Upload
others
View
0
Download
0
Embed Size (px)
Citation preview
DATE :
SUBJECT:
FROM :
TO
UNITED STATES ENVIRONMENTAL PROTECTION AGENCYENVIRONMENTAL SCIENCE CENTER
701 MAPES ROADFORT MEADE, MD 20755-5350
February 13, 2003
Region III Data Q/L Reviewy/v
Fredrick Foreman)]/Region III ESAT RPO (3ES20)
Romuald RomanRegional Project Manager (3HS22)
SDMSOocJD2065975
Attached is the organic data validation report for the Valmont TCEsite (Case #: R31385, SDG#: 216587) 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#: 0144
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 M A R T
DATE:
SUBJECT:
FROM:
TO:
OVERVIEW
February 13, 2003
Level M3 Organic Data Validation for DAS R31385SDG: 216587Site: Valmont TCE
MichaelSenior Data Reviewer
Fredrick ForemanESAT Regional Project Officer
»Mahboobeh Mecanic 'Senior Oversight Chemist
DAS R31385, Sample Delivery Group (SDG) 216587, consisted of ten (10) aqueous samples submittedto Southwest Research Institute (SWRI) for fluorinated surfactants (perfluorooctanoic acid andperfluorooctanyl sulfonate) analyses. Samples included one (1) field blank, one (1) rinsate blank andone (1) field-duplicate pair. Samples were analyzed according to EPA SW-846, Solvent Extractable Non-volatile Compounds by High Performance Liquid Chromatography/Thermospray/Mass Spectrometry(HPLC/TS/MS), Method 8321 A, modified. Samples were analyzed through Delivery of Analytical Services(DAS) program.
SUMMARY
Data were validated according to Region III Modifications to the National Functional Guidelines forOrganic Data Review, Level M3. All samples were successfully analyzed for all target compounds.
NOTES
No positive results were reported for target compounds in field . rinsate or method blanksassociated with this Case.
Target compounds detected below Contract Required Quantitation Limits (CRQLs) werequalified "J" on the Data Summary Forms (DSFs).
Perfluorooctanyl sulfonate (PFOS) calibration standards indicated two distinct peaks for thePFOS anion. Peaks were designated PFOS1 and PFOS2 by the laboratory and both peaks wereassigned the theoretical concentration of PFOS in the standards. Sample data also indicatedtwo peaks when PFOS anion was present. Laboratory calculated PFOS concentration insamples by averaging concentrations calculated from the two peaks. Samples VM-GW21-01,VM-MW10A-01 and VM-MW12S-01 were the only samples reporting positive PFOS results.
Page 2 of 2
All data for DAS R31385, SDG 216587, were reviewed in accordance with Region III Modifications to theNational Functional Guidelines for Organic Data Review, September 1994.
ATTACHMENTS
1)2)3)4)5)
Appendix AAppendix BAppendix CAppendix DAppendix E
Glossary of Data Qualifier TermsData Summary FormsChain of Custody RecordsLaboratory Case NarrativeLaboratory-prepared Results Forms
DCN:R31385rpt.wpd
Appendix A
Glossary of Data Qualifiers
GLOSSARY OF DATA QUALIFIER CODES (ORGANIC)
CODES RELATED TO IDENTIFICATION(confidence concerning presence or absence of compounds)
U = Not detected. The associated number indicates approximate sampleconcentration necessary to be detected.
NO CODE = Confirmed identif ication.
B = Not detected substantially above the level reported in laboratory or Heldblanks.
R = Unusable result. Analyte may or may not be present in the sample.Supporting data necessary to confirm result.
N = Tentative identification. Consider present. Special methods may beneeded to confirm its presence or absence in future sampling efforts.
CODES RELATED TO OUANT1TATION(can be used for both positive results and samplequantitation limits):
J = Analyte present. Reported value may not be accurate or precise.
K = Analyte present. Reported value may be biased high . Actual value isexpected to be lower.
L = Analyte present. Reported value may be biased low. Actual value isexpected to be higher.
UJ = Not detected, quantitation l imi t may be inaccurate or imprecise.
UL = Not detected, quantitation l i m i t is probably higher.
OTHER CODES
NJ = Qual i ta t ive identification questionable due to poor resolution.Presumptively present at approximate q u a n t i t y .
0 = No ana ly t i ca l result .
Appendix B
Data Summary Forms
DATA SUMMARY FORM: FLUOROSURFACTANTS Page_1 of 1
Case #: R31385
Site.
Lab.:
SDG: 216587
VALMONT TCE
SWRI
Number of Soil Samples 0
Number of Water Samples 10
Sample Number :
Sampling Location'
Field QC:
Matrix .
Units:
Date Sampled .
Time Sampled : ,
Dilution Factor
Target analyte
Perfluorooctanoic acid (PFOA)
Perflu'orooctanyl sulfonate (PFOS)
CRQL
020
020
FB-01
FB-01
Field Blank
Water
ug/L
11/18/02
0845
10
Result
•
Flag
RB-01
RB-01
Rtnsate Blank
Water
ug/L
11/18/02
0835
10
Result Flag
VM-GW21-01
VM-GW21-01
Water
ug/L '
11/18/02
1310
10
Result
0067
0094
Flag
J
J
VM-MW1 10-01
VM-MW11D-01
Water
ug/L
11/18/02
1110
10
Result
'
Flag
VM-MW11S-01
VM-MW11S-01
Water
ug/L
11/18/02
1030
1 0
Result
0043
Flag
J
CRQL = Contract Required Quantitation Limit
To calculate sample quantitation limits' (CRQL * Dilution Factor)
SEE NARRATIVE FOR CODE DEFINITIONS
Revised 09/99
Sample Number .
Sampling Location.
Field QC:
Matrix :
Units :
Date Sampled :
Time Sampled .
Dilution Factor .
