\ \ o '/ UNITED STATES ENVIRONMENTAL PROTECTION AGENCY ENVIRONMENTAL SCIENCE CENTER 701 MAPES ROAD FORT MEADE, MD 20755-5350 S °MS DOC/O 2065645 DATE : September 4, 2002 SUBJECT: Region III Data QA_Review FROM : Fredrick Foremai Region III ESAT l^PO (3ES20; TO : Romuald Roman Regional Project Manager (3HS22) r- Attached is the inorganic"data validation report for the Valmont TCE site (Case #: 30647, SDG#: MC002, MC0035, MC0069, MC0078, MC0109, MC0128, MC0143M MC0153) completed by the Region III Environmental Services Assistance Team (ESAT) contractor under the direction of Region III ESD. If you have any questions regarding this review, please call me at (410) 305-2629. Attachments cc: Neil Teamerson (Tetratech NUS) TO File: 0007 TDF#: 0746 OFFICE OF ANALYTICAL SERVICES AND QUALITY ASSURANCE Internet Address (URL) • http://www.epa.gov Recycled/Recyclable ••Printed with Vegetable Oil Based Inks on Recycled Paper (Minimum 30% Postconsumer)
132
Embed
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY '/o · MC0069 Se MC0078 Se Matrix spike recoveries were low (
This document is posted to help you gain knowledge. Please leave a comment to let me know what you think about it! Share it to your friends and learn new things together.
Transcript
\\o'/
UNITED STATES ENVIRONMENTAL PROTECTION AGENCYENVIRONMENTAL SCIENCE CENTER
701 MAPES ROADFORT MEADE, MD 20755-5350
S°MS DOC/O2065645
DATE : September 4, 2002
SUBJECT: Region III Data QA_Review
FROM : Fredrick ForemaiRegion III ESAT l PO (3ES20;
TO : Romuald RomanRegional Project Manager (3HS22)
r-
Attached is the inorganic"data validation report for the ValmontTCE site (Case #: 30647, SDG#: MC002, MC0035, MC0069, MC0078,MC0109, MC0128, MC0143M MC0153) completed by the Region IIIEnvironmental Services Assistance Team (ESAT) contractor under thedirection of Region III ESD.
If you have any questions regarding this review, please call me at(410) 305-2629.
Attachments
cc: Neil Teamerson (Tetratech NUS)
TO File: 0007 TDF#: 0746
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)
Lockheed Martin Environmental ServicesUS EPA Environmental Science Center701 Mapes Road Ft. Meade, MD 20755-5350Telephone 410-305-3037 Facsimile 410-305-3597
L O C K H E E D HI A R
DATE: August 29,2002
SUBJECT: Inorganic Data Validation (IM2 Level)Case: 30647SDGs: MC0002,MC0035,MC0069,MC0078,MC0109,MC0128,
MC0143.MC0153Site: Valmont TGE
FROM:
TO:
OVERVIEW
Kenneth W. CurryInorganic Data Reviewer
Fredrick ForemanESAT Region 3 Project Officer
Mahboobeh Mecanic *Senior Oversight Chemist
Case 30647, Sample Delivery Groups (SDGs) MC0002, MC0035, MC0069, MC0078, MC0109,MC0128, MC0143 and MC0153, from the Valmont TCE site consisted of one hundred thirty-one (131) soil samples and four (4) associated aqueous blanks analyzed for total metals andcyanide (CN~) in addition one (1) aqueous blank was analyzed for total metals only. All sampleswere analyzed by CompuChem (LEBRTY). The sample set included two (2) rinsate blanks, three(3) field blanks and eight (8) field duplicate pairs. Samples were analyzed in accordance withContract Laboratory Program (CLP) Statement of Work (SOW) ILM04.1 through RoutineAnalytical Services (RAS) program.
SUMMARY
All samples were successfully analyzed for all Target Analyte List (TAL) parameters with theexception of those listed under "Major Problem". Areas of concern with respect to data usabilityare listed below.
One (1) field blank was collected 6/24/02 while the remaining field and rinsate blanks werecollected 6/28/02. The samples were collected 6/24/02,6/26/02,6/27/02 and 6/28/02. Due tothe sampling dates of the blanks, the highest detected concentration of an analyte in the rinsateand field blanks were utilized by the reviewer to assess these data for blank contamination.
Data in this case have been impacted by outliers present in laboratory, field and rinsate blanks,sample cooler chest temperature as well as matrix spike, laboratory duplicate, ICP serial dilution,continuing calibration verification, laboratory control sample and Contract Required DetectionLimit (CRDL) standard analyses. Details of these outliers are discussed under "Major and MinorProblems"; specific samples affected are outlined in "Table 1A" and qualified analytical resultsfor all samples are summarized on Data Summary Forms (DSFs).
Page 2 of5
MAJOR PROBLEM
Matrix spike recoveries were extremely low (<30%) for antimony (Sb) in SDG MC0002 and formanganese (Mn) in SDG MC0143. Reported results for these analytes in these SDGs may bebiased extremely low. The "L" qualifier for Mn in SDG MC0143 has been superseded by "J"on the DSFs. Quantitation limits for Sb in SDG MC0002 were rejected and qualified "R".
MINOR PROBLEMS
Continuing Calibration (CCB), Preparation (PB), Field (FB) and/or Rinsate (RB) Blanks hadreported results greater than the Instrument Detection Limits (DDLs) for analytes listed below.Reported results in affected samples which are less than or equal to five times (<5X) blankconcentrations may be biased high and have been qualified "B" on DSFs.
MC0035 CCB aluminum (Al), barium (Ba), Ca, iron (Fe), magnesium (Mg)PB zinc (Zn), CN'
MC0069 CCB Sb, beryllium (Be)FB Ni, NaRB Ca, Mg,
MC0078 CCB Sb, BeFB . Ni,NaRB Ca, Mg,
MC0109 FB Ni,NaRB Ca, Mg,
MC0128 CCB BeFB • Ni, NaRB Ca,CN'
MC0143 CCB Sb, BeFB Ni,NaRB Ca, Mg,
MC0153 CCB Be, thallium (Tl)FB copper (Cu), Ni, NaRB Ca, Mg,
Page 3 of5
Continuing calibration and/or preparation blanks had negative values greater than the absolutevalue of the EDLs for analytes listed below. Reported results less than two times (<2X) theabsolute value of the blank and quantitation limits for these analytes in affected samples may bebiased low and have been qualified "L" and "UL", respectively, on the DSFs unless supersededby "B".
CRDL standard recoveries were low (<90%) for analytes listed below. Low recoveries mayindicate negative biases for results detected near detection limits due to an unstable baseline.Reported result which are <2XCRDL and quantitation limits for these analytes in affectedsamples may be biased low and have been qualified "L" and "UL", respectively, on the DSFs.
SPG Analvte(s)MC0035 lead (Pb)MC0069 Se,zinc(Zn)MC0078 ZnMC0128 SeMC0153 Se,Zn
CRDL standard recoveries were high (>110%) for analytes listed below. High recoveries mayindicate positive biases for results detected near detection limits due to an unstable baseline.Reported results which are <2XCRDL for these analytes in affected samples may be biased highand have been qualified "K" on the DSFs unless superseded by "B".
SPG Analyte(s)MC0002 arsenic (As), Se, ZnMC0069 SeMC0078 Se
Matrix spike recoveries were low (<75%) for analytes listed below. Reported results andquantitation limits for these analytes in these SDGs may be biased low and have been qualified"L" and "UL", respectively, on the DSFs unless superseded by "B".
Matrix spike recoveries were high (>125%) for Pb and Mn in SDG MC0002 as well as for Pb inSDG MCO 109. Reported results for this analyte in these SDGs may be biased high and havebeen qualified "K" on the DSFs.
Relative Percent Differences (RPDs) for laboratory duplicate analyses were outside control limits(35% RPD, ±2CRDL) for As in SDG MC0069 and for Mn in SDG MC0143. Reported resultsfor these analytes in these SDGs are estimated and have been qualified "J" on the DSFs.
Percent Differences (%Ds) for ICP serial dilution analyses were outside control limits (>10%)for analytes listed below. Reported results for these analytes are estimated and have beenqualified "J" on the DSFs unless superseded by "B".
Recoveries of Na in the Laboratory Control Sample (LCS) analyses in SDGs MC0002, MC0109,MC0128 and MC0143 were outside the upper control limit. Reported results for this analyte inthis SDG may be biased high. The "K" qualifier for this outlier has been superseded by "B" onthe DSFs.
The sample coolers had interior temperatures of 7.1 °C and /or 8.0 °C for samples analyzed inSDGs MC0002, MC0035, MC0143 and MC0153 when received by the laboratory. Reportedresults and quantitation limits for CM" in affected samples may be biased low and have beenqualified "L" and "UL", respectively, on the DSFs unless superseded by "B". Due tothermostability of metals, no other data were qualified based on the sample cooler cheststemperature.
Matrix spike recoveries were low (<75%) while CRDL standard recoveries were high (>110%)for Hg in SDG MC0128 and for Se in SDG MCO143, producing opposing bias effects for resultsdetected near detection limits due to an unstable baseline. Reported results which are <2XCRDLfor these analyte? in affected samples in these SDGs are estimated and have been qualified "J" onthe DSFs.
A continuing calibration verification standard recovery was high for Al in SDG MCO 153.Reported results for this analyte in affected samples in this SDG may be biased high and havebeen qualified "K" on the DSFs.
NOTES
The laboratory duplicate results for Mn and Zn in SDG MC0002 as well as for Cr and Fe in SDGMCO 143 were outside the contractual control limit of 20% RPD, ±CRDL. However, the resultsfor these analytes were within the control limit of 35% RPD, ±2XCRDL utilized for datavalidation of soil samples in Region 3. No data were qualified based on these outliers.
Page 5 of 5
The matrix spike recovery for Mn in SDG MC0002 was not considered outside the QC limits bythie laboratory since the result would round down to the upper limit. Laboratory Form Is do notindicate a matrix spike outlier for this analyte in this SDG. The reviewer considered this result asbeing outside the upper QC limit and qualified results accordingly.
Field blank, sample MC0185, was not analyzed for CN". This sample was listed on the Chain ofCustody (COC) record for CN' analysis.
Reported results for the field duplicate pairs were within 35% RPD, ±2XCRDL for all analytesexcept for those listed below.
Data for Case 30647, SDGs MC0002, MC0035, MC0069, MC0078, MC0109, MC0128,MC0143 and MC0153, were reviewed in accordance with National Functional Guidelines forEvaluating Inorganic Analyses with Modification for use within Region in.
