep, blank analyzed for: each 20 samples? [ / 3 __

each batch? [ IX } _._

each matrix type? [ _ ] _

both AA and ICP whsi both are used for same analyte? [ __ ] _

if no for any of the above, flag as estimated (J)all associated positive data <10 x IDLs for wnichprep, blank was not analyzed.

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

A.I. 9.5. 2 Is concentration of psrep. blank greater than ORELwhen IEL is less than or equal to CRCL? _If yes, is the ccncmtration of the sample with theleast ccix:entrated analyte less than 10 times theprep, blank value? " __ C_J

SR302itOO

OPERATING FROCEEURE Page 12 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program . Nuflber: Hi-;- 2Appendix A.1: Data Assessment - Contract Revision: 10Ccrnpliance (Total Heview - Inorganics)

__ _aCffll?: If yes, reject (red-line? all associated data

greater than CROL concentration but less than tentimes the prep, blank value found in the raw data.

A. 1.9. 5. 3 Do concentrations of prep, blank fall below two timeswhen IEL is greater than CREL? t _ ] _

If no, reject (red-line) all positive datathat has a concentration less than 10 tinesthe prep- blank value in the raw data.

A- 1.9. 5. 4 Is concentration of prep, blank below the negative O?DL? _ [ ,/X]ACTICK: If yes, reject (red-line) all associated data

that has a concentration less than 10xCK3L.

A.I. 9. 6 Form IV (1CP Interfergrce QiecK ggpple)

A. 1.9. 6.1 Present and ccrrplete? [it 3 _

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

Was 2CS analyzed at beginning and end of run<or at least twice every 8 hours)?ACTICK: If no, flag as estiinated (J) all sanples for

which AL, Ca, Fe, or Mg is higher than in ICS.

A.l.8.6.2 Circle all values on Data Satrary Sheet that are morethan **• 20* of true or established mean value. Are allInterference Check Sanple results inside of controllimits <* 20%)? -,If no, is concentration of Alf Ca, re, or Mg lewthan in ICS? I _ J

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 **dch ICS recovery is lessthan 50%; if ICS recovery is above 150%, rejectpositive results only (not flagged with a "11").

SIMCftRD QFCT7OTNG H4JLLUURE Page 13 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HX*-2appendix A.1: Data Assessment - Contract Revision: 10cerrpliance (Itotal Review - Inorganics)

2E5 ID

( Note: Not required for Ca, Mg, K, and Na (both matrices) , Al, and Fe(soil only.)

! A.l.9.7.1 Present and complete for: each 20 sanples? [ ft6 __

If Y®5. flag »H positive data less than4 x spike *tted as estimated (J) for whichfield blank was used as spiked sample.

Matrix spite analysis should be performed on afield blank *ten it is the only aqueous sanple in SDG.

A. 1.9.7. 3 Circle all values en Data 9aimary Sheet that are outsidecontrol limits (75% to 125*). Are all recoveries /vwithin control limits? ru I _ ]If no, is sarple conceitraticn greater than or equalto four times spike ccnceitration? I _ ]

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

•ach matrix type? I/y 1 _ _ _

aach cone, range (i.e. low, med. , high)? [ _ ] _ _ V"

For bo-th AA and ICP when both are used for sameanalyte? " [ _ ]

If no for any of the above, flag asestiireted (J) all positive data lessthan four times spiking level forwhich spiked sample was not analyzed.

If one spiked sample was analyzed for morethan 20 sanples, then first 20 samplesanalyzed do not have to be flagged as

- estimated (J).

A.l.9.7.2 Was field blank used for spiked sample? _

CF2J&JING ffiDCHJURE Page 14 o: 35

'Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: *Hw-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Ifctal Review - Inorganics)

A.I.9.7.5 Soil/SedimentAre any spike recoveries:

(a) less than 10%? _ [_](b) between 10-74%? __ [_]

(c) between 126-200%? __ {__]

(d) greater than 200%? __ [_]

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

Are results outside the control limits (75-125%) _,flagged with "N" on Form I ' s and Form VA? [ 0(]

£CIlfl$: If no, write in the Contract - Problem/Nan -Ccrrpliance section of "Data Assessment Narrative".

A.I. 9.7. 4 AoueoosAre any spike recoveries:

(a) less than 30%? _ .

(b) between 30-74%? Q( ( __ ] __

(c) between 126-150%? __

<d) greater than 150%? _

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".

CPERAJIN3 HOCEDURE Page 15 oi 35

itle: Evaluation of Metals Data for the Date: Feb. 199:-contract Laboratory Program Number: H>;-2

A.1: Data Assessment - Contract Revision: 10(TOtal Revi - Inorganics)

t.1.9.8 yprm VJ

If TO, art all results outside the control lijnitswith an * en Form Ifs and VI?

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

1. KTO is not calculable for an anaiyte of thesanple - duplicate pair when both values areless than EX.

Substitute HL for CRCL when IEL > 'CKX*

L.9*8.1 Present and cotrplete for: each 20 sanples? [ 3 _ _,sash matrix type? fr/ 1 _ _

•ach concettraticn range (i.e. low, mad., high)? [__] __ 'V

and ICP when both are used for sane anaiyte? [ ] CVf—— — jt .If no for any the above, flag as estimated (J)all data X3S3L* for which duplicate sarrple wasnot analyzed.1. If one duplicate sanple was analyzed formore than 20 sanples, then first 20 sanples do nothave to be flagged as estijnated.2. If percent solids for soil sanple and its duplicatediffer by more than 1%, prepare a Form VI for eachduplicate pair, report concentrations in Hg/Lon wet weight basis and calculate PPD or Differencefor each anaiyte,

.9.8.2 Was field blank used for duplicate analysis? _ tp J 't_

• If yes, flag all tota >O*DL* as estiratedtJ) for which field blank was used as duplicate.

Duplicate analysis should be performed ona field blank wh&i it is the only aqueoussanple in 3DG.

A.1.9.B.3 Are all values within control limits (KTO 20% or

S3BNDWO CFEBAJING PRCX2UURE Page 16 Ol 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: H>;-2Appendix A.I: Data Assessnent - Contract Revision: 10Corrpliance (Total Review - Inorganics)

2. If lab duplicate result is rejectable dueto coefficient of correlation of MS ,analytical spike recovery, or duplicateinjections criteria, do not apply precisioncriteria.

A. 1.9.8.4 Is any value for sample duplicate pair less than CRDL*and other value greater than or equal to 10 x *CRDL?

ACTICK: If yes, flag the associated data asestimated (J).

A.I.9.8.5 AqueousCircle all values on Data Summary Sheet that are:

RPD > 50%, orDifference > ± OTDL*

Is any RTO greater than 50% where sample and duplicateare both greater than or equal to 5 times *CRDL? 2V

Is any "difference between sample and duplicate greaterthan *CREL where sample and/or duplicate is less than5 times *O*DL?

If yes, flag the associated data as estijnated.

A.I. 9, 8. 6 Soil/SedunentCircle all values on Data Surtnary Sheet that are:

RTO > 100%, or •

Difference > 2 x O?DL*Is any PPD (where sample and duplicate are bothgreater than or equal to 5 times *O3DL) :

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

* Substitute IEL for CH3L when TDL > OREL.** Use absolute values of sample and duplicate to calculate

the difference.

H)

ioo%? [ _ J

Ii Page 17 oi 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: H.%-2Appertfix A.I: Data Assessment - Contract Revision: 10Ccrrpliance (Itxtal Review - Inorganics)

A.I* 9. 9. 3 Aqueous

&>If yes, flag the associated data as estimated.

A.I.9.9 ifllflfl duplicates

A.I.9.9.1 Were field Silicates analyzed? t__] _ _ (V_

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

ld£: 1- Bo not calculate RTO when both values areless than IDL.

2. Flag all associated data only for fieldduplicate pair.

A. 1.9.9.2 Is any value for sample duplicate pair less than *CRDLother value greater than or equal to 10 x *CRDL? __ [_ . 3

If yes, flag the associated data as estijnated.

Circle all values on Form VI for field duplicates that are:RTO > 50%, or

Difference > ± CRDL*is any RTO greater than 50% where sample and digaicateare both greater than or equal to 5 times *OT3L? __ [_ J CxIs any **differerce between sairple and duplicate greaterthan *CREL where sanple and/or diplicate is less than5 tim« *CREL? __ [_ .]

the associated data as estijnated.

* Substitute IEL for C*EL whai ITL > CSEL.

** Use absolute values of sample and delicate to calculate the difference.

STANDARD OFEBMTNG PROCEDURE Page 18 c: 35

Title: Evaluation of Metals Data for the Date: Feb. 1993Contract laboratory Program Number: K.-;-2~Appendix A.1: Data Assessment - Contract Revision: 10Compliance (Ittal Review - Inorganics)

IES

A.I. 9. 9. 4f Circle all values on Form VI for field duplicates that are:) RPD >100%, or

Difference > 2 x CRDL*Is any RFC (where sample and duplicate are bothgreater than 5 times *O*DL) :

A. 1.9. 10 Ftorm VII {l nr r f GontTDl Sarrple) (Mate: LCS - notrequired for aqueous Hg and cyanide analyses.)

A. 1.9. 10.1 Was one LCS prepared and analyzed for:every 20 water sanples? I IX]

every 20' solid sanples? [ _ ]

both AA and ICP when both are used for same analyte? [ _ ]

if HD for any of the above, prepare TelephoneRecord Log and contact laboratory for sutaittalof results of LCS. Flag as estimated (J) alldata for which 1CS was not analyzed.

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

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

>2x *CRDL? __ [ ] X"

: If yes, flag the associated data as estimated.

* Substitute IEL for OCL when HL >

**Use absolute values of sample and duplicate to calculate the difference.

/SR302U07

SWCftRD OPERATING PROCEDURE Page 19 o: 35

Title: Evaluation of Metals Data for the Date: Feb.Contract Laboratory Program Number: H.vAppendix A.I: Data Assessment - Contract • Revision: 10Ccrrpliance (Total Review - Inorganics)

A. 1.9.10.2 Aqueous LCSCircle all LCS values outside control lijnits(80 - 120%- except aqueous Ag and Sb).

Is any LCS recovery: less than 50%?

between 50% and 79%?

betveen 121% and 150%?

greater than 150%?

Less than 50%, reject (red-line) all data;betveen 50% and 79%, flag all associated dataas estimated (J); between 121% and 150%, flag

I a l l positive (not flagged with a "U") resultsas estimated; greater than 150%, reject allpositive results.

A. 1.9.10.3 Solid LCS

IK7TE: 1. If "Found" value of LCS is rejectable due to duplicateinjections or analytical spike recovery criteria,regardless of LCS recovery, flag the associated dataas estijrated <J).

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

Is LCS "Found1* value higher than the controllimits on Form VII? __ I 1

if yes, qualify all associated positive dataas estimated.

is LCS "Found" value lower than the Controllimits en Form VII? __ I J

If yes, qualify all associated data asestimated.

OFERAITOG raOdUUr?£ Page 20 c: 35

Title: Evaluation of Metals Data for the Date: Feb. 199*Contract Laboratory Program Number: ik:-2~*Appendix A.I: Uata Assessment - Contract Revision: 10Conpliance (Itotal Review - Inorganics)

A.I. 9. 11 Form DC tIQ> Serial Dimticnl -

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

A. 1.9. 11-1 Was Serial Dilution analysis performed for: ^each 20 samples? IJ .1 _

each iratrix type? [CK 3 __

each concentraticn range (i.e. low, med.)? [ _ ] __

If no for any of the above, flag all positivedata greater than or equal to lOxIDLs asestimated (J) for which Serial Dilution Analysiswas not performed, and summarize the deficiencyon the DPO report.

A.I. 9. 11. 2 Was field blank(s) used for Serial Dilution Analysis? __ [./V]

ACT1CTJ: If yes, flag all associated data 2 10 x Id-as estimated (JJ.

NC7l£: Serial dilution analysis should be performedon a field blank wnen it is the only aqueoussarrple in SDG.

A.l.9.11.3 Are results outside control limit flagged with an "E"an Form I *s and Form IX when initial concentration on «Form IX is equal to 50 tijnes IDL or greater. [_] _

acnfXJ: If no, write in the ccntract-prcblaoAicn-corrpliance section of the "Data AssessnentNarrative".

Circle mil values en Data Sumary Sheet that are outsidecontrol limit for initial concentrations equal to or greaterthan 10 x FT-p only. Are any I difference values:

2 100%? ^ [._] _

CREATING ITOCEDURE Page 21 Of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: H>-;-2~Appendix A.I: Data Assessment - Contract Revision: 10Corqpliance (Total Review - Inorganics)

Flag as estimated (J) all associated equalto or greater than lOxIDLs for which percentfiifferexre is greater than 10% but lessthan 100%. Reject (red- line) all associatedsarrple results equal to or greater thanlOxIELs for which K> is greater than orequal to 100%.

i A. i . 9 . 12 FUrn g frtnnic PteCTfrE-ion (MO *"*?I "A. 1.9. 12.1 Are duplicate injections present an furnace raw data

<€xcept during full Method of Standard Addition) fori each sarrple analyzed ijy GFAA? [X. ]

acncm: If no, reject the data on Form I's for whichi duplicate injections were not performed.

A.I. 9. 12. 2 Do the duplicate injection readings agree within 20%I Relative Standard Deviation (RSD) or Coefficient ofI Variation (CV) for concentration greater than CRDL?

Was a dilution analyzed for sanple with post digestion| spike recovery less than 40%? [ _ ]I -

If no for any of the above, flag all the; associated data as estimated (J).

A. 1.9. 12. 3 Is *post digestion spike recovery less than 10% orgreater than 150% for any result? (J L_ O<L [. _3i ^

If y Sf reject (red-line) the affected data ifrecovery is <10%; reject data not flagged with*U* if spike recovery is >150%.

Reject the data only if the affected sanpie wasnot subsequently analyzed by Method of StandardAddition.

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

OFEBATUgG PROCEDURE Page 22 c: 35

Title: Evaluation of Metals Data for the Date: Feb 1990Contract Laboratory Program Number: *hv;-2~Appendix A.I: Data Assessnent - Contract Revision: 10Corrpliance ('Total Review - Inorganics )

A.I. 9. 13 Etorm VIII (MgthDd Of fthanrffipfl

A.l.9.13.1 Present? f (Xl

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

If yes, write request en Telephone Record logand contact laboratory for sutmittal of Form VIII.

A.I. 9. 13. 2 Is coefficient of correlation for Ma less than 0.990 forany sarrple?

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

A.I. 9. 13. 3 Was *MSA required for any sanple but not performed?

. Is coefficient of correlation for MSA less than 0.995?

Are MS calculations outside the linear range of thecalibration curve generated at the beginning of the ^analytical run? _ L?\

J£H£E: If yes for any of the above, flag allthe associated data as estimated (J).

A. 1.9. 13. 4 Was proper quantitation procedure follcved correctlyas outlined in the SOW on page E-16 through £-17? fie ] __

If no, note exception xmder contract problarv/I non-carpiiance of data assessment narrative,

or prepare a separate list.

A. 1.9. 14 Pi!?gPlVBl/*Tttj*J

7L 1*9. 14.1 Were any analyses performed for dissolved as well astotal analytes en the same sample(s).Were any analyses performed for inorganic as well as total{organic * inorganic) analytes on the same sampie(s)?

is not required on LCS and prep, blank.

flR3021)l I

SWCRHD OPESAnNG PROCUXJRE Pace 23 Cf 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: H~;-2~Appendix A.1: Data Assessnent - Contract - Revision: 10Corrpliance (Itatai Review - Inorganics)

———— - „ ___ •"

M2IE: 1. If yes* prepare a list ccrparing differencesbetween all dissolved (or inorganic) andtotal analytes. Ocrpute the differences asa percent of the total analyte only whendissolved concentration is greater than CKOLas well as total concentration.

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

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

A. 1.9. 14. 2 is the concentration of any dissolved (or inorganic)analyte greater than its total concentration bymore than 10%? • _

A.I. 9. 14. 3 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration bymore than 50%?

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

A, 1,9. 15 Fttrm T to IX

A* 1.9. 15.1 Are all the Form I through Form IX labeled with:Laboratory name?

Case/SAS nuntoer?sanple No.? fO 3

SC No.? [ ]

Contract No.? [ 1

Correct units? LX ]

Matrix?

if no for any of the above, note undercontract problem/non-ccrrpliance sectionof the "Data Assessnent Narrative".

OPERATING PROCEDURE Page 24 o: 35

Title: Evaluation of Metals Data for the Date: Feb.Contract Laboratory Program Number: K-;

! Appendix A.I: Data Assessment - Contract Revision: 10Ccrrpliance (Itotal Review - Inorganics)

2LS ffi K A"A. 1.9.15.2 Do any ccrputation/transcription errors exceed 10% of

reported values on Forms I-IX for:

(NOTE: Check all forms against raw data.)

<a) all analytes analyzed by ICP? __ [ -V_] _<b> all analytes analyzed try GFAA? _ [_XJ _

(c) all analytes analyzed by AA Flame? _ [__) •<

(d) Mercury? __

(e) Cyanide? __

ACTIdJ: If yes, prepare Telephone Log, ccntactlaboratory for corrected data andcorrect errors with red pencil areainitial.

A.l.9.16 Form I (Field Blank) -

Circle all field blank values on Data Surmary Sheetthat are greater than OS2L, 2 x JDL when IDL > CHDL,

Do concentrations of field blank(s) fall below CKDL(or 2 x IDL when HJL > CRDL) for all parameters ofassociated aqueous and soil sanples? [_]

If ix), was field blank value already rejected due toother QC criteria?

if nof reject (except field blank results)all associated positive sairple data lessthan or equal to five times the field blankvalue.

flR302M3

OFE3AHN3 PROOTURE Page 25 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: K/;-Appendix A.I: Data Assessment - Contract Revision: aoCcrpliance (Sbtal Review - Inorganics)

A.I. 9. 17.1 Is verification report present for:

Instrument Detection Limits (quarterly)?

TCP Interelanent correction Factors (annually)? [ Xl\/ICP Linear Ranges (quarterly)? [ jc ]

If no, contact ISO of the lab.

A.I.9.17.2 Form X (Instrument Detection Limits) - (Note: IDL is rotrequired for cyanide.)

Are TTE..S present for: all the analytes? [ t\] _

all the instruments used? [_/Y ]v~ ~ — -

For both AA and ICP vnen both are used for sameanalyte? " [_] _ VATTICT4; If re for any of the above, prepare

TelepJx ie Record Log and contactlaboratory.

Is HX greater than CRDL for any analyte? _ [

If yes, is the concentration on Form I of the sanpleanalyzed on the instrument whose IDL exceeds O DL,greater than 5 x IEL? [__] __

If nop flag as estimated all valuesless than five times HL of the instrumentvhose HL exceeds CRCL.

Yi

OPERATING FKXEnjRE Page 26 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: His-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance Cltital Review - Inorganics)

— —— -_._^_._

A.I.9.17.3 Form XI (Tiinfftr Ranges)

Was any sample result higher than high linear rangeof JCP.

