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3 GLP10-01-02 Interim Report 25: Analysis of PFOS, PFHS and PFBS in Sediments Collected from the Jeffries Property Study Title 3M Environmental Laboratory Analytical Protocol GLP10-01-02: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program Data Requirement EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 Study Director Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way W est Chester, PA 19380 Phone: 610-701-3761 Principal Analytical Investigator Cleston C. Lange, Ph.D. 3M Environmental Laboratory Interim Report Completion Date Upon Signing Performing Laboratory 3M Environmental Health and Safety Operations Environmental Laboratory 3M Center, Bldg 260-05-N-17 St. Paul, MN 55144 Project Identification GLP10-01-02-25 Total Number of Pages 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property This page has been reserved for specific country requirements. Page 2 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property GLP Compliance Statement Report Title: GLP10-01-Q2 Interim Report 25: Analysis for PFOS, PFHS and PFBS in Sediments Collected from the Jeffries Property. 3M Environmental Laboratory Analytical Protocol GLP-1001-02: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program. This analytical phase was conducted in compliance with Toxic Substances Control Act (TSCA) Good Laboratory Practice (GLP) Standards, 40 CFR 792, with the exceptions listed below Exceptions to GLP compliance: o The reference substances were not all characterized under GLPs. o Because these are environmental samples and the study analytical In nature only, there was no specific test substance or control substance for this study. Page 3 of 24 Study: GLP10-01-Q2, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Q uality Assurance Statement Report Title: GLP10-01-Q2 Interim Report 25: Analysis for PFOS, PFHS and PFBS in Sediments Collected from the Jeffries Property. 3M Environmental Laboratory Analytical Protocol GLP-10-Q1-02: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program. This interim analytical report and the accompanying data were audited by the 3M Environmental Laboratory Quality Assurance Unit (QAU), as indicated below. The findings were reported to the principal investigator (P.I.), laboratory management and study director. Study Dnspection Pates 6/7/2012-6/8/2012 Phase Interim Report and Data P.l. 6/8/2012 Bate Reported to Study Pirector Management Study Breetoo- 6/13/2012 6/13/2012 Page 4 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Ta b l e o f Co n t e n t s GLP Compliance Statement.......................................................................................................................3 Quality Assurance Statement.....................................................................................................................4 Table of Contents........................................................................................................................................5 List of Tables................................................................................................................................................6 1 Study Information.................................................................................................................................7 2 Sum m ary..............................................................................................................................................8 3 Introduction...........................................................................................................................................9 4 Test, Control and Reference Substances.........................................................................................10 5 Test System........................................................................................................................................ 11 6 Method Summary............................................................................................................................... 11 6.1 M ethods................................................................................................................................. 11 6.2 Sample Receipt..................................................................................................................... 11 6.3 Sample Preparation...............................................................................................................12 6.4 Percent Soil Moisture Determination....................................................................................13 6.5 LC/MS/MS Analysis...............................................................................................................13 7 Analytical Results ............................................................................................................................... 