ATTACHMENTS
INFORMATION REGARDING REPORT CONTENT
Table 1A is a summary of qualifiers applied to the laboratory- generated results during datavalidation.
TABLE 1A SUMMARY OF QUALIFIERS ON DATA SUMMARY FORMS AFTERDATA VALIDATION
TABLE IB CODES USED IN COMMENTS COLUMN OF TABLE 1AAPPENDIX A GLOSSARY OF DATA QUALIFIER CODESAPPENDIX B ~ DATA SUMMARY FORMSAPPENDIX C CHAIN OF CUSTODY (COC) RECORDSAPPENDIX D LABORATORY CASE NARRATIVES
MSB = Matrix spike recoveries were extremely low (<30%) [% recoveries are inparenthesis]. Reported results may be biased extremely low. Quantitation limitsare unusable.
CRH = CRDL standard recoveries were high (>110%) [% recoveries are in parenthesis].Reported results which are <2XCRDL may be biased high.
RB = Rinsate blanks had results > IDL (results are in parenthesis). Reported resultswhich are less than five times (<5X) blank concentrations may be biased high.
MSH = Matrix spike recoveries were high (>125%) [% recoveries are in parenthesis].Reported results may be biased high.
ISD = Percent differences (%Ds) for ICP serial dilution analyses exceeded control limits(10%) [% Ds are in parenthesis]. Reported results are estimated.
FB = Field blanks had results > DDLs (results are in parenthesis). Reported results whichare less than five times (<5X) the blank concentration may be biased high.
MSL = Matrix spike recoveries were low (<75%) [% recoveries are in parenthesis].Reported results and quantitation limits may be biased low.
CCB = Continuing calibration blanks had results > IDLs (results are in parenthesis).Reported results which are less than five times (<5X) the blank concentration maybe biased high. !
LCH = Laboratory Control Sample (LCS) recoveries were high (>120%) [% recoveries arein parenthesis]. Reported results may be biased high.
CHT = The sample cooler temperature was outside the required temperature range (4 °C ±2°C) [sample cooler temperature is in parenthesis]. Reported results andquantitation limits may be biased low.
PEN = Preparation blanks had negative results with absolute values greater than the IDLs(results are in parenthesis). Reported results less than two times (<2X) the absolutevalue of the blank and quantitation limits may be biased low.
CRL = CRDL standard recoveries were low (<90%) [% recoveries are in parenthesis].Reported results which are <2XCRDL and quantitation limits may be biased low.
PB = Preparation blanks had results > IDLs (results are in parenthesis). Reported resultswhich are less than five times (<5X) the blank concentration may be biased high.
Page 2 of 2
TABLE IBCODES USED IN COMMENTS COLUMN
DUP = The Relative Percent Difference (RPD) for the laboratory duplicate analysis wasoutside control limits (35%, ±2XCRDL) [RPD is in parenthesis]. Reported resultsare estimated.
CBN = Calibration blanks had negative results with absolute values greater than the IDLs(results are in parenthesis). Reported results less than two times (<2X) the absolutevalue of the blank may be biased low.
CVH = Continuing calibration verification standard recoveries were high (>110%) [%recoveries are in parenthesis]. Reported results may be biased high.
APPENDIX A
Glossary of Qualifier Codes
GLOSSARY OF DATA QUALIFIER CODES (INORGANIC)
CODES RELATED TO IDENTIFICATION(confidence concerning presence or absence of analytes):
U = Not detected. The associated number indicates approximate sample concentrationnecessary to be detected.
(NO CODE) = Confirmed identification.
B = Not detected substantially above the level reported in laboratory or field blanks.
R = Unusable result. Analyte may or may not be present in the sample. Supporting datanecessary 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 is expected to belower.
L = Analyte present. Reported value may be biased low.Actual value is expected to be higher.
[ ] = Analyte present. As values approach the IDL the quantitation may not be accurate.
UJ = Not detected, quantitation limit may be inaccurate or imprecise.
UL = Not detected, quantitation limit is probably higher.
Concentration: L = Low, M = Low/Medium, H = High Type/Designate:Composite = C, Grab = G
Metals and Cyanide
ature
*S
Chain of Custody Seal Number:
v/ \/Custody Seal lntact?> 1 Shipment Iced Y
I
FR Number: 3-424838327-062502-0001 | A o $ > p 4 y:f> p y f\1 results. Requests for preliminary results will increase analytical costs. i^r^fiwf' ^ 8%%>^"*>. n W % 'K & ^Laboratory Analytical Services Support, 2000 Edmund Halley Dr., Reston, VA. 20191-3436 Phone 703/264-9348 Fax 703/264-922 F2V5.0.66 Page 2 of 3
SEPA USEPA Contract Laboratory ProgramInorganic Traffic Report & Chain of Custody Record
Date Shipped: 6/25/02
Carrier Name: FedEx
Airbill: 828684709982
Shipped to: Liberty Analytical501 Madison AvenueGary NC 2751 3(919)379-4080
Chain of Custody RecordRelinquished By (Date / Time)
1£LAY\ -X 6/l5/oL '00
2
3
4
Sampler —rs. vvl \ •Signature' •!••* -SM ^ \
/R§Ce|ved By [) (Date / Time)
/teftM\(lulli9 tofa'Crts~ I W>
Case No: 30647
DAS No: 1SDGNo: MCjoo^MCjooesL.For Lab Use Only ' COLab Contract No: VO^ xfoOCfeS £",
07/22/02 01:59 PM Subject: inorganic portion of 30647, Valmont TCE: need Regional copies ofsome COC's and memo to file
Dear Neil: We need the Regional copies of the COC/TR's 3-424838327-062502-001 pages onethrough three. We need the field QC information and duplicate pairs.
Memo to file needed for the following errors/discrepancies:1. Sampler did not sign/relinquish COC pages 2 and 3 of 3-424838327-070102-002. You need to state inthe memo who relinquished the samples and the date and time of relinquishment.2. Sample MC0005 was listed on COC page one of 3-424838327-062502-01 but was not shipped, per labdocumentation. -The lab did receive sample MC0004, tag 3-115 sampled 6-24-02 @ 9:55 from stationlocation SB-DOO-0206 which is not listed on the COC. Sampler will please delete MC0005 and addMC0004 by memo to file.3. Tag 3-878 was crossed off on the lab copy of the COC for sample MC0185 but the cyanide analysiswhich would have been done on this aliquot was not crossed off. Also the cross through was no dated.The lab analyzed the total metals aliquot only. Sampler will please indicate who cancelled the cyanidealiquot and on what date and confirm that the cyanide analysis and tag 3-878 were indeed cancelled, ifthat was the intent.4. Tags listed on the COC for sample MC0078 are 3-423 and 3-515. Tag number 3-423 is incorrect. Theactual tag number is 3-424.5. Tags listed on COC for MC0073 are 3-402 and 3-523. Tag #3-4-3 is incorrect on the COC. The actualtag number for MC0073 is 3-404.6. Neither the tag nor the COC list a sample collection time for MC0087.
For the very large number of samples collected on the inorganic portion of this case alone, thedocumentation errors were minimal. Good job.
Judy SnyderESAT Auditor, Region 3Lockheed Martin Environmental Services701 Mapes RoadFt. Meade, MD 20755-5350Phone 410-305-3015Fax 410-305-3095
TETRA TECH NUS, INC.600 Clark Avenue, Suite 3 • King of Prussia, PA 19406-1433(610) 491-9688 • FAX (610) 491-9645 • www.tetratech.com
Subject: Memo to FileCase Number 30647Valmont TCE,J-iazleton, Pennsylvania
Dear Ms. Snyder:
This is a memo to correct documentation errors for the Valmont TCE sampling event.
• Sampler Neb Dedic should have signed and relinquished pages 2 through 5 forCOC 3-424838327-070102-002 on 07/01/02 at 20:00.
• The inorganic soil sample MC0005 listed on Traffic Report (TR) # 3-424838327-062502-01 for TM/CNanalysis is incorrectly listed. A correction should be made to list sample MC0004 collected on 6/24/02 at09:55 instead of sample MC0005 collected on 6/24/02 at 10:00.
• Sampler Neb Dedic crossed off the tag # 3-878 for sample MC0185, the cyanide analysis should also havebeen crossed off and the changes should have been initialed and dated by the sampler.
• Tags listed on the COC for sample MC0078 are 3-423 and 3-515. Tag number 3-423 is incorrect. The actualtag number is 3-424.
• Tags listed on the COC for sample MC0073 are 3-403 and 3-523. Tag # 3-403 is incorrect on the COC. Theactual tag number for MC0073 is 3-404.
/• The collection time for sample MC0087 was 13:40 on 6/26/02, this information was mistakenly omitted from
the COC and the lag.
We apologize for the inconvenience. Please do not hesitate to call if you have any questions.
Respectfully,
Daniel Hartigan
DH/vh
Romuald Roman (EPA Region 3)Neil Teamerson (TtNUS)File No. 3.2
I forgot to send you an e-mail about this. Sample MC0185 is listed as TM/CN, -but we only received TM. If youtake a look at the traffic report the sampler marked the CN tag number out, but did not nnark the CN off from theanalysis colume. Please see attachment.
Melissa StevensEPA Coordinator(919)379-4081CompuChem a division of Liberty [email protected]
•"> ! PX<~ *-»*
07/16/02
TETRA TECH NUS, INC.600 Clark Avenue, Suke 3 • King of Prussia, PA 19406-1433 /• /(610) 491-9688- FAX (610) 491-9645. www.tetratech.com '' / Jin
• />/*nPHIL-16367 ; ///V^7'-
\ / A 5 " r% '\ T-'I <r~* i f°*t «..*,'. . • ' " * • • •'!''•'Project Number 4192 V AlJ DATUM 8 CCr Y -
July 2, 2002
Ms. Betty Ann JefferyUnited States Environmental Protection Agency, Region 3Office of Analytical Services and Quality AssuranceThe Environmental Science Center701 Mapes RoadFort Meade, Maryland 20755-5350
Subject: Case Number 30647Valmont TCEMemo to File
Dear Ms. Jeffery: '
In response to sample listing issue regarding the-case # 30647:
The inorganic soil sample MC0005 listed on Traffic Report (TR) # 3-4248327-062502-0001 forTM/CN analysis is incorrectly listed. A correction should be made and list sample MC0004collected on 6/24/02 at 09:55 instead the sample MC0005 collected on 6/24/02 at 10:00.