"Was any sample result hitler than the highestcalibration standard for ncsrfCP parameters? __ [ /yl

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

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

A.I.9.18 Parcart Soli

Is soil content in sediment(s) less than 50%? _ [_ ]

ACTia7: If yes, qualify as estimated all datanot previously rejected or flagged dueto other QC criteria.

ATTACHMENT IVDPO REPORT

INORGANIC REGIONAL DATA ASSESSMENT

CASE NO, .- _____ SITELABORATORY ffftr. p. (A h NO. OF SAMPLES/ -

Q MATRIX 3> uaAfczSDG>* ^ ______________ REVIEWER (IF NOT ESD)

SOW* n 7 ___________________ REVIEWERS NAME\4 JDPO: ACTION _____ FYI &/ ______ COMPLETION DATE /-

O « Data had no problems/or qualified due to minor problems.M -= Data qualified due to major problems.Z = Data unacceptable.X -= Problems, but do not affect data.

ACTION ITEMS: I ~ TX)g fo

DATA ASSESSMENT SUMMARY

ICP AA Hg CYANIDE

I. HOLDING TIMES Q O O &

2. CALIBRATIONS . O & O • O

3. BLANKS O Q . O Q

4. ICS 0

5- LCS Q ...... G"

6. • DUPLICATE ANALYSIS Q3* Q @ _fi

7. MATRIX SPIKE Q Q ' O O

8. MSA O

9. SERIAL DILUTION 0 S

10. SAMPLE VERIFICATION Q Q . # r>

II. OTHER QC (} n G O

12. OVERALL ASSESSMENT Q __H 0 &

NOTABLE PERFORMANCE:

III

ATTACHMENT VSUPPORT DOCUMENTATION

I

NO SUPPORT DOCUMENTATION

5R302M9

III STANDARD CHLORINE

CASE 9008L253

This quality assurance review is based upon a review of the datagenerated from one water sample, one field blank, and one tripblank collected on 08/01/90 and analyzed by Roy F. Weston, Inc.d£or TCL Volatile, Semivolatile, Pesticide/PCB, and special listtarget compounds.

The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.

Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.

QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9008L253Page 2 of 5

EVALUATION BY FRACTION

•?! * Volatiles

Holding TimeSurrogate RecoveryMS/MSDBlankGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)StandardsSpectra QualityChromatographyData Completeness

OVERVIEW

This portion of the case consisted of one water sample, one fieldblank, one trip blank. The samples were analyzed for TCL volatiletarget compounds.

All surrogate recoveries, internal standard areas, and calibrationdata met EPA CLP QC criteria. Minor problems associated with thesample analyses are listed in the following section.

ISSUES

The method blank contained common contaminants methylene chlorideand acetone at levels less than 3x the CRQL. The trip and fieldblanks contained the same compounds. For these compounds, sampleresults that are less than CRQL, are believed to be not detectedand reported at the CRQL. All other results were greater than theCRQL but less than lOx the blank level. The results are consideredlaboratory artifacts and are not detected. They are flagged "U" inthe data summary.

The %RSD for acetone in the initial calibration exceeded the 30% QClimit. The associated sample results are already qualified inreference to the method blank contamination. No additionalqualification is applied.

Lr



II. Bage/Neutral/Acids

___ Holding Time___ Extraction Time___ Surrogate Recovery___ Blank_J_ MS/MSD___ GC/MS TuningX Initial CalibrationX Continuing Calibration___ Compound ID (HSL, TIC)X Standards___ Spectra Quality___ Chromatography___ Data Completeness

OVERVIEW

This portion of the case consisted of one water sample and onefield blank analyzed for special list semivolatile targetcompounds.

All blank spike recoveries, surrogate recoveries/ and calibrationdata met EPA CLP QC criteria- The samples and blanks were free oftarget compounds. Minor problems associated with the sampleanalyses are listed in the following section.

ISSUES

The chrysene and perylene internal standard areas were below QClimits for sample GW 4-0-1 OR6A. This sample was also analyzed asthe matrix spike/spike duplicate and similar internal standardoutliers were found. This sample is exhibiting a matrix effect.The data usability is not affected and no qualification is applied.

Several compounds had %RSD and/or %D exceed the 30% and 25% QClimits in the initial and continuing calibrations. All associatedguantitation limits are qualified estimated and flagged "UJ".

The pyrene matrix spike/spike duplicate recoveries were above theQC limits. This compound was not detected in the originalanalysis, therefore no qualification is applied.



.III. Pesticides/PCB

___ Holding Time___ Extraction Time___ Surrogate Recovery_X_ MS/MSD___ BlankX Linearity CalibrationX DDT/Endrin Degradation___ Analytical Sequence___ DBC Retention Time___ Continuing Calibration___ Retention Time Window___ Standards___ Chromatography___ HSL Compounds___ Data Completeness

OVERVIEW

This portion of the case consisted of one water sample and onefield blank. These samples were analyzed for TCL Pesticide/PCBtarget compounds.

All surrogate recoveries, blank spike recoveries, retention time,and calibration data met EPA CLP QC criteria. Positive targetcompound results were not detected in the samples and the blank.Minor problems associated with the sample analyses are listedbelow.

ISSUES

Several compounds had %RSD exceeded the 10% QC limit on theconfirmation column. Since this column is not used for sampleresult quantitation, no qualification is applied.

The following matrix spike recoveries are outside the QC limits.Also, all %RPD were outside criteria. These compounds were notfound in the original sample analysis. The data usability is notaffected, and no qualification is applied.

Compound % Recovery Lower Limit

Gamma-BHC 45 564,4-DDT 32 38

ifr QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9008L253Page 5 of 5

There was a coeluting non-target compound that interfered with theguantitation of 4,4-DDT.

The 4,4-DDT/Endrin breakdown were calculated incorrectly for bothguantitation and confirmation columns. The corrected results arereported on the attached Form VIII Pest-1. All breakdown criteriais met.

flR302l»2lt

1II

INFORMATION REGARDING DATA

The data have been reviewed according to EPA CLP FunctionalGuidelines for Evaluating Organic Analyses. All data are validatedwith regard to usability.

If you have any questions or comments on this data review, pleasecall Kelly M. Spittler or Zohreh Hamid at (215)524-6100.

ATTACHMENTS

1. Attachment I - Glossary of Data Qualifier Codes.

2. Attachment IX - Data Summary. This includes:

a) A summary of all positive results for the targetanalytes with the qualifier codes, if applicable;

b) All usable detection limits (qualified "Rn).

3. Attachment III - Support Documentation

RR302U25

ATTACHMENT IGLOSSARY OF DATA QUALIFIER CODES

I GLOSSARY OF DATA QUALIFIERS

( CODES RELATING TO IDENTIFICATION


0 =* NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELI REPORTED IN LABORATORY OR FIELD BLANKS.

R «. UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.

N ^ NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.

(NO CODE) « CONFIRMED IDENTIFICATION

COSES RELATING TO OUANTITATION

(can be used for both positive results and sample quantitationlimits):

J «• ANALYTE PRESENT. REPORTED VALUE MAY NOT. BEACCURATE OR PRECISE.

L - ANALYTE PRESENT. REPORTED VALUE MAY BEBIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.

UJ - THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.

UL - NOT DETECTED. QUANTITATION LIMIT MAY BE IHIGHER.

OTHER CODES

Q NO ANALYTICAL RESULT.

ATTACHMENT IIDATA SUMMARIES

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ATTACHMENT IIISUPPORT DOCUMENTATION

""3021,35

I 2780

PESTICIDE EVALUATION STANDARD SUMMARY

Lab Name: Rov F> Weston, Inc. Contract: 2267-09-02-OODg

Ca»e No.: STANDARD CHLORINE______ GC Sample ID: 08089013

RFW Lot NO.s 9008L253

Instrument ID: £3______ OC Column ID: 2250/2401

Dates of Analyses: 08/08/90 to 08/09/90

Evaluation Check for Linearity

1| PESTICIDEI

f ALDRIN1 BNDRIN1 4,4'-DDT1 OBC1

| CALIBRATION1 FACTOR| EVAL MIX A

| 3972281| 10600531 590008| 5451491

CALIBRATIONFACTOREVAL MIX B

41291111079097660401539627

CALIBRATIONFACTOREVAL MIX C

4P728971094805702906536204

j %RSD |!(</- 1(10.0%) j—— 11 2.0|1 1.6|1 a.a|1 o.sj1 1

(1) If > 10.0% RSD/ plot a standard curve and determine the ngfor each sample in that set from the curve.

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

1 11 11 1

OlflNIT. EVAL MIX B)02 j EVAL MIX BJ

1 i

DATE |ANALYZED i

i108/08/90 |08/09/90 !

J

| TIME || ANALYZED |

1 11 1519 || 0103 |1 1

ENDRIN

0.00.0

| 4r4'-DDT | COMBINED1 1 (2)

| |

(2) See Form Instructions.

FORM VIII PEST-1 11/88 Rev,

I28

8DPESTICIDE EVALUATION STANDARD SUMMARY

* Lab Nome: Roy F* Weaton, lac- Contract: 2267-09-02-0000 '

1 Case No.: STANDARD d&ORINg______ GC Sample ID: 08089014

RFW Lot NO.: 90.Q8L253

Instrument IDs i£______ GC Column ID: SP2100

Date* of Analyses: OS/09/90 to 08/09/90


PESTICIDE

ALDRINENDRIN4,4'-DDTDBG

| CALIBRATIONj FACTORj EVAL MIX A

| 2867125! 915416| 631723| 536287i


33262011008029785836560534


35898491086803894371582087

| %RSD |!<</- 1|10.0%)j

1 H.2|1 8.5|I 17.1|1 4.1|I 1

(1)

(!) If > 10.0% RSD, plot a standard curve and determine the ngfor each sample in that set from the curve.

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

11I

INIT. EVAL MIX B)EVAL MIX BJ

1

DATE ]ANALYZED

108/09/90 |08/09/90

!

| TIME || ANALYZED j

i 1| 0914 || 1836 j1 t

ENDRIN | 4, 4 '-DOT | COMB IN1 1 (2)

1 1

j*f£

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-02 1 EVAL MIX B 08/09/90 1836 | \^ G J \/-xi _____ i(2) See Form Instructions.

FORM VIII PEST-1 11/88 Rev.

SEMIVOLATILE AND VOLATILE ANALYSES

UPPER POTOMAC MONITOR WELLS MW-11,MW-12 AND OR-6B

STANDARD CHLORINECASE 9008L254

This quality assurance review is based upon a review of the datagenerated from three water samples and one trip blank collected on07/31/90 and 08/01/90 and analyzed by Roy F. Weston, Inc. for*«pecial list Volatile and Semivolatile target compounds.

The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPArs ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.




I. Volatiles

___ Holding Time___ Surrogate Recovery_X_ MS/MSD___ Blank___ GC/MS Tuning___ Initial Calibration___ Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality_____ Chromatography___ Data Completeness

OVERVIEW - - - - - -

This portion of the case consisted of three water samples and onetrip blank analyzed for benzene, toluene, chlorobenzene andethylbenzene.

The samples and blanks were free of target compounds.

The surrogate recoveries, internal standard areas, and calibrationdata met EPA CLP QC criteria.

A matrix spike/spike duplicate sample was not analyzed with thisbatch of samples. The matrix spike/spike duplicate associated withthese samples is sample GW 4-0-1 OR6A from RFW batch 9008L253-001.All spike recoveries were within EPA QC limit.

The samples were free of tentatively identified compounds.


I


XI. Base/Neutral/Acids

___ Holding Time___ Extraction Time___ Surrogate Recovery___ Blank_X_ MS/MSD___ GC/MS Tuning___ Initial Calibration___ Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness

OVERVIEW

This portion of the case consisted of three water samples analyzedI for a special list of semivolatile target compounds.

The samples and blank were free of target compounds.

j The surrogate recoveries, blank spike recoveries, internal standardareas, and calibration data met EPA CLP QC criteria.

A matrix spike/spike duplicate sample was not analyzed with thisbatch of samples. The matrix spike/spike duplicate associated withthese samples is sample GW 4-0-1 ORGA from RFW batch 9008L253-001.The pyrene spikes recoveries exceeded the QC limit. This compoundwas not on the target list, therefore no qualification is. applied.

AR302UI




ATTACHMENTS


2. Attachment II - Data Summary. This includes:


b) All usable detection limits (qualified ,HRM).

II1





U = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.

R = UNRELIABLE RESULT, ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.



CODES RELATING TO QUANTITATION

(can be used for both positive results and sample guantitationlimits):


L = ANALYTE PRESENT. REPORTED VALUE MAY BEBIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.


UL = NOT DETECTED. QUANTITATION .LIMIT MAY BEHIGHER.

OTHER CODES

NO ANALYTICAL RESULT.

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VOLATILE, SEMIVOLATILE, PESTICIDE/PCB,AND METALS ANALYSES

COLUMBIAMONITOR WELL C-30

STANDARD CHLORINECASE 9008L257

This quality assurance review is based upon a review of the datagenerated from five water samples collected on 08/03/90 andanalyzed by Roy F. Weston, Inc, for TCL Volatile, Pesticide/PCBand special list Semivolatile target compounds.

The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults*


IQA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9008L257Page 2 of 4


I. Volatiles

Holding Time.Surrogate RecoveryMS/MSDBlankGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)StandardsSpectra QualityChromatographyData Completeness

OVERVIEW

This portion of the case consisted of five water samples that wereanalyzed for TCL volatile target compounds.

All surrogate recoveries, internal standard areas, and calibrationdata met EPA CLP QC criteria. Minor problems associated with thesample analyses are listed below.

ISSUES

The method blank contained common contaminants methylene chlorideand acetone at levels less than 3x the CRQL. Sample results forthese compounds that are less than CRQL are considered not detectedand are reported at the CRQL. Results greater than the CRQL butless than lOx the blank level are considered laboratory artifactsand are flagged "U". The acetone result in sample GW7-0-1-C30 isgreater than lOx the blank level and is considered true value.

Acetone and 2-butanone had %RSD and/or %D exceed the 30% and 25% QClimits in the initial and continuing calibrations. Most acetoneresults are qualified due to blank contamination, however all non-detects for acetone and 2-butanone are qualified estimated andflagged "UJ».

This batch did not have a matrix spike/spike duplicate. However,the matrix spike sample from batch 9008L253-001 is associated withthese samples. All matrix spike criteria were met.

tII QA ORGANIC DATA REVIEW

STANDARD CHLORINECASE 9008L257Page 3 of 4


11. Base/Neutral/Acids

___ Holding Time___ Extraction Time___ Surrogate Recovery___ Blank___ MS/MSD

1 ___ GC/MS TuningX Initial Calibration

j X Continuing Calibration1 ___ Compound ID (HSL, TIC)

___ Standards___ Spectra Quality___ Chromatography___ Data Completeness

I OVERVIEW

I T h i s portion of the case consisted of four water samples which wereanalyzed for special list Semivolatile target compounds.

All surrogate and blank spike recoveries, internal standard area| and calibration data met the EPA CLP QC criteria. Also the blankI is free of target compounds. Minor problems associated with the

sample analyses are listed below.

Several compounds had %RSD and/or %D exceed the 30% and 25% QClimits in the initial arid continuing calibrations. All associatedsample quantitation limits are qualified estimated and flagged "UJ"in the data summary.

A matrix spike/spike duplicate was not analyzed with this batch ofsamples. However, the matrix spike analyzed in batch 9008L253-001is associated with these samples. The pyrene matrix spike/spikeduplicate recoveries exceeded the QC limits. This compound was notdetected in the samples; therefore, no qualification is applied.

Several compounds were detected in samples GW7-0-1-C30 and GW7-1-1-C30 as tentatively identified compounds. These compounds were notdetected in the blank; therefore no qualification is applied.

AR302t(5l



III. Pesticides/PCB

Holding TimeExtraction TimeSurrogate RecoveryMS/MS DBlankLinearity CalibrationDDT/Endrin DegradationAnalytical SequenceDBC Retention TimeContinuing CalibrationRetention Time WindowStandardsChromatographyHSL CompoundsData Completeness

OVERVIEW

This portion of the case consisted of four water samples which wereanalyzed'for TCL Pesticide/PCB target compounds.

All surrogate recoveries and calibration data met EPA CLP QCcriteria. Also the method blank and samples were free of targetcompound contamination. Minor problems associated with the sampleanalyses are listed below.

ISSUES

A matrix spike/spike duplicate was not analyzed with this batch ofsamples. The matrix spike/spike duplicate 9008L253-001 isassociated with these samples. The Gamma-BHC and 4,4-DDT spikerecoveries were below the QC limits. Since spike recoveries haveadvisory limits, no qualification is applied. A blank spike/spikeduplicate was also analyzed and four %RPD were outside limits. Thedata usability is not affected.

The 4,4-DDT/Endrin breakdown were calculated incorrectly for bothguantitation columns. The corrected results are reported on theattached Form VII Pest-1. All breakdown criteria is met.

I

REGARDING DATA

The data have been reviewed according to EPA CLP Functional'Guidelines for Evaluating Organic Analyses. All data are validatedwith regard to usability.


ATTACHMENTS




b) All usable detection limits (qualified "R").



COPES RELATING TO IDENTIFICATION


U = NOT DETECTED,. SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.

R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.



CODES RELATING TO OUANTITATION . . ..



L = --- -ANALYTE PRESENT. REPORTED VALUE MAY BEBIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.


UL = NOT DETECTED. QUANTITATION LIMIT MAY BEHIGHER.

OTHER CODES

NO ANALYTICAL RESULT,

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I 8D «PESTICIDE EVALUATION STANDARD SUMMARY *->0

Lab Name: Rov F, Wegton, Inc. Contract: 2267-09-02-0000

Case No.: STANDARD CHLORIKB______ GC Sample ID: 08089013

RFW Lot No.s 9008L257

Instrument ID: 13______ GC Column ID: 2250/2401



PESTICIDE

ALDRINENDRIN4,4'-DDTDBC

| CALIBRATION |j FACTOR |j EVAL MIX A |

| 3972281 || 1060053 || 590008 || 545149 |1 1

| CALIBRATION || FACTOR || EVAL MIX B |

| 4129111 || 1079097 || 660401 || 539627 |! 1

| CALIBRATION| FACTORj EVAL MIX C

| 4072897| 1O94B05| 702906| 536204I

| *RSD |!<</- 1|10.0%)|__l1 2.0|1 i-6lI S.8|1 0.8J1 I

(1)

(1) If > 10.0% RSDr plot a standard curve and determine the ngfor each sample in that set from the curve.

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

j DATE j TIME j ENDRIN | 4,4'-DDT | COMBINEDj ANALYZED j ANALYZED j j I (2)

01INIT. EVAL MIX B| 08/08/90 | 1519 | 0.0 |021 EVAL MIX B j 08/09/90 j 0103 | 0.0 j^-, 8.5


eFORM VIII PEST-1 11/88 Rev.