14 7.1 Calibration .............................................................................................................................. 14 7.2 Limits of Quantitation (LO Q s)...............................................................................................16 7.3 Continuing Calibration...........................................................................................................16 7.4 Blanks..................................................................................................................................... 16 7.5 Laboratory Control Spikes (LCSs)........................................................................................16 7.6 Laboratory Matrix Spikes (LM Ss).........................................................................................18 7.7 Percent Moisture Determinations.........................................................................................18 7.8 Individual Analytical Sample Results....................................................................................19 Page 5 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property 8 Conclusion..........................................................................................................................................22 9 Data/Sample Retention......................................................................................................................23 10 List of Attachments.............................................................................................................................23 11 Signatures...........................................................................................................................................23 Lis t o f Ta b l e s Table 1. Results for Jeffries Property Sediments......................................................................................8 Table 2. LMS Recovery for Jeffries Property Sediments..........................................................................9 Table 4. Instrument Information................................................................................................................13 Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053)...................................................... 14 Table 6. Mass Transitions..........................................................................................................................14 Table 7. PFOS Calibration Summary....................................................................................................... 15 Table 8. PFHS Calibration Summary....................................................................................................... 15 Table 9. PFBS Calibration Sum m ary....................................................................................................... 15 Table 10. LCS Results (PFOS, linear + branchedisom er).....................................................................17 Table 11. LCS Results (PFHS, linear + branchedisom er).................................................................... 17 Table 12. LCS Results (PFBS)..................................................................................................................17 Table 13. Analytical Method Uncertainties.............................................................................................. 18 Table 14. Percent Moistures for Jeffries Property Sediments................................................................ 19 Table 15. Individual PFOS Results for Jeffries Property Sediments..................................................... 19 Table 16. Individual PFHS Results for Jeffries Property Sediments...................................................... 20 Table 17. Individual PFBS Results for Jeffries Property Sediments...................................................... 