We apologize for the erroneous sample listing on the Chain of Custody documents and causingthe discrepancy. Thank you for your cooperation and please contact us if you need additionalinformation in solving this issue.
Respectfully,
Neb DedicEarth Scientist
ND/vh
Roman Romuald (EPA Region 3)Dan Slizys (EPA Region 3)Holly Rogers (CLASS)
Sent: Friday, June 28, 2002 9:23 AMSubject: Region 03 | Case 30647 | Lab LIBRTY | Issue TR/COC discrepancy - sample level | FINALAlice,
Following is the resolution from Region 3 regarding the TR discrepancy issuefor Case 30647. Per the Region, the lab should note the issue in theCase/SDG narrative and proceed with the analysis of the samples. Thesampler has been instructed to write a memo to file to clear up thediscrepancy.
Please let me know if you have any other questions or problems.
The Region III CST Brokerage is waiting for the field personnel to respondto this issue. The field personnel are the only ones that can resolve thisissue. They will have to write a memo to file for TR/COC discrepancy.The lab should proceed with the analysis of samples and document this issuein the case narrative.
Original MessageFrom: [email protected] [mailto:[email protected]]Sent: Thursday, June 27, 2002 1:09 PMTo: Rogers, Holly; [email protected]; [email protected];[email protected]: Betty Ann Jeffery (E-mail); John Kwedar (E-mail); Khin-Cho Thaung(E-mail)Subject: Re: NEW ISSUE | Case.30647 | Lab LIBRTY | Issue TR/COC discrepancy- sample level
Everyone,
The field personnel will have to investigate and resolve this sampleidentity issue on TR/COC. They are requested to provide feedback assoon as possible so analysis of samples would not be impeded.
Original MessageFrom: Rogers, HollySent: Wednesday, June 26, 2002 2:23 PMTo: Betty Ann Jeffery (E-mail); Dan Slizys (E-mail); John Kwedar (E-mail);Khin-Cho Thaung (E-mail)Subject: NEW ISSUE | Case 30647 | Lab LIBRTY | Issue TR/COC discrepancy -sample levelImportance: High
Following is an email from LIBRTY regarding samples received on 6/26 forCase 30647.
s
Soil sample MC0005 was listed on the TR for TM/CN analysis but was notreceived by the lab. However, the lab did receive soil sample MC0004, whichwas not listed on the TR. The sample collection date and,time listed forsample MC0005 is 6/24 09:55. The sample collection date and time listed onthe tag for sample MC0004 is 6/24 10:00.
Original MessageFrom: Alice Evans [mailto:[email protected]]Sent: Wednesday, June 26, 2002 1:53 PMTo: Rogers, HollySubject: Case 30647Importance: High
Holly,
Liberty received 20'soils and 1 water for Total Metals and Cyanides on06/26/02.
1. Received sample MC0004 which is not listed on the Traffic Report. Thesample Date is 06/24/02, the time collected is 09:55 (label on thebottle). Soil - 8 oz jar. Tag no. 3-115.
279
t)6/28/02
2. Sample MC0005 is listed on the Traffic Report but we did not receivedthe sample (date collected: 06/24/02, Time 10:00) Soil.
Thanks,Alice
Alice EvansCompuChem/Liberty501 Madison AveCary,NC 27513919-379-4080
Sent: Wednesday, July 03, 2002 10:19 AMSubject: Region 03 | Case 30647 | Lab LIBRTY | Issue TR/COC discrepancy - sample level | FINALAlice, , u
Following is the resolution from Region 3 regarding the TR discrepancy forCase 30647. Per the Region, the lab should document the issue in theCase/SDG narrative and proceed with the analysis of the samples.
I f - y o u have any other questions or problems, please let me know.
Original MessageFrom: [email protected][mailto:[email protected]]Sent: Wednesday, July 03, 2002 10:12 AMTo: Rogers, HollyCc: Dan Slizys (E-mail) ; John Kwedar (E-mail); Khin-Cho Thaung (E-mail)Subject: Re: NEW ISSUE I Case 30647 | Lab LIBRTY I Issue TR/COC discrepancy- sample level
Holly, the lab must document the TR/COC discrepancy in the case narrativeand continue with the analysis.. Thanks
Original MessageFrom: Rogers, HollySent: Monday, July 01, 2002 1:08 PM OO1
381
07/11/02
Page 2 of 2
To: Betty Ann Jeffery (E-mail); Dan Slizys (E-mail); John Kwedar (E-mail);Khin-Cho Thaung (E-mail)Subject: NEW ISSUE I Case 30647 | Lab LIBRTY | Issue TR/COC discrepancy -sample levelImportance: High
This is Jessica Brown, Holly is out for the day.
Per LIBRTY, the sample collection time was not listed on the TR/COC,received 6/29/02, for sample MC0087, Case 30647. Please advise on how thelab should proceed.
Thanks,Jessica
11:07AM 7/01/02Jessica Brown, SMO, spoke with" Alice Evans, LIBRTY, concerning Case 30647.The sample collection time was not listed on the TR/COC for sample MC0087.
Holly RogersDynCorp Systems and Solutions LLCCLP Coordinator for Regions 3 & 9703-264-9526holly, [email protected] <iuailto:holly. roqers@dyncorp. com>
382
07/11/02
Region III Sample Scheduling Request Form
RASCASENo:CT1363 / 3O (s>^=^
Date:
DAS No:
Data Validation Level: M-3 *f "$. r^J - 3_
Site Name: Valmont Rlitmlil'Jl ParltSitc- / CL-fc:
~~ TA I— •-•-xE.' 'sl ^ f C«-/'J>A-1» A-<4_ //3^>9
'A( fOi^tc^lS / Cc/3ru<^-£- ' f 5 ™ f)
\
MATRIX
Soil
AQ
AQ
^0. /
^J l" *")/\ \i<_
NOTE: Data validation levels M3 & IM2 require justification. QC field samples must be included as part of total number of samples.
1. Special Instructions: Send results to: Neil Teamerson, Tetra Tech NUS 600 Clarke Ave., Ste. 3, King of Prussia, PA 194062. Objectives / Project Plan ID / Permit ID: validated data used later for risk assessment: (Not Drinking Water)3. Program / Project / Permit Reporting Limits According to method used.4. DQO (QC Requirements) According to method used.
Teamerson, Neil" To: Lisa Penix/ESC/R3/USEPA/US@EPA<TeamersonN@TTNus. cc:Com> Subject: FW: Valmont Soil Samples
08/20/02 11:14 AMVALIDATOR'S COPY
> Original Message> From: Teamerson, Neil> Sent: Friday, August 16, 2002 1:21 PM> To: '[email protected]'> Subject: Valmont Soil Samples>> MC0031 (SS-DUP-01) is the dup of MC0030 (SS-G500-0002)>> MC0018 (SB-DUP-01) is the dup of MC0017 (SB-J250-0709)>> Neil Teamerson> Tetra Tech NUS, Inc. (TtNUS)> 600 Clark Avenue, Suite 3> King of Prussia, PA 19406-1433> (610) 491-9688> .(610) 491-9645 (facsimile)> [email protected]
APPENDIX D
Laboratory Case Narrative
Lab Name: COMPUCHEM
Lab Code: LIBRTY
U. S, EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Comments: THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN "E" TO INDICATE SERIALDILUTION RESULTS WHICH ARE NOT WITHIN CONTROL LIMITS:
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 the computer-readable datasubmitted on diskette has been authorized by the Laboratory Manager or the Manager's designee, asverified by the following signature.
Signature ;•
Date:
Name:
Title:
iCOVER PAGE - IN ILM04.1
U. S. EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Lab Name: COMPUCHEM \ Contract: 68W00082
Lab Code: LIBRTY Case No.: 30647 SAS No.: SDG No.: MC0002
SOW No. : ILM04.1
EPA Sample No. Lab Sample ID.
MC0033 MC0002-62
Were ICP interelement corrections applied? Yes/No YES
Were ICP background corrections applied? Yes/No YESIf 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:MACTTTT.CiTTTM
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 the computer-readable datasubmitted on diskette has been authorized by the Laboratory Manager or the Manager' s designee, asverified by the following signature.
Signatures —T *- ^ •/ • L yV-X . Name:
f] f] QDate: (Ju (x/ ' C/-U (L. Title:
71
COVER PAGE - IN ILM04.1
CompuChema Division of Liberty Analytical Corp.•501 Madison Avenue Cary.NC 27513
SDG NARRATIVECASE # 30647 SDG # MC0002
CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of twenty (20) soil samples was received into thelaboratory information management system (LIMS) on June 26, 2002; intact and in good condition \vithChains of Custody (COC) Records in order, unless otherwise noted in any attachments or QualityAssurance Notices. Sample ID's reported in this data package are noted by the receiving department on theCOC if they differ from those listed by the samplers on the COC.
The samples were analyzed, in accordance with EPA - CLP Statement of Work (SOW) document ILM04.1for CLP TAL total metals and cyanide.
The correlation coefficients for the mercury and cyanide analytical runs are confirmed to be > 0.9950.
The cooler temperature bottle was present with samples received on June 26, 2002; and sampletemperature was 7.1 degrees Celsius.
LIBRTY did not receive sample MC0005 (with collection date and time 06/24/02 - 10:00) as listed on theTraffic Report but received sample MC0004 (with collection date and time 06/24/02 - 9:55). "
The Laboratory Control Sample (LCS) for sodium analyzed outside the control limits established for thatanalyte. Sodium is present in the LGS below the CRDL. Thus, the control limits are only advisory limits.
EQUATIONS FOR SOLID SAMPLE CALCULATIONS:
Client sample MC0020 is used for illustration.
Any sample result that is < the instrument detection limit (IDL) will be entered at the IDL for thatanalyte.
ICP Equation:Equation for obtaining metals sample results in mg/Kg as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb).