•37PESTICIDE EVALUATION STANDARD SUMMARY

Lab Name: Rov F- Weaton, Inc. Contract: 2267-09*02-0000 •

Case No.; STANDARD CHLORINE______ GC Sample ID: 08089014

RFW Lot No.: 90081,257

Instrument ID: 14______ GC Column ID: SP2100

Dates of Analyses; 08/09/90 to 08/09/90


1| PESTICIDE1

f ALDRIN1 ENDRIN1 4,4'-DDTi DBC1

| CALIBRATION |j FACTOR j| EVAL MIX A j

| 2867125 1| 915416 || 631723 || 536287 |1 I


33262011008029785836560534


35898491086803894371582087

%RSD

10. 0% )smmmmmK

11.28.517.14.1

(1) If > 10.0% RSDf plot a standard curve and determine the ngfor each sample in that set from the curve.

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

02INIT. EVAL MIX

EVAL MIX

1 DATEj ANALYZED

1B| 08/09/90BJ 08/09/90

1

TIMEANALYZED

09141836

ENDRIN | 4r4'-DDT | COMBINED1 1 (2)

1 1

1 \J*\ 5.1i r-'(2) See Form Instructions.


STANDARD CHLORINESD6 #CLP257


The laboratory's portion of SDG #CLP257 consisted of eight watersamples analyzed for TAL metals by Roy F. Weston, Inc.

The laboratory reported no problems with the receipt and analysisof the samples received on 08/03/90.


Minor Issues

The post-digestion spike recoveries for As, Se, Pb, and Tl werebelow the CLP control limits. All associated sample results arequalified as estimated and considered to be biased low.

The data package does not include matrix spike, duplicatedigestiop, and serial dilution samples. These QC samples wereprepared in the same digestion batch but reported in a separatedata package. These forms are included with this package. As aresult of these QC samples, the associated sample results:

1. For Pb are estimated and considered to be biased low dueto a low matrix spike percent recovery.

2. For Zn is estimated due to a high duplicate digestionrelative percent difference.

3. For Ca is estimated due to a high serial dilution percentdifference

TABLE I

Sample # Analyte -j-DL -QL Comments

All samples Pb J UJ 1All samples Zn J — 2All samples Ca J UJ 390082570019008257009 As, Pb, Tl J UJ 4

9008257003 Se, Tl - UJ 4

90082570049008257004 Tl UJ 49008257008

9008257006 Pb, Tl - UJ 4

Comments

1. Due to a low matrix spike percent recovery indicating alaboratory or matrix spike problem, all associated sampleresults are qualified as estimated and considered to be biasedlow.

2. Due to a duplicate digestion outside of the CLP controllimits, all associated sample results are qualified asestimated.

3. Due to a high serial dilution percent difference, allassociated sample results are qualified as estimated.


Note;


Information Regarding Report Content








ATTACHMENT IGLOSSARY OP DATA QUALIFIERS




U - NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.• ••

R » UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.

N » NEGATED COMPOUND WAS CONSIDERED AS NOT .PRESENT IN THE SAMPLE.


CODES RELATING TO OUANTITATION

(can be used for both positive results and sample guantitationlimits) :

J - ANALYTE PRESENT. REPORTED VALUE MAY NOT BE. ACCURATE OR PRECISE.

L « ANALYTE PRESENT. REPORTED VALUE MAY BE ._. . ._BIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.

' ' --UJ - THE REPORTED QUANTITATION LIMITS ARE

QUALIFIED ESTIMATED.

UL - NOT DETECTED. QUANTITATION LIMIT MAY BEHIGHER. . _

OTHER CODES

Q NO ANALYTICAL RESULT


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OPERATING FKXH3URE Page 4 01 35

Title: Evaluation of Metals Data for the Date- FebContract Laboratory Program Number: 'Appendix A.I: Data Assessment - Cdntract Revision: 10Coipliance (Itotal Review - Inorganics)

A. 1.2 Iteoord of QcnMTJC3tigi ffron RSCC) - Present?

: If no/ request from RSCC.

A.1.3 Trip Report - Present and ccrplete? [ _ ]

i : If no, contact RSCC for trip report.

I A. 1.4 Sarrple Traffic Report. - Present or on file?

m Legible?1' £din>7." If no, request frcm Regional Sanple Control

Center (RSCC).

" A.I. 5 Cover Page - Present? [jXj

I Is cover page prcperly filled in and signed by the labmanager or the manager's designee? l_£C]

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

Do nun-bars of sanples correspond to runbers en Recordof Conrunication? [ __ ]

, Do sanple rurbers on cover page agree with satplemirtiers en:

1 (a) Traffic Report Sheet? [ ]

f <£>) Ponn I's? lot]If no for any of the above, contact RSOC forclarification.

JffiS ffi

?: If no, contact RSCC.

OPESAxrNG JTOCEZJURE Page 5 ox 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: HK-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Ibtai Reviev - Inorganics)

A.1.6 ftorm T (Final Data) - Are all Form I's present and conplete?

, aCDSU: If no, prepare telephone record log and contactlaboratory for sutmittal.

Are correct units (ug/1 for vaters and wg/Xg for soils) /indicated on Form I's? tx 1

Are soil sanple results for each parameter corrected forpercent solids? [ __ ]

Are O7* sarrple « s and corresponding laboratory sanpieID t s the same as on the Cover Page, Form I's andin the raw data? M>O Ak ^>o tf>f\ & *t, tfa$<. t

Are ccrputat ion/transcript ion errors less than 10%of reported values? [

Are all "less than IDLH values properly coded with "Un? [Oc ]

Was a brief physical description of sanples given onForm I's? I PC 1

were the result qualifiers used correctly with finaldata?

aerial If no for any of the above, prepare TelephoneRecord Log, and contract laboratory forcorrected data.

Were any sarrples diluted beyond requirements of contract?

If yes, were dilutions noted on Term I's? [_] _If no, note underof tfte"Data Assessment Narrative"*

XI.7 Holding Times - (aqueous and soil samples )

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

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

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

To

OPERATOR raOCHXJRE Page 6 O1 35

Title: Evaluation of Metals for the Contract Date: Feb. 1990Laboratory Program Number: *H/*-2Appendix A.I: Data Assessnent - contract Revision- 10Ccrpiiance (total Review - Inorganics)

ffi

Other Metals analysis (6 months). . . . exceeded? _H2I£: Prepare a list of all sanples and analytes

for which holding times have been exceeded. Specifythe lumber of days frcm date of collection to the dateof preparation (fron raw data). Attach to checklist.

acnaj: If yes, reject (red-line) values less thanInstrument Detection Limit (II2L) and flagas estijnated (J) the values above EX eventhough sample(s) was preserved properly.

A. 1.8 Rav Data

A.l.8.1 Digestion Log* for flame AA/ICP (Form 5QII) present? [ft/ ] _

Digestion Log for furnace AA Form XIII present? IJ J _ _

I Distillation Log for mercury Form XIII present? [ 3 _ _

Distillation Log for cyanides Form XIII present? [ <X 3 __

Are pH values (pH<2 for all metals, pH>12 for cyanide) ^present? [^ 3 __Weights, dilutions and volunes used to obtain values.

Percent solids calculation present for soils/sediments? [ __ 3 _

Are preparation dates present en Digestion Log? [J£] _XI. 8.2 Mgasuronant r«ad out record praseit? ICP [Q/ } _

Tlame AA [ _ ] _ -V_Furrace AA

Mercurycyanides

STANDARD OPERATDC FRXEDURE Page 7 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: 'HW-2Appendix A.1: Data Assessment - Contract Revision: :oCompliance (Sfctal Review - Inorganics)

__ _ ___

A.1.8.3 Are all raw data to support all sample analyses artiQC operations present?

Legible? • [_Prpperly labeled? [r ]

If no for any of the above, write TelephoneRecord Log and contact laboratory. Flag metaldata as estimated if pH of sanple is greaterthan 2. Flag cyanide data as estimated if pHsanple is less than 12.

A. 1 * 9 PH'Ua Va'*irtaticn and

A. 1.9.1is record of at least 2 point calibrationpresent for 2CP analysis? EX 3Is record of 5 point calibration present forHg analysis?

If no for any of the above, write in theContract FroblavNon-Conpliance section ofthe "Data Assessment Narrative"*

A.1.9.1*2 Is record of 4 point calibration present for:Flame AA? [_]

Furnace AA? K- 3Cyanides? t ot 1

If less than 4 standards are measured in absorbanrenode, then the remaining standards in concentrationmode must be run ijmadiately after calibration andbe within ±10* of true value*For all AA (except Hg) and cyanide analyses, onecalibration standard is at CKX level. If not,write in the Contract-PrdblaVNon-Conpliance sectionof the "Data Assessment Narrative".

CREATING PROCEDURE Page 8 oi 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: *HW-2Appendix A.I: Data Assessnent - Contract Revision: 10Ccrnpliance (itotal Review - Inorganics)

JES

MUffi: Flag associated data as estimated if standardsare not within ±10% of true values (except CTOLcalibration standard)* Do not flag the data asestimated in linear range indicated by goodrecovery of standard.

A. 1.9. 1.3 Is correlation *coefficient less than 0.995 for:Mercury Analysis? _ [V ]

Cyanide Analysis? U/_ 3—— ^T

Atonic Absorption Analysis? _ [y( ]

yes» flag the associated data as estiirated.

A. 1.9. 2 TQTTR II A (Jnitifll 3Ti3 COntiinilTH CfU3l3ri1ti.gi

A. 1.9.2.1 Present and corplete for every metal and cyanide? [

Present and ccrplete for AA and ICP when both areused fof* same analyte? {

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

A.I.9.2.2 Circle all values on data sumary sheet that areoutside contract windows. Are all calibrationstandards (initial and continuing) within controllimits?

Metals 90-110% t.

Hg - 80-120% [

Cyanides 85-115% [

Ine reviewer will calculate correlation coefficient.

STANDARD OPERATING FKOCEXJRE Page 9 of 33

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: HI-;-2Appendix A.I: Data Assessnent - Contract Revision: 10Corpliance (Total Review - InDrganics)

SES IDFlag as estimated (J) all positive data (notflagged with a "U") analyzed between acalibration standard with %R between 75-89%(65-79% for Hg; 70-84% for CU) or 111-125%(121-135% for Hg; 116-130% for W) recovery an3nearest 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% (OS, 70-130%; Hg,65-135%). Qualify five samples on either side ofverification standard out of control limits.

Was continuing calibration performed every 10 samplesor every 2 hours? ,

anZflH: If no, flag the excess samples (eleventh andup) data as estimated (J).

was ICV for cyanides distilled?

ACTIQ'J: If nor write in the Contract-PrQbleWNDn-Corrpliancesection of the "Data Assessnent Narrative".

A. 1.9.3 Form II B CCTTT. fftyriflfflS fpr AA and ICP) —

A. 1.9.3,1 Was a CRDL standard (CRA) analyzed after initialcalibration for all AA metals (except Ho)? I

*Was a mid-range calib* verification standard distilledand analyzed for cyanide analysis? [__]

Was a 2xCTOL ( or 2XIZZ. when IDL>CKDL} analyzed (CRI)for each ICP run? _

s: OU for AL,Ba,Ca,Fe,Mg,Na,or K is not required.)

If no for any of the above, flag as estimatedall data falling within the affected ranges.

affected ranges are:AA Analysis - **ltue Value ± CTCLICP Analysis - **ltue Value * 2OTLCN Analysis - **l*ue Value + 0.5 x True Value.

.* Find the results of mid-range standard in the raw data.value of CRA, CM or mid-range standard. Substitute itL for CRDL when 1DL > CRDL.

SOMCftKD OPERATING HOCEDURE Page 10 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HW-2~Appendix A.1: Data Assessnent - Contract Revision: 10Compliance (TOtal Reviev - inorganics)

A.l.9.3.2 Was oa analyzed after ICV/ICB and before the finalCCV/CCB, and for every four hours of IO> run?

If no, write in Contract. Section of the "Data Assessnent Narrative11.

A. l. 9. 3* 3 Circle all values en sunrary sheet that are outsideacceptance winctows.

Are CRA and Q*I standards within control limits:Metals 80 - 120%R?

Is mid-range standard within control limits:cyanide 80 - 120%R?

ACTION Flag as estimated all data within the affectedranges if the recovery of the standard isbetween 50-79%; flag only positive data ifthe recovery is between 121-150%; reject(red line) all data if the recovery is lessthan 50%; reject only positive data if therecovery is greater than 150%.

A.1,9-4.1 Present and conplete? " ['. !x 3For both AA and ICP when both are used for same analyte? I P( ]

Was an initial calibration blank analyzed? [ 3Was a continuing calibration blank analyzed afterevery 10 «arpl«s or every 2 hours (whichever is morefrequent)? [PCI

2CHSXJ: If no, prepare Telephone Record Log, contactlaboratory and write in the contract-problans/non-ccrpliarce section of the Data AssessmentNarrative.

[_3 _ _

CPEBAUNG TOXEDURE Page 11 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Ntsnber: K*-2Appendix A.1: Data Assessment - Contract Revision: 10Compliance (Tfctal Review - Inorganics)

A.1,9.4.2 Circle all calibration blank values on Data Sumary Sheetthat are above CKCL (or 2 x KL when H2L > CREL), Areall calibration blanks (when zxx.<GROL) less than or equalto Contract Required Detection Limits (CRDL}? I

Are all calibration blanks less than two timesInstnment Detection Limit (when HLX302L)? [_J

ania : If no for any of the above, flag as estijrated (J)all positive data less than or equal tocalibration blank values analyzed betweencalibration blank with value over CRDL (or 2xIDL>and nearest good calibration blank. Flag fivesamples on either side of the calibration blank.

A.I.9.5 FORM in (Preparaticn Blank) -(Note: OJie preparation blank for mercury is the sameas the calibration blank,)

A.I.5.5.1 Was one prep, blank analyzed for: each 20 sanples? Ik<3 __ __

each batch? fc/ 3 _._ _each matrix type? [_] _ gf

\both AA and ICP when both are used for same analyte? I_]

If no for any of the above, flag as estimated (J)all associated positive data <10 x ULs for wnichprep, blank was not analyzed.If cnly one blank was analyzed for morethan 20 sanples, then first 20 sanpies analyzeddo not have to be flagged as estimated (JJ.

A. 1.9.5.2 Is concentration of prep, blank greater than OELwhen nx is less than or equal to CRCL? _If yes, is the concentration of the sanple with theleast concentrated analyte less than 10 times theprep, blank value? _

II SMCftRD CFEPKTI2C ranTFTTURE Page 12 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program . Number: K-;-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Itrtal Review - Inorganics)

aCTKK: If yes, re ject (red-line ) all associated datagreater than O£L concentration tut less than tentines the prep, blank value found in the raw data.

A. 1.9. 5. 3 Do concentrations of prep, blank fall below two timesUX- when m, is greater than CREL? [ _ ]

aOISH: If no, reject (red-line) all positive datathat has a concentration less than 10 timesthe prep, blank value in the raw data.

A. 1.9. 5. 4 Is concentration of prep, blank below the negative GRDL? _

if yes, reject (red-line) all associated datathat has a concentration less than KtoOOJL.

I

A. 1.9. 6 Fonn IV (1CP Interference

A. 1.9. 6.1 Present and conplete? [3/1

(NOTE: Nat required for furnace AA, flame AA, mercury,cyanide and Ca, Mgr K and Na. )

Was ICS analyzed at beginning and end of run /<or,at least twice every 8 hours)? [£\ 3

adlfltJ: If no, flag as estimated (J) all samples foruhich AL, Ca, Fe, or Mg is higher than in ICS.

A.l.8.6.2 Circle all values en Data Sunrary Sheet that are worethan + 20% of true or established mean value. Are allInterference OiecX Sarple results inside of control ,limits (* 2Q\)? . LX.l

If no, is ocncsitnticn of Al, Ca, Pe, or Mg lowerthan in ICS? [__)

if nor 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">.

SR302U82

I s W C f c R D OPERAITOG ITOCEEURE Page 13 Ol 35.-mt*.Title: Evaluation of Metals Data for the Date: Feb. 1990

Contract laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 10Corrpliance (total Review - Inorganics)

ffi

A.l.9.7: Utot required for Ca, Mg, K, arri Na (both matrices) , Al, and Fe

(soil only. )

A. 1.9. 7.1 Present and coipiete for: each 20 sanples? [ __ ]

each matrix type? [ _ ]each cone, range (i.e. low, med. f high)? [ _ ]

Tor both AA and ICP irfien both are used for sameanalyte? [ _ ]

If no for any of the above, flag asestimated (J) all positive data lessthan four times spi)cing level forwiii en spiked sample was not analyzed.

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

A. 1.9. 7. 2 Was field blanX used for spiked sanple? __

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

NOTE: Matrix spike analysis should be performed on afield blank when it is the only aqueous sample in SDG.

A. 1.9*7. 3 Circle mil values en Data Sunnary Sheet that are oitsidecontrol limits (75% to 125%). Are all recoverieswithin centre! limits? _ I _ 3If no, is sarple concentration greater than or equalto four times spike concentration? [ __ ]

If yes, disregard spike recoveries for analytesvhose concent rat icns are greater than or equalto four times spike added. If no, circle thoseanalytes on Form V for vhich sample concentrationis less than four times the spike concentration.

STWCftRD OPERATING JTOCEXJRE Page 14 o: 35

Title: Evaluation of Metals Data for the ' Date: Feb. 1990Contract laboratory Program Number: Hw-2Appendix A.I: Data Assessment - Contract Revision: 10Corpliance (Total Review - Inorganics)

A.I.9.7.5 Soil/SedimentAre any spike recoveries:

(a) less than 10%? _ [_](b) between 10-74%? _ [_]

(c) between 126-200%? __ I__]

<d> greater than 200%? _ [_]If less than 10%, reject all 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 "U"; if greater than 200%,reject all associated data not flagged with a "U".

Are results outside the control limits (75-125%)flagged with "N" en Form I's and Form TO? [_] _ Qf

ACTION: If no, write in the Contract - Fr6blen/Non -Carpliance section of "Data Assessment Narrative".

A.I.9.7.4 SoueoosAre any spike recoveries: ~/

(a) less than 30%? __ [_ J ^

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

(c) between 126-150%? _ [_ J

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

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".

OFE33ATING raDCEXJSE Paae 15 oi 35fI itle: Evaluation of Metals Data for the Date: Feb. 1990

Contract Laboratory Program Number: Kw-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Total Revi&* - inorganics)

1. 1.9.8 TPrrn VT

v.l. 9. 8.1 Present and corplete for: each 20 sanples? { _ ]

difference < +CEDL)? [__]

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

If no, write in the Contract - Problars/Non-Corpliance section of "Data Assessnent Narrative".

MOTE: i. KPD is not calculable for an analyte of thesanple - duplicate pair when both values areless than IEL.

Substitute IEL for CREL when IEL > CRDL.

each matrix type? [__] _ 9\

each concentration range (i.e. low, road., high)? [__] __ y

both AA and ICP \foen both are used for same analyte? [__] _

2CEL3$: If no for any the above, flag as estimated (J)all data >CRDL* for which duplicate sartple wasnot analyzed.

*tote: l. If one duplicate sanple was analyzed fornore than 20 sartples, then first 20 sanples do nothave to be flagged as estimated.2. If percent solids for soil sanple and its duplicatediffer try more than 1%, prepare a Form VI for eachduplicate pair, report concentrations in Hg/Lon wet weight basis and calculate RTO or Differencefor each analyte.