Target analyte
Perfluorooctanoic acid (PFOA)
Perfluorooctanyl sulfonate (PFOS)
CRQL
020
020
VM-MW14S-01
VM-MW14S-01
Dupl ofVM-MW41S-01
Water
ug/L
11/18/02
0800
1.0
Result Flag
VM-MW41S-01
VM-MW41S-01
Dupl ofVM-MW14S-01
Water
ug/L
11/18/02
0815
10
Result Flag
VM-MW10A-01
VM-MW10A-01
Water
ug/L
11/21/02
1135
10
Result
069
064
Flag
VM-MW12S-01
VM-MW12S-01
Water
ug/L
11/19/02
1415
1 0
Result
022
008
Flag
J
VM-MW15S-01
VM-MW15S-01
Water
ug/L
1 1/20/02
1720
1 0
Result Flag
CRQL = Contract Re '.uired Quantitation Limit
To calculate sample quantitation limits- (CRQL * Dilution Factor)
Sr-E NARRATIVE FOR CODE DEFINITIONS
Revised 09/99
oEPVX USEPA Contract Laboratory Program Reference case: QGeneric Chain of Custody aa*nx *™** IY
Region:Project Coda:Account Code:CERCLIS ID:tnill in-
3
4192
wfjlll lUf
Site Name/State: ValmontTCE (R31385XPAProject Leader:Action:Sampling Co:
SAWLENo.
FB-01
RB-01
VM-JIW2I-01
VM-«AvV11D-01
VM-MW11S-01
VM-MW14S-01
VM-MLV4IS-01
Neil fearnereonRemedial InvestigationTetra Teoh NUS. Inc
MATRIX/ CONCSSAMPLER TYPE
Field QC/ L/GEric Hinkle
Reid QC/ L/GEric Hinkle
Ground Waterf L/GEnc HinMB
Ground Walerf L/GEric HinWe
Ground Waterf L/GEricHinWe
Ground Water/ L/GEric Hinkle ~
Ground Water/ L/GEric Hinkle
ANALYSIS/TURNAROUND
PFOS/PFOA (21)
PFOS/PFOA (21)
PFOS/PFOA (21)
PFOS/PFOA (21)
PFOS/PFOA (21)
PFOS'PFOA(21)
PFOS(PFOA(21)
Date shipped: 11/19(02 Chain of Custody Record SSL^^gS^LCsuriBrNama: FedE* jf^—ys^QAirbill: 828684646973 Relinquished By (Date /Time) Received By (Date /Time)
Shipped to: Southwest Research 1 .s-̂ S&^K /{•Ff̂ £- /̂ P** *Institute ^~ — : ^ ~~~ ~~ ~~~ ————— ——6220 Culefara Road 2San antonio TX 78238 ——————— ——(210)522-2169 3
4
TAG No/ STATION SAMPLE COLLECT QCPRESERVATIVE LOCATION DATETTIME SAMPLE No. Type
3-541 (Ice Only) (1) F6-01 S: 11/18/02 845 Fiald Blank
3r540 (Ice Only) d) RB-01 S: 11/18/02 835 Rinsate
3-556 (Ice Only) (1) VM-GW21-01 S: 11/18/02 13:10
3-605 (Ice Only) d) VM-MVV1 10-01 S: 11/1ST02 11:10
3-644 (Ice Only), 3-545 VM-MW11S-Q1 S. 11/18/02 1030 MSfl̂ SO(Ice Only). 3-546 (Ice
Only) (3)3-542 (loa Only) (1) VM-MW14S-01 S: 11/18/02 8.00
3-543 (Ice Only) (1) VM-MW41S-01 S: 11/18/02 8.15 Duplicate oJVM-MW14S-01
Shipment for CaseComplete? N
Analysis Key:
PFOS/PFOA = Perftuc
Sample(s) to be used for laboratory QC:
VM-MW11S-01
AddHional Sampler Signature(s):
Concentration: L = ̂ M = \mlmaumt H = H,gh Type/ueagnate: (
>rooctanyt sullonafe
TR Number: 3-424838327-1 1 1902-0003'K praviam preilrniiKiry mutts. Reqmsta for preliminary result* witl increase analytical cort*.Send Copy to: Contract Laboratory Analytical Services Support. 2000 Edmund Halley Or., Reston,
i)mposrte = C, Grab = G
Chain o) Custody Seal Number:
Aifa
Shipment Iced
REGION COPV A. 201 91 -3436 Phone 703/264-9348 Fax 703/264-922 " f?v« » «« o>~
Vt
4 «*•*
&ER/V USEPA Contract Laboratory ProgramGeneric Chain of Custody
Region: 3Project Code: 4ig2Account Code:CERCL15 ID:Spill ID:SiteN le/Slate: Valmont TCE (R31385VPA
Project Leader: Neil TearwrsonAction: Remedial Investigation
Sampling Co: TetraTechNUS.Inc
Date Shipped: 11/21KJ2
Carrier Name: FedExAirbill: 826564646756
Shipped to: Southwest ResearchInstitute6220 Culebra RoadSan antonloTX 78238(210)522-2169
Reference Case: |-%
aienl No: K31M5 \\̂
Chain of Custody RecordRelinquished By (Date / Time)
1 ̂ **&&&- Ml** *S«2
3
4
Sampler -. ^^^Snnature- r-̂ ^^s&ji&£- • .oigiiamru.̂ ,'̂ Sjrj9f^ *-
Received By (Dale / Time)
MATRIX/ CONG/ ANALYSIS/ TAG No7 STATION SAMPLE COLLECT QCSAMPLE No. SAMPLER TYPE TURNAROUND PRESERVATIVE LOCATION DATE/TIME SAMPLE No. T>pe
" Vlil-iwvi/10A-0 Ground Watej/ UG PFOSTPFOA (21)1 Eric Hinkle
Ground Vtfaterf UG PFOS/PFOA (21)EficHmkle
VM-MW15S-0 Ground Water/ UG PFOS.rpFOA(21)1 Eric HinWa
VM-MW1QA-01 S: 11/21/0^ 11353-740 (toe Only) (1)
3-615 (Ice Only) (1) VM-MW12S-01 -S: 11/19/02 14.15
3-730 (loe Only )(1) VM-MW15S-01 S: 11/20/02 1720
Shipment for CaseComplete? Y
Analysis Key:
PFOS/PFOA = Perflut
Sample(s) to be used for laboratory QC: Additional Sampler Signatures):
Concentration: L = {MI M c low/Medium| H = High lyp^Lteagnate: composite = C. Grab - G
Chain of Custody Seal Number
Shipment teed
irooctanyJ sultanate
TR dumber 3-424838327-112102-0001PffprLviOMi pralirninafy rasulU. R«quesU forpmlimmary ravulU will Increase analytical costs.Send Copy to: Contract Laboratory Analytical Services Support, 2000 Edmund Halley Dr., Heston, VA. 20191-3436 Phone 703/264-9343 Fax 70 #264-922
»>' * « H* tulff a i!F2VS.0.66 Papa 1 of 1
U.S. EPA Region III Sample Scheduling Request Form
RAS CASE No: DAS No: R31385
Date: 09/23/02 Data Validation Level: M3
Site Name: Valmont TCE
NSFNo:
EPA Lab Reply:
Cost: c
Address: Deer Run Road City: West Hazleton State: PA
Latitude: 40 58" 04" Longitude: 76 00' 56"
Program: SUPERFUND CERCLIS No: PAD982363970
Account No: 02T03N50102D031MCO01 Operable Unit:
Preparen Megan Ritchie RPM/PO:Romuald Roman
Phone: 610-491-9688 Phone: 215-814-3212
FAX: 610-491-9645 FAX: 215-814-3002
E-mail: [email protected] E-mail: Romuald [email protected]
Anal +Val Data TAT:42 days
Activity: RI/FS
Spill ID:
Site Leaden Neil Teamerson
Phone: 610-491-9688
FAX: 610-491-9645
E-mail: [email protected]
EPA CO: Al Pinero Contract Type: RAC 3 Prime: Tetra Tech NUS Sub:
Lab Assignment Date: Analytical TAT: 21 days
Organic Lab:
Inorganic Lab:
SAMPLES
10
METHOD
SW-846 8270C
/2wadA
Ship Date From: 10/28/02
Ship Date To: 11/15/02
Carrier:
PARAMETER
PFOA/PFOS (perfluorooctanyl sulfonate) f ^/ Q *~f-3>
%y 7~flZ>4^. *-/̂ c$> /L£&tte4&& ^ #£i&7jZ5L/
Appendix D
Laboratory Case Narratives
SwRI Case NarrativeClient: EPA Region III Case R31385SDG: 216587(FB-01) 010003SwRI Project Number: 06053.08.005SwRI Work Order Number: 23463,23483Page 2
Tuning ofLC/MS:
Negative mode electrospray check tune was performed prior to analysis of the calibrationstandards and samples. Peak width and mass axis were checked to verify the mass calibration ofthe instrument.