C x D x VConcentration (% solids) (mg/Kg)
W x SWhere
C = concentration (ug/L)D = dilution factorV = final volume in liters after sample preparationW = weight in grams of wet sampleS = % solids/100
Example: aluminum result ug/L to mg/Kg.52195.07 ug/L (C) x 1 (D) x 0.2 L(V)
= 11943.95 mg/Kg reported as 11900 mg/Kgl .Og(W) x 0.874 (S)
Mercury Equation:
Equation for obtaining mercury sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/L HgB = wet weight of sampleD = dilution factor to bring sample into analysis rangeE = % solids/100F = final volume in liters (0.1 L)
Example: mercury result ug/L to mg/Kg0.1307 ug/L (A) x 1(D) x 0.1 (F)
= 0.0748 mg/Kg reported as 0.075 mg/Kg0.2 g(B) x 0.874 (E) :
Cyanide Equation:
Equation for obtaining cyanide sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/LCNB = wet weight of sampjeD = dilution factor to bring sample into analysis rangeE = %solids/100F = final volume in liters (0 05 L)
Example: cyanide result ug/L to mg/Kg0.887464 ug/L (A) x 1 (D) x 0.05 L (F)
= 0.0508 mg/Kg reported as 0.051 mg/Kgl.OOg(B) x 0.874 (E)
SAMPLE IDs:f
The following customer IDs are associated with this SDG:
MC0002 MC0004 MC0012 MC0014 MC0015 MC0017
MC0018 MC0020 MC0021 MC0022 MC0023 MC0024
MC0025 MC0027 MC0028 MC0029 MC0030 MC0031
MC0032 MC0033
7
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 (LCSS & PBS) were found to be within acceptable rangesand all field samples were prepared and analyzed within the contract specified holding times.
MATRIX RELATED QUALITY CONTROL:
The sample matrix spike, CCN = WG18450-1 (MC0020S) was found to be outside CLP control limits forantimony, lead, and selenium. The reported concentrations for these analytes are flagged with an "N" onall associated Form 1 and on Form 5a.
An "N" indicates a matrix-related interference in the sample preparation procedure &/or analysis for theflagged analyte. This is normally the consequence of a relatively high anionic content in the sample or (forsome sediments) an inconsistent sample matrix relative to that analyte.
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.
Post-digestion spikes are mandatory for analytes demonstrating unsatisfactory matrix spike recoveriesduring ICP analysis (excluding silver). The results of such spikes are presented on Form 5b.
Unsatisfactory recovery of post-digestion spikes of this type do not have bearing upon the aforementioned"N" flags, but may indicate interference during analysis &/or a solution matrix which is hostile to theanalyte in question.-
Satisfactory recovery of an analyte in a post-digestion spike of this type implies interference by therequired preparation procedure or in the sample matrix itself. Lack of uniformity for an analyte insediments will also result in satisfactory recovery of post-digestion spikes after failure in the related matrixspike.
The sample matrix duplicate, CCN = WG 18450-2 (MC0020D) was outside CLP control limits formanganese and zinc. The reported concentrations for these analytes are flagged with a "*" on allassociated Form 1 and on Form 6.
A "*" indicates a non-homogeneous sample matrix in regard to the flagged analyte. This is normally theconsequence of a relatively coarse texture or of a mixed-matrix in sediment samples.
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 = MC0002-50 (MC0020L) was performed in accordance withCLP requirements for ICP analysis.
The adjusted sample concentrations were outside CLP control limits for magnesium and zinc, which areflagged with an "E" on all associated Form 1, the Cover Page and Form 9.
8
An "E" indicates that a chemical or physical interference effect was encountered during the analysis of theflagged analyte. As a result of this interference, all values for the analyte in the same matrix must beconsidered to be estimated quantities.
CLP control limits for serial dilution are defined as a deviation less than or equal to 10% in the dilution-adjusted concentrations from the original values for all analyte concentrations with values greater thanfifty (50) times their respective Instrument Detection Limit (IDL) in the original sample.
The laboratory manager or his designee, as verified by the following signature has authorized release of thedata contained in this hard copy data package.
Thomas R. ColeData Reviewer IIJuly 9, 2002
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
DATA REPORTING QUALIFIERS FOR INORGANICS
On Form I, under the column labeled "C" for concentration qualifier and "Q" for qualifier, each result is flagged with the specific datareporting qualifiers listed below, as appropriate. Up to five qualifiers may be reported on Form I for each analyte.
The C (concentration) qualifiers used are:
U: This flag indicates the analyte was analyzed for but not detected. This reported value was obtained from a reading thatwas less than the Instrument Detection Limit (1DL). The 1DL will be adjusted to reflect any dilution and, for soils, the
percent moisture.
B: This flag indicates the analyte was analyzed for and the reported value was obtained from a reading that was less than theContract Required Detection Limit (CRDL) but .greater than or equal to the Instrument Detection Limit (IDL).
The Q qualifiers used are:
E: This flag indicates an estimated value. This flag is used:
1. When the serial dilution (a five fold dilution for CLP and a five fold dilution for SW-846 method 601 OB) results arenot within 10%. The analyte concentration must be sufficiently high (minimally a factor of SOX above the IDL inthe original sample).
2. When the analytical spike recovery associated with the sample is below 40% after two successive dilutions byGraphite Furnace Atomic Absorption (GFAA).
M: This flag applies to GFAA analyses for concentrations greater than the Contract RequiredDetection Limit (CRDL). This flag is only used for GFAA if the analytical sample or analyticalspike duplicate injection reading is not within 20% of the Relative Standard Deviation (RSD).
N: This flag indicates the sample spike recovery is outside of control limits:
*: This flag is used for duplicate analysis when the sample and the sample duplicate results are notwithin control limits.
S: This flag applies to GFAA analyses to indicate the reported value was determined by theMethod Of Standard Addition (MSA).
\V: This flag applies to GFAA analyses when the post-digestion spike (analytical spike) is out of control limits (85% -115%),while sample absorbance is less than 50% of "spike" absorbance ["spike" is defined as (absorbance or concentration ofspike sample) minus (absorbance or concentration of the sample)].
+; This flag applies to GFAA analyses when the correlation coefficient for the MSA is less than 0.995 after two MSAanalyses.
NOTE: Entering "S", "W", or"+" is mutually exclusive. No combination of these qualifiers can appear in the same field for ananalyte.
The extensions: D, S, SD, L. A, added to the end of the client ID represent as follows:D: matrix duplicateS: matrix spikeSD: matrix spike duplicateL: serial dilution ,A: post digestion spike
Were ICP interelement corrections applied? Yes/No YES
Were ICP background corrections applied? : Yes/No
If yes-were raw data generated beforeapplication of background corrections? Yes/No NO
Comments:
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: (Lj&vK jiia^S? (j^e££J~ Name: . feWVeS. W
Date: // _ 7 / / (f Id 2 _ Title: "Se VN \C> r
COVER PAGE - IN ILM04.1
CompuChema Division of Liberty Analytical Corp.'501 Madison Avenue Gary, NC 27513
SDG NARRATIVECASE # 30647 SDG # MC0035
CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of five (5) water samples was received into thelaboratory information management system (LIMS) on June 26,29, and July 2, 2002 intact and in goodcondition with Chain of Custody (COC) Records in order, unless otherwise noted in any attachments orQuality Assurance Notices. The temperature of the samples received on June 26, 2002 was 7.1°C. Thetemperature of the samples received on June 29,2002 was 3°C. The temperature of the samples received onJuly 2, 2002 was 8°C. Cooler temperature indicator bottles were present with all shipments.
Sample MC0185 is listed on the Traffic Report as TM/CN. It appears that the Sampler crossed out the tagnumber for the Cyanide fraction. The Laboratory only received a TM fraction for this sample, and onlyreported results for TAL metals.
All samples in this SDG are identified on the Traffic Report as Field QC. No matrix related QC sampleswere analyzed.
The samples were analyzed, in accordance with EPA CLP Statement of Work (SOW) document ILM04.1for the complete Inorganic Target Analyte List (TAL).
The correlation coefficient for the mercury and cyanide analytical runs are 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 |ig/L (ppb).
C x F
1
Where
C = concentration (ug/L)
F = final volume in liters after sample preparation
I = initial volume in liters
Example: Aluminum result in ug/L
30.92848 ug/L (C) x 0.05 L (F)-- = 30.92848 ug/L reported as 30.9 ug/L0.05 L (I)
Equation for obtaining cyanide sample results in ug/L as presented on FORM I data sheets from instrumentacquired results in ug/L (ppb).
C x F x D
I
Where
C = concentration (ug/L) CN
F = final volume
D = dilution factor to bring sample into analysis range
I = initial volume in liters
Example: cyanide result in ug/L
0.390252 ug/L (C) x 1 (D) x 0.05 L (F)= 0.390252 ug/L reported as 0.60 ug/L *
0.05 L (F)
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)
1 = initial volume in liters
Example: Mercury result in ug/L
0.0882 ug/L (C) x 1 (D) x 0.1 (F)= 0.0882 ug/L reported as 0.10 ug/L *
* This result reported down to the IDL.
SAMPLE IDs:The following customer IDs are associated with this SDG:MC0035 MC0141 MC0142 MC0184 MC0185
INSTRUMENTAL QUALITY CONTROL:
All calibration verification solutions (ICV & CCV), blanks (IGB, & CCB), and interference check samples(1CSA & 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.
The laboratory manager or his designee, as verified by the following signature has authorized release of thedata contained in this hard copy data package.
I forgot to send you an e-mail about this. Sample MC0185 is listed as TM/CN, but we, only received TM. If youtake a look at the traffic report the sampler marked the CN tag number out, but did not mark the CN off from theanalysis colume. Please see attachment.
Melissa Stevens•EPA Coordinator(919)379-4081CompuChem a division of Liberty [email protected]
807/16/02
U. S. EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
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:. K-
Date: iJijt / b,
Name:
Title: \) \AJ-t l\ 4 )
•COVER PAGE - IN ILM04.1
U. S. EPA - CLP
COVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Lab Name: COMPUCHEM Contract: 68W00082
Lab Code: LIBRTY Case No.: 30647 SAS No.: SDG No.: MC0069
SOW No.: ILM04.1
EPA Sample No. Lab Sample ID.
MC0089 . MC0069-20
Here ICP interelement corrections applied? Yes/No YES
Were ICP background corrections applied? Yes/No YESIf yes-were raw data generated beforeapplication of background corrections? Yes/No NO
Comments:
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.:_ jksMo L Kr • ( JJj2— Name: I /Vl U/LS ./H
Date: JltiL, ' *> . /7*OQ<s*- Title:
COVER PAGE - IN ILM04.1
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Gary, NC 27513
SDG NARRATIVECASE # 30647 SDG # MC0069
CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of twenty (20) soil samples was received into thelaboratory information management system (LIMS) on June 29, 2002; intact and in good condition with
• Chains of Custody (COC) Records in order, unless otherwise noted in any attachments or QualityAssurance Notices. Sample ID's reported in this data package are noted by the receiving department on theCOC if they differ from those listed by the samplers on the COC.
The samples were analyzed, in accordance with EPA - CLP Statement of Work (SOW) document ILM04.1for CLP TAL total metals and cyanide.
