DATE

SUBJECT

FROM

TO

UNITED STATES ENVIRONMENTAL PROTECTION AGENCYENVIRONMENTAL SCIENCE CENTER

701 MAPES ROADFORT MEADE MD 20755 5350

SDMS DocID 2032264

March 4, 2002

Region III Data QA Review

Fredrick Forema/Vn/Region III ESAT^RPO (3ES20)

Marjone EastonRegional Project Manager (3HS31)

RECEIVEDMAR 13 2002

Removal Enf & Oil SectionUSEPA Wheeling Office

Attached is the inorganic data validation report for the Big John'sSalvage/Hoult Road Site (Case 30178, SDG# MC03S5) completed by theRegion III Environmental Services Assistance Team (ESAT) contractorunder the direction of Region III ESD

If you have any questions regarding this review or the change informat, please call me at(410) 305-2629

Attachment

cc Younus Burham (E & E)

TO 0001 TDF # 2228

OFFICE OF ANALYTICAL SERVICES AND QUALITY ASSURANCE

Internet Address (URL) http //www epa govRecycled/Recyclable Printed with Vegetable Oil Based Inks on Recycled Paper (Minimum 30 / Postconsumer) AR107529

Lockheed Martin E n v i r o n m e n t a l ServicesUS EPA Env i ronmen ta l Science Cenier701 Mapes Road Ft Meade MD 0755-53501 I t p h o n t - J 0 3 0 5 3 0 3 7 Facs imi le 4 10 305 3597

LOCKHEED MA

DATE February 22 2002

SUBJECT Level IM2 Inorganic Data ValidationCase 30178 SDG MC03S5Site Big John Salvage Hoult Road

FROM Mahboobeh Mecanic^ ̂Senior Oversight Chemist

TO Fredrick ForemanESAT Region 3 Project Officer

Kenneth W CurrySenior Data Reviewer

OVERVIEW

Case 30178 Sample Delivery Group (SDG) MC03S5 consisted of three (3) aqueous samplesSubmitted to Compuchem (LIBERTY) for total metals analysis The sample set included one (1) fieldduplicate pair Samples were analyzed according to Contract Laboratory Program (CLP) Statement ofWork (SOW) ILM04 1 through the Routine Analytical Services (RAS) program

SUMMARY

All samples were successfully analyzed for all analytes Data in this Case have been impacted byoutliers present in laboratory blanks serial dilution and Contract Required Detection Limit (CRDL)standard analyses Details for these outliers are discussed under Minor Problems and qualifiedanalytical results for all samples are summarized on a single Data Summary Form (DSF)

MINOR PROBLEMS

• Preparation (PB) and/or Continuing Calibration Blanks (CCBs) had reported results greaterthan Instrument Detection Limits (IDLs) for antimony (Sb) beryllium (Be) cadmium (Cd) andmercury (Hg) Reported results for these analytes in affected samples which are less than orequal to five times ( 5X) blank concentration may be biased high and have been qualified Bon the DSF

• Recovery of a CRDL standard was low (<90%) for selenium (Se) Low recoveries mayindicate negative biases for results detected near detection limits due to an unstable baselineThe quantitation limits for Se in affected samples MC03S6 and MC03S7 may be biased lowand have been qualified UL on the DSF

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Page 2 of 2

• Recoveries of CRDL standards were high for Cd (> 110%) and Hg (> 130%) Highrecoveries may indicate positive biases for results detected near detection limits due to anunstable baseline Reported results which are less than two tune CRDL (<2XCRDL) for theseanalytes may be biased high and have been qualified "K" unless superseded by "B" on DSF

• Percent Differences (%Ds) for the ICP serial dilution analysis were outside the control limits(10%) for potassium (K) and sodium (Na) These outliers may indicate chemical or physicalinterferences impacting the analyses of these analytes Reported results for K and Na werequalified as estimated "J" on the DSF

