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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.

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


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


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


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


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


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


335-67-1 Perfluorooctanoic acid (^0.043 f)Perfluorooctanyl sulfonate 0.20 U


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)


Page 1 of 1 FORM I

SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Data Reporting Form

010034


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


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


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)


Page 1 of I FORM I


}

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



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)


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


U Indicates compound was analyzed for, but not detected Report the minimum detection limit for the sample with U (e g 1OU)


Page 1 of 1 FORM I


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


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


335-67-1 Perfluorooctanoic acid 0.20 U




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)


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


^^&&~ 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


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


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


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


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


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


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 Sample ID: LCSSystem ID: 216923


LCSCone

Compound (ug/L)Perfluorooctanoic acidPerfluorooctanyl sulfonate

2.002.00

LCSRecovery

(ug/L)1.701.60

MS%

REC8580

QCLIMITS%REC50-15050-150

FORM III


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


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.


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)


Page 1 of I FORM 1

SOUTHWEST RESEARCH INSTITUTEPFOA/PFOS Analysis Matrix Spike/Duplicate Recovery

010014


Client Sample ID: VM-MW11S-01System ID: 216591


SPIKEADDED


2.002.00

SAMPLECONC(ug/L)0.0430.20 U

MSCONC

(ug/L)1.681.52

MS%

REC8276


SPIKEADDED


2.002.00

MSDCONC(ug/L)

1.591.42

MSD%

REC7771


%RPD

67

QCLIMITS%RPD

2525

FORM III


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



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


.1 Indicates an estimated value


Page 1 of 1 FORM I


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






Page I of 1 FORM I


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



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

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