XI.9,8,2 Was field blank used for duplicate analysis? _ [. _]

AcnCMr* if yes, flag all data X3S3L* as estimated(J} for which field blank was used as duplicate.

MOTE: Duplicate analysis should be performed ona field blank when it is the only aqueoussanple in SDG.

A. 1.9.8.3 Jure all values within control limits (RTO 20% or y

OFEEAUNG tMJLUXJRE Page 16 o: 35

Title: Evaluation of Metals Data for the ' Date: Feb. 1990Contract Laboratory Program Number: Hv-2Appendix A.I: Data Assessnent - Contract Revision: 10Coipliance (Itrtal Review - Inorganics)

. . __ .^

2. If lab duplicate result is rejectable dueto coefficient of correlation of MSA,

•w-- analytical spike recovery, or duplicateinjections criteria, do not apply precisiancriteria.

A. 1.9.8,4 Is any value for sanpie duplicate pair less thanOinL* ^and other value greater than or equal to 10 x *CHEL? __ [_ ] '~\

ACTION; If yes, flag the associated data asestimated {J).

A.I.9.8.5 frgueousCircle all values on Data Sunrary Sheet that are:

RPD > 50%, orDifference > * CREL*

Is any RPD greater than 50% where sanpie and duplicateare both greater than or equal to 5 tiroes *CRDL? _ [_ J

Is any **difference between sarrple and duplicate greaterthan *O?DL where sanpie and/or duplicate is less than5 times *CRDL? _ [_ _]

If yes, flag the associated data as estimated.

j A.I.9.8.6 Soil/SediinentCircle all values en Data Sumary Sheet that are:

RTO > 100%, orI - .Difference > 2 x CREL*

Is any FTO (where sanpie and duplicate are bothgreater than or equal to 5 times *CKCL) :

> 100*?

Is any "difference between sanpie ana duplicate(where sanpie and/or duplicate is less than 5x*CKDL)

* Substitute IEL for OREL when HL > CREL.** Use absolute values of sanpie and duplicate to calculate

the difference.

OPERATING FRuumURE Page 17 oi 3s

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: B%-2Appendix A.I: Data Assessment - Contract Revision: 10Ccrnpliance (TOtaJ Review - Inorganics)

if yes, flag the associated data as estiirated.

if yes, flag the associated data as estimated.

A.I. 9*9 Field ZVnlicaties

A.I. 9. 9.1 Were field (placates analyzed? [ __ ] _ _ J<

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

1- Do not calculate RFD when both values areless than IDL.


.1.9.9.2 Js any value for sanple duplicate pair less thanand other value greater than or equal to 10 x *O*DL? _ [_ _ ]

ACTIgJ: If yes, flag the associated data as estineted.

A.I.9.9.3

Circle all values on Form VT for field duplicates that are:RTO > 50%, or

Difference > ± CTOL*

Is any RTO greater than 50% where sanple and duplicateare both greater than or equal to 5 times *CRDL? __ [_ .]

Is any **difference between sarple and duplicate greaterthan *O*DL where sanple and/or duplicate is less than5 time« *CTEL? __ [_ .3

* Substitute IEL for CKX when ITL > OCL.

** Use absolute values of sanple and duplicate to calculate the difference.

flR302U87

STANDARD CFE33ATIN3 PROCEDURE Page 18 c: 35

Title: Evaluation of Metals Data for the Date: Feb. 199-.Contract laboratory Program Number: K.V-Z"Appendix A.I: Data Assessment - Contract Revision: ibCorrpliance (Itftal Reviev - Inorganics)

Circle all values on Form VI for field duplicates that are:RTO >100%, or

Difference > 2 x CTOL*

Is any RTO (where sarrple anc3 delicate are bothgreater than 5 times *O?DL) :

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

>2X *CRDL?

If yes, flag the associated data as estinated.

A. 1.9. 10 Form VIT {JflKratory <TPTTtirPl SPFT g) (Note: LCS - notrequired for aqueous Hg and cyanide analyses.)

A- 1.9. 10.1 Was one LCS prepared and analyzed for:every 20 water sarrples? [fevery 20* solid sairples? [ _ ]

both AA and ICP when both are used for same analyte? [ _ ]

If no for any of the above, prepare TelephoneRecord log and contact laboratory for sutmittalof results of LCS. Flag as estirated (J) alldata for which LCS was not analyzed.

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

EDA.I. 9. 9. 4 goi 1

* Substitute IEL for < L when IEL > CREL.

**Use aJ olute values of sanple and (plicate to calculate the difference.

QPEBATOOG FROOEDU3E Page 19 o: 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HX-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (lotal Review - Inorganics)

A. 1.9. 10. 2 Jtoueous ITSCircle all LCS values outside control limits(80 - 120%- except aqueous Ag and Sb).

Is any LCS recovery: less than 50%? _ La(J _between 50% and 79%? __

between 121% and 150%? _

greater than 1.50%? _

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.

kA.1.9.10.3 Solid LC5

i- 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 IEL of an analyte is equal to or greater thantrue value of LCS, disregard the "Action" belov eventhough LCS is out of control limits.

Is LCS "Found" value higther than the controllijruts on Form VII? __ [_ _]

if yes, qualify all associated positive dataas estimated.Is LCS "Found" value lover than the Controllimits on Form VII? __ [_ J

if yes, qualify all associated data asestimated.

AR3Q2489

SIANEARD OPERATING PROCEIXJHE - " Page 20 c: 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: h>;-2Appendix A.I: Data Assessnerrt - Contract Revision: 10Compliance (Itotal Review - Inorganics)

j*

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

A. 1.9.11-1 Was Serial Dilution analysis performed for: (each 20 samples? ~ [__] ^_ _

each matrix type? [_] _ _ y

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

Arngj: If no for any of-the above, flag all positivedata greater than or equal to lOxIDLs asestimated (J) for which Serial Dilution Analysiswas not performed, and surrmarize the deficiencyon the DPO report.

A.I.9.11.2 Was field blan)c(s) used for Serial Dilution Analysis? _ [__J

If yes, flag all associated data 2 10 x IDLas estimated (J).

Serial dilution analysis should be performedon a field blank when it is the only aqueoussample in SDG.

A-1.9.11.3 Are results outside control lijnit flagged with an "E"on Form I's and Form IX when initial concentration onForm IX is equal to 50 times EX or greater. {_] _

ACTIONS if no, write in the contract-problamAion-compliance section of the "Data AssessmentNarrative".

A.l.9.11.4 Circle all values en Data Sismary Sheet that are outside; control limit for initial Concentrations equal to or greater1 than 10 x TTT-e only. Are any % difference values:

> 10%? __ I_]

2 100%? __ [._]

CFEKAHNG PTOCmUR£ Page 21 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: HV>2~Appendix A.1: Data Assessment - Contract Revision: 10Ccrnpiiance ClbtaJ. Review - Inorganics)

2ESFlag as estimated (J) all associated equalto or greater than lOxIELs for vfcicn percentdifference is greater than 10% but lessthan 100%. Reject (red-line) all associatedsample results equal to or greater thanlOxEXs for which PD is greater than orequal to 100%.

A. 1 . 9 . 12 f JffTTaCg fttTUT fltePTtti0"1 f^Al OC

A.I. 9. 12*1 Are duplicate injections present in furnace raw data(except during full Method of Standard Addition) foreach sample analyzed try GF7A?

fiCIIflB-* If no, reject the data on Form I's for whichduplicate injections were not performed.

A. 1.9. 12. 2 Do the duplicate injection readings agree within 20%Relative Standard Deviation (RSD) or Coefficient ofVariation (CV) for concentration greater than CH3L? [ >J ] _ _ _

Was a di lution analyzed for sample with post digestionspike recovery less than 40%? [ .y ] _ _ X.

Acnac: If no for any of the above, flag all theassociated data as estimated ( J) *

A. 1.9- 12. 3 Is *post digestion spike recovery less than 10% orgreater than 150% for any result?

ACTION If yes, reject (red-line) the affected data ifrecovery is <10%; reject data not flagged with•U" if spite recovery is >150%,

Reject the data only if the affected sample wasnot subsequently analyzed by Method of StandardMdition.

* Post digestion spike is not required en the pre-digestion spiked sample.

SIMTORD CFEBATIN3 FTOCEXJRH Page 22 o: 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: hv;-2Appendix A.I: Data Assessnent - Contract Revision: 10Corpliance (Ttotal Kevi©*/ - Inorganics)

A.I. 9. 13 ytonn VITT fMgtfrod of

A.I.9.13.1 Present?

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

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

XI. 9. 13. 2 Is coefficient of correlation for MS less than 0.990 forany sanple? - __ [1\J

ACTION: If yesr reject (red-line) affected data.

A.I. 9. 13-3 Was *MS required for any sanple but not performed? _

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

Are M calculations outside the linear range of thecalibration curve generated at the beginning of the A,analytical run? _ 1L\ ]

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

A. 1.9. 13, 4 Was proper quantitation procedure follcved correctlyas outlined in the SOW on page E-16 through E-17? [Cxj __

ACTIC13: If no, note exception under contractnon-conpliance of data assessment narrative,or prepare a separate list.

A.I. 9. 14

XI. 9. 14.1 Were any analyses performed for dissolved as well astotal analytes en the same sanple(s). /\f [ _ 3

Were any analyses performed for inorganic as well as total(organic * inorganic) analytes on the same sanple(s)? __

* MSR is not required en l£S and prep, blank.

S3?»NDARD OPERATING mXEOJRE Page 23 cf 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: nl-i"Appendix A.1: Data Assessment - Contract Revision: 10Ccrpliance (Total Review - Inorganics)

}£S - gj-H2ZE: 1. If yes, prepare a list ccnparing differences

between all dissolved (or inorganic) andtotal analytes, Oonpute the differences asa percent of the total analyte only whendissolved concentration is greater than CKDLas well as total concentration.

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

3. At least one preparation blank, 1CS, and ICSshould be analyzed in each analytical run.

A.I.9.14.2 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration byJrore than 10%? _ [_ _] J<

A.1.9.14.3 Is the concentration of any dissolved (or inorganic)anaJyte greater than its total concentration byrore than 50%? _

ACT1CK: If nore than 10%, flag both dissolved (orinorganic) and total values as estijTBted (J);if more than 50%, reject (red-line) the datafor both values.

A.I.9.15 Form I tr> IX

A.I.9.15.1 Are all the Form I through Form IX labeled with:laboratory name? t.°<J

Case/S&S number?

sanple No. ?cnr? No.?

Contract No.? [ __ ] __ °C

Correct units?

Matrix?

If no for any of the above, note undercontract probJeVnon-corpliance sectionof the "Data Assesanent Narrative".

SIWCftRD OPEKATOC TOCEZKJRE Page 24 c: 35

Title: Evaluation of Metals Data for the .Date: Feb. 1990Contract Laboratory Program Number: t£-;-2~Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Ttotal Review - Inorganics}

„ ^——

A. 1.9.15.2 Do any cor utation/transcription errors exceed 10% ofreported values on Forms I-IX for:

(NOTE: deck 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? _

ACTldh If yes, prepare Telephone Log, contactlaboratory for corrected data andcorrect errors with red pencil andinitial.

A.l.9.16 Form 1 (Field l nfr* -

Circle all field blank values on Data Summary Sheetthat are greater than CRDL, 2 x IDL when IDL > CRDL.

Do concentrations of field blank<s> fall below(or 2 x IDL when H3L > O*EL) for all parameters ofassociated aquecus and soil sanples? [__]

If no, was field blank value already rejected due toother QC criteria? [_]

If no, reject (except field blank results)all associated positive sample data lessthan or equal to five times the field blankvalue.

I S T T t f O A R D OPERATING R*XmJ'RE Page 25 of 35^

Title: Evaluation of Metals Data for the Date: Feb. 1990'Contract Laboratory Program Number: K.-;-2*Appendix A.I: Data Assessnent - contract Revision: 10Corrpliance (Itotal Review - Inorganics)

A. 1.9.17 TOTTfi X, XI,, XII (Verif jc

A.I.9.17.1 Is verification report present for:

Instronent Detection Limits (quarterly)?

ICP Interelement Correction Factors (annually)?

ICP Linear Ranges (quarterly)?

If no, contact EffO of the lab.

A.l*9.17.2 Form X (Instrument Detection Limits) - (Note: IDL is notrequired for Cyanide.)

Are TIK..S present for: all the analytes? [ V ]

all the instruments used? [

For both AA and ICP when toth are used for sameanalyte? ' [_]

aCUCE: If no for any of the above, prepareTelepixme Record Log and contactlaboratory.

Is HZ. greater than OtCL for any analyte? _

If yes, is the concentration on Form I of the sampleanalyzed on the instrument whose IEL exceeds CRDL,greater than 5 x IEL? {__J

If no, flag as estimated all valuesless than five times IEL of the instilmentwhose IEL exceeds CRDL.

OPERATING FRXHXJRE Page 26 of 33

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: K«-2Appendix A.I: Data Assessment - Contract Revision: 10Ccnpliance (Tttal Review - Inorganics)

. - . —;_ _

A. 1.9.17.3 Form XI (Linear Ranges)

Was any sanple 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, vas thesample diluted to obtain the result on Form I? [>A] _ _

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

Is soil content in sediinent(s) less than 50%? t ]— —If yes, qualify as estineted all datanot previously rejected or flagged dueto other QC criteria.


CASE NO. In 6 OK _____________ SITELABORATORY S ggJovi ^mu.ILL NO. OF SAMPLES/

MATRIX ^ *

6. DUPLICATE ANALYSIS & ___^ O

O « Data had no problems/or qualified due to minor problems.M - Data qualified due to major problems.Z « Data unacceptable.X « Problems, but do not affect data.

ACTION ITEMS: ________________________________

AgEASjJF CONCERN: &£> «s

"Tli/ K'kci/

(Af 2 t~>~?__________________ REVIEWER (IF NOT ESD) ___

SOW*_____7 7________________ REVIEWER'S NAME J J&#.j'be* sDPO: ACTION _____ FYI X______ COMPLETION DATE /-JV -y


ICP AA Hg CYANIDE

1. HOLDING TIMES ^ & & CJ

2. CALIBRATIONS . V ___/ & ' ~ &

3. BLANKS ^ ^ ^ ^

4. ICS *' _

5. LCS , /:' O

7. MATRIX SPIKE O O Q Q

8. MSA O

9. SERIAL DILUTION (J

10. SAMPLE VERIFICATION Q O~" -~~& >?

11. OTHER QC Q O Q _<?_

12. OVERALL ASSESSMENT O O £> ^


II


AR302500

STANDARD CHLORINE8DG ICLP360


The laboratory's portion of SDG #CLP360 consisted of six watersamples analyzed for TAL metals by Roy F. Weston, Inc.



Minor Issues —

The matrix spike percent recoveries for As, Se, and Tl were belowthe CLP control limits. All associated sample results arequalified as estimated and are considered to be biased low.

The duplicate digestion relative percent difference (RPD) for Feand 2n were above the CLP control limits. All associated sampleresults are qualified as estimated.

The serial dilution percent differences for Ca, Fe, Mn, and Na wereabove the CLP control limits. All associated sample results arequalified as estimated.

The post matrix spike percent recoveries for Pb were above the CLPcontrol limits. All associated sample results are qualified asestimated and are considered to be biased high.

The post-digestion spike percent recoveries for Se and Tl werebelow the CLP control limits. All associated sample results arequalified as estimated and are considered to be biased low.

r-n t

TABLE I

Sample # Analvte +DL -QL Comments

Se, Tl UJ 1Fe, Zn J UJ 2

Ca, Fe, Mn, Na J — 39008L360039008L36007 Pb J UJ 5

All samples Se UJ 49008L360002 Tl UJ 4

1. Due to a low matrix spike percent recovery indicating alaboratory or matrix spike problem, all associated sampleresults are qualified as estimated and considered to be biasedlow. ^

2. Due to a duplicate digestion outside of the CLP control flimits, all associated sample results are " qualified asestimated.

3. Due, to a high serial dilution percent difference, allassociated sample results are qualified as estimated.


5. Due to a high post-digestion percent recovery, all associatedsample results are qualified as estimated and are consideredto be biased high.

Note;


Information Regarding Report Contest


Inorganic Attachments .__.._-.




4. Appendix B - DPO Report - This addresses laboratory complianceissues with' respect to the statement of work.


I1I

ATTACHMENT IGLOSSARY OF DATA QUALIFIERS

1GLOSSARY OF DATA QUALIFIERS



0 = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELf REPORTED IN LABORATORY OR FIELD BLANKS.

R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.



CODES RELATING TO QUANTITATION



L . = ANALYTE PRESENT. REPORTED VALUE MAY BEBIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.

UJ = * - THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.

0L = NOT DETECTED. QUANTITATION LIMIT MAY BEHIGHER.

OTHER CODES


I1I


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ICFEBA3TOG J*OOEUR£ Page 7 of 35

Title: Evaluation of Metals Data for the Date: Feb 1990'Contract Laboratory Program Number: 'HW-ZAppendix A.I: Data Assessnent - Contract . Revision: aoCtirpliance (Ttrtal Review - Inorganics)

t£) N/A

A. 1.8. 3 Are all raw data to support all sanple analyses ardQC operations present? [. ]

- [ X ]

Properly labeled? [j( ]

If no for anyjof the above, write telephoneRecord Log and contact" laboratory/ >iag metaldata as estimated if pH of sanple is greaterthan 2. Flag cyanide data as estimated if pHsanple is less than 12.

A. 1.9 Data Vaiirtatjcn and

A. 1.9-1 naii brat ion

A. 1.9.1.1 Is record of at least 2 point calibrationpresent for ICP analysis? ['X 3

Is record of 5 point calibration present forHg analysis? [ y ]

If no for any of the above, write in theContract ProblenvNon-Ccrpliance section ofthe •'Data Assessnent Narrative".

Furnace AA? [ Vl __

Cyanides?1 less than 4 standards are measured in absorbancenode, th@i the remaining standards in concent-rationmode nust be run inrnediately after calibration andbe" within ±10* of "true value.For all AA (except Hg) and Cyanide analyses, onecalibration standard is at CKEL level, if not,write in the COTtract-PrbblerVIton-Ccnpliance sectionof the "Data Assessnent Narrative".

AR3025.I2

OPERATING FKXZDURE Page 8 OJ 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HW-2Appendix A.1: Data Assessment - Contract Revision: 10Compliance (TOtal Review - Inorganics)

IE W ELS

Flag associated data as estimated if standardsare not within +10% of true values (except CKDLcalibration standard). Do not flag the data asestimated in linear range indicated by goodrecovery of standard.

A. 1.9.1.3 Js correlation coefficient less than 0.995 for:

Mercury Analysis? __ [_*0 _

Cyanide Analysis? __ [_ '3 _

Atonic Absorption Analysis? _ [ ] _

: If yes, flag the associated data as estiirated.