NOTES

• Rounding rules used by the laboratory on the Form Is did not conform to the SOWrequirements Rounding rules specified in the SOW were used by the reviewer to reportconcentrations on DSFs Form Is for analytes impacted were corrected by the reviewer

• Matrix spike recovery was high for Se No positive results were reported for this analyte andno data were qualified based on this outlier

All data for Case 30178 SDG MC03S5 were reviewed in accordance with the Region in Modificationto the Inorganic National Functional Guidelines April 1993

ATTACHMENTS

APPENDK A Glossary of Data Qualifier CodesAPPENDDCB Data Summary FormsAPPENDDC C Chain-of Custody RecordsAPPENDK D Laboratory Case Narrative

DCN 30178 MC03S5Nar

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Page 1 of 1

Case 30178 SDGMC03S5

TABLE 1ASUMMARY OF QUALIFIERS ON DATA SUMMARY

FORM AFTER DATA VALIDATION

NON-

ANALYTE

Sb

Be

Cd

Hg

K

Se

Na

SAMPLESAFFECTED

MC03S5

MC03S7

MC03S5

MC03S6 MC03S7

All samples

All Samples

MC03S6 MC03S7

All samples

POSITIVEVALUES

B

B

K

B

B

J

J

DETECTEDVALUES BIAS

High

High

High

High

High

UL Low

COMMENTS*

CCB (2 2 /ig/L)

CCB (0 4 /ig/L)

CRH(111 7% 113

CCB (0 3 /ig/L)CRH(1138% 114

PB (0 112 /ig/L)CRH (140%)

ISD (16 4%)

CRL (89 0%)

ISD (109%)

8%)

5%)

* See explanation of comments in Table IB

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ORIGINAL

Page 1 of 1

TABLE IBCODES USED IN COMMENTS COLUMN

CCB = Continuing Calibration Blanks had results > IDL (the results are in parenthesis)Reported results which are <5X the blank concentration may be biased high

CRH = CRDL standard recoveries were high ( %recovenes are in parenthesis) Reported resultswhich are <2XCRDL may be biased high

PB = The Preparation Blank had a result > IDL (the result is in parentheses) Reportedresults which are < 5X the blank concentration may be biased high

ISD = Percent Difference (%D) for the ICP serial dilution analysis was outside the QC limit(10%) [%D is in parenthesis] Reported results are estimated

CRL = A CRDL standard recovery was low (% recovery is in parenthesis) Quantitation limitsmay be biased low

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X

Appendix A

Glossary of Data Qualifier Codes

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ORIGINAL

GLOSSARY OF DATA QUALIFIER CODES

CODES RELATED TO IDENTIFICATION(confidence concerning presence or absence of analytes)

U = Not detected The associated number indicates approximate sampleconcentration necessary to be detected

(NO CODE) = Confirmed identification

B = Not detected substantially above the level reported in laboratory or fieldblanks

R = Unreliable result Analyte may or may not be present in the sampleSupporting data necessary to confirm result

CODES RELATED TO OUANTITATION(can be used for both positive results and sample quantitation limits)

J = Analyte Present Reported value may not be accurate or precise

K= Analyte present Reported value may be biased high Actual value isexpected to be lower

L = Analyte present Reported value may be biased low Actual value isexpected to be higher

[ ] = Analyte present As values approach the IDL the quantitation may not beaccurate

UJ = Not detected, quantitation limit may be inaccurate or imprecise

UL = Not detected, quantitation limit is probably higher

OTHER CODES

Q = No analytical result

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X

Appendix B

Data Summary Forms

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DATA SUMMARY FORM INORGANIC Page 1 of 1