LC/MS Analysis and Calibration:
Negative mode electrospray LC/MS in selected-ion-monitoring mode was used in the analysis ofPFOA and PFOS. Reverse phase HPLC conditions were used in eluting the perfluorocompounds. Since these perfluoro compounds do not contain any chromophores, diode arraydetector was turned off during the LC/MS analysis.
Five point calibration curve was used for the quantitation of perfluorooctanoic acid (PFOA) andperfluorooctanyl sulfonate (PFOS). Calibration range was from 0.20-0.0lu,g/mL. Thepotassium salt form of PFOS was used in the calibration standards. The concentration valueswere adjusted to reflect only the anion of PFOS. Two peaks were observed in the calibrationstandard for PFOS. Both peaks were assigned the theoretical concentration of PFOS in thecalibration standards. External standard calibration with linear fit was used in the five pointcalibration. Correlation values were above 0.999 for the target analytes and surrogate. Responseratios (RF) for all the calibration standards were reported on the Form VI- and Form VII.Response ratios were obtained by dividing the area of the peak with the concentration of theanalyte.
Continuing calibration standard (O.lug/mL) was analyzed in the middle and also at the end of thesequence. Percent differences were all less than 15% in both continuing calibration standards.
Target analyte Quantitation:
Two peaks were observed in the calibration standard for PFOS. The two peaks were labeled asPFOS1 and PFOS2. The average value between the two peaks were reported as theconcentration of PFOS in the samples. As for PFOA, only one peak was observed in thecalibration standards, however, two peaks were observed in the samples with PFOA hits such assamples VM-MW10A-01 and VM-MW12S-01. Only the peak at elution time 9.3mm wasquantitated as PFOA.
Sample calculation:
File ID: VI127218 Sample: VM-MW10A-01 Extract Volume: 4mLAnalyte: PFOS Sample volume: 0.2L
SwRI Case NarrativeClient: EPA Region III Case R31385SDG: 216587(FB-01)SwRI Project Number: 06053.08.005SwRI Work Order Number: 23463,23483Page 1
010002
SwRI CASE NARRATIVE
1. Ten (10) samples were received for TDG analysis by Method 8321:
SwRI ID216587216588216589216590216591216592216593216834216835216836
Customer IDFB-01RB-01VM-GW21-01VM-MW11D-01VM-MWHS-01VM-MW14S-01VM-MW41S-01VM-MW10A-01VM-MW12S-01VM-MW15S-01
MatrixWATERWATERWATERWATERWATERWATERWATERGROUND WATERGROUND WATERGROUND WATER
Samples were received at SwRI on November 20 and 22, 2002 for a twenty-one (21) dayhardcopy turnaround time from Validated Time of Sample Receipt (VTSR).
Quality Control Identification:LCSVM-MW11S-01MS/MSD
ANALYSIS FOR METHOD 8321:
LC/MS analysis of Pefluorooctanoic acid (PFOA) and Pefluorooctanyl sulfonate (PFOS)
Extraction:
An aliquot of 200mL was removed from each sample and was extracted using CIS solid phaseextraction (SPE) cartridges. Extraction procedure was based on the article by Moody et al.1
Prior to extraction, perfluorononanoic acid (PFNA) was added to the water sample as theextraction surrogate. The sample was passed through a CIS SPE cartridge and was eluted withtwo aliquots of 2mL of methanol. The final volume was adjusted to 4mL and the extract wasanalyzed by negative mode electrospray LC/MS. Contact of samples and extracts with glasssurfaces should be minimized because the perfluoro compounds easily bind to glass.Polypropylene containers were used during extraction, storage and analysis.
SwRI Case NarrativeClient: EPA Region III Case R31385 010004SDG: 216587(FB-01)SwRI Project Number: 06053.08.005SwRI Work Order Number: 23463,23483Page 3
Average value of PFOS1 and PFOS2:(0.040632 + 0.0233462) / 2 = 0.031989 u^g/mL in extract
Concentration of PFOS in the water sample:0.031989ng/mLx4mL/0.2L = 0.64ug/L
Laboratory Method Blank:
One laboratory method blank (SwRI ID: 216922) was generated to cover both work orders.Contamination was not observed in the blank.
Laboratory Control Standard (LCS):
Recoveries of PFOA and PFOS were above 75%.
Surrogate Recoveries:
The surrogate recoveries ranged from 60-105%. Since no QC limits were established for theperfluoro compounds in water samples, an advisory limit of 50-150% was used.
Matrix Spike Recoveries:
All the matrix spike recoveries were above 70%. Since no QC limits were established for theperfluoro compounds in water samples, an advisory limit of 50-150% was used.