The correlation coefficients for the mercury and cyanide analytical runs are confirmed to be > 0.9950.
The cooler temperature bottle was present with samples received on June 29, 2002; and sampletemperature was 3.0 degrees Celsius.
The collection time is missing from the Traffic Report for sample MCOOS7. Per Region 3, the sample wasanalyzed.
EQUATIONS FOR SOLID SAMPLE CALCULATIONS:
Client sample MC0073 is used for illustration.
Any sample result that is < the instrument detection limit (IDL) will be entered at the IDL for thatanalyte.
ICP Equation:
Equation for obtaining metals sample results in mg/Kg as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb).
C x D x VConcentration (% solids) (mg/Kg)
W x SWhere
C = concentration (ug/L) ,D = dilution factorV = final volume in liters after sample preparationW = weight in grams of wet sampleS = %solids/100
Example: aluminum result ug/L to mg/Kg.28361.53 ug/L (C) x 1 (D) x 0.2 L (V)
=6178.98 mg/Kg reported as 61 SO mg/Kg1.0 g(W) x 0.918 (S)
Mercury Equation:
Equation for obtaining mercury sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/L HgB = wet weight of sampleD = dilution factor to bring sample into analysis range •E = % solids/100
. F = final volume in liters (0.1 L)Example: mercury result ug/L to mg/Kg0.10 ug/L* (A) x 1(D) x 0.1 (F)
= 0.05447 mg/Kg reported as 0.054 mg/Kg*0.2 g(B) x 0.918 (E)
* The result is reported down to the instrument detection limit.
Cyanide Equation:
Equation for obtaining cyanide sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/LCN 'B = wet weight of sampleD = dilution factor to bring sample into analysis range
• E = % solids/100F = final volume in liters (0 05 L)
Example: cyanide result ug/L to mg/Kg1.204136 ug/L (A) x 1 (D) x 0.05 L (F)
= 0.06558 mg/Kg reported as 0.066 mg/Kgl.OOg(B) x 0.918 (E)
SAMPLE IDs:
The following customer IDs are associated with this SDG:
MC0069 MC0070 MC0071 MC0072 MC0073 MC0074
MC0075 MC0076 MC0077 MC0079 MC0080 MC0081
MC0082 MC0083 MC0084 MC0085 MC0086 MC0087
MC0088 MC0089
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 (LCSS & PBS) were found to be within acceptable rangesand all field samples were prepared and analyzed within the contract specified holding times.
MATRIX RELATED QUALITY CONTROL:
The sample matrix spike, CCN = WG18532-1 (MC0073S) was found to be outside CLP control limits forantimony, manganese, mercury, and thallium. The reported concentrations for these analytes are flaggedwith an "N" on all associated Form 1 and on Form 5a.
An "N" indicates a matrix-related interference in the sample preparation procedure &/or analysis for theflagged analyte. This is normally the consequence of a relatively high anionic content in the sample or (forsome sediments) an inconsistent sample matrix relative to that analyte.
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.
Post-digestion spikes are mandatory for analytes demonstrating unsatisfactory matrix spike recoveriesduring ICP analysis (excluding silver). The results of such spikes are presented on Form 5b.
Unsatisfactory recovery of post-digestion spikes of this type do not have bearing upon the aforementioned"N" flags, but may indicate interference during analysis &/or a solution matrix which is hostile to theanalyte in question.
Satisfactory recovery of an analyte in a post-digestion spike of this type implies interference by therequired preparation procedure or in the sample matrix itself. Lack of uniformity for an analyte insediments will also result in satisfactory recovery of post-digestion spikes after failure in the related matrixspike.
The sample matrix duplicate, CCN = WG 18532-2 (MC0073D) was outside CLP control limits for arsenic.The reported concentration for this analyte is flagged with a "*" on all associated Form 1 and on Form 6.
A "*" indicates a non-homogeneous sample matrix in regard to the flagged analyte. This is normally theconsequence of a relatively coarse texture or of a mixed-matrix in sediment samples.
was inside CLP control limits for the requested analytes.
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 = MC0069-5 (MC0073L) was performed in accordance withCLP requirements for ICP analysis.
The adjusted sample concentrations were inside CLP control limits for the requested analytes.
7
CLP control limits for serial dilution are defined as a deviation less than or equal to 10% in the dilution-adjusted concentrations from the original values for all analyte concentrations with values greater thanfifty (50) times their respective Instrument Detection Limit (IDL) in the original sample.
The laboratory manager or his.designee, as verified by the following signature has authorized release of thedata contained in this hard copy data package.
Thomas R. ColeData Reviewer IIJuly 16, 2002
8
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
DATA .REPORTING QUALIFIERS FOR INORGANICS
On Form I, under the column labeled "C" for concentration qualifier and "Q" for qualifier, each result is flagged with the specific datareporting qualifiers listed below, as appropriate. Up to five qualifiers may be reported on Form I for each analyte.
The C (concentration) qualifiers used are:
U: This flag indicates the analyte was analyzed for but not detected. This reported value was obtained from a reading thatwas less than the Instrument Detection Limit (IDL). The IDL will be adjusted to reflect any dilution and. for soils, the
percent moisture.
B: This flag indicates the analyte was analyzed for and the reported value was obtained from a reading that was less than theContract Required Detection Limit (CRDL) but greater than or equal to the Instrument Detection Limit (IDL).
The Q qualifiers used are:
E: This flag indicates an estimated value. This flag is used:
1. When the serial dilution (a five fold dilution for CLP and a five fold dilution for SW-S46 method 601 OB) results arenot within 10%. The analyte concentration must be sufficiently high (minimally a factor of SOX above the IDL inthe original sample).
2. When the analytical spike recovery associated with the sample is below 40% after two successive dilutions byGraphite Furnace Atomic Absorption (GFAA).
M: This flag applies to GFAA analyses for concentrations greater than the Contract RequiredDetection Limit (CRDL). This flag is only used for GFAA if the analytical sample or analyticalspike duplicate injection reading is not within 20% of the Relative Standard Deviation (RSD).
N: This flag indicates the sample spike recovery is outside of control limits:
*: This flag is used for duplicate analysis when the sample and the sample duplicate results are not ,within control limits.
S: This flag applies to GFAA analyses to indicate the reported value was determined by theMethod Of Standard Addition (MSA).
\V: This flag applies to GFAA analyses when the post-digestion spike (analytical spike) is out of control limits (85% - 115%),while sample absorbance is less than 50% of "spike" absorbance ["spike" is defined as (absorbance or concentration ofspike sample) minus (absorbance or concentration of the sample)]. "
+: This flag applies to GFAA analyses when the correlation coefficient for the MSA is less than 0.995 after two MSAanalyses.
NOTE: Entering "S", "W", or"+" is mutually exclusive. No combination of these qualifiers can appear in the same field for ananalyte.
The extensions: D, S, SD, L. A, added to the end of the client ID represent as follows:D: matrix duplicateS: matrix spikeSD: matrix spike duplicateL: serial dilutionA: post digestion spike
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:
Date:
Name:
Title:
COVER PAGE - IN ILM04.1
U.S. EPA-CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
•Lab Name: COMPUCHEM Contract: 68W00082
Lab Code: LIBRTY Case No.: 30647 SAS No.: SDG No. : MC0078
SOW No.: ILM04.1
EPA Sample No. Lab Sample ID.
MC0108 MC0078-33
Were ICP interelement corrections applied? Yes/No
Were ICP background corrections applied? \ Yes/NoIf yes-were raw data generated beforeapplication of background corrections? Yes/No NO
Comments:
I certify that this data package is in compliance with the terras 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.
Yl g -JSignature : ( M&yY &l ^g-J^ Name :
>
Date: // 7 / / g'/dZ- _ Title:
COVER PAGE - IN ILM04.1
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
SDG NARRATIVECASE # 30647 SDG # MC0078
CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of twenty (20) soil samples was received into thelaboratory information management system (LIMS) on June 29,2002 intact and in good condition withChain of Custody (COC) Records in order, unless otherwise noted in any attachments or Quality AssuranceNotices. The temperature of the samples upon receipt was 3°C, as determined from the cooler temperatureindicator bottle.
The samples were analyzed, in accordance with EPA CLP Statement of Work (SOW) document ILM04.1,for the complete Inorganic Target Analyte List (TAL).
The correlation coefficient for the mercury and cyanide analytical runs are confirmed to be > 0.9950.
EQUATIONS FOR SOLED SAMPLE CALCULATIONS:
Equation for obtaining metals sample results in mg/kg as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb).
C x V
W x S
Where
C = concentration (ug/L)
V = final volume in liters after sample preparation
W = weight in grams of wet sample
S = % solids/100
Example: aluminum result ug/1 to mg/kg.
30976.51 ug/L(C) x 0.2 L(V)
l.Og(W) x 0.890 (S)= 6961.013 mg/kg reported as 6960 mg/kg
Equation for obtaining cyanide sample results in mg/kg as presented on FORM I data sheets frominstrument acquired results in ug/LXppb).
C x D x V
W x S
Where
C = concentration of cyanide (ug/L)
W = wet weight of sample
D = dilution factor to bring sample into analysis range
S = % solids/100
V = final volume in liters
Example: cyanide result ug/L to mg/kg
1.399607 ug/L (C) x 1 (D) x 0.05 L (V)
l.Og(W) x 0.890 (S)= 0.07863 mg/kg reported as 0.079 mg/kg
' Equation for obtaining mercury sample results in mg/kg as presented on FORM 1 data sheets frominstrument acquired results in ug/L (ppb). .
C x D x V
W x S
Where
C = concentration (ug/L)
W = wet weight of sample
D = dilution factor to bring sample into analysis range
S = %solids/100
V = final volume in liters
Example: mercury result ug/L to mg/kg
0.0165 ug/L(C) x 1 (D) x 0.1 L (V)= 0.0093 mg/kg reported as 0.056 mg/kg *
0.2 g (W) x 0.890 (S)
* This result reported down to the IDL. f
SAMPLE IDs:The following customer IDs are associated with this SDG:MC0078 MC0090 MC0091 MC0092 MC0093 MC0094 MC0095 MC0096 MC0097MC0098 MC0099 MC0100 MC0101 MC0102 MC0103 MC0104 MC0105 MC0106MC0107 MC0108
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 (LCSS & PBS) were found to be within acceptable rangesand all field samples were prepared and analyzed within the contract specified holding times.
MATRIX RELATED QUALITY CONTROL:
The sample matrix spike, CCN = WG18530-1 (MC0078S) was found to be outside CLP control limits forAntimony, Manganese and Thallium.