21 Page 6 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property 1 Study Information Sponsor 3M Company Sponsor Representative Gary A. Hohenstein Environmental Manager Special Projects, EHS Operations Bldg 224-5W-03 St. Paul, MN 55144 Phone: (651) 737-3570 gahoh enstein@ m m m .com Study Director Jaisimha Kesari, P.E., DEE W eston Solutions, Inc. 1400 Weston Way W est Chester, PA 19380 Study Analytical Testing Facility 3M EHS Operations Environmental Laboratory Building 260-5N-17 St. Paul, MN 55144 Study Personnel (3M Environmental Laboratory) Cleston C. Lange, Ph.D., Principal Analytical Investigator William K. Reagen, Ph.D., Laboratory Manager Patrick Kenney, Laboratory Technician (Pace Analytical, Professional Services) Marlene Heying, Laboratory Technician (Pace Analytical, Professional Services) Study Dates Study Initiation: March 08, 2010 Interim Analytical Initiation: March 12, 2012 Interim Analytical Completion: May 29, 2012 Interim Report Completion: Upon final Signatures Location of Archives All original raw data and analytical reports have been archived at the 3M Environmental Laboratory according to 40 CFR Part 792. The test substance and analytical reference standard reserve samples are archived at the 3M Environmental Laboratory according to 40 CFR Part 792. Page 7 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property 2 Summary This interim report provides the PFOS, PFHS and PFBS concentration results for five sediment samples collected in March 2012 at the Jeffries property in northern Alabama. In addition, one travel blank (trip blank), containing between10-25 grams of control soil in a sample bottle, accompanied the sample bottles to and from the site and was also analyzed for quality control purposes. Samples were logged into the 3M Environmental Laboratory information management system (LIMS) under project GLP10-01-01-26 and cross referenced to this project GLP10-01-02-25 for additional fluorochemical sulfonates analysis. Four aliquots of sample were removed from each sample bottle and accurately weighed for extraction. The first and second aliquot served as analytical sample and duplicate analytical sample. The third and fourth aliquots were fortified with nominal 20.0 and 200 ng each of PFOS (linear isomer), PFHS (linear isomer) and PFBS as a low and high laboratory matrix spike (LMS), respectively. Three aliquots of the trip blank were taken, with the third prepared as a single LMS that was fortified with nominal 1.00 ng each of PFOS (linear isomer), PFHS (linear isomer) and PFBS. Samples were extracted and analyzed per method ETS8-053 by liquid chromatography with triple quadrapole mass spectrometric detection (LC/MS/MS). The LMS recovery results provided a measure of the data accuracy. The relative percent difference (RPD) of the duplicate analytical sample results was used to assess the data precision. The percent moisture of each soil was also determined as part of the study. The PFOS, PFHS and PFBS concentrations are summarized in Table 1. The PFOS, PFHS and PFBS recoveries from the LMS samples are summarized in Table 2. The average data accuracy and standard deviation determined from LMS results was 107% + 7.9% for PFOS, 105% + 7.2% for PFHS and 106% + 5.2% for PFBS. The analytical method uncertainty (95% CI) was determined at + 7.3% for PFOS, + 10% for PFHS and + 12% for PFBS. Table 1. Results for Jeffries Property Sediments 3M LIMS ID [d] Sample ID Average Concentration (ng/g; dry) PFOS PFHS PFBS GLP10-01-01-26-001 JPAL SD TRIP1 0 0000 BLQ BLQ BLQ GLP10-01-01-26-002 JPAL SD ET01 0 0000 3.95 BLQ BLQ GLP10-01-01-26-003 JPAL SD ET02 0 0000 8.59 BLQ BLQ GLP10-01-01-26-004 JPAL SD ET02 DB 0000 10.0 BLQ BLQ GLP 1 0 - 0 1 - 0 1 - 2 6 - 0 0 5 JPAL SD ET03 0 0000 12.1 BLQ BLQ GLP 1 0 -0 1 - 0 1 - 2 6 - 0 0 6 JPAL SD ET04 0 0000 23.8 BLQ BLQ All LMS recovery results were within acceptance criteria of 100 + 30% Average concentration of duplicate analytical result reported; RPDs of duplicates were less than 10% The analytical method uncertainty was determined from LCS results at + 12% for PFBS, + 10% for PFHS and + 7.2% for PFOS Concentration values are shown at 3 significant figures, but more precise data was used for data calculations. BLQ; analyte response was lower than the analyte response of the lowest standard (LLOQ) which was the nominal 0.500 ng calibration standard (i.e. less than nominal 0.50 ng/g) Page 8 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 2. LMS Recovery for Jeffries Property Sediments 3M LIMS ID [b] Sample ID GLP10-01-01-26-001 Low GLP10-01-01-26-002 Low GLP10-01-01-26-002 High GLP10-01-01-26-003 Low GLP10-01-01-26-003 High GLP10-01-01-26-004 Low GLP10-01-01-26-004 High GLP10-01-01-26-005 Low GLP10-01-01-26-005 High GLP10-01-01-26-006 Low GLP10-01-01-26-006 High JPAL SD TRIP1 0 0000 LMS JPAL SD ET01 0 0000 LMS Low JPAL SD ET01 0 0000 LMS High JPAL SD ET02 0 0000 LMS Low JPAL SD ET02 0 0000 LMS High JPAL SD ET02 DB 0000 LMS Low JPAL SD ET02 DB 0000 LMS High JPAL SD ET03 0 0000 LMS Low JPAL SD ET03 0 0000 LMS High JPAL SD ET04 0 0000 LMS Low JPAL SD ET04 0 0000 LMS High Average Recovery Standard Deviation RSD LMS Recovery (%) PFOS PFHS PFBS 130% 125% 105% 102% 105% 114% 103% 103% 103% 104% 102% 110% 104% 105% 103% 105% 100% 105% 104% 103% 98.5% 111% 105% 108% 108% 107% 104% 105% 108% 115% 104% 97.0% 101% 107% 105% 106% 7.9% 7.2% 5.2% 7.4% 6.8% 4.9% LMSs were fortified with PFOS, PFHS and PFBS (linear isomers only) at nominal 20.0 ng (low) and 200 ng (high). The LMS for the trip blank was fortified at nominal 1.0 ng each of Pf Os , PFHS and PFBS Recovery values are shown at 3 significant figures, but more precise data was used for data calculations. 