Reference:
1. Determination of perfluorinated surfactants in surface water samples by two independentanalytical techniques: liquid chromatography/tandem mass spectrometry and 19F NMR.Moody CA, Kwan WC, Martin JW, Muir DC, Mabury SA. Anal Chem 2001 May15;73(10):2200-6.
SwRI Case NarrativeClient: EPA Region III Case R31385 01 0 0 0SDG: 216587(FB-01) I. 1U UISwRI Project Number: 06053.08.005SwRI Work Order Number: 23463,23483Page 4
"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 has been authorized bythe Director or his designee, as verified by the following signature. This report shall not bereproduced except in full, without the written approval of SwRI."
Jo^rin BoydjManager DateQuality Assurance UnitDivision 01
"Sloboda, Russell" To: Judy Snyder/ESC/R3/USEPA/US@EPA Subject: RE: additional forms needed by ttnus for Valmont TCE and Frankli n
Slag for risk asses, data base12/27/0203:51 PM
For the project data being used for risk assessment:
Electronic data summary forms are needed for organic and inorganic data.This allows importing of data into a database without resorting to manualdata entry. Sample detection or quantitation limits are required for riskassessment statistical calculations but because of past precedents Region 3does not add these numeric "U" values to the data summary. Therefore,additional laboratory documentation is needed. We start with the electronicdata summary and then use multiplicative factors and generic detectionlimits from the laboratory Forms to back calculate and fill in the missingdetection limits, and afterwards check our work against the Form I's.
Organic Data --We need Form Is so we can reproduce the sample quantitationlimit. No other laboratory forms are needed for the risk assessment oforganic data.
Inorganic data --We need Form Is so we can look up sample detection limitsand also the instrument detection limit form (Form 10), and the samplepreparation weight forms (Form 13) for all analytes and all SDGs.
Original MessageFrom: Snyder.Judy®epamail.epa.gov [mailto:[email protected]]Sent: Friday, December 27, 2002 3:23 PMTo: Sloboda, RussellCc: Teamerson, Neil; Ritchie, MeganSubject: additional forms needed by ttnus for Valmont TCE and Franklin Slagfor risk asses, data base
We are processing an extremely large case (case number 31112) from ValmontTCE, full organic suite, at present. I know you guys said you needed FormI's, Form X's and Form XIII's for the inorganic cases we dealt with a coupleof months ago for a risk assessment data base. Russ mentioned two sites thatrequired more than data summary forms -Valmont TCE and Franklin Slag. I want to be sure we supply what youneed, this time on the first go-round. What Form numbers do you needfor the organic data besides the Form I's for this organic Valmont TCE datawhich will be entered in a risk assessment data base by you? The Forms youneed will be included with the validation report.************Judy SnyderESAT Auditor, Region 3Lockheed Martin Environmental Services701 Mapes RoadFt. Meade, MD 20755-5350Phone 410-305-3015Fax 410-305-3095
Form Is
010017SOUTHWEST RESEARCH INSTITUTEPFOA/PFOSAnalysis Data Reporting Form
Client: EPA Region III
Case: R31385
SDG- 216587
Matrix: Water
Extract Volume (mL)' 4
pH:6 I
CAS No.
Client Sample ID: FB-01System ID: 216587
Instrument: LC/MS VL
Filename: VI127207Sample Volume (mL). 200
Compound
Project Number: 06053.08.005
Date Received: Nov 20, 2002
Date Extracted: Nov 25, 2002
Date Analyzed: Nov 27, 2002 15-27
Dilution Factor: 1
ug/L
335-67-1 Perfluorooctanoic acidPerfluorooctanyl sulfonate
0.20 U0.20 U
DATA REPORTING QUALIFIERS
B Tins flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration rangeJ Indicates an estimated value
U Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of 1 FORM I
Q10021SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client- EPA Region III Client Sample ID: RB-01 Project Number: 06053.08.005
Case: R31385 System ID: 216588 Date Received: Nov 20, 2002
SDG. 216587 Instrument: LC/MS VL Date Extracted- Nov 25,2002
Matrix. Water Filename: V1127208 Date Analyzed: Nov 27, 2002 15:45Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1
pH:6.1
CAS No. Compound ug/L335-67-1 Perfluorooctanoic acid 0.20 U
Perfluorooctanyl sulfonate 0.20 U
DATA REPORTING QUALIFIERSB This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration range
) Indicates an estimated "ilue
U Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 1OU)based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of I FORM 1
010025SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region IIICase: R31385SDG: 216587Matrix: WaterExtract Volume (mL)- 4pH: 6.3
CAS No.
Client Sample ID: VM-GW21-01System ID: 216589Instrument: LC/MS VLFilename: VI127209Sample Volume (mL)- 200
Compound
Project Number: 06053.08.005Date Received: Nov 20, 2002Date Extracted: Nov 25, 2002Date Analyzed: Nov 27, 2002 16:04Dilution Factor. 1
335-67-1 Perfluorooctanoic acid
Perfluorooctanyl sulfonate
DATA REPORTING QUALIFIERS0 This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration range
J Indicate., an estimated valueU Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of I FORM I
010028SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region III Client Sample ID: VM-MW11D-01 Project Number. 06053.08.005Case: R31385 System ID. 216590 Date Received: Nov 20, 2002SDG: 216587 Instrument: LC/MS VL Date Extracted: Nov 25, 2002Matrix: Water Filename: VII27210 Date Analyzed: Nov 27, 2002 16:22Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1pH: 6.0
CAS No. Compound ug/L
335-67-1 Perfluorooctanoic acid 0.20 U
Perfluorooctanyl sulfonate 0.20 U
DATA REPORTING QUALIFIERSB "Fins flag ts used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration range
J Indicates an estimated value
U Indicates compound was analyzed for, but not detected. Report the minimum detection limit for the sample with \J (eg IOU)based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of 1 FORM I
010031SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region III Client Sample ID: VM-MWllS-01 Project Number: 06053.08.005Case. R31385 System ID: 216591 Date Received: Nov 20, 2002SDG: 216587 Instrument: LC/MS VL Date Extracted: Nov 25, 2002Matrix: Water Filename: V1127211 Date Analyzed: Nov 27, 2002 16:40Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1
PH- 6 0
CAS No. Compound ug/L
335-67-1 Perfluorooctanoic acid (^0.043 f)Perfluorooctanyl sulfonate 0.20 U
DATA REPORTING QUALIFIERSB This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
C Tins flag indicates compounds whose concentrations exceed the calibration range
J Indicates nn estimated valueU Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of 1 FORM I
SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
010034
Client: EPA Region III
Case: R31385
SDG: 216587
Matrix: Water
Extract Volume (mL): 4
pH: 6.0
CAS No.
