LEVEL IM2 INORGANIC DATA VALIDATION REPORT (COVER … · ESAT Region 3 Project Officer Kenneth W...
Transcript of LEVEL IM2 INORGANIC DATA VALIDATION REPORT (COVER … · ESAT Region 3 Project Officer Kenneth W...
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
AR107530
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
AR107531
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
AR107532
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
AR107533
X
Appendix A
Glossary of Data Qualifier Codes
AR107534
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
AR107535
X
Appendix B
Data Summary Forms
AR107536
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
AR107537
Appendix C
Cham-of-Custody Records
AR107538
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
AR107539
Appendix D
Laboratory Case Narrative
AR107540
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
AR107542
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
AR107543
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
AR107544