A. 1.9. 2 Fprm II A (IfUtifll iffti CcritJJuJpgT Cr*l JlTratiro Verificaticn)-

.1.9.2.1 Present and ccrplete for every metal and cyanide? [c/ ]•

Present and ccrpiete for AA and ICP ien both areused for same analyte? [ __ ]

ACTT QN: if no for any of the above, prepare TelephoneRecord Log and contact laboratory.

A.l.9.2.2 Circle all values on data sistmary sheet that areoutside contract winders. Are all calibrationstandards (initial and continuing) within controllijnits?

Metals 90-110% IX }Hg - 80-120% f X ]

qyanides 85-115% [ V]

Ine reviewer will calculate correlation coefficient.

flR3025{3

OFERATIN3 PROCEDURE Page 9 Of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: Hi-;-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Total Review - Inorganics)

Flag as estimated (J) all positive data (notflagged with a "IT) analyzed between acalibration standard with %R between 75-89%(65-79% for Hg; 70-84% for OJ) or 111-125%(121-135% for Hg; 116-130% for CN) recovery andnearest good calibration standard. Qualify results<IUL 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 orOCV is outside the range 75-125% (O*, 70-130%; Hg,65-135%). Qualify five samples on either side ofverification standard out of control limits.

Was continuing calibration performed every 10 samplesor every 2 hours? [_X ]

ACTIQC: If no, flag the excess samples (eleventh andup) data as estimated (J).

Was ICV for cyanides distilled? [ _ J

If no, write in the Contract-Problem/Non-Corpliancesection of the "Data Assessnent Narrative".

A. 1.9. 3 florin II B (OCTf p*y»r*fc|rtte fOT AA and

A. 1.9. 3.1 Was a CRDL standard (CKA) analyzed after initialcalibration for all AA metals (except Ha)?

*Was a nud-range calib. verification standard distilledand analyzed for cyanide analysis? [ __ ]

Was a 2xCRDL ( or 2x771. vftien IELX35EL) analyzed (Qtt) ,for each JCT run? C_] _ —(NDte: GRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.)

ACTION if no for any of the above, flag as estiratedall data falling within the affected ranges.The affected ranges are:AA Analysis - **ltue Value ± PELICP Analysis - **ltue Value + 2CRCLW Analysis - **Itue Value + 0.5 x Itue Value.

Tina the results of mid-range standard in the raw data.*True value of ORA, CRI or mid-range standard. Substitute IEL for CRDL when IDL > CRDL.

4R3025.lt

CFESAUNG TOXEDURE Page 10 of 35

Title: Evaluation of Metals Data for the Date: Feb 1990Contract Laboratory Program Number: "wc-i"Appendix A.1: Data Assessnent - Contract Revision: 10Osrpliance (I&tal Review - inorganics)

3ES IDA. 1.9.3.2 Was CRI analyzed after ICV/ICB and before the final

CCV/CCT, and for every four hours of ICP run?

If no, vrite in ContractSection of the "Data Assessnent Narrative11.

.l. 9*3.3 Circle all values en sutmaiy Sheet that are outsideacceptance

Are CSA and OS standards within control lijnits:Metals 80 - 120%R? [__]

is mid-range standard within control limits:__. _ Cyanide 80 - 120%R? [_]

ACTION: Flag as estijiated all data within the affectedranges if the recovery of the standard isbetween 50-79%; flag only positive data ifthe recovery is between 121-150%; reject<r©d line) all data if the recovery is lessthan 50%; reject only positive data if therecovery is greater than 150%.

A.I.9-4 Form III (Initial and OontiTnina Calibration Blanlcsl

A.I.9.4.1 Present and ccnplete? I.X.]

For toth AA and ICP when both are used for same analyte? [ __ ] _ V

Was an initial calitoaticn blsnfc analyzed? [X ] __ _

Was a continuing calibration blank analyzed afterevery 10 swples or every 2 tours (whichever is more

ACTION; If no, prepare Ttel hone Record Log, contactlaboratory and write in the contract-problems/ncn-corpliance section of the Data AssessmentNarrative.

AR3025I5

OPERATING PROCEDURE Page 11 of 35

Title: Evaluation of Metals Data for the Date; Feb. 1990Contract Laboratory Program Nurriber: Hw-2jpendix A.1: Data Assessnent - Contract Revision: 10Compliance (2t>tal Review - Inorganics)

_ _ _ _ _

A. 1.9.4.2 Circle all calibration blank values en Data Surrary Sheetthat are above O£L (or 2 x m when HfL > Ott). Areall calibration blanks (when IEL<aS2L) less than or equalto Contract Required Detection Limits (OREL)? { XJ _ _

Are all calibration blanks less than tw timesInstrument Detection Limit (when TDLXTOL)? [__] _

ACHfltf: If no for any of the above, flag as estinated (J)all positive data less than or equal tocalibration blank values analyzed betweencalibration blank with value over CRDL (or 2xlDL)and nearest good calibration blank. Flag fivesanples on either side of the calibration blank.

A.l.9.5 FraM yil (Praaaratian Bl nk) -

(Note: !rte preparation blank for mercury is the sameas the calibration blank.)

A.I.9.5.1 Was one prep, blank analyzed for: each 20 sanpies? [ X'3 ___

.. . -- - •""" " each batch? I__] _._

each matrix type? [_] _ .xx

both AA and ICP when both are used for same analyte? [_] _ V

If no for any of the above, flag as estimated (J)all associated positive data <10 x IDCs for whichprep, blank was not analyzed.if only one blank was analyzed for morethan 20 sarrples/ then first 20 sanples analyzeddo not have to be flagged as estimated (J).

A. 1.9.5.2 Is concentration of prep, blank greater than OELwhen IDL is less than or equal to CREL? _If yes, is the concentration of the sairple with theleast concentrated analyte less than 10 times theprep, blank value? __

/5R3025/6

GRIKATING Hfl I >1 URE Page 12 of 35

Title; Evaluation of Metals Data for the _ Date: Feb. 1990Contract laboratory Program . Number: H-:-2Appendix A.1: Data Assessment - Contract Revision: 10Compliance (Ttotal Review - Inorganics)

reject (red-line) all associated datagreater than CRDL concentration but less than tentimes the prep, blank value found in the raw data.

A.l.9.5.3 Do concentrations of prep, blank fall below two timesIEL when HH- is greater than CRX? [_ ]

&313?: If no, reject (red-line) all positive datathat has a concentration less than 10 timesthe prep, blank value in the raw data.

A.I.9.5.4 Is concentraticn of prep, blank below the negative CREL? _ [_] _

acnoa: If yes, reject (red-line) all associated datathat has a concentration less than lOxCRDL.

A.I.9.6.1 Present and corplete? [ y/ ] __

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

Was ICS analyzed at beginning and end of run(or at least twice every 8 hours)? [ X] _ _ACTION If no, flag as estimated (J) all samples for

vhich ALff Ca, Fe, or Mg is higher than in ICS.

A.1.8.6.2 Circle all valxies on Data Satwary Sheet that are morethan •*• 20\ of true or established mean value. Are allInterference Greek Sarple results inside of controllimits <+ 2Q\}? C^J _

If no, is concentration of Al, Cat Fef or Mg lowerthan in ICS? [ _ 1

if no, flag as estiiiatad (J) those positiveresults for which ICS recovery is between 121-150%;flag all sanple results as estimated if ICSrecovery falls within 50-79X; 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").

AR3025I7

SlfcNBftRD GYRATING JKXHXJRE Page 13 Ot 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number; HW-2Appendix A.I: Data Assessment - Contract Kevision: 10Compliance (Itotal Review - Inorganics)

JOES ffi

( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe(soil only.)

A.I.9.7.1 Present and raipiete for: each 20 samples? [ > ] __

each matrix type? [_] __

each cone, range (i.e. lov, med., high)? [_] __ w

For both AA and ICP when both are used for sameanalyte? [__3

If no for any of the above, flag asestimated (J) all positive data lessthan four tunes spiking level forwhich spiked sample was not analyzed.

If one spiked sample was analyzed for morethan 20 sanpies, then first 20 sarrpiesanalyzed do not have to be flagged as

- • estimated (JK

A. 1.9.7.2 Was field blank used for spiked sanple? _

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

Matrix spite analysis should be perfonned on afield blank when it is the only aqueous sample in SDG,

A.l.9.7.3 Circle all values on Data Surmary Sheet that are outsidecontrol limits (75% to 125%). Are all recoveries

. within control limits? I_]If no, is sarple concentration greater than or equalto four times spike concentration? t__]

If yesr disregard spiJce recoveries for analytesvhose concentrations are greater than or equalto four times spike added. If no, circle thoseanalytes en Form V for which sample concentrationis less than four times the spike concentration.

OPERATING fWXHXJRE Page 14 o: 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HK-2Appendix A.I: Data Assessment - Contract Revision: 10Corpliance (ItJtal Review - Inorganics)

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

ACTKU; If no,"write in the Contract - Prbblen/Non -Ocrpliance section of "Data Assessnent Narrative*1.

A.l.9.7.4 ftoueousAre any spike recoveries:

(a) less than 30%?

(b) between 30-74%?

(c) between 126-150%?

<d) greater than 150%? ,X [__]

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

A.I. 9, 7. 5Are any spiXe recoveries:

(a) less than 10%? _ [ _ ](b) between 10-74%? __ [ _ ]

(c) between 126-200%? _ [ _ ] X

(d) greater than 200%? _ [ _ 1If less than 10%, reject all associated data; if

between 10-74% p 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".

flR3025j9

OFSSCTOC PROCEDURE " -"- Page 15 02 35

Evaluation of Metals Data for the . Date: Feb. I9?jContract laboratory Program Number: K>--2

t ^ appendix A.I: Data Assessrent - Contract Revision: 10j compliance (Ifctal Review - Inorganics)

a11 data >CK3L* as estimated(J) for which field blank was used as duplicate.

Duplicate analysis should be performed ona field blank when it is the only aqueoussairple in SDG.

A. 1.9. 8.3 Are all values vithin ccntrol lijnits (RPD 20% ordifference < iOSL)? I __ ]

If no, are all results ootsi<te the control limitsflagged %dth an * on Form l«s and VI?tcnSBi If no, write in the contract - Problems/Nan-

Ccnpliance section of "Data Assessnent Narrative*.

MOTE* i. RTO is not calculable for an analyte of thesanple - duplicate pair when both values areless than IEL.

* Substitute IEL for CKDL when TOL >

IB IL2>.1.9.8 ytem VT (Mft T*g*lieat*»gl

.1.9.8.1 Present and corplete for: each 20 sanples? [X ] __ _ .

each matrix type? [ __ ] _ y>

©adh concentration range (i.e. low, mad., high)? [ __ ] _ ±'_.

both AA and ICP \faen both are used for same analyte? [ _ ]

If no for any the above, flag as estimated (J)all data >o*DL* for which duplicate sairple wasnot analyzed.1- If one duplicate sanple was analyzed forirore than 20 sanples, then first 20 samples 60 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 Hg/Lon wet weight basis and calculate PTO or Differencefor each analyte.

A.l.9.8.2 Was field blanX used for duplicate analysis? _

flR302520

OPESA31N3 ITOCEDURE Page 16 o: 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: H«-2Appendix A.I: Data Assessment - Contract Revision: 10Ccrpliance (Itrtal Reviev - Inorganics)

If yes, flag the associated data as estajrated.

A.I, 9. 8. 6 Soil/SedijnentCircle all values en Data Sumary Sheet that are:

RTO > 100%, or

Difference > 2 x

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

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

* Substitute irL for O*EL when 3TL > OCL.** Use absolute values of sanple and duplicate to calculate

the difference-

ffiS MD

2. If lab duplicate result is rejectable dueto coefficient of correlation of MS ,analytical spike recovery, or duplicateinjections criteria, do not apply precisioncriteria.

A. 1,9. 8, 4 Is any value for sample duplicate pair less than CRDL*and other value greater than or equal to 10 x *CRDL? __

Hfift: If yes, flag the associated data asestimated (J).

A.I, 9. 8. 5 AqueousCircle all values on Data Summary Sheet that are:

RPD > 50%, orDifference > ± OREL*

Is any RTO greater than 50% where sample andduplicate .are both greater than or equal to 5 times *CRDL? [ A ]__ V

Is any **difference between sanple anc3 duplicate greaterthan *CKDL where sanple and/or duplicate is less than5 times *CRDL? __

> 100%? __ I__]

[ _.] _}

•RR3025Z1

S3WTORD CFEKAUNG FTOCEDURE Page 17 oi 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: hV.'-2Appendix A.I: Data Assessm it - Contract Revision: 10Ccrpliance (TtJtal Review - Inorganics)

. . . : - " JESS I DIf yes, flag the associated data as estimated.

A.I. 9. 9.1 Were field duplicates analyzed? [ _ J _ _

2d2?: If yes, prepare a Form VI for each aqueous fieldduplicate pair. Prepare a Form 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 each -analyte.

H2IE: 1- ED not calculate PPD when both values areless than IDL.


!A.l.9.9.2 Is any value for sample duplicate pair less than *OTXand other value greater than or equal to 10 x *CRDL? __ [_

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

A.I. 9. 9. 3 Aqueous

Circle all values on Form VT for field duplicates that are:RPD > 50%, or

Difference > ± C3S3L*

Is any RPD greater than 50% where sample and duplicateare both greater than or equal to 5 tunes *CRDL? __ l_ .] ^

Is any **difference between sample and duplicate greaterthan *OQX where sample and/or duplicate is less than5 times *CRCL? __ [_ J :~

If yesf flag the associated data as estiirated.

* Substitute HX for CPQL when IEL > O7EL.

** Use absolute values of sample and duplicate to calculate the difference.

BR302522

STANDARD OrasSHJG FTOCHX3RE Page 18 c: 35

Title: Evaluation of Metals Data for the Date: Feb. 199-'Contract laboratory Program Number: h"-;-z"Appendix A.I: Data Assessnent - Contract . Revision: 10Corpliance (Stotal Review - Inorganics)

fiA. 1.9. 9. 4

Circle all values en Form VI for field (Implicates that are:RTO >100%, or

Difference > 2 x CREEL*

Is any RTO (where sarrple and duplicate are bothgreater than 5 tires *CTOL) :

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

>2x

If yes, flag the associated data as estiinated.

A. 1.9.10 Fbrm VTT (T Tr?ratprv CfrrftJPl SfTPie) (Note: LCS - notrequired for aqueous Hg and cyanide analyses.)

A.I,9.10.1 Was cine LCS prepared and analyzed for:every 20 water sanples? [ >A. " * ~"every 20* solid sanples? [_]

both AA and IO* when both are used for same analyte? [_] _ _ V

If no for any of the above, prepare TelephoneRecord Log and contact laboratory for sumittalof results of LCS. Flag as estimated (J) alldata for which LCS was not analyzed.

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

* Substitute TDL for OREL when HL >

"Use absolute values of sample and duplicate to calculate the difference.

flR302523

QFEEATBrj PR l H*JR£ Page 19 01 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program . Number: HX-i"Appendix A.I: Data Assessment * Contract Revision: 10Coipliance (total Review - Inorganics)

A. 1.9. 10. 2Circle all LCS values outside control limits(80 - 120%- except aqueous Ag and Sb).

Is any LCS recovery: less than 50%?



greater than 150%?

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

fA.l.9.10.3 Solid LCS

i. if "Found" value of LCS is rejectable due to duplicateinjections or analytical spiXe recovery criteria,regardless of LCS recovery, flag the associated dataas estiiTBted (J).

2. If inL of an analyte is equal to or greater thantrue value of LCS, disregard the " tian" 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 estijnated.Is LCS "Found" value lower than the Controllimits en Form VII? __ I_ J

if yes r qualify all associated data asestimated.

OPERATING FRQC3X3HE Page 20 c; 35

Title: Evaluation of Metals Data for the Date: Feb. 199.-Contract Laboratory Program Number: h>;-2~Appendix A.I: Data Assessnent - Contract Revision: 10appliance (3btal Review - Inorganics)

2ES £& K/R

A.I.9.11 ltonn.JX flg> Serial

If no, write in the contract-problan/non-conpliance section of the "Data AssessmentNarrative".

&.1.9.11.4 Circle all values on Data SunrBry Sheet that are outsidecontrol limit for initial Concentrations equal to or greaterthan lO^t TTTje cnly. Are any % difference values:

100%?

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

A.l.9.11.1 Was Serial Dilution analysis perfonred for: ^each 20 samples? [LA ]each matrix type? I_]

each concentration range (i.e. low, med.)? [_] __ ^\-

ACTICK: If no for any of the above, flag all positivedata greater than or equal to lOxIDLs asestimated (J) fcr which Serial Dilution Analysiswas not performed, and summarize the deficiencyon the DPO report.

A. 1.9.11.2 Was field blank(s) used for Serial Dilution Analysis? _

ACT!OS; If yes, flag all associated data 2 10 x IDLas estimated (J),

M2ZE: Serial dilution analysis should be performedon a field blank when it is the only aqueoussanple in SDG.

A.I.9,11.3 Are results outside control lijnit flagged with an "E"on Form Ifs and Form IX when initial concentration on ,Form IX is equal to 50 times IDL or greater. .V ]

flR302525

OPERATING fTOCEIXJRE Page 21 of 35

Title: Evaluation of Metals Data for the Date; Feb. 190-,Contract Laboratory Program ' Number: H.v-2*-Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Ifctal Review - Inorganics)

Flag as estimated (J) all associated equal•to or greater than lOxIDLs for which percentdifference is greater than 10% but lessthan 100%. Reject (red-line) all associatedsample results equal to or greater thanlOxHE-s for which FD is greater than orequal to 100%.

A. 1 . 9 . 12 FurnQC? ?\fJU7 flfaTfrrfrEi i (AA) Op

A. 1.9. 12.1 Are duplicate injections present in furnace raw data(except during full Method of Standard Mdition) foreach sample analyzed £y GFAA? [X ]

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

A. 1.9. 12. 2 Do the delicate injection readings agree within 20%Relative Standard Deviation (RSD) or Coefficient of *Variation (CV) for concentration greater than CRDL? [DC 1

Was a dilxition analyzed for sample with post digestion yspike recovery less than 40%? [ A]

?SCTICM; If no for any of the above, flag all theassociated data as estimated (J).

A.l.9.12.3 Is *post digestion spike recovery less than 10% orgreater than 150% for arry result? _

ArncM: if yes, reject <red-line) the affected data ifrecovery is <10%; reject data not flagged with•U" if spike recovery is >150%.

fflffi: Reject the data only if the affected sample wasnot subsequently analyzed by Method of StandardAddition.

* Post digestion spike is not required en the pre-digestion spiked sample.

AR302526

SIANEftRD OPEKATHC FTOCEDURE Page 22 o: 35

Title: Evaluation of Metals Data for the . - Date: Feb. 1990Contract Laboratory Program Number: *hv-2Appendix A.I: Data Assessment - Contract _ Revision: 10Compliance (Ttotal Review - Inorganics)

If y*3* write request on Teleptane Record Logand contact laboratory for sutmittal of Form VIII.

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

A.l.9.13.4 Was proper quantitation procedure followed correctlyas outlined in the SOW on page E-16 through £-17?