Case* 30178

Site

Lab

SDG MC03S5

BIG JOHN SALVAGE HOULT ROAD

LIBRTY

Number of Soil Samples 0

Number of Water Samples 3

Sample Number

Sampling Location

Field QC

Matrix

Units

Date Sampled

Time Sampled

Dilution Factor

ANALYTE

ALUMINUM

ANTIMONY

ARSENIC

BARIUM

BERYLLIUM

CADMIUM

CALCIUM

CHROMIUM

COBALT

COPPER

IRON

LEAD

MAGNESIUM

MANGANESE

MERCURY

NICKELiPOTASSIUM

SELENIUM

SILVER

SODIUM

THALLIUM

VANADIUM

ZINC

CRDL

2006010

20055

5000

1050

25100

3

5000

150240

5000

510

5000

105020

MC03S5

BJSW-06

Water

ug/L

2/11/2002

1335

1 0

Result

19000

[24]

[20]

[328]

[22]

[21]

141000

394[477]

29598500

13121700

3860

[013]

841[4840]

15300

[50]

[309]

385

Flag

B

K

B

J

J

MC03S6

BJSW-07

DUP (MC03S7)

Water

ug/L

2/11/2002

1345

10Result

4600

[281]

[21]

[13]

94400

[263]

[53]

103000

4821200

7050

[012]

[348]

[3940]

21900

[91]

606

Flag

B

B

J

UL

J

MC03S7

BJSW-08

DUP (MC03S6)

Water

ug/L

2/1 1/2002

1400

1 0

Result

4480

[18]

[275]

[20]

[13]

91400

[12]

[254]

[53]

99700

51

20700

6860

[014]

[345]

[3960]

21500

107

582

Flag

BB

B

JUL

J

Result Flag Result Flag

CRDL = Contract Required Quantitation Limit

To calculate sample quantitation limits (CRDL Dilution Factor)

Action Level Exists SEE NARRATIVE FOR CODE DEFINITIONS

Revised 09/99

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Appendix C

Cham-of-Custody Records

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Chain of Custody RecordRehnqinshedfby (Signature)

Relinquished by (Signature) v

Relinquished by (Signature)

Date /Time

Dal

Dat

a/Time

a/Time

Received by (Signature)

Received by (Signature)

Received for Laboratory by(Signature)

Relinquished by (Signature)

Relinquished by (Signature)

Date /Time

1Distribution Green Region Copy Pink CLASS Copy ~""EPA Form 9HO-1

White Lab Copy for Return to Region Yellow Lab Copy lor Return to CLASS

Date)

Date)

Time

Time, , ^ J n t , , " 'P '

Received by4 {Signature) f ' ,

Remarks Is custody seal intact? Y/N/none

(8 /99 ) See Raveraa for AddWonal Standard kjtnieoo a\"lyy' See Havana for Purpoae Code DefMUona

on /i one

COHI

CMcHO

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Appendix D

Laboratory Case Narrative

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U S EPA-CLPCOVER PAGE INORGANIC ANALYSES DATA PACKAGE

Lab Name COMPUCHEM Contract 68W00082

Lab Code LIBRTY Case No 30178 SAS No SDG No MC03S5

SOW No ILM04 1

EPA Sample No Lab Sample ID

MC03S5 MC03S5-1MC03S5D WG15778-2MC03S5S WG15778-1MC03S6 MC03S5-2MC03S7 MC03S5-3

Were ICP interelement corrections applied7 Yes/No

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

Comments THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN E TO INDICATE SERIALDILUTION RESULTS WHICH ARE NOT WITHIN CONTROL LIMITS POTASSIUM and SODIUM

I certify that this data package is in compliance with the terms and conditions of thecontract, both technically and for completeness, for other than the conditions detailedabove Release of the data contained in this hardcopy data package and in thecomputer-readable data submitted on diskette has been authorized by the Laboratory Manager orthe Manager s designee as verified by the following signature