Client Sample ID: VM-MW14S-01
System ID: 216592
Instrument: LC/MS VL
Filename: VI127216
Sample Volume (mL): 200
Compound
Project Number: 06053.08.005
Date Received: Nov 20, 2002
Date Extracted: Nov 25,2002
Date Analyzed: Nov 27, 2002 18:11
Dilution Factor: 1
ug/L
335-67-1 Perfluorooctanoic acidPerfluorooctanyl sulfonate
0.20 U0.20 U
DATA REPORTING QUALIFIERS
B This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration range <
i Indicates an estimated value.U Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of I FORM I
010038SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
}
Client: EPA Region III Client Sample ID: VM-MW41S-01 Project Number: 06053.08.005Case: R31385 System ID: 216593 Date Received: Nov 20,2002SDG: 216587 Instrument: LC/MS VL Date Extracted. Nov 25, 2002Matrix: Water Filename: VI127217 Date Analyzed: Nov 27, 2002 18:29Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1pH: 6.0
CAS No. Compound ug/L335-67-1 Perfluorooctanoic acid 0.20 U
Perfluorooctanyl sulfonate 0.20 U
DATA REPORTING QUALIFIERSB Phis flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported-at a secondary dilution factorE This flag indicates compounds whose concentrations exceed the calibration rangeJ Indicates an estimated value.U Indicates compound was analyzed for , but not detected Report the minimum detection limit for the sample with U (e g 10U)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of 1 FORM I
010042SOUTHWEST RESEARCH INSTITUTEPFOA/PFOSAnalysis Data Reporting Form
Client: EPA Region III Client Sample ID: VM-MW10A-OI Project Number: 06053.08 005Case: R31385 System ID: 216834 Date Received: Nov 22, 2002SDG:216587 Instrument: LC/MS VL Date Extracted: Nov 25, 2002Matrix: Water Filename: V1127218 Date Analyzed: Nov 27, 2002 18:47Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1pH: 6.0
CAS No. Compound
335-67-1 Perfluorooctanoic acid
Perfluorooctanyl sulfonate
DATA REPORTING QUALIFIERSB This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factorE This flag indicates compounds whose concentrations exceed the calibration range
J Indicates an estimated value
U Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 1OU)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of 1 FORM I
010045SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region III Client Sample ID: VM-MW12S-01 Project Number: 06053.08.005Case: R31385 System ID: 216835 Date Received: Nov 22, 2002SDG: 216587 . Instrument: LC/MS VL Date Extracted: Nov 25,2002Matrix: Water Filename: V1127219 Date Analyzed: Nov 27, 2002 19:05Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1pH: 6.4
CAS No. Compound ug/L_^335-67-1 Perfluorooctanoic acid
SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region III Client Sample ID: VM-MWI5S-01 Project Number: 06053.08.005Case: R31385 System ID: 216836 Date Received: Nov 22, 2002SDG: 216587 Instrument: LC/MS VL Date Extracted: Nov 25, 2002Matrix. Water Filename: VI127220 Date Analyzed: Nov 27, 2002 19:23Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1pH:6.1
CAS No. Compound ug/L
335-67-1 Perfluorooctanoic acid 0.20 U
Perfluorooctanyl sulfonate 0.20 U
DATA REPORTING QUALIFIERSB This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration range
J Indicates an estimated valueU Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of 1 FORM I
ATTACHMENT 2
Support Documentation
VVtKA ubtKA Contract Laboratory ProgramGeneric Chain of Custody
Date Shipped: 11/19/02Carrier Name: FedEx
Airbill: 828684646973
Shipped to- Southwest ResearchInstitute6220 Culebra RoadSan antonio TX 78238(210) 522-2169
Chain of Custody RecordRelinquished By (Date / Time)
^^&&~ It-lt-oz- I6>*=>2
3
4
Sampler ^*. sî *&^^Signature: ££~/s^*£.Received By (Date / Time)
f/^L *.£*-J(s &^c^z" \\jzt/i3Z~.o^2^~
-'
Reference CasClient No: R31385 1
SDG No: 1
For Lab Use OnlyLab Contract No:
Unit Price:
Transfer To:
Lab Contract No:
Unit Price:
MATRIX/ CONC/ ANALYSIS/ TAG No / STATION SAMPLE COLLECT FOR LAB USE ONLYSAMPLE No. SAMPLER TYPE TURNAROUND PRESERVATIVE LOCATION DATE/TIME SAMPLE No. Sample Condition On Receipt
AFPA USEPA Contract Laboratory ProgramGeneric Chain of Custody
Date Shipped: 11/21/02
Carrier Name: FedEx
Airbill: 828684646756
Shipped to: Southwest ResearchInstitute6220 Culebra RoadSan antonio TX 78238(210)522-2169
Chain of Custody RecordRelinquished By (Date / Time)
1 ̂ ^^- /W-02. /$2
3
4
Sampler ^—* .ff-rf^Signature' ^^—-^V^ .̂ —Received By (Date / Time)
J/a/M/L/MX2T ///S2/OJL /U/ ' r f r
Reference CasClient No: R31385 |
SDG No: I
For Lab Use OnlyLab Contract No:
'Unit Price:
Transfer To:
Lab Contract No:
Unit Price:
MATRIX/SAMPLE No. SAMPLERSAP*
CONG/ ANALYSIS/TYPE TURNAROUND
TAG No./ STATION - SAMPLE COLLECT FOR LAB USE ONLYPRESERVATIVE LOCATION DATE/TIME SAMPLE No. Sample Condition On Receipt
\/VM-MWnUA-(J1 larouna Water/ L/lj rrUo/rTUA (zl). Eric Hmkle
J/VM-MW12S-01 Ground Water/ L/G PFOS/PFOA (21)Eric Hmkle
/VM-MW15S-01 Ground Water/ L/G PFOS/PFOA (21)* Eric Hmkle
(ice uniy) (i) VM-MWiUA-01 .o. 11/^1/0^ 11:00
v/3-3-615 (Ice Only) (1), VM-MW12S-01 S: 11/19/02 14:15
-730 (Ice Only) (1) VM-MW15S-01 S' 11/20/02 17:20
"faA f>2.