ACTION If no, note exception under contract prdblan/nan-carpi iance of data assessnent narrative,or prepare a separate list*

A.I. 9. 14

* KSA is not required en LCS and prep, blank.

AR302527

A.I. 9. 13 Yttnn VTTT (Method of Stanrfar*

A.i. 9.13.1 Present?-If no, is any Form I result coded with "S" or a "•«•"? _ [_ ]

, 1.9. 13. 2 Is coefficient of correlation for M less than 0.990 forany sanple? . _ 1=20 _


A. 1.9. 13. 3 Was *WSA required for any sanple but not perforred? __ [_V ] _

Is coefficient of correlation for MS less than 0.995? _

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

A. 1.9. 14.1 Were any analyses performed for dissolved as well astotal analytes en the same sairplets). x I _ ]Were any analyses performed for inorganic as well as total{organic + inorganic) analytes en the same sanple(s)? __

OPERATING raOO-ZXJRE Pace 23 cf 25

Title: Evaluation of Metals Data for the - Date: Feb. 199--Contract Laboratory Program Number: H>;-i"Appendix A.I: Data Assessment - Contract Revision: 10Ccrpliance (Dotal Review - Inorganics)

H3IE: 1. If yes, prepare a list ccrparing differencesbetween all dissolved (or inorganic) andtotal analytes, Compute the differences asa percent of the total analyte only whendissolved concentration is greater than O*DLas 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 ICSshould be analyzed in each analytical run.

A.l.9.14.2 Is tne concentration of any dissolved (or inorganic)analyte greater than its total concentration bymore than 10%? • __

A.I.S. 14.3 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration bymore than 50%? _ [JXj

&CH£L3: If more than 10%, flag both dissolved (orinorganic) and total values as estiirated (J);if more than 50%, reject (red-line) the datafor both values.

A. 1.9.15 Ftorm I to DC

A.I.9.15.1 Are all the Form I tJirough Form IX labeled with: .Laboratory name? IX ] _ _

Case/SAS number? fEPA sample No.?

SDG NX? EX]

Contract No.? [ __ ]

Correct units? l&( ]

Matrix?

If no for any of the above, note undercontract problsVhon-corpliance sectionof the "Data Assessnent Narrative".

AR302528

SIWCftRD OPERATING iVUGJJURE Page 24 o: 35

Title: Evaluation of Metals Data for the Date: Feb. 199:Contract Laboratory Program Number: K-;-2

I A p p e r K i i x A.I: Data Assessnent - Contract Revision: 10Corpliance (total Review - Inorganics)

2LS

A.I.9,15.2 Do any corputation/transcription errors exceed 10% ofreported values en Forms I-IX for:


(a) all analytes analyzed by IO>? __

(b) all analytes analyzed by GFAA? _

(c) all analytes analyzed by 7A Flame? _ t__] j/

(d) Mercury? _

<e) Cyanide? __

If yes, prepare Telephone Log, contactlaboratory for corrected data andcorrect errors with red pencil anainitial.

A.l.9.16 Form T (Fii

Circle all field blank values on Data Surrrary Sheetthat are greater than CRnL, 2 x IDL when HJL > OiliL.

Do concentrations of field blank(s) fall belcw CTOL(or 2 x IEL when ICL > CRCL) for all parameters ofassociated aguecus and soil ssnples?

If no, was field blank value already rejected doe toother QC criteria?

if no, reject (except field blank results)all associated positive sanpie data lessthan or equal to five times the field blankvalue.

flR302529

i• STATOARD OPEJ&TING FBQCHXJRE Page 25 of 33

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: Kl-;-2"Appendix A.I: Data Assessment - Contract Revision: 10Corrpliance (TtotaJ. Review - Inorganics)

A.I.9.17 Ffrrm X. XI,.XII (Verification of Instjunental Rarangters).

A.I.9.17.1 Is verification report present for:

Instrument Detection Limits (quarterly)? [X ]

ICP Interelanent Correction Factors (annually)?

ICP Linear Ranges (quarterly)?

ACTICU: If no, contact DFO of the lab.

A. 1.9.17.2 form X (Instrument Detection Limits) - (Note: IDL is notrequired for cyanide.)

Are TT7T.S present for: all the anaiytes? [,

all the instruments used? [.

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

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

Is IDL greater than CKL for any analyte? _ [A. J

If yes, is the concentration on Form I of the sanpleanalyzed on the instrument whose UL, exceeds CRDL,greater than 5 x IEL? [__] __

If no, flag as estimated all valuesless than five tires EX of the instrumentvtx>se IEL exceeds


Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: HW-ZAppendix A.I: Data Assessment - Contract Revision: 10Compliance (Ttotal Review - Inorganics)

2S5 ffiA. 1.9.17.3 Form XI (Lir r pgnaes)

was any sample result higher than high linear rangeof ICP.Was any sample result higher than the highestcalibration standard for non-IOP parameters? __ [ y"

If yes for any of the above, was the ^sample diluted to obtain the result on Form I? [_] _

'SCXlSfti If no, flag the result reported on Form Ias estimated(J). '

A-l.9.18 p&rcgrt Solids Of

Is soil content in sedijnent{s) less than 50%? _ [_ ] ,

If yes, qualify as estimated all datanot previously rejected or flagged dueto other QC criteria.

BR30ZS31


AR302532

I INORGANIC REGIONAL DATA ASSESSMENT

CtiCASE NO. _________ SITELABORATORY ( >£VfT'Vi - L/i <LnS\ > ', lit

sow* 7DPO: ACTION v FYI X

NO. OF SAMPLES/MATRIX ' ff , *t>v >REVIEWER (IF NOT ESD)

REVIEWER'S NAME 2^. rv/_fr&-UCOMPLETION DATE -<a — _ -^ / -13S -fif

DATA ASSESSMENT SUMMARY4,

i . HOLDING TIMES

2. CALIBRATIONS3. BLANKS

4, ICS

5. LCS

6. DUPLICATE ANALYSIS

7. MATRIX SPIKE

8. MS A

9. SERIAL DILUTION

10. SAMPLE VERIFICATION

11. OTHER QC

12. OVERALL ASSESSMENT

O ~ Data had no problems/or qualified dueM « Data qualified due to major problems.Z * Data unacceptable.X * Problems, but do not affect data.

ACTION ITEMS:

ICP AA Hg CYANIDE

rl O {) 00 O 0 . o0 0 0: 0O0 o0 O O o0 0 D o

n0o - r-r r> o0 0 C: 0n o o o

to minor problems.

AREAS OF CONCERN:ff-v ^•*" t-

,


flR302533

If


RR30253U


RR302535

I

VOLATILE, SEMIVOLATILE, PESTICIDE/PCBAND METALS ANALYSES

COLUMBIAMONITOR WELL TW-6A

STANDARD CHIORINECASE 9008L360

This quality assurance review is based upon a review of the datagenerated from four water samples collected on 08/10/90 andanalyzed by Roy F. Weston, Inc. for TCL Volatile and special listSemivolatile, and Pesticide/PCB target compounds.



RR302537



I. Volatiles

___ Holding TimeX Surrogate Recovery_X_ MS/MSD_JC_ Blank___ GC/MS TuningX Initial CalibrationX Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness

OVERVIEW

This portion of the case consisted of four water samples receivedat Roy F. Weston, Inc. on 08/10/90. The samples were analyzed forTCL Volatile target compounds. Problems associated with the sampleanalyses are listed below.

ISSUES

The method blank contained common contaminant methylene chloride ata level less than 5x the CRQL. The associated samples containedthe same compound at levels less than lOx the blank level.Therefore, the sample results are considered laboratory artifacts,and are flagged "U" in the data summary.

Sample GW 22-0-1 TW6A had the toluene and bromofluorobenzenesurrogate recoveries below the EPA CLP QC limits. The sample wasalso analyzed as a matrix spike/spike duplicate and similar resultswere obtained. The sample is exhibiting a matrix effect. Allpositive results and quantitation limits are qualified estimatedand flagged "J" and "UJ".

Several compounds had %RSD and/or %D exceed the 30% and 25% EPA CLPQC criteria in the initial and continuing calibrations. Allpositive results and quantitation limits are qualified estimated.

1R302538


The %RPD for chlorobenzene exceeded the spike recovery QC limit forsample GW 22-0-1 TW6A. This was detected at a high level in theoriginal sample analysis and since spike recoveries have advisorylimits, no qualification is applied.

Samples GW 22-0-1 TW6A MS/MSD and GW 22-1-1 TW6A required 200-folddilutions due to high levels of target and non-target compounds.The data usability is not affected, no qualification is applied.

Dichlorobenzene isomers were detected as tentatively identifiedcompounds in several samples. These compounds are on thesemivolatile TCL list and should not be reported as a TIC on thevolatile list.

BR302539



II. Base/Neutral/Acids

___ Holding Time___ Extraction Time___ Surrogate Recovery_J£_ BlankX MS/MSD___ GC/MS TuningX Initial CalibrationX Continuing Calibration

Compound ID (HSL, TIC)JC_ Standards___ Spectra Quality__ Chromatpgraphy___ Data Completeness

1 OVERVIEW

This portion of the case consisted of three water samples. The1 samples were analyzed for TCL Semivolatile and special list target

compounds. Problems associated with the sample analyses are listedin the following section.

! ISSUES

The chrysene and perylene internal standards were below QC limitsfor samples GW 22-0-1 TW6AMS, GW 22-0-1 TW6AMSD, and GW 22-1-1TW6A. The QC samples are exhibiting a matrix effect. Sample GW22-1-1 TW6A was reanalyzed but not reported; therefore, thecompound results quantified with these standards are qualifiedestimated.

Several compounds had %RSD and/or %D exceed the 30% and 25% QClimits in the initial and continuing calibrations. The associatedquantitation limits are qualified estimated.

Samples GW 22-0-1 TW6AMS/MSD and GW 22-1-1 TW6A required 200-folddilutions because they contained high levels of target compounds.The surrogate and spike recoveries were diluted out. The datausability is not affected and no qualification is applied.


All blank spike recoveries were within EPA CLP QC criteria.However the %RPD for pentatchlorophenol exceeded the QC criteria.-This compound was not detected in the sample analyses and spikerecoveries have advisory limits. Therefore, the data usability isnot affected and no qualification is applied.

The method blank contained common contaminant bis(2-ethylhexyl)phthalate at a level less than the CRQL. Sample GW 22-0-3 TW6Acontained this compound at a level less than the CRQL. The resultis considered not detected and a laboratory artifact. It isreported at the CRQL in the data summary.

flR3025l»l



-III* Pesticides/PCS

___ Holding Time___ Extraction TimeX Surrogate Recovery

_X__ MS/MSD___ BlankX Linearity CalibrationX DDT/Endrin Degradation___ Analytical Sequence___ DBC Retention TimeJK_ Continuing Calibration_X_ Retention Time Window___ Standards___ Chromatography___ HSL Compounds___ Data Completeness

OVERVIEW

This portion of the case consisted of three water samples. Thesamples were analyzed for TCL Pesticide/PCB target compounds.Problems associated with the sample analyses are listed in thefollowing section.

ISSUES

Samples GW 22-0-1 TW6A, GW 22-0-1 TW6A MS/MSD, and GW 22-1-1 TW6Arequired 2-fold dilutions due to high levels of non-targetcompounds. Sample results may be biased low. No qualification hasbeen applied.

The following samples had inference problems from non-targetcompounds that inhibited the proper recovery of surrogate compounddi-n-butylchlorendate: GW 22-0-1 TW6AMS, GW 22-0-1 TW6AMSD, GW 22-1-1 TW6A and PBLKLE0846-MB1. Positive sample results were notdetected for these samples, however, the spike recoveries were allbelow QC limits. These QC samples were re-extracted 19 days out ofholding time; however, most spike recoveries were still below QClimits. These outliers are probably due to the presence of non-target compounds and the matrix of the samples. No qualificationis applied.

RR3025U2


One blank spike recovery was outside the QC limits. The blank QCsamples are better examples of the long term precision and accuracyof the analytical method.

Several compounds had %RSD exceeded the 10.0% QC limit for theconfirmation column. Since this column is not used forquantitation, the data usability is not affected.

Several compounds had %D exceeded the 15% and 20% QC limits on thequantitation and confirmation columns. These standards wereanalyzed at the end of the analytical sequence, therefore nosamples are associated with them. No qualification is applied.

The retention time for 4,4-DDT in Ind A 08/31/90 at 05:55 exceededthe established retention time window. The standard was alsoanalyzed at the end of the analytical sequence. The sample resultsare not affected.

The 4,4-DDT/Endrin breakdowns were calculated incorrectly for bothquantitation and confirmation columns. The corrected results arereported on the attached Form VIII Pest-1. All breakdown criteriais met.

INFORMATION REGARDING DATA _


If you have any questions or comments on this data review, pleasecall Kelly M. Spittler or Zohreh Hamid at (215)524-6100,

ATTACHMENTS






I[




U ^ NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.

R ^ UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.



CODES REIATING TO OUANTITaTION


J ~ ANALYTE PRESENT. REPORTED VALUE MAY-NOT BEACCURATE OR PRECISE.

L « ANALYTE PRESENT. REPORTED VALUE MAY BEBIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.

DJ « THE REPORTED QUANTITATION LIMITS ARE -QUALIFIED ESTIMATED.

UL « NOT DETECTED. QUANTITATION LIMIT MAY BEHIGHER.

OTHER CODES

Q NO ANALYTICAL RESULT.

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AR302550

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^302553

II



Lab Name: Rov F. Weston, Inc. Contract: 2267-09-02-0000

Case No.: STANDARD CHLORINE______ _ GC Sample ID: 08309013

RFW Lot No.: 9008L360

Instrument ID: 13______ GC Column ID: 2250/2401



| | CALIBRATION | CALIBRATION | CALIBRATION | %RSD |j PESTICIDE I FACTOR | FACTOR | FACTOR |{</- |j j EVAL MIX A j EVAL MIX B j EVAL MIX C JIO.0%) j

ALDRIN_____________| 4977875 | 4920253 | 4899509 | 0.8JENDRIN_____________ | 1539869 | 1475759 j 1449323 | 3.114,4'-DDT___________| 873656 j 923173 | 962915 | 4.9| (1)DBG________________I 745269 715595 705560 2.9

{1} If > 10.0% RSD, plot a standard curve and determine the ngfor each sample in that set from the curve.


111102 |03|

1

1 11 I

i 1UNIT. EVAL MIX Bf| EVAL MIX B|| EVAL MIX B|I i

DATE |ANALYZED |

|08/30/90 i08/30/90 |08/31/90 !

1

| TIME || ANALYZED j

1 1| 1002 || 1952 || 0340 |1 1

ENDRIN | 4,4'-DDT | COMBINED1 I (2)

| |0.0 1 - ND frTS 11.5 j 3 A j&£ 10-5 | r. r*- j

1 ^ 1



flR302555


Lab Name: Rov F» Weston, Inc. Contract: 2267-09-02-0000

Case No.t STANDARD CHLORINE______ GC Sample ID: 08309014

RFW Lot No.t 90Q8L360

Instrument IDs 14______ GC Column ID: SP2100



|| CALIBRATION | CALIBRATION | CALIBRATION | %RSD || PESTICIDE | FACTOR j FACTOR j FACTOR j(</» || I EVAL MIX A I BVAL MIX B j EVAL MIX C |10.0%) |

| ALDRIN_____________| 2271013 | 2586463 | 2805933 | 10.51j ENDRIN_____________| 679362 j 708279 | 753120 | 5.2|j 4,4'-DDT___________j 502257 | 623301 j 708571 | 17.0| (1)DBC________________ 458356 466502 475615 I 1.81

(1) If > 10.0% RSD, plot a standard curve and determine the ngfor each sample in that set from the curve.

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

| DATE j TIME j ENDRIN | 4,4'-DOT | COMBINEDj ANALYZED j ANALYZED j j j (2)

01|INIT. EVAL MIX BI 08/30/90 | 1004 | | | <f 4 JfrrT L,^02 j EVAL MIX_B| 08/30/90 j 1954 j j j ||/j i3<< F ^03j BVAL MIX BJ 08/31/90 | 0342 j | ' - - "

I______________I_________I_________I_________I_________



flR302556


Lab Name: Rov F« Weston/ Inc. Contract: 2267-09-02-0000

Case No.s STANDARD CHLORINE _____ GC Sample ID: Q90_79013

RFW Lot No. t 9008L360

Instrument IDt 13 ______ GC Column ID: 2250/2401

Dates of Analyses: 09/07790 to 09/07/90


1| PESTICIDE1

i ALDRIN1 ENDRIN| 4,4'-DDT1 DEC1

| CALIBRATION| FACTOR1 EVAL MIX A

| 4691641| 1364103t 665056t 6295781


48605631350197736910614033


47199771331899780164619290

| %RSD |!<</- I|10.0%) 1mmmmmmw |

1 l.»|1 1-2|1 8.0|1 1-31I I

(1)

(1) If > 10.0% RSD, plot a standard curve and determine the ngfor each sample in that set from the carve.


0102

111

INIT. EVAL MIX B|EVAL MIX BJ

1

DATEANALYZED

09/07/9009/07/90

TIME |ANALYZED j

11359 |2323 |

1

ENDRIN | 4, 4 '-DOT | COMBINED1 1 (2)

I lo.o u \ y*? \ .,,, MI*-' r,.>r"



/IR302557

IIII

3380


Lab Namex Rov F» Weaton, Inc. Contract: 22 7-09-02-0000

CAB* NO.J STAHDASP CHLORINE_____ GC Sample ID: 09079014

RFW Lot No. i 9008L360

Instrument ID: 1£______ GC Column IDs SP210D



PESTICIDE

ALDRINENDRIN4,4'-DDTDBC

| CALIBRATION1 FACTOR1 EVAL MIX A

| 1937805| 628768I 481600| 3978071


2410241702869623965426104

CALIBRATION | %R5DFACTOR j {</«EVAL MIX C J10.0%)

2754027 | 17.3*7S7666 | 11.3745528 | 21.4461669 | 7.5

1

(1) If > 10.0% R5D, plot a standard curve and determine the ngfor each sample in that set from the curve.


02

I11

INIT. EVAL MIX B|EVAL MIX BJ

1

DATEANALYZED

09/07/9009/07/90

TIMEANALYZED

14012326

ENDRXN | 4,4'-DDT | COMBINED1 1 (2)

| | U-5 Jttf\ lc<7 2<*r1 1


<D

FORM'VIII PEST-1 11/88 Rev.

BR302558

I

VOLATILE, SEMIVOLATILE, PESTICIDE/PCBAND METALS ANALYSIS

STAR ENTERPRISE WELL OR-6A(POST-PUMP TEST SAMPLING)

DELAWARE CITY, DELAWARE FACILITY

4R302559

1

STANDARD CHLORINESDG #CLP104


•?The laboratory' s portion of SDG fCLP104 consisted of one watersample analyzed for TAL metals by Roy F. Weston, Inc.



Minor Issues

The matrix spike percent recovery for Pb was below the CLP controllimits. All associated sample results are qualified as estimatedand are considered to be biased low.