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 = WG18530-2 (MC0078D) was found to be inside CLP control limitsfor the requested analytes.
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 = SDIMC0078-1 (MC0078L) was performed in accordancewith CLP requirements for 1CP analysis.
The adjusted sample concentrations were inside CLP control limits for the requested analytes.
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.
The laboratory manager or his designee, as verified by the following signature has authorized release of thedata contained in this hard copy data package.
James E. MedlinSenior ChemistJuly 16,2002
8
U. S. EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Comments: THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN "E" TO INDICATE SERIALnTT.ITTTON RESULTS WHICH ARE NOT WTTHIN CONTROL LIMITS:MAGNESIUM . _
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 the computer-readable datasubmitted on diskette has been authorized by the Laboratory Manager or the Manager's designee, asverified by the following signature.
Signatur
Date:
Name:
Title:
COVER PAGE - IN
IN&it.
1L 3
ILM04.1
U. S. EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Lab Name: COMPUCHEM Contract: 68W00082
Lab Code: LIBRTY Case No.: 30647 SAS No.: SDG No.: MC0109
SOW No. : ILM04.1
EPA Sample No. Lab Sample ID.
MC0131S WG18531-1
Were ICP interelement corrections 'applied? Yes/No YES
Were ICP background corrections applied? ' Yes/No YESIf yes-were raw data generated beforeapplication of background corrections? Yes/No NO
Comments: THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN "E" TO INDICATE SERIALDTT.1TTTON RESULTS WHICH ARE NOT WTTHTN CONTROL T.TMTTS; ._
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 the computer-readable datasubmitted on diskette has been authorized by the Laboratory Manager or the Manager's designee, asverified by the following signature.
&• -Signatur^^/A^-ViMA**- **• - \_0\$_ Name:
Date: I / < A - / V , 1.5, d-Cfl&t Title: Uwf-" J\^£AJUJ^-^\. \{ ~f.Q I y
COVER PAGE - IN ILM04.1
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
SDG NARRATIVECASE # 30647 SDG # MC0109
CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of twenty (20) soil samples was received into thelaboratory information management system (LIMS) on June 29,2002; intact and in good condition withChains of Custody (COC) Records in order, unless otherwise noted in any attachments or QualityAssurance Notices. Sample ID's reported in this data package are noted by the receiving department on theCOC if they differ from those listed by the samplers on the COC.
The samples were analyzed, in accordance with EPA - CLP Statement of Work (SOW) document ILM04.1for CLP TAL total metals and cyanide.
The correlation coefficients for the mercury and cyanide analytical runs are confirmed to be > 0.9950.
The cooler temperature bottle was present with samples received on June 29,2002; and sampletemperature was 3.0 degrees Celsius.
The Laboratory Control Sample (LCS) for sodium analyzed outside the control limits established for thatanalyte. Sodium is present in the LCS below the CRDL. Thus, the control limits are only advisory limits.
EQUATIONS FOR SOLID SAMPLE CALCULATIONS:
Client sample MC0131 is used for illustration.
Any sample result that is < the instrument detection limit (IDL) will be entered at the IDL for thatanalyte.
ICP Equation:
Equation for obtaining metals sample results in ing/Kg as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb).
C x D x VConcentration (% solids) (mg/Kg)
. W x SWhere
C = concentration (ug/L)D = dilution factorV = final volume in liters after sample preparationW = weight in grams of wet sampleS = %solids/100
Example: aluminum result ug/L to mg/Kg.41422.58 ug/L (C) x 1 (D) x 0.2 L(V)
=9511.5 mg/Kg reported as 9510 mg/Kgl.Og(W) x 0.«71(S)
Mercury Equation:
Equation for obtaining mercury sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/L HgB = wet weight of sampleD = dilution factor to bring sample into analysis rangeE = %solids/100F = final volume in liters (0.1 L)
Example: mercury result ug/L to mg/Kg0.10 ug/L* (A) x 1(D) x 0.1 (F)
= 0.0574 mg/Kg reported as 0.057 mg/Kg*0.2 g(B) x 0.871(E)
* The result is reported down to the instrument detection limit.
Cyanide Equation:
Equation for obtaining cyanide sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/L CNB = wet weight of sampleD = dilution factor to bring sample into analysis rangeE = % solids/100 ''F = final volume in liters (0 05 L)
Example: cyanide result ug/L to mg/Kg0.656435 ug/L (A) x 1 (D) x 0.05 L (F)
= 0.03768 mg/Kg reported as 0.038 mg/Kgl.OOg(B) x 0.871(E)
SAMPLE IDs:
The following customer IDs are associated with this SDG:
MC0109 MC0110 MC0111 MC0112 MC0113 MC0114
MC0115 MC0116 MC0117 MC0113 MC0119 MC0120
MC0121 MC0122 MC0123 MC0124 MC0125 MC0126V
MC0127 MC0131
7
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 (LCSS & PBS) were found to be within acceptable rangesand all field samples were prepared and analyzed within the contract specified holding times.
MATRIX RELATED QUALITY CONTROL:
The sample matrix spike, CCN = WG18531-1 (MC0131S) was found to be outside CLP control limits forantimony and lead. The reported concentrations for these analytes are flagged with an "N" on allassociated Form 1 and on Form 5a.
An "N" indicates a matrix-related interference in the sample preparation procedure &/or analysis for theflagged analyte. This is normally the consequence of a relatively high anionic content in the sample or (forsome sediments) an inconsistent sample matrix relative to that analyte.
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.
Post-digestion spikes are mandatory for analytes demonstrating unsatisfactory matrix spike recoveriesduring ICP analysis (excluding silver). The results of such spikes are presented on Form 5b.
Unsatisfactory recovery of post-digestion spikes of this type do not have bearing upon the aforementioned"N" flags, but may indicate interference during analysis &/or a solution matrix which is hostile to theanalyte in question.
Satisfactory recovery of an analyte in a post-digestion spike of this type implies interference by therequired preparation procedure or in the sample matrix itself. Lack of uniformity for an analyte insediments will also result in satisfactory recovery of post-digestion spikes after failure in the related matrixspike.
The sample matrix duplicate, CCN = WG 18531-2 (MC0131D) was inside CLP control limits for therequested analytes.
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 = MCO109-20 (MC0131L) was performed in accordance withCLP requirements for ICP analysis.
The adjusted sample concentrations were outside CLP control limits for magnesium, which is flagged withan "E" on all associated Form 1, the Cover Page and Form 9.
An "E" indicates that a chemical or physical interference effect was encountered during the analysis of theflagged analyte. As a result of this interference, all values for the analyte in the same matrix must beconsidered to be estimated quantities.
8
CLP control limits for serial dilution are defined as a deviation less than or equal to 10% in the dilution-adjusted concentrations from the original values for all analyte concentrations with values greater thanfifty (50) times their respective Instrument Detection Limit (IDL) in the original sample.
The laboratory manager or his designee, as verified by the following signature has authorized release of thedata contained in this hard copy data package.
omas R. ColeData Reviewer IIJuly 15, 2002
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
DATA REPORTING QUALIFIERS FOR INORGANICS
On Form I, under the column labeled "C" for concentration qualifier and "Q" for qualifier, each result is flagged with the specific datareporting qualifiers listed below, as appropriate. Up to five qualifiers may be reported on Form I for each analyte.
The C (concentration) qualifiers used are:
U: This flag indicates the analyte was analyzed for but not detected. This reported value was obtained from a reading thatwas less than the Instrument Detection Limit (IDL). The IDL will be adjusted <o reflect any dilution and, for spils, the
percent moisture.
B: This flag indicates the analyte was analyzed for and the reported value was obtained from a reading that was less than theContract Required Detection Limit (CRDL) but greater than or equal to the Instrument Detection Limit (IDL).
The Q qualifiers used are:
E: This flag indicates an estimated value. This flag is used:
1. When the serial dilution (a five fold dilution for CLP and a five fold dilution for SW-846 method 601 OB) results arenot within 10%. The analyte concentration must be sufficiently high (minimally a factor of SOX above the IDL inthe original sample).
2. When the analytical spike recovery associated with the sample is belo\\ 40% after two successive dilutions byGraphite Furnace Atomic Absorption (GFAA).
M: This flag applies to GFAA analyses for concentrations greater than the Contract RequiredDetection Limit (CRDL). This flag is only used for GFAA if the analytical sample or analyticalspike duplicate injection reading is not within 20% of the Relative Standard Deviation (RSD).
N: This flag indicates the sample spike recovery is outside of control limits:
*: This flag is used for duplicate analysis when the sample and the sample duplicate results are not .within control limits.
S: This flag applies to GFAA analyses to indicate the reported value was determined by theMethod Of Standard Addition (MSA).
\V: This flag applies to GFAA analyses when the post-digestion spike (analytical spike) is out of control limits (85% - 115%),while sample absorbance is less than 50% of "spike" absorbance ["spike" is defined as (absorbance or concentration ofspike sample) minus (absorbance or concentration of the sample)].
+: This flag applies to GFAA analyses when the correlation coefficient for the MSA is less than 0.995 after two MSAanalyses.
NOTE: Entering "S", "W", or"+" is mutually exclusive. No combination of these qualifiers can appear in the same field for ananalyte.
The extensions: D, S, SD, L. A, added to the end of the client ID represent as follows:D: matrix duplicateS: matrix spikeSD: matrix spike duplicateL: serial dilutionA: post digestion spike
Were ICP background corrections applied?If yes-were raw data generated beforeapplication of background corrections?
Yes/No YES
'• Yes/No YES
Yes/No NO
Comments: THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN "E" TO INDICATE SERIAL' nTT.TTTTQN TJF.SULTS WHTCH ARE NOT WITHIN CONTROL T.TMTTS:
ZiNC : =
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 the computer-readable datasubmitted on diskette has been authorized by the Laboratory Manager or the Manager's designee, asverified by the following signature.
Signature :r
Date:
I Name:
Title:
COVER PAGE - IN
/ AoTlAAS K - L
JAt/i, K £k>
ILM04.1
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
SDG NARRATIVECASE # 30647 SDG # MC0128
CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of eleven (11) soil samples was received into thelaboratory information management system (LIMS) on June 29,2002; intact and in good condition withChains of Custody (COC) Records in order, unless otherwise noted in any attachments or QualityAssurance Notices. Sample ID's reported in this data package are noted by the receiving department on theCOC if they differ from those listed by the samplers on the COC.