o>-*o
Shipment for CaseComplete'-'Y
Analysis Key:
PFOS/PFOA = Perfluoro
Sample(s) to be used for laboratory QC:
fiff*
Additional Sampler Signature(s):
A//*"
Cooler TemperatureUpon Receipt:
Concentration: L = Low, M = Low/Medium, H = High Type/Designate:Composite = C, Grab = G
Chain of Custody Seal Number:
^Custody Seal Intact? Shipment Iced
octanyl sulfonate
TR Number: 3-424838327-112102-0001felifflinary results. Requests for preliminary results will increase analytical costs. &=^^Contract Laboratory Analytical Services Support, 2000 Edmund Halley Dr., Reston, VA. 20191-3436 Phone 703/264-9348 Fax 703/264-922
•YF2V5.0.66 Page 1 of 1
SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
010054
Project Number: 06053.08 005Instrument: LC/MS VL
Case. R31385 SDG:2I6587Column: Agilent Zorbax SB C-18150mm x 2.1 mm, 5 micron
RF1 RF2 RF3 RF4 RF5Analysis DateAnalysis Time
Lab File IDCompoundPFOAPFOS1PFOS2PFNA (surrogate)
11/27/0213:38
V1127201RF1
6819104155051242418908207
11/27/0213:56
V1127202RF2
7053684169951224275956498
11/27/0214:14
V1127203RF3
7032744066661211833982985
11/27/0214:32
V1127204RF4
71794243113912987821098644
11/27/0214:51
V1127205RF5
75141147613213759171312482
Mean71198142928712706451051763
%RSD3.66.47.812.3
Page 1 of 1 FORM VI
Method C:\HPCHEM\1\METHODS\PFOA.M
Calibration Table 010055MPA only
Calib. Data Modified
CalculateBased on
Rel. Reference WindowAbs. Reference WindowRel. Non-ref. WindowAbs. Non-ref. WindowUncalibrated PeaksPartial CalibrationCorrect All Ret. Times
Curve TypeOriginWeight
Recalibration SettingsAverage ResponseAverage Retention Time
Wednesday, November 27, 2002 4:29:28 PM
External StandardPeak Area
20.000 %1.000 min ,5.000 %1.000 minnot reportedYes, identified peaks are recalibratedNo, only for identified peaks
LinearIgnoredEqual
Average all calibrationsFloating Average New 75%
Calibration Report Options :Printout of recalibrations within a sequence:
Calibration Table after RecalibrationNormal Report after Recalibration
If the sequence is done with bracketing:Results of first cycle (ending previous bracket)
Signal 1: MSDl 369, EIC=368.7:369.7Signal 2: MSDl 499, EIC=498.7:499 . 7Signal 3: MSDl 419, EIC = 418.7:419 . 7
RetTime Lvl Amount[mm] Sig [ug/mL]
Area Amt/Area Ref Grp Name
7.331
7.673
7.894
8.081
11 5
4321
2 5432J_
2 54321
3 54321
l.OOOOOe-22.00000e-25.00000e-2l.OOOOOe-12.00000e-ll.OOOOOe-22.00000a-25.00000e-2l.OOOOOe-12.00000e-ll.OOOOOe-22.00000e-25.00000e-2l.OOOOOe-12.00000e-ll.OOOOOe-22.00000e-25.00000e-2l.OOOOOe-12.00000e-l
7514.123051.43588e43.51638e47 .05365e41.36382e54761.309088622.786132.03333e44.16995e48.31011e41.37592e42.59756e46.05916e41.22428e52.48484e51.31248e42.19729e44.91493e49.56500e41.81641e5
1.33083e-61.39287e-61.42192e-61.41770e-61.46647e-62.10026e-62.31944e- :2.45902e-62.39811e-62.40671e-67.26788e-77.69952e-78.25196e-78.16810e-78.04882e-77.61915e-79.10213e-71.01731e-61.04548e-61.10107e-6
1 PFOA
2 PFOS1
2 PFOS2
3 PFNA
Group summary :
Jroup 1 ( ?r-0rt ) -Group members:
PFOA with retention time 7.331 minGroup 2 ( PFOS ) :
L.CMS VT, 1 1 /?"7
Method C:\HPCHEM\1\METHODS\PFOA.M
Group members:PFOS1 with retention time 7.673 minPFOS2 with retention time 7.894 min
Group 3 ( PFNA (Surr) ) :Group members:
PFNA with retention time 8.081 min
1 Warnings or Errors :
Warning : Overlapping peak time windows at 7.673 min, signal 2
010056
Peak Sum Table
***No Entries in table***
Area j
120000-
100000-
80000-^
60000-
40000
20000
0
Calibration Curves
0.1Amount[ug/mL]
0.2
PFOA at exp. 'RT: 7.331MSD1 369, EIC=368.7:369.7Correlation: 0.99987Residual Std. Dev.: 973.34907Formula: y = mx V b
m: 679517.81538b: 1147.72220x: Amount[ug/mL]y: Area
f~ Area :I 80000-^
"T01
-Amo.unt[ug/mL]_
PFOS1 at exp. RT: 7.673MSD1 499, EIC=498.7:499.7Correlation: 0.99994Residual Std. Dev.: 420.21359
y = mx + b413745.13415
258.96033x: Amount[ug/mL]y: Area
Formula:
PFOS2 at exp. RT: 7.894MSD1 499, EIC=498.7:499.7Correlation: 0.99990Residual Std. Dev.: 1584.48046Formula: y = mx + b
m: 1.23599e6b: 312.17896x: Amount[ug/mL]y: Area
CMS VL 11/27/2002 4:30:23 PM AYY
Method C:\HPCHEM\1\METHODS\PFOA.M
150000-
125CXXH
100000-:
75000 -:
50000-
PFNA at exp. RT: 8.081MSD1 419, EIC=418.7:419.7Correlation: 0.99986Residual Std. Dev.: 1342.26083Formula: y = mx + b
m: 889073.09165b: 4737.98078x: Amount[ug/mL],y: Area
010057
VL 11/27/2002 4 : 3 0 : 2 3 PM AYY
Data File C:\HPCHEM\1\DATA\PFOA\V1127201.D Sample Name: PFOA/OS 0.2ug/mL
Injection DateSample NameAcq. Operator
Acq. MethodLast changedAnalysis MethodLast changed
11/27/2002 1:38:57 PMPFOA/OS 0.2ug/mLAYY
C:\HPCHEM\1\METHODS\PFOA.M11/27/2002 1:34:13 PM by AYYC:\HPCHEM\1\METHODS\PFOA2.M11/28/2002 7:39:50 AM by AYY
Seq. LineLocation
InjInj Volume
1Vial 21
10 fil010058
fcfcJZJtZMSD1 TIC, MS File (PFOAW1127201 D) APl-ES, Neg, SIM, Frag: 85 (TT)35000 -i
30000 -.