The post matrix spike percent recoveries for Pb and Se were belowthe CLP control limits. All associated sample results arequalified as estimated and are considered to be biased high.

The post-digestion spike percent recoveries for Tl was above theCLP control limits. All associated sample results are qualified asestimated and are considered to be biased low.

flR302560

Sample # Analyte -fDL -QL Comment:s

9010L104-001 Pb - UJ 1,2

Se UJ 2Tl UJ 3

Comments

1. Due to a low matrix spike percent recovery indicating alaboratory or matrix spike problem, all associated sampleresults are qualified as estimated and considered to be biasedlow.

2. Due to a low post-digestion percent recovery, all associatedsample results are qualified as estimated and are consideredto be biased low.

3. Due to a high post-digestion percent recovery, all associatedsample results are qualified as estimated and are consideredto be biased high.

QR302561

The reported IDL and linear range data were from the wrong quarter.Although this is contractually non-compliant, the data should beconsidered acceptable.

Regarding Report Content





3 . Appendix A - Data Validation Form for Inorganics



"R302562

ATTACHMENT IGLOSSARY OF DATA QUALIFIERSm

SR302563

II

I


I CODES RELATING TO IDENTIFICATION

(confidence concerning presence or absence of compounds):

0 » NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVEL( R E P O R T E D IN LABORATORY OR FIELD BLANKS.

*R - UNRELIABLE RESULT- ANALYTE MAY OR MAY NOT BE

PRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.



CODES RELATING TO OUANTITATION


J «• ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.

L « ANALYTE PRESENT. REPORTED VALUE MAY BEBIASED LOW. ACTUAL VALUE IS EXPECTED TO BEHIGHER.

UJ - THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.

UL = NOT DETECTED. QUANTITATION LIMIT MAY BEHIGHER.

OTHER CODES


/1R302561*


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M302567

CFEB?aTN3 PROCEDURE Page 4 Ol 35

Title: Evaluation of Metals Data for tJie Date: Feb. 1990Contract Laboratory Program NL&rjber: *H*-2Appendix A.I: Data Assessment - Contract Revision: 10Cerpliance (Total Revi&* - Inorganics)

ACTIO3: If no for any of tte above, contact RSOC forclarification.

A. 1.4 anplg Traffic Report - Present or on file? [_]

Legible? [ ]

ACTICH: If no, request frcm Regional Sanple ControlCenter {RSCCJ.

A. 1.5 Qpver Page - Present? I A }

Is cover page properly filled in and signed try the labmanager or the manager's designee? [X ]

AcnoM! if no, prepare Telephone Record Log, andcontact laboratory.

Do numbers of sarrples correspond to nirters en Recordof CcrTTuaicaticn?

Do sanple inters en cover page agree with sanplerunbers on: /

U) Traffic Report S»et? I.vri(b) Form I»s? I x]

&R3Q2568

XES ffiA. 1.1 QantJTgE Qotrpliance Scroaniiio yacprt (OCS) * Present? [ __ ] __ V.

: If no, contact RSCC.

A. 1.2 pscprrj pf QgnffUnJCStJOI (fron.RgpT) - Present? [ __ ] >/

! If no, request frcm RSCC,

A. 1.3 Trip Rgport - Present and corpiete? [ _ ] __ ^

If 3io, contact RSCC for trip report.

CPEKAIUgG PROCEDURE Page 5 o: 35

Title: Evaluation of Metals Data for tne Date: Feb. 1990Contract Laboratory Program Number: H«-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Itrtal Review - Inorganics)

ND N/&

A.l.6 Ftorm I (Final Data) - Are all Form I's present and conplete? [X.] _ _ _

aCHflN: If no, prepare telephone record log and contactlaboratory for su&nittal.

Are correct omits (ug/1 for waters and ing/kg for soils) ,indicated on Form I's? [ X] _ _

Are soil sample results for each parameter corrected forpercent solids? [ _ ] _ X

Are HA sarrple f s and corresponding laboratory sanpleID t s the same as on the Cover Page, Form I's and .in tfte raw data? u^ s*^ <-^ '««- *«-^< V* cf? fc/u , [ -^ ] __ _.._

.*Are cornputation/transcription errors less than 10%of reported values? [ 3 _

Are all "less than H2L" values prc3perly coded with "U"? [ X 3 f_

Was a brief physical description of sanples given on ,Form I's? [X ] _

were the result qualifiers used correctly with finaldata? I X] _

ACTICK: if no for any of the above, prepare TelephoneRecord log, and contract laboratory forcorrected data.

Were any sanples diluted beycnd requiranents of contract? __ IV

If yes, were dilutions noted en Item I's? [_] _amen: If no, note under CcrttTKrt-Problarv cn-Conpliance

of theTfeta Assessment Narrative".

Xl.7 tifrldirn Timaff - (aqueous and soil samples )(Examine sanple traffic reports and digestion/distillation logs.)

Mercury analysis (2B days). ...... exceeded? __

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

5R302569

OPERATING FRDCEHJRE Page 6 oi 35

Title: Evaluation of Metals for the Contract Date: Feb. i990Laboratory Program Number: HW-2Appendix A.I: Data Assessment - Contract Revision: 10Ccnpliance (Ttotal Reviev - Inorganics)

A. 1.8 R3K

A. 1.8.1 'Digestion Log* for flame ftA/ICP (Form XIII) present? [ x ]

Digestion Log for furnace AA Form XIII present? [ y ]

Distillation Log for mercury Form XIII present? [>( 1

Distillation Log for cyanides Form XIII present? [ ]

Are pH values (p«<2 for all metals, p«>12 for cyanide)present f [ ]

Weights, dilutions and volunes used to obtain vali s.

Percent solids calculation present for soils/sediments? [ _ ]

Are preparation dates present on Digestion Log? I > ]

. 8.2 Measuremsit r«ad out record present? ICP I 1

RR302570

ffi N/AOtter Metals analysis (6 months), . . . exceeded? _ [jl ] _

Prepare a list of all samples and analytesfor which holding times have been exceeded. Specifythe nurrber of days frtm date of collection to the dateof preparation (fron raw data). Attach to checklist.

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

Plane AA [ _ ] _ yrumace AA i^f ] _ _Mercury

Cyanides

CFEEATOG H?O3DURE Page 7 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: 'HWAppendix A.I: Data Assessnent - Contract Revision: 10Compliance (Ttotal Review - Inorganics)

——————— ffi

A.I. 8. 3 Are all raw data to support all sanple analyses andQC operations present? [ / ]

Legible? - [ ]

. Properly Labeled? ««. A **/ ' & *-„{, fa\ [ c ]

If no for any of the above, write TelephoneRecord Log and contact laboratory. Flag metaldata as estimated if pH of sarrple is greaterthan 2. Flag cyanide data as estimted if jflsanple is less than 12.

A. 1.9 Data V^iiflfttion and

A. 1.9.1

1,9.1.1 Is record of at least 2 point calibrationpresent for ICP analysis? [ X ]

Is record of 5 point calibration present forHg analysis? [ X ]

ftCna*: If no for any of the above, write in theContract Problan/Nan-Corpliance section ofthe "Data Assessnent Narrative".

A.l.9.1.2 Is record of 4 point calibration preseit for:Flare AA? f_]Furnace AA? [V]Cyanides? fXj

1. If less than 4 standards are measured in absorbancemode, then the ranaining standards in concentrationmode mist be run immediately after calibration andbe within ±10% of true value.

2. For all AA (except Hg) and Cyanide analyses, onecalibration standard is at OOX level. If not,write in the Contract-ProblarvWon-Cornpliance sectionof the "Data Assessnent Narrative".

flR30257l

CREATING FRQCTOJRE Page 8 01 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HW-2Appendix A.I: Data Assessnent - Contract Revision: 10Corpliance (total Review - Inorganics)

Flag associated data as estimated if standardsare not within ±10% of true values (except CK2Lcalibration standard). Do not flag the data asestimated in linear range indicated by goodrecovery of standard.

A.I. 9. 1.3 Is correlation coefficient less than 0.995 for:

Mercury Analysis?

The reviewer win calculate correlaticn coefficieit.

ID

Cyanide Analysis? __ [

Atonic Absorption Analysis? _ [

ACTICK: If yes, flag the associated data as estiitated.

A. 1.9. 2 Fprm II A (Tjut3tU__and jTtim1_iy7

A.l.9.2,1 Present and ccnplete for every metal and cyanide? [ <?] _

Present and ccnplete for and ICP vhen both are „used fof same analyte? [__] _ _.

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

A.I. 9. 2.2 Circle all values on data sxanrary sheet that areoutside contract windows. Are all calibrationstandards (initial and continuing) within controllimits?

Metals 90-110X f ~x* 3 __

Hg - 80-120*

Cyanides 85-115% [ v 3 __

(IR302572

STANDARD OPERATING PROCEDURE Page 9 of 35

Title; Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: Bv-2Appendix A.I: Data Assessment - Contract Revision: 10Coipliance (Total Review - Inorganics)

Flag as estimated (J) all positive data (notflagged 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 OJ) recovery andnearest good calibration standard. Qualify results<ICL 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% (Otf, 70-130%; Hg,65-135%). Qualify five samples on either side ofverification standard out of control limits.

Was continuing calibration performed every 10 sanplesor every 2 hours? [X J

aCHfltf: If no, flag the excess samples (eleventh artfup) data as estimated (JJ.

Was ICV for cyanides distilled? [_ J

££H£1$: If no, write in the Contract-Problan/Ndn-Compliancesection of the "Data Assessnent Narrative".

A, 1.9.3.1 Was a OT3L standard (CRA) analyzed after initialcalibration for all AA metals (except Ho)? I XJ

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

a 2xOSX ( or 2xHL. when HEXREL) analyzed (CRI)for each ICP run?(Note: CRI for AL,Ba,Ca,Fe,*g,tta,or K is not required.)

2QI2J: If no for any of the above, flag as estimatedall data falling within the affected ranges.2fte affected ranges are:AA Analysis - **True Value ± CREXICP Analysis - **Ttue Value + 2CRDLW Analysis - **7tue Value ± 0.5 x True Value.

* Find the results of mid-range standard in the raw data.value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL.

flR302573


Title: Evaluation of Metals Data for the Date: Feb. 199Contract Laboratory Program Number: B%*-2~Appendix A.1: Data Assessnent - Contract Revision: 10Compliance (Total Review - Inorganics)

__ _ .

A. 1.9.3.2 Was OU analyzed after ICV/ICB and before the finalCCV/CCB, and for every four hours of JCP run? EX 3 _

31£1?: If no, write in Contract Problan/NcDv-CcnplianceSection of the "Data Assessnent Narrative".

A. 1.9.3.3 Circle all values en surmary Sheet that are outsideacceptance windows,

Are CRA and CRT standards within control limits:Metals 80 - 120%R? [__ ] __

Is mid-range standard within control limits:Cyanide 80 - 120%R? [_] _

Flag as estimated all data within the affectedranges if tne recovery of the standard isbetween 50-79%; flag only positive data ifthe recovery is between 121-150%; reject<red line) all data if the recovery is lessthan 50%; reject only positive data if therecovery is greater than 150%.

A.l.9.4 Form III (Initial and Oont5r^™p

A.I.9.4.1 Present and cotplet€? [ X'l

For both AA and ICP when both are used for same analyte? [__]

Was an initial calibration blank analyzed? [_Xj __ _

Was a continuing calibration blank analyzed afterevery 10 sarples or every 2 hours (whichever is morefrequent)? L>£] __ _.

If no, prepare Telephone Record Log, contactlaboratory and write in the contract-problems/rerv-corpliance section of the Data AssessmentNarrative.

OPERATING FROCEDURE Page 11 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: Htf-2Appendix A.I: Data Assessment - Contract Revision: 10Compliance (Tbtal Review - Inorganics)

"~ woXI. 9.4. 2 Circle all calibration blank values on Data Surmsry Sheet

that are above CRTL (or 2 x IEL when EX > CRDL). Areall calibration blanks (when HSxCRDL) less than or equalto Contract Required Detection Limits <CHDU? f Jxf] _

Are all calibration blanks less than two timesInstrument Detection Limit (wJien H3LX3?nL)? [ __ ] _

aniBJ: If no for any of the above, flag as estimated (J)all positive data less than or equal tocalibration blank values analyzed betweencalibration blank with value over OS2L (or 2xIDL)and nearest good calibration blank. Flag fivesamples on either side of the calibration blank.

A.I. 9. 5 FCSfrl III (Preparation Blapk) -

(Note: Trie preparation blank for mercury is the sameas the calibration blank. }

A.I. 9. 5.1 Was one prep, blank analyzed for: each 20 samples? [ >O __

each batch? [ _ ] _

each matrix type? [ _ ] _AA and ICP vtfien both are \ased for same analyte? [ _ ] _ X

If no for any of the above, flag as estimated (J)all associated positive data <10 x HLs for vtiichprep, blank was not analyzed.

I22Z£: If oily one blank was analyzed for morethan 20 sarrples, then first 20 sarrples analyzeddo not have to be flagged as estimated ( J) .

A.l.9.5.2 Is concentration of pwp. blank greater than CRDLwhen IEL is less than or equal to CRDL? _ [_2<3 _ .If yes, is the concentration of the sanple with theleast concentrated analyte less than 10 times theprep, blank value? _ [_._! -£S

AR302575

If no, is cencaitraticn of Al, Ca, Fc, or Mgthan in ICS? [__]

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 "ID*

SMCftRD CKRATING FRXEDURE Page 12 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990contract Laboratory Program . Number: 'K-.'-ZAppendix A.I: Data Assessment - Contract Revision: 10Compliance (Tbtal Review - Inorganics)

JES ffi N/A"2Cna$: If yes, reject (red-line) all associated data

greater than CECIL concentration but less than tentimes the prep, blank value found in the raw data.

A.l.9.5.3 Do concentrations of prep, blank fall below two timesEX when EX is greater than OTX? [_ ] __ _X

tCnGE: If no, reject (red-line) all positive datathat has a concentration less than 10 timesthe prep, blank value in the raw data.

A. 1.9.5.4 Is ccnc rtraticn of prep, blank belcv the negative CREEL? _ [X ] _

i HO?: If yes, reject (red-line) all associated datathat has a concentration less than lOxCRDL.

A.l.9.6.1 Present and ccrrplete? [ X ] _

(NOTE: Not required for furnace 2&, flame AA, mercury,cyanide and Car Mg, K and Na.)

Was ICS analyzed at beginning and end of run(or ,at least twice every 6 hours)? [ V] _

ACTION: if no, flag as estimated (J) all sanples forwhich AL, Ca, Fe, or Mg is higher than in ICS.

.8.6.2 Circle all values en Data Surrmary Sheet that are morethan + 20% of true or established mean value. Are allInterference Check Sanple results inside of controllimits <+ 20%)? I

flR302576

OPERATING FKXETURE Page 13 ot 33

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HW-2Appendix A.1: Data Assessnent - Contract Revision: 10Corrpliance (Total Review - Inorganics)

2E5 LD

A.l.9.7 KCT V A (Spited Saccle Recovery - Pre gestiofi/prg-pigtillrtJTI?-( Note: Not required for Ca, Mg, K, and Na (toth matrices), Ai, and Fe(soil only.)

A.l. 9.7.1 Present and coiplete for: each 20 sanples? [ X'] __

each matrix type? [__] _ _

each cone, range (i.e. low, mad., high)? [_] __

Tor both AA and ICP when toth are used for sameanalyte? [_] __

If no for any of tte above, flag asestimated (J) all positive data lessthan four times spiking level forvhich spiked sanpie was not analyzed.

If one spiked sample was analyzed for ircrethan 20 sanples, then first 20 sanpiesanalyzed do not have to be flagged asestiroted (J).

A.1.9.7.2 Was field blank used for spiked sanple? __ t_>0 _

If yesr flag all positive data less than4 x spike added as estimated (J) for whichfield blank was used as spiked sanple.Matrix spite analysis should be performed on afield blank whan it is the only aqueous sanple in SEC.

A. 1.9.7.3 Circle all values en Data Sunnary Sheet that are outsidecontrol limits (75% to 1251L Are all recoverieswithin control limits? p fj [_]If no, is sarple concentration greater than or equalto four tiines spike concentration? [_]

If yes, disregard spike recoveries for analytes•whose concentrations are greater than or equalto four times spike added. If no, circle thoseanalytes en Form V for which sairple concentrationis less than four times the spike concentration.

/JR302577

OFEEAITNG TOCEEURE Pace 14 o* 35I

Title: Evaluation of Metals Data for the Date: Feb. 1990I Contract Laboratory Program Nurrtoer: HW-2I Appendix A.1: Data Assessment - Contract __ Revision: 101 Ccrpliance (Ototal Review - Inorganics)

2£S~jg————— '

I

Are results outside the control limits (75-125%)I flagged with "N" en Form I»s and Form VA? [__] _

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

; A.l.9.7.4 aqueousAre any spike recoveries:

(a) less than 30%? __ [J<_]

(b) between 30-74%? J>C [_]

j <c) between 126-150%? _(d) greater than 150%? __

IIf 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.I.9.7.5 Soil/SedijnentAre any spike recoveries:

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

(b) between 10-74%? "r" _ [_](c) between 126-200%? _ [_] X-

If less than 10%, reject all associated data; ifbetween 10-74%, flag all 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 «UM. ^_.

flR302578

Corrpliance section of "Data Assessment Narrative".

1. RTO is not calculable for an analyte of thesanple - duplicate pair when both values areless than IGL.

Substitute IEL for CRDL when HL > OttJL.

'OPERATING H?OCEDURE Page 15 oi 35

Evaluation of Metals Data for the . Date: Feb. 1990contract Laboratory Program Number: h»2Appendix A.I: Data Assessment - contract " Revision: 10Ccrpliance (HJtal Revi ; - Inorganics)

25 1C ILS1.1.9.8 ypnn VT fiat* Duplicates)

v.l.9.8.1 Present and ccrplete for: each 20 samples? -each natrix type? [ __ ]

each concentration range (i.e, low, mad., high)? [ __ )

both AA and IQ> when both are used for same analyte? [ __ ]

ACTICI3: If no for any the above, flag as estimated (J)all data >CPDL* for which duplicate sanple wasnot analyzed.

Note: i. If one duplicate sanple was analyzed formore than 20 sanples, then first 20 sarrples 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 Hg/Lon wet weight basis and calculate RTO or Differencefor each analyte.

Xl-9,8.2 Was field blank used for duplicate analysis? __

• If yesf flag all data >CRDL* as estimated( J) for which field blank was used as duplicate.

Duplicate analysis should be performed ona field blank when it is the only aqueoussanple in SDG.

A. 1.9.8. 3 Are all values within control limits (RTO 20% ordifference < iIf no, are all results outside the control lijnitsflagged with an * en Form I's and VI? t __ 1 . _

If no, write in the Contract - Frcblenis/Non-

^302579

OPERATING H4JCEUURE Page 16 o: 35

Title: Evaluation of Metals Data for the Date: Feb. 1993Contract Laboratory Program Number: H«-2Appendix A.I: Data Assessment - Contract Revision: 10Corpliance (Total Review - Inorganics)

2ES JSD

2. If lab duplicate result is rejectable dueto coefficient of correlation of MSk,analytical spike recovery, or duplicateinjections criteria, do not apply precisioncriteria.