The samples were analyzed, in accordance with EPA - CLP Statement of Work (SOW) document ILM04.1for CLP TAL total metals and cyanide.
The correlation coefficients for the mercury and cyanide analytical runs are confirmed to be > 0.9950.
The cooler temperature bottle was present with samplesTeceived on June 29, 2002; and sampletemperature was 3.0 degrees Celsius.
The sampler did not designate as sample for MS/MSD. LIBRTY selected sample MC0128 for QC.
The Laboratory Control Sample (LCS) for sodium analyzed outside the control limits established for thatanalyte. Sodium is present in the LCS below the CRDL. Thus, the control limits are only advisory limits.
EQUATIONS FOR SOLID SAMPLE CALCULATIONS:
Client sample MC0128 is used for illustration.
Any sample result that is < the instrument detection limit (IDL) will be entered at the IDL for thatanalyte.ICP Equation:Equation for obtaining metals sample results in mg/Kg as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb).
C x D x VConcentration (% solids) (mg/Kg)
W x SWhere
C = concentration (ug/L)D = dilution factorV = final volume in liters after sample preparationW = weight in grams of wet sampleS = %solids/100
Example: aluminum result ug/L to mg/Kg.34365,69 ug/L (C) x 1 (D) x 0.2 L (V)
= 7446.5 mg/Kg reported as 7450 mg/Kgl.Og(W) x 0.923(8)
Mercury Equation:
Equation for obtaining mercury sample results in mg/Kg as presented on fORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/L HgB = wet. weight of sampleD = dilution factor to bring sample into analysis rangeE = % sol ids/100F = final volume in liters (0.1 L)
Example: mercury result ug/L to mg/Kg0.1253 ug/L (A) x 1 (D) x 0.1 (F)
= 0.06788 mg/Kg reported as 0.068 mg/Kg0.2 g(B) x 0.923 (E)
Cyanide Equation:
Equation for obtaining cyanide sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/L CNB = wet weight of sampleD = dilution factor to bring sample into analysis rangeE = % solids/100F = final volume in liters (0 05 L)
Example: cyanide result ug/L to mg/Kg0.60 ug/L* (A) x 1 (D) x 0.05 L (F)
= 0.0325027 mg/Kg reported as 0.033 mg/Kg*l.OOg(B) x 0.923 (E)
* The result is reported down to the instrument detection limit.
SAMPLE IDs:
The following customer IDs are associated with this SDG:
MCOI28 MC0129 MC0130 MC0132 MC0133 MC0134
MC0135 MC0136 MC0137 MC0138 MC0139
INSTRUMENTAL QUALITY CONTROL:
All calibration verification solutions (ICY & CCV), blanks (1CB, & GCB), 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 (LCSS & PBS) were found to be within acceptable rangesand all field samples were prepared and analyzed within the contract specified holding times.
MATRIX RELATED QUALITY CONTROL:
The sample matrix spike, CCN = WG18589-1 (MC0128S) was found to be outside CLP control limits forantimony and mercury. The reported concentrations for these analytes are flagged with an "N" on allassociated Form 1 and on Form 5a.
An "N" indicates a matrix-related interference in the sample preparation procedure &/or analysis for theflagged analyte. This is normally the consequence of a relatively high anionic content in the sample or (forsome sediments) an inconsistent sample matrix relative to that analyte.
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.
Post-digestion spikes are mandatory for analytes demonstrating unsatisfactory matrix spike recoveriesduring ICP analysis (excluding silver). The results of such spikes are presented on Form 5b.
Unsatisfactory recovery of post-digestion spikes of this type do not have bearing upon the aforementioned"N" flags, but may indicate interference during analysis &/or a solution matrix which is hostile to theanalyte in question.
jSatisfactory recovery of an analyte in a post-digestion spike of this type implies interference by therequired preparation procedure or in the sample matrix itself. Lack of uniformity for an analyte insediments will also result in satisfactory recovery of post-digestion spikes after failure in the related matrixspike.
The sample matrix duplicate, CCN = WG 18589-2 (MC0128D) was inside CLP control limits for therequested analytes.
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 = MCO128-1 (MC0128L) was performed in accordance withCLP requirements for ICP analysis.
VThe adjusted sample concentrations were outside CLP control limits for zinc, which is flagged with an "E"on all associated Form 1, the Cover Page and Form 9.
An "E" indicates that a chemical or physical interference effect was encountered during the analysis of theflagged analyte. As a result of this interference, all values for the analyte in the same matrix must beconsidered to be estimated quantities.
CLP control limits for serial dilution are defined as a deviation less than or equal to 10% in the dilution-adjusted concentrations from the original values for all analyte concentrations with values greater thanfifty (50) times their respective Instrument Detection Limit (IDL) in the original sample.
7
The laboratory manager or his designee, as verified by the following signature has authorized release of thedata contained in this hard copy data package.
Thomas R. ColeData Reviewer IIJuly 12, 2002
8
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
DATA.REPORTING QUALIFIERS FOR INORGANICS
On Form I, under the column labeled "C" for concentration qualifier and "Q" for qualifier, each result is flagged with the specific datareporting qualifiers listed below, as appropriate. Up to five qualifiers may be reported on Form I for each analyte.
The C (concentration) qualifiers used are;
U: This flag indicates the analyte was analyzed for but not detected. This reported value was obtained from a reading thatwas less than the Instrument Detection Limit (IDL). The IDL will be adjusted to reflect any dilution and, for soils, the
percent moisture.
B: This flag indicates the analyte was analyzed for and the reported value was obtained from a reading that was less than the "Contract Required Detection Limit <CRDL) but .greater than or equal to the Instrument Detection Limit (IDL).
The Q qualifiers used are:
E: This flag indicates an estimated value. This flag is used:
" 1. When the serial dilution (a five fold dilution for CLP and a five fold dilution for SXV-846 method 6010B) results arenot within 10%. The analyte concentration must be sufficiently high (minimally a factor of SOX above the IDL inthe original sample).
2. When the analytical spike recovery associated with the sample is below 40% after ruo successive dilutions byGraphite Furnace Atomic Absorption (GFAA).
M: This flag applies to GFAA analyses for concentrations greater than .the Contract RequiredDetection Limit (CRDL). This flag is only used forGFAA if the analytical sample or analyticalspike duplicate injection reading is not within 20% of the Relative Standard Deviation (RSD).
N: This flag indicates the sample spike recovery is outside of control limits:
*: This flag is used for duplicate analysis when the sample and the sample duplicate results are not:within control limits.
S: This flag applies to GFAA analyses to indicate the reported value was determined by theMethod Of Standard Addition (MSA).
W: This flag applies to GFAA analyses when the post-digestion spike (analytical spike) is out of control limits (85% -115%),while sample absorbance is less than 50% of "spike" absorbance ("spike" is defined as (absorbance or concentration ofspike sample) minus (absorbance or concentration of the sample)].
+; This flag applies to GFAA analyses when the correlation coefficient for the MSA is less than 0.995 after two MSAanalyses.
NOTE: Entering "S", "W", or"+" is mutually exclusive. No combination of these qualifiers can appear in the same field for ananalyte.
The extensions: D, S, SD, L. A, added to the end of the client ID represent as follows:D: matrix duplicateS: matrix spikeSD: matrix spike duplicateL: serial dilutionA: post digestion spike
Method Codes:P. ICP PLASMACV: MERCURY COLD VAPOR AA .,CA: MIDI-DISTILLATION SPECTROPHOTOMETRICF: FURNACE AA
U. S. EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Comments: THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN "E" TO INDICATE SERIALDILUTION RESULTS WHICH ARE NOT WITHIN CONTROL LIMITS : ZINC.
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:
Date:
Name:
Title:
COVER PAGE - IN ILM04.1
U. S. EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Lab Name: COMPUCHEM Contract: 68WO0082
Lab Code: LIBRTY Case No. : 30647 SAS No. : SDG No. : MC0143
SOW No.: ILM04.1
EPA Sample No. Lab Sample ID.
MC0163 MC0143-20
Were ICP interelement corrections applied? Yes/No
Were ICP background corrections applied? •• Yes/NoIf yes-were raw data generated beforeapplication of background corrections? Yes/No NO
Comments: THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN "E" TO INDICATE SERIALDILUTION RESULTS WHICH ARE NOT WITHIN CONTROL LIMITS : ZINC.
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: /^L^^^ Name: J^VY\-eS YY\&d\ln
Date:C
7/7*7 /<9<3 _ Title: S^n JQC
COVER PAGE - IN ILM04.1
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
SDG NARRATIVECASE # 30647 SDG # MC0143
CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of twenty (20) soil samples was received into thelaboratory information management system (LIMS) on July 2, 2002 intact and in good condition withChain of Custody (COC) Records in order, unless otherwise noted in any attachments or Quality AssuranceNotices. The temperature of the samples upon receipt was 8°C, as determined from the cooler temperatureindicator bottle. '
The samples were analyzed, in accordance with EPA CLP Statement of Work (SOW) document ILM04.1,for the complete Inorganic Target Analyte List (TAL).
The correlation coefficient for the mercury and cyanide analytical runs are confirmed to be > 0.9950.
EQUATIONS FOR SOLDD SAMPLE CALCULATIONS:
Equation for obtaining metals sample results in mg/kg as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb).
C x V
W x S
Where
C = concentration (ug/L)
V = final volume in liters after sample preparation
W = weight in grams of wet sample
S = %solids/100
Example: aluminum result ug/1 to mg/kg.
42130.18 ug/L (C) x 0.2 L(V)= 9629.755 mg/kg reported as 9630 mg/kg
l.Og(W) x 0.875 (S)
Equation for obtaining cyanide sample results in mg/kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
C x D x VV
W x S
Where '
C = concentration of cyanide (ug/L)
W = wet weight of sample
D = dilution factor to bring sample into analysis range
S = %solids/100
V = final volume in liters
Example: cyanide result ug/L to mg/kg
1.246421 ug/L (C) x 1 (D) x 0.05 L (V)= o.071224 mg/kg reported as 0.071 mg/kg
l .Og(W) x 0.875(8)
Equation for obtaining mercury sample results in mg/kg as presented on FORM I data sheets frominstrument acquired results in Ug/L (ppb).
C x D x V
W x S .
Where
C = concentration (ug/L)
W = wet weight of sample
D = dilution factor to bring sample into analysis range
S = % solids/100
V = final volume in liters
Example: mercury result ug/L to mg/kg
0.0892 ug/L(C) x 1 (D) x 0.1 L (V)= 0.0510 mg/kg reported as 0.057 mg/kg *
0.2 g (W) x 0.822 (S)
7This result reported down to<he IDL.