Signature V T ^ l f ^ , ^/ f ^ T Name __ g.WVe-'S ](YWlUv\

jl/zJdz _ Title *Sey\\or £/W^s4r 3

COVER PAGE - IN ILM04 1AR107541

CompuChema Division of Liberty Analytical Corp501 Madison Avenue Gary NC 27513

SDG NARRATIVECASE # 30178 SDG # MC03S5

CONTRACT # 68W00082

The indicated Sample Delivery Group (SDG) consisting of three (3) water samples was received into thelaboratory information management system (LIMS) on February 13 2002 intact and in good conditionwith Cham of Custody (COC) Records in order unless otherwise noted in any attachments or QualityAssurance Notices The temperature of the samples upon receipt was 4 C as determined from the coolertemperature indicator bottle

The samples were analyzed in accordance with EPA CLP Statement of Work (SOW) document ILM04 1for the complete Inorganic Target Analyte List (TAL) metals

The correlation coefficient for the mercury analytical run is confirmed to be > 0 9950

EQUATIONS FOR LIQUID SAMPLE CALCULATIONS

Equation for obtaining metals sample results in ug/L as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb)

C x F

I

Where

C = concentration (ng/L)

F = final volume in liters after sample preparation

I = initial volume in liters

Example Aluminum result in ug/L S^f1' MC0!>->S

18955 42 ug/L (C) x 0 05 L (F)= 18955 42 ug/L reported as 19000

0 05 L (I)

5

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OR/GJNAL

Equation for obtaining mercury sample results in ug/L as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb)

C x D x F

I

Where

C = concentration (ug/L) Hg

D = dilution factor to bring sample into analysis range

F = final volume in liters (0 1 L)

I = initial volume in liters

Example Mercury result in ug/L- *~^

0 1288 ug/L(C) x 1 (D) x 0 1 (F) 0 \ * °= ZZ2 u^g/L reported as 0 13 ug/L

0 1 L (I)

SAMPLE IDsThe following customer IDs are associated with this SDGMC03SS MC03S6 MC03S7

INSTRUMENTAL QUALITY CONTROL

All calibration verification solutions (ICV & CCV) blanks (ICB & CCB) and interference check samples(ICSA & ICSAB) associated with this data were confirmed to be within EPA CLP allowable limits

SAMPLE PREPARATION QUALITY CONTROL

The sample preparation procedure verifications (LCSW & PBW) were found to be within acceptableranges and all field samples were prepared and analyzed within the contract specified holding times

MATRIX RELATED QUALITY CONTROL

The sample matrix spike CCN = WG15778 1 (MC03S5S) was found to be outside CLP control limits forSelenium

CLP control limits for matrix spike recoveries are set at 75% to 125% of the analyte quantity added unlessoriginal sample concentrations exceed the true values of these spikes by a factor of four or more In thiscase affected analytes are not flagged even if recoveries are outside percentage recovery control limits

The sample matrix duplicate CCN = WG15778 2 (MC03S5D) was inside CLP control limits for therequested analytes

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CLP control limits for duplicate determinations are +/ 20% Relative Percent Difference (RPD) forconcentrations greater than or equal to five times the CRDL in both the original and duplicate samples and+/ the CRDL for concentrations less than five times the CRDL The RPD is not calculated if both theoriginal and duplicate values fall below the IDL

A five fold serial dilution of sample CCN = SDIMC03S5 1 (MC03S5L) was performed in accordancewith CLP requirements for ICP analysis

The adjusted sample concentrations were outside CLP control limit for Potassium and Zinc which areflagged with an E on all associated Form I and Form IX

CLP control limits for serial dilution are defined as a deviation less than or equal to 10% in the dilutionadjusted concentrations from the original values for all analyte concentrations greater than fifty (50) timestheir respective Instrument Detection Limit (IDL) in the original sample

An E flag indicates that a chemical or physical interference effect was encountered during the analysis ofthat analyte As a result of the interference all values for that analyte in the same matrix must beconsidered estimated values

The laboratory manager or his designee as verified by the following signature has authorized release of thedata contained in this hard copy data package

fames E Medhn/Senior ChemistFebruary 15 2002

1

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