A.I. 9. 8. 4 j.i> oiiy v<3j.ue 2Ui ocoj i tHJ.tr uuf.u.xwa»5 JJ&J..L j.e»a u*±u \-ru-u_-- ,.,/and other value greater than or equal to 10 x *O3JL? __ l/\ ] V_

If yes, flag the associated data asestimated (J).

A.I. 9. 8.5Circle all values on Data Summary Sheet that are:

RPD > 50%, orDifference > ±

Is any RTO greater than 50% vhere sanpie and duplicateare both greater than or equal to 5 tiines *O*DL?

Is any **difference between sairpie and duplicate greaterthan *CRDL where sanpie and/or duplicate is less than5 tiJnes *CRDL?

If yes, flag the associated data as estixrated.

A. 1.9. 8. 6 Soil/SediinentCircle all values en Data Sumary Sheet that are:

RPD > 100%, or

Difference > 2 x CTCS-*

Is any KPD (where sairpie and duplicate are bothgreater than or equal to 5 times *Q£L) :

> 100%? _ [ _ ]

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

* Substitute IEL for CRDL when HE- >** Use absolute values of sanpie and duplicate to calculate

the difference.

5R302580

OPERATING FRQCUXJRE Page 17 oi 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Numtier: Hi-;-zAppendix A.I: Data Assessment - Contract Revision: 10Compliance (Total Review - Inorganics)

XE5 IDIf yes, flag the associated data as estijnated.

A. 1.9. 9 Field

A. 1.9.9.1 Were field duplicates analyzed? [__] _ ±,

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

1. Do not calculate RTO when both values areless than IDL.


v. 1.9.9.2 Is any value for sample duplicate pair less than *CRDLand other value greater than or equal to 10 x *CRDL? _ [_ J x

ACTIC13: If yes, flag the associated data as estimated,

A.I.9.9.3 Equeous

Circle all values on Form VI for field duplicates that are:RTO > 50%, or

Difference > ± CREL*Is any RPD greater than 50% where sample and duplicateare both greater than or equal to 5 times *OTL? __ [_ J X

Is any **difference between sample and duplicate greater 1than *CREL where sample and/or duplicate is less than \5 times *OTX? __ [_ J __

If yes, flag the associated data as estimated.

* Substitute IDL for CREEL when HL > C3CL.

** Use absolute values of sample and duplicate to calculate the difference.

&R302581

SJBNDftRD CPEBA31N3 PROCEDURE Page 18 o: 35

Title: Evaluation of Metals Data for the Date: Feb. 199%Contract Laboratory Program Number: "K.-;-::"Appendix A.I: Data Assessnent - Contract Revision: 10Corpliance (Ttotal Review - Inorganics)

A. 1.9. 9. 4

Circle all values on Form VI for field Silicates that are:RTO >100%, or -

Difference > 2 x CKDL*

Is any RTO (where sarrple and duplicate are bothgreater than 5 times *O?DL), :

. >100%? _ [_ 3 ^

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

>2x *CRDL? __ [_ ] ^

If yes, flag the associated data as estiirated.

1 A.I. 9. 10 Ftorm VII fT.a>y*ratory Contrpl Sry>le> (Note: LCS - notrequired for aqueous Hg and cyanide analyses. )

A.1,9.10.1 Was one LCS prepared and analyzed for:1 f every 20 water samples?

every 20* solid samples? { _ ] _ _ >(

I both AA and ICP when both are used for same analyte? [ _ ] _ . y

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

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

* substitute nx for' "Use absolute values of sample and duplicate to calculate the difference.

fiR302582

JfcQIEDURE Page 19 01 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: HX-2Appendix A.I: Data Assessment - Contract Revision: 10Ccrpliance (Total Review - Inorganics)

A. 1.9.10.2 toueous LCSCircle all LCS values outside control limits(80 - 120%- except aqueous Ag and Sb).

Is any LCS recovery: less than 50%? _ [_X]

5 tetween 50% and 79%? __

between 121% and 150%? _

greater than 150%? ;_ [_)£] __

f feCIIfltf: Less than 50%, reject (red-line) all data;\ between 50% and 79%, flag all associated data

as estimated (J); between 121% and 150%, flag\ all positive (not flagged with a "U") results| as estimated; greater than 150%, reject all

positive results.

A.I.9.10.3 Solid LCS

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

2. If IISL 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? __ I_ J

If yes, qualify all associated positive dataas estimated*is LCS "Found" value lower than the Controllimits on Form VII? __ [__ J __

If yes/qualify all associated data asestimated.

IOPERAIING PRCnZTUZE Page 20 c: 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract laboratory Program Number: "to;-2"

A.1: Data Assessnent - Contract Revision: 10(Itotal Review - Inorganics)

A.I.9.11

ELSE: Serial dilution analysis is required onlyfor initial concentrations equal to orgreater than 10 x HX*.

A-1.9.11.1 Was Serial Dilution analysis performed for:each 20 sanples? [_

each natrix type? [_]

each concentration range (i.e. low, med.)? [_] __ v/

ACTION: If no for any of-the above, flag all positivedata greater than or equal to lOxIDLs asestijrated (J) for which Serial Dilution Analysiswas not performed, and sunroarize the deficiencyon the JDFO report.

A. 1.9.11.2 Was field blank(s) used for Serial Dilution Analysis?

If yes, flag all associated data > 10 x IELas estimated (J).

Serial dilution analysis Should be performedon a field blank wften it is the only aqueoussanple in SDG,

A.l.9.11.3 Are results outside control limit flagged with an "E"on Form Ifs and Form IX when initial concentration onForm IX is equal to 50 times US- or greater* [_] _

ACTION If no, write in the ccntract-probl«o/tion-conpliance section of the "Data AssessnentNarrative".

A.l-9.11.4 Circle all valises on Barta Suwnary Sheet that are outsidecontroU.imit for initial concentrations equal to or greater

only. Are any \ difference values:

S2ANLARD CFEBATING FKXEEURE Page 21 of 35

Title: Evaluation of M&tals Data for the Date: Feb. 1990Contract laboratory Program Number: H/>2~Appendix A.I: Data Assessnent - Contract Revision: 10Corpliance (Ttrtal Review - Inorganics)

Flag as estimated (J) all associated equalto or greater than lOxEXs for which percentdifference is greater than 10% tut lessthan 100%. Reject (red-line) all associatedsample results equal to or greater thanlOxIELs for which K> is greater than orequal to 100%.

A. 1.9. 12 FUmac*? fttgnic Absorption (AA) pc ftryUYSifi

A. 1.9. 12.1 Are duplicate injections present in furnace raw data(except during full Method of Standard Mdition) foreach sample analyzed ty GF7A? [ V ] _

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

A.I. 9. 12,2 Do the duplicate injection readings agree within 20%Relative Standard Deviation (RSD) or Coefficient ofVariation (CV) for concentration greater than CRDL? [ X] __ _

Was a dilution analyzed for sanple with post digestionspike recovery less than 40%? [ _ ] _ _

3IflK: If no for any of the above, flag all theassociated data as estimated ( J) .

A. 1.9, 12- 3 Is *post digestion spike recovery less than 10% orgreater than 150% for any result? _

ACTI CM; If yes. reject <red-line) the affected data ifrecovery is <10%; reject data not flagged with

if spite recovery is >150%.

Reject the data only if the affected sanple wasnot subsequently analyzed ty Method of StandardMditicn.

* Post digestion spike is not required an the pre-digestion spiked sanple.

5R302585——————

CFEBATHvG PROCEDURE Page 22 OJ 35

Title: Evaluation of Metals Data for the • Date: Feb. 1990-Contract Laboratory Program Number: 'nv;-2appendix A»l: Data Assessment - Contract Revision: 10Ccnpliance (TOtal Review - Inorganics)

10A. 1.9. 13 fOnn VIII (MsthDd Of ffl-anrtart W'.im I SLlltS)

A.I. 9. 13.1 Present? [ __ )

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

If yes, vrite request en Telephone Record Logand contact laboratory for sutaittal of Fora VIII.

. 1.9. 13. 2 Is coefficient of correlation for MS less than 0.990 forany sarrple?


A. 1.9. 13. 3 Was *MSA required for any sarrple but not performed?

Is coefficient of correlation for MS less than 0.995?

Are MS calculations outside the linear range of thecalibration curve generated at the beginning of theanalytical run? _ [_ _}

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

A. 1.9. 13. 4 Was proper quantitation procedure followed correctly -as outlined in the SOW on page E-16 through E-17? [ x ]

IT" H. ~~.~~

if no, note exception under contract problan/non-corrpliance of data assessnent narrative,or prepare a separate list.

A. 1.9. 14 p 5 1 yfiyj ital or Inpnpgn firtfli ftnftiYtCr *~

A. 1.9. 14.1 Were any analyses performed for dissolved as veil astotal analytes en the same sanple(s). __ [ _ ] >C

Were any analyses performed for inorganic as well as total{organic * inorganic! analytes on the same sample(s)? __ [ _ ]

* MS* is not required en I£S and prep, blank.

SR302586

OPERATING FKXEXJRE Page 23 cf 35

Title: Evaluation of Metals Data for the Date: Feb.Contract laboratory Program Number: H.-:Appendix A.1: Data Assessnent - Contract Revision: 10Ccrpliance (Ttotal Review - Inorganics)

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

2. Apply tf>e following questions cnly 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.l.9.14.2 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration fcyirore than 10%? _ [_ _] y/

A. 1.9.14.3 Is the concentration of any dissolved (or inorganic)analyte greater than its total concentration by .more than 50%? _ [ ] y

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

*A.I.9.15 Form I to IX

A. 1.9.15.1 Are all the Form I through Form DC labeled with:Laboratory name? [^f 3 _ _.

Case/ff£ number? f X ] _ _ __

EFA sanple No.? [.X 1 _._ _

SDC ND.?Contract No.? [__] __ V

Correct xmits? \2? ] __ _

Matrix?

If no for any of the above, note undercontract problenvton-carpliance sectionof the "Data Assessment Narrative".

OFEKAIXN3 JTOCUXJRE Page 24 o: .35

Title: Evaluation of Metals Data for the ' Date: Feb. 1990Contract laboratory Program Number: H«-2~Appendix A.I: Data Assessnent - Contract Revision: 10Compliance (Total Review - Inorganics)

A. 1-9.15.2 DD any captation/transcription errors exceed 10% ofreported values on Forms I-IX for:


(a) all analytes analyzed by ICP? __ [

(b) all analytes analyzed by GFfcA? _ [_ ] _

(c) all analytes analyzed by wv Flame? _ t__3 xT

(d) Mercury? __ [y(_] _

(e) Cyanide? _ [ vi] _

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

A.l.9.16 Form I (Field Blank) -

Circle all field blank values on Data Sunrary Sheetthat are greater than O*DL, 2 x UJL when IDL > DCL.

Do concentrations of field blank(s) fall below(or 2 x IEL when IDL > O EL) for all parameters ofassociated aqueous and soil samples? [__] _ V

If no, was field blank value already rejected due toother QC criteria? [__]

If no, reject (except field blank results)all associated positive sample data lessthan or equal to five times the field blankvalue.

HR302588

IOPERATING FEOCHJjRE Page 25 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: HA-2Appendix A.I: Data Assessment - Contract Revision: 10Corrpliance <7t?tal Review - Inorganics)

A. 1.9. i? ffrrm K. ?g, gi (Variflcatiqn of InsuurantalA.l. 9.17.1 Is verification report present for:

Instrument Detection, Limits (quarterl(?) yr* r- &<£»,** —ICP Interelerent Correction Factors (annually)? [ x 3

w fICP Linear Ranges (quarterly)? [ X ]

if no, contact DPO of the lab.

A.I.9.17.2 Form X (Instrument Detect ion. Limits) - (Note: IDL is notrequired for Cyanide.)

Are IHLs present for: all the analytes? [ V 3

all the instruments used?

For both AA and ICP when both are used for sameanalyte? " [ _ ] _ V-

aCTia : If no for any of the above, prepareTelephone Record log and contactlaboratory.

Is US- greater than CTOL for any analyte? _ I A" ] _

If yes, is the concentration on Form I of the_sampleanalyzed on the instrument wnose IDL exceeds CRDL,greater than 5 x IEL? [__] _

if no, flag as estimated all valuesless than five times IEL of the instrumentwhose ICL exceeds CKCL.

4R302589

OPERATING FROCEIXJRZ Page 26 of 35

Title: Evaluation of Metals Data for the Date: Feb. 1990Contract Laboratory Program Number: Hw-2Appendix A.I: Data Assessnent - Contract Revision: 10Ccrpliance (Itotal Review - Inorganics)

A.I.9.17.3 Fonn XI (Line&r-Ranees)

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, vas thesanple diluted to obtain the result on Form I? [_] _ _

ACTICH: If no, flag the result reported on Form Ias estiirated{J). '

Is soil content in sedirent(s) less than 50%? _ [_ ]

Jf yes, qualify as estijnated all datanot previously rejected or flagged dueto other QC criteria.

flR302590

I[


1R30259I


CASE NO. Lstf 6OK_______________ SITELABORATORY UJp (-£ c\

SDG# CLP/& sow* 7 £7DPO: ACTION FYI 3*

NO. OF SAMPLES/MATRIX / <* u t s-REVIEWER (IF NOT ESD)

REVIEWER'S NAME IT)/ Gnfl - LCOMPLETION DATE / - - fr -fPf••• " —————— r-i —————————


I. HOLDING TIMES2. CALIBRATIONS3. BLANKS

4. ICS

5. LCS

6. DUPLICATE ANALYSIS '

7. MATRIX SPIKE

8. MSA

9. SERIAL DILUTION10. SAMPLE VERIFICATIONII. OTHER QC12. OVERALL ASSESSMENT

O * Data had no problems/or qualified dueM = Data qualified due to major problems.Z = Data unacceptable.X & Problems, but do not affect data.

ACTION ITEMS: & T<D S'i kfr 5^/6- /

ICP AA Hg CYANIDE

O O 6 <^

o 0 0 • 00 '"" 0 u OOo o£>'0 0' o 0

o0 0 O &0 O* O o0 0 o n

to minor problems.

L« ^ l^n^/i^S &\ )t c\fC *.c>d +*T"?&fa&ssA J&£.& fa- ***£ v s y f /£* , ~~ //>--,( Me-4ClJ? i*\ \) £s~\

^ / r SP i TJ? if " &

AREAS£F CONCERN:"v" _-* ~ .*"

.


II


flR302593

STANDARD CHLORINECASE 90101*104

This quality assurance review is based upon a review of the datagenerated from one water sample and one trip blank collected on10/11/90 and analyzed by Roy F. Weston, Inc. for TCL Volatile,Semivolatile, and Pesticide/PCB target compounds.



/1R302595



I- Volatiles

___ Holding TimeX Surrogate Recovery___ MS/MSD_X_ Blank___ GC/MS TuningX Initial CalibrationJC_ Continuing Calibration___ Compound ID (HSL, TIC)__ Standards___ Spectra Quality__ Chromatography___ Data Completeness

OVERVIEW

This portion of the case consisted of one water sample and one tripblank. The samples were analyzed for TCL Volatile targetcompounds.

All internal standard area and calibration data met the EPA CLP QCcriteria. Minor problems associated with the sample analyses arelisted below.

ISSUES

The toluene-da surrogate recovery exceeded the EPA QC limit forsample OR-6AMS. The sample was analyzed as OR-6AMSD and there wereno surrogate outliers. The toluene spike recovery for OR-6AMS alsoexceeded QC criteria. Sample results/spike recoveries for thissample may be biased high. However, no qualification is applied.

The method blank contained common contaminants methylene chlorideand acetone at levels less than 4x the CRQL. The trip blank alsocontained methylene chloride. Sample results above the CRQL, butless than lOx the blank level are flagged "U" and considered alaboratory artifact. The acetone result in sample OR-6A is greaterthan lOx the blank level and is considered a true value.

The %RSD and/or %D for several compounds exceeded the 30% and 25%QC limits in the initial and continuing calibrations. Allassociated positive results and guantitation limits are qualifiedestimated J and UJ.

J5R302596


II. Base/Neutral/Acids

___ Holding Time___ Extraction Time___ Surrogate Recovery_X_ Blank___ MS/MSD___ GC/HS TuningX Initial CalibrationX Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness

OVERVIEW

This portion of the case consisted of one water sample analyzed fora special list of semivolatile target compounds.

All surrogate and matrix spike recoveries, internal standard area,and calibration data met EPA CLP criteria. Minor problemsassociated with the sample analyses are listed below.

The method blank contained common contaminant bis(2-ethylhexyl)phthalate at a level less than 2x the CRQL. Sample OR-6A contained this compound above the CRQL, but less than lOx theblank level. Therefore, the result is considered a laboratoryartifact and is flagged "U".

Several compounds had %RSD and/or %D exceed the 30% and 25% QClimits in the initial and continuing calibrations. The associatedquantitation limits are qualified estimated and flagged "UJ" in thedata summary.

The blank spike recovery for 4-chloro-3-methylphenol exceeded theQC limit. Since spike recoveries have advisory limits, and allmatrix spike recoveries were within QC limits, no qualification isapplied.

flR302597



3*1• Pesticides/PCB

___ Holding Time___ Extraction Time___ Surrogate Recovery___ MS/MSD___ Blank___ Linearity CalibrationX DDT/Endrin Degradation___ Analytical Sequence___DBC Retention TimeX Continuing Calibration___ Retention Time Window___: Standards___ Chromatography___ HSL Compounds___ .Data Completeness

OVERVIEW

This portion of the case consisted of one water sample analyzed forTCL Pesticide/PCB target compounds.

The surrogate recoveries, blank spike recoveries, and calibrationdata met EPA CLP QC criteria. Minor problems associated with thesample analyses are listed below.

ISSUES ~"~

Sample OR-6A required a 2-fold dilution due to high levels of non-target compounds. Positive target compound results were notdetected in this sample. Sample results may be biased low. Noqualification is applied.

Several compounds had %D exceed the 15% and 20% QC limits on thequantitation and confirmation columns. Most affected standardswere analyzed after the samples. Several standards are associatedwith the samples, however, positive target compound results werenot detected. Therefore, no qualification is applied.

Several compounds had retention times exceed the established QClimit; however, the data usability is not affected. Noqualification is applied.


The 4,4-DDT/Endrin breakdown were calculated incorrectly for bothcolumns. The corrected results are reported on the attached FormVIII Pest-1. All breakdown criteria were met with the exception ofEval Mix B 11/07/90 at 03:28. There were no samples associatedwith this standard. No qualification is applied.

Three matrix spike recoveries were outside QC limit. Since spikerecoveries have advisory limits and target compounds were notdetected, no qualification is applied.

AR302599




ATTACHMENTS , - • - : - - -

1. Attachment I - Glossary of.Data Qualifier Codes.




3, Attachment III - Support Documentation

AR302600

semspub.epa.gov · i standard chlorine bdg #clp253 data reviewer: douglas godfrey data supervisor:...

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