25000-
20000-
15000-
10000-
5000-
0-.10 11
MSD1 369, EIC=368.7:369.7 (PFOA\V1127201 D) APl-ES, Neg, SIM, Frag: 85 (TT)
20000-:
17500-;
15000 4
12500-!
10000-i
7500-3
5000^
2500-3
8
35000
30000
25000
20000
15000
10000
5000
10 11MSD1 499, EIC=498 7 499 7 (PFOAXV1127201 D) APl-ES, Neg, SIM, Frag- 85 (TT)
mm
10 11MSD1 419, EIC=418.7.419 7 (PFOAW1127201.0) APl-ES, Neg, SIM, Frag: 85 (TT)
25000 -j
20000 -
15000
10000-
5000-
0-1~\—10 11 mm
CMS VL 12 /2 /2002 4 : 4 2 : 2 1 PM GAA
010068SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Project Number: 06053.08.005Instrument: LC/MS VL
Case: R31385 SDG: 216587Column: Agilent Zorbax SB C-18150mm x 2.1 mm, 5 micron
Lab File ID: V1127214
Compound
Analysis Date: 11/27/02Initial Date: 11/27/02
Analysis Time: 17:34Initial Time: 13:38 14:51
MeanRRF RF4 %DPFOAPFOS1PFOS2PFNA (surrogate)
71198142928712706451051763
7166964432301339650982383
0.73.25.4-6.6
Page I of 1 FORM VII
010072SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Project Number: 06053.08.005Instrument: LC/MS VL
Case: R31385 SDG: 216587Column: Agilent Zorbax SB C-18 150mm x 2.1 mm, 5 micron
Lab File ID: V1127221 Analysis Date: 11/27/02Initial Date: 11/27/02
Compound Mean RRF RF4
Analysis Time: 19:41Initial Time: 13:38 14:51
%DPFOAPFOS1PFOS2PFNA (surrogate)
71198142928712706451051763
7267584700011454140986545
2.19.514.4-6.2
Page 1 of 1 FORM VII
SwRI LabsClient: EPA REGION IIIProject 06053.08005Case: R31385
(E8321) PFOA/OS WATER SOLID-PHASE EXTRACTION
SDG: 216587Work Order: 23463,23483
010091
DATE EXTRACTEDANALYSTS INVOLVED
SURROGATE SOL. IDVITX SPK SOL. IDEXTRACTS LOCATION
CHEMICAL.BRAND &LOT#
11/25/02ALICE YAU (SP.SU.FV)HAMED EDRISI (SW.SU)PFNA SURR 1 67-01 -98BIO020PFOA/OS MS 167-02-98BIO020FREEZER #48 XVII C-1 AY/HE1 1/25/02
OZARKA WATER LOTS2403536B&J METHANOL LOT#BY081C18 SUPELCO LOT3SP2638E
NOTE
ADDITIONAL NOTE
EXT CODE 1EXTRACTION FLOWCHART
PIPET Eppendorf 10-100uL S N.339512
ALL SAMPLES WERE PASSEDTHROUGH C18 BY VACUUM AT 5psiE8321200mL >» FV4000uL MEOH
System ID
216587216588216589216590216591216591216591216592216593216834216835216836216922216923
Type
MSMSD
Customer ID
FB-01RB-01VM-GW21-01VM-MW11D-01VM-MW11S-01VM-MW11S-01VM-MW11S-01VM-MW14S-01VM-MW41S-01VM-MW10A-Q1VM-MW12S-01VM-MW15S-01WQC BLANKLCS
PH
6.16.16.36.06.06.06.06.06.06.0646.16.060
SAMPLEVOL (ML)
200200200200200200200200200200200200200200
SURROGATE SOLVOL
100 uL100 uL100 uL100 uL100 uL100 uL100 uL100 uL100 uL100 uL100 uL100 uL100 uL100 uL
MTX SPK SOLVOL
0 uL0 uL0 uL0 uL0 uL
100 uL100 uL
0 uL0 uL0 uL0 uL0 uL0 uL
100 uL
FVMETHANOL
(UL)40004000400040004000400040004000400040004000400040004000
Page created Nov 25 2002 1.54PM by HEdnsiBook- EXTRACTION LAB, Volume. EXT-2002, Page 737 (Section 1 of 1)
Approved by SUSANA GONZALEZ on Dec 2 2002 11 02AM
Date Printed- 12/03/2002
ver (07/17/2002)
010012
SOUTHWEST RESEARCH INSTITUTESystem Monitoring Compound Recovery
Project Number: 06053.08.005 Case: R313 85 SDG: 216587
SMC1Sample ID (PFNA) OutWQC BlankFB-01RB-01VM-GW21-01VM-MW11D-01VM-MW11S-01VM-MW11S-01 MSVM-MW11S-01 MSDVM-MW14S-01VM-MW41S-01VM-MW10A-01VM-MW12S-01VM-MW15S-01LCS
10570649360868176756190808891
00000000000000
Advisory QC LimitsSMC1 (PFNA) = Perfluorononanoic acid (50-150)
FORM II-A
010013
SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Laboratory Control Spike Recovery
Client: EPA Region III
Client Sample ID: LCSSystem ID: 216923
Project Number: 06053.08.005
LCSCone
Compound (ug/L)Perfluorooctanoic acidPerfluorooctanyl sulfonate
2.002.00
LCSRecovery
(ug/L)1.701.60
MS%
REC8580
QCLIMITS%REC50-15050-150
FORM III
010081SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client- EPA Region III Client Sample ID: LCS Project Number: 06053.08.005
Case:R31385 System ID: 216923 Date Received: NA
SDG: 216587 Instrument: LC/MS VL Date Extracted: Nov 25, 2002
Matrix: Water Filename: VI127215 Date Analyzed: Nov 27,2002 17:53
Extract Volume (mL): 4 Sample Volume (mL): 200 , Dilution Factor: 1
pH: 6.0
CAS No. Compound ug/L335-67-1 Perfluorooctanoic acid 1.7
Perfluorooctanyl sulfonate 1.6
DATA REPORTING QUALIFIERS
B This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor.