SAMPLE IDs:The following customer IDs are associated with this SDG:MC0143 MC0144 MC0145 MC0146 MC0147 MC0148 MC0149 MC0150 MC0151MC01S2 MC0154 MC01S5 MC01S6 MC0157 MCOI58 MC0159 MC0160 MC0161MC0162 MC0163
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 (LCSS & PBS) were found to be within acceptable rangesand all field samples were prepared and analyzed within the contract specified holding times. The Sodiumresult for the LCSS is above the control'limit. The True Value for Sodium is below the CRDL and thecontrol limits are stated to be advisory only.
MATRIX RELATED QUALITY CONTROL:
The sample matrix spike, CCN = WG18575-1 (MC0152S) was found to be outside CLP control limits forAntimony, Manganese and Selenium.
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 = WG 18575-2 (MC0152D) was found to be outside CLP control limitsfor Chromium, Iron and Manganese.
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 = SDIMC0143-10 (MC0152L) was performed in accordancewith CLP requirements for ICP analysis.
The adjusted sample concentration was outside CLP, control limits for Zinc, which is flagged 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.
Comments: THE FOLLOWING ANALYTES HAVE BEEN FLAGGED WITH AN "E" TO INDICATE SERIALDILUTION RESULTS WHICH ARE NOT WITHIN CONTROL LIMITS:
rHTtnMTTTM, PDTRSSTTJM '
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 the computer-readable datasubmitted on diskette has been authorized by the Laboratory Manager or the Manager's designee, asverified by the following signature.
Signature: _
Date:
Name:
Title:
COVER PAGE - IN
-UJ^ \-tJT, JL
ILM04.J
U. S. EPA - CLPCOVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Lab Name: COMPUCHEM Contract: 68WOOO82
Lab Code: LIBRTY Case Ho. : 30647 SAS No. : SDG No. : MC0153
SOW No. : ILM04.1
EPA Sample No. Lab Sample ID.
MC0182 MC0153-34
Here ICP interelement corrections applied? Yes/No YES
Were ICP background corrections applied? • Yes/No YESIf 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:
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 the computer-readable datasubmitted on diskette has been authorized by the Laboratory Manager or the Manager' s designee, asverified by the following signature.
K - (j>*JL Name: / /WWA£ A - Cfif JjSignature: ^/fK^jjU- K - (J^UL Name: / nfrfW4£ A- - (-fit &
i
Date: . LUULu I / O . 2 0^/^~ Title:
COVER PAGE - IN ILM04.1
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
SDG NARRATIVE
CASE # 30647 SDG # MC0153CONTRACT # 68W00082
The indicated Sample Delivery Group (SDG) consisting of twenty (20) soil samples was received into thelaboratory information management system (LIMS) on July 2, 2002; intact and in good condition withChains of Custody (COC) Records in order, unless otherwise noted in any attachments or QualityAssurance Notices. Sample ID's reported in this data package are noted by the receiving department on theCOC if they differ from those listed by the samplers on the COC.
The samples were analyzed, in accordance with EPA - CLP Statement of Work (SOW) document ILM04.1for CLP TAL total metals and cyanide.
The correlation coefficients for the mercury and cyanide analytical runs are confirmed to be > 0.9950.
The cooler temperature bottle was present with samples received on July 2,2002; and sample temperaturewas 8.0 degrees Celsius.
EQUATIONS FOR SOLID SAMPLE CALCULATIONS:
Client sample MC0153 is used for illustration.
Any sample result that is < the instrument detection limit (IDL) will be entered at the IDL for thatanalyte.
ICP Equation:
Equation for obtaining metals sample results in mg/Kg as presented on FORM I data sheets from ICPinstrument acquired results in ug/L (ppb).
C x D x VConcentration (% solids) (mg/Kg)
W x SWhere
C = concentration (ug/L)D = dilution factorV = final volume in liters after sample preparationW = weight in grams of wet sampleS = %solids/100
Example: aluminum result ug/L to mg/Kg.48942.08 ug/L (C) x 1 (D) x 0.2 L (V)
= ll276.98 mg/Kg reported as 11300 mg/Kgl .Og(W) x 0.868(5)
Mercury Equation:
Equation for obtaining mercury sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D .x F
B x EWhere
A = ug/L HgB = wet weight of sampleD = dilution factor to bring sample into analysis rangeE = % solids/100F = final volume in liters (0.1 L)
Example: mercury result ug/L to mg/Kg0.10 ug/L* (A) x 1 (D) x 0.1 (F)
= 0.05760 mg/Kg reported as 0.058 mg/Kg*0.2 g (B) x , 0.868 (E)
* The result is reported down to the instrument detection limit.
Cyanide Equation:
Equation for obtaining cyanide sample results in mg/Kg as presented on FORM I data sheets frominstrument acquired results in ug/L (ppb).
A x D x F
B x EWhere
A = ug/L CNB = wet weight of sampleD = dilution factor to bring sample into analysis rangeE = % solids/100F = final volume in liters (0 05 L)
Example: cyanide result ug/L to mg/Kg0.60 ug/L* (A) x 1 (D) x 0.05 L (F)
= 0.03456 mg/Kg reported as 0.035 mg/Kg*l.OOg(B) x 0.868 (E)
* The result is reported down to the instrument detection limit.
SAMPLE IDs.
The following customer IDs are associated with this SDG:
MC0153 MC0164 MC0165 MC0166 MC0167 MC0168
MC0169 MC0170 MC0171 MC0172 MC0173 MC0174
MC0175 MC0176 MC0177 MC0178 MC0179 MC0180
MC0181 MC0182
7
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 (LCSS & PBS) were found to be within acceptable rangesand all field samples were prepared and analyzed within the contract specified holding times.
MATRIX RELATED QUALITY CONTROL:
The sample matrix spike, CCN = WG18576-1 (MC0153S) was found to be outside CLP control limits forantimony and thallium. The reported concentrations for these analytes are flagged with an "N" on allassociated Form 1 and on Form 5a.
An "N" indicates a matrix-related interference in the sample preparation procedure &/or analysis for theflagged analyte. This is normally the consequence of a relatively high anionic content in the sample or (forsome sediments) an inconsistent sample matrix relative to that analyte.
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.
Post-digestion spikes are mandatory for analytes demonstrating unsatisfactory matrix spike recoveriesduring ICP analysis (excluding silver). The results of such spikes are presented on Form 5b.
Unsatisfactory recovery of post-digestion spikes of this type do not have bearing upon the aforementioned"N" flags, but may indicate interference during analysis &/or a solution matrix which is hostile to theanalyte in question.
Satisfactory recovery of an analyte in a post-digestion spike of this type implies interference by therequired preparation procedure or in the sample matrix itself. Lack of uniformity for an analyte insediments will also result in satisfactory recovery of post-digestion spikes after failure in the related matrixspike.
The sample matrix duplicate, CCN = WG18576-2 (MC0153D) was inside CLP control limits for therequested analytes.
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 = MC0153-15 (MC0153L) was performed in accordance withCLP requirements for ICP analysis.
The adjusted sample concentrations were outside CLP control limits for calcium, chromium, andpotassium, which are flagged with an "E" on all associated Form 1, the Cover Page and Form 9.
An "E" indicates that a chemical or physical interference effect was encountered during the analysis of theflagged analyte. As a result of this interference, all values for the analyte in the same matrix must beconsidered to be estimated quantities.
8
CLP control limits for serial dilution are defined as a deviation less than or equal to 10% in the dilution-adjusted concentrations from the original values for all analyte concentrations with values greater thanfifty (50) times their respective Instrument Detection Limit (IDL) in the original sample.
The laboratory manager or his designee, as verified by the following signature has authorized release of thedata contained in this hard copy data package.
Thomas R. ColeData Reviewer IIJuly 16,2002
CompuChema Division of Liberty Analytical Corp.501 Madison Avenue Cary.NC 27513
DATA REPORTING QUALIFIERS FOR INORGANICS
On Form I, under the column labeled "C" for concentration qualifier and "Q" for qualifier, each result is flagged with the specific datareporting qualifiers listed below, as appropriate. Up to five qualifiers may be reported on Form I for each analyte.
The C (concentration) qualifiers used are;
I): This flag indicates the analyte was analyzed for but not detected. This reported value was obtained from a reading thatwas less than the Instrument Detection Limit (IDL). The IDL will be adjusted to reflect any dilution and, for soils, the
percent moisture.
B: This flag indicates the analyte was analyzed for and the reported value was obtained from a reading that was less than theContract Required Detection Limit (CRDL) but greater than or equal to the Instrument Detection Limit (IDL).
The Q qualifiers used are:
E: This flag indicates an estimated value. This flag is used:
1. When the serial dilution (a five fold dilution for CLP and a five fold dilution for SW-846 method 601 OB) results arenot within 10%. The analyte concentration must be sufficiently high (minimally a factor of SOX above the IDL inthe original sample).
2. When the analytical spike recovery associated with the sample is below 40% after two successive dilutions byGraphite Furnace Atomic Absorption (GFAA).
M: This flag applies to GFAA analyses for concentrations greater than the Contract RequiredDetection Limit (CRDL). This flag is only used for GFAA if the analytical sample or analyticalspike duplicate injection reading is not within 20% of the Relative Standard Oeviation-(RSD).
N: This flag indicates the sample spike recovery is outside of control limits:
*: This flag is used for duplicate analysis when the sample and the sample duplicate results are not .within control limits.
S: This flag applies to GFAA analyses to indicate the reported value was determined by theMethod Of Standard Addition (MSA).
\V: This flag applies to GFAA analyses when the post-digestion spike (analytical spike) is out of control limits (85% -115%),while sample absorbance is less than 50% of "spike" absorbance ["spike" is defined as (absorbance or concentration ofspike sample) minus (absorbance or concentration of the sample)].
+: This flag applies to GFAA analyses when the correlation coefficient for the MSA is less than 0.995 after two MSAanalyses.
NOTE: Entering "S", "W", or "+" is mutually exclusive. No combination of these qualifiers can appear in the same field for ananalyte.
\
The extensions: D, S, SD, L. A, added to the end of the client ID represent as follows:D: matrix duplicateS: matrix spikeSD: matrix spike duplicateL: serial dilutionA: post digestion spike
Method Codes:P: ICP PLASMACV: MERCURY COLD VAPOR AA 1 f)CA: MIDI-DISTILLATION SPECTROPHOTOMETRIC •*-f: FURNACE AA