E This flag indicates compounds whose concentrations exceed the calibration range
J Indicates an estimated valueU Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of I FORM 1
SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Matrix Spike/Duplicate Recovery
010014
Client: EPA Region III
Client Sample ID: VM-MW11S-01System ID: 216591
Project Number: 06053.08.005
SPIKEADDED
Compound (ug/L)Perfluorooctanoic acidPerfluorooctanyl sulfonate
2.002.00
SAMPLECONC(ug/L)0.0430.20 U
MSCONC
(ug/L)1.681.52
MS%
REC8276
QCLIMITS%REC50-15050-150
SPIKEADDED
Compound (ug/L)Perfluorooctanoic acidPerfluorooctanyl sulfonate
2.002.00
MSDCONC(ug/L)
1.591.42
MSD%
REC7771
QCLIMITS%REC50-15050-150
%RPD
67
QCLIMITS%RPD
2525
FORM III
010084SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region III Client Sample ID: VM-MW11S-01 MS Project Number: 06053.08.005
Case. R31385 System ID' 216591MS Date Received: Nov 20,2002
SDG: 216587 Instrument: LC/MS VL Date Extracted: Nov 25, 2002Matrix: Water Filename: V1127212 Date Analyzed: Nov 27, 2002 16:58
Extract Volume (mL). 4 Sample Volume (mL): 200 Dilution Factor: 1
pH: 6.0
CAS No. Compound ug/L335-67-1 Perfluorooctanoic acid 1.7
Perfluorooctanyl sulfonate 1.5
DATA REPORTING QUALIFIERS
B This flag is used when the analyte is found in the blank as well as the sample
D This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration range
.1 Indicates an estimated value
U Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page 1 of 1 FORM I
010087SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region III Client Sample ID: VM-MW11S-01 MSD Project Number: 06053.08.005Case:R31385 System ID: 216591MSD Date Received: Nov 20, 2002SDG: 216587 Instrument: LC/MS VL Date Extracted: Nov 25, 2002Matrix: Water Filename: VI127213 Date Analyzed: Nov 27,2002 17:16Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor- 1pH- 6.0
CAS No. Compound . ug/L
335-67-1 Perfluorooctanoic acid 1.6
Perfluorooctanyl sulfonate 1.5
DATA REPORTING QUALIFIERSB This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factor
E This flag indicates compounds whose concentrations exceed the calibration range
J Indicates an estimated value
U Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 10U)based on necessary concentration dilution action (This is not necessarily the instrument detection limit)
Page I of 1 FORM I
010077SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form
Client: EPA Region III Client Sample ID: WQC Blank Project Number: 06053.08.005Case: R31385 System ID: 216922 Date Received: NASDG: 216587 Instrument: LC/MS VL Date Extracted: Nov 25,2002Matrix: Water Filename: V1127206 Date Analyzed: Nov 27,2002 15:09Extract Volume (mL): 4 Sample Volume (mL): 200 Dilution Factor: 1pH: 6.0
CAS No. Compound ug/L335-67-1 Perfluorooctanoic acid 0.20 U
Perfluorooctanyl sulfonate 0.20 U
DATA REPORTING QUALIFIERSB This flag is used when the analyte is found in the blank as well as the sampleD This flag identifies a compound reported at a secondary dilution factorE This flag indicates compounds whose concentrations exceed the calibration rangeJ Indicate.s an estimated valueU Indicates compound was analyzed for , but not detected. Report the minimum detection limit for the sample with U (e g. 10(J)
based on necessary concentration dilution action (This is not necessarily the instrument detection limit).
Page 1 of 1 FORM I
010015
SOUTHWEST RESEARCH INSTITUTEBlank Summary
Blank ID: WQC Blank 216922Project Number: 06053.08.005Instrument: LC/MS VL
Case: R31385Filename: VI127206
This Blank Applies to the Following Samples
Sample ID SwRIID Lab File ID
SDG:216587Date Analyzed: Nov 27, 2002 19:23
AnalyzedWQC BlankFB-01RB-01VM-GW21-01VM-MW11D-01VM-MW11S-01VM-MW11S-01 MSVM-MW11S-01 MSDVM-MW14S-01VM-MW41S-01VM-MW10A-01VM-MW12S-01VM-MW15S-01LCS
216922216587216588216589216590216591
216591MS216591MSD
216592216593216834216835216836216923
V1127206V1127207V1127208V1127209V1127210V1127211V1127212V1127213V1127216V1127217V1127218V1127219V1127220V1127215
11/27/0215:0911/27/0215:2711/27/0215:4511/27/0216:0411/27/0216:221 1/27/02 16:401 1/27/02 16:5811/27/0217:1611/27/0218:1111/27/02 18:2911/27/0218:4711/27/0219:0511/27/02 19:2311/27/02 17:53
FORM IV
0%524: AR2023850%526: AR2023851%231: AR2023861%233: AR2023862%236: AR2023872%238: AR2023873%241: AR2023883%243: AR2023884%246: AR2023894%248: AR2023895%251: AR2023905%253: AR2023906%256: AR2023916%258: AR2023917%261: AR2023927%263: AR2023928%266: AR2023938%268: AR2023939%271: AR2023949%273: AR20239410%276: AR20239510%278: AR20239511%281: AR20239611%283: AR20239612%286: AR20239712%288: AR20239713%291: AR20239813%293: AR20239814%296: AR20239914%298: AR20239915%301: AR20240015%303: AR20240016%306: AR20240116%308: AR20240117%311: AR20240217%313: AR20240218%316: AR20240318%318: AR20240319%321: AR20240419%323: AR20240420%326: AR20240520%328: AR20240521%331: AR20240621%333: AR20240622%336: AR20240722%338: AR20240723%341: AR20240823%343: AR20240824%346: AR20240924%348: AR20240925%351: AR20241025%353: AR20241026%356: AR20241126%358: AR20241127%361: AR20241227%363: AR20241228%366: AR20241328%368: AR20241329%371: AR20241429%373: AR20241430%376: AR20241530%378: AR20241531%381: AR20241631%383: AR20241632%386: AR20241732%388: AR20241733%391: AR20241833%393: AR20241834%396: AR20241934%398: AR20241935%401: AR20242035%403: AR20242036%406: AR20242136%408: AR20242137%411: AR20242237%413: AR20242238%416: AR20242338%418: AR20242339%421: AR20242439%423: AR20242440%426: AR20242540%428: AR20242541%431: AR20242641%433: AR20242642%436: AR20242742%438: AR20242743%441: AR20242843%443: AR20242844%446: AR20242944%448: AR20242945%451: AR20243045%453: AR20243046%456: AR20243146%458: AR202431