3 Introduction The soil analyses results reported herein were conducted as part of the Phase 3 Environmental Monitoring and Assessm ent Program for the 3M facility located in Decatur, Alabama. The objective of the overall program is to gain information regarding concentrations of perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate (PFHS) and perfluorobutane sulfonate (PFBS) in various environmental media such as groundwater, soils and sediments that are associated with and near the Decatur facility. Reported herein are the results from analysis of sediments collected from the Jeffries property. The samples were collected by Weston Solutions, Inc. personnel in February 2012 and shipped to the 3M Environmental Laboratory for quantitative analysis of PFOS, PFHS and PFBS. One soil travel blank (trip blank) accompanied the sample bottles to the site, during collection and during samples shipment and was analyzed to evaluate for any potential contamination of samples during the sample shipment and collection period. This report describes the sample shipment, receipt, extraction and quantitative LC/MS/MS analysis procedures conducted for determination of PFOS, PFHS and PFBS in the sediment samples that were received. Additionally, included in this report are the assessment of the analytical precision and accuracy for the reported PFOS, PFHS and PFBS concentration results based on duplicate analytical sample results and laboratory matrix spike (LMS) recovery results, respectively. The recovery results for a stable isotope labeled 13C4-PFOS surrogate recovery standard (SRS) that was added to each soil aliquot prior to extraction, and the determined percent moisture content of each soil, are also included herein. Page 9 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property 4 Test, Control and Reference Substances This study does not have a test substance in the classic sense of a GLP study because this study was purely analytical in nature. The reference and control substances are listed in Table 3. Table 3. Reference Substances Reference ID Chemical Name Chemical Formula Use Source Expiration Date Storage Conditions Chemical Lot Number TCR Number Physical Description Purity Reference ID Chemical Name Chemical Formula Use Source Expiration Date Storage Conditions Chemical Lot Number TCR Number Physical Description Purity PFOS (linear) PFOS (linear + branched) PFHS (linear) n -P e rflu o ro o c ta n e -1 Sulfonate Potassium Salt Perfluorooctane Sulfonate Potassium Salt n -P e rflu o ro h e x a n e -1 -s u lfo n a te Sodium Salt n-CsFi7SO3 K C 8F 17S O 3 K n-C6F13SO3 Na Reference Standard for Calibration and LMSs Reference Standard for LCSs R eference S tandard for C alibration and LM Ss W ellington Laboratories 3M W ellington Laboratories 1 0 /1 8 /1 8 1 2 /1 4 /1 6 3/25/18 Frozen Frozen Frozen LPFOSKBM06 171 LPFHxSAM08 T C R 0 8 -0 0 0 1 -1 /1 T C R -6 9 6 T C R 0 8 -0 0 1 8 -1 /1 C ry s ta llin e W h ite P ow der C ry s ta llin e 98% PFHS (linear + branched) n -P e rflu o ro h e x a n e -1 sulfonate Potassium Salt n-C6Fi3S3 K Reference Standard for LCSs 3M 8 6 .4 % PFBS (predominantly linear) P e rflu oro buta ne-1 -sulfo nate P otassium S alt n-C4F9S3 K R e fe re n ce S ta n d a rd fo r All PFBS 3M >98% 13C4-PFOS [1 ,2 ,3 ,4-13C 4 ]-P e rflu o ro o cta n e 1-Sulfonate Sodium Salt 13C412C4F17SO3 Na S u rro g a te W ellington Laboratories 2/12/17 Frozen NB 120067-69 T C R -0 8 3 W hite Powder 98.6% 1 /1 0 /1 7 Frozen 101 T C R -1 21 W h ite P ow der 9 6 .7 % 9/8/2013 Frozen MPFOS0910 T C R 1 0 -0 0 4 4 -2 /9 Liquid; M ethanol solution > 9 8 % [a] Page 10 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Reference ID Chemical Name Chemical Formula Use Source 13C8-PFOS [13C s]-P e rfiu o ro o cta n e -1 Sulfonate Sodium Salt 13CsF17SO3 Na Internal Standard for PFOS W ellington Laboratories 13C3-PFHS [13C 3 ]-P e rflu o ro h e x a n e -1S ulfo na te S odium Salt 13C 3 12C 3 F 1 3 S O 3 N a Internal S tandard for PFHS W e llin g to n Laboratories 18O2-PFBS [18O 2 ]-P e rflu o ro b u ta n e -1S ulfonate A m m onium Salt C 4FgS18O 216O N H 4 Internal Standard for PFBS RTI International Expiration Date 9/28/2013 9 /2 8 /2 0 1 3 3/9/15 Storage Conditions -20C -20C -20C Chemical Lot Number 092310 092310 11546-107-2 TCR Number TCR10-0048-3/16, 4/16 T C R 10-0048-3/16, 4/16 T C R -1 0 4 2 Physical Description Liquid; M ethanol solution Liquid; M ethanol solution Liquid; M ethanol solution Purity > 9 8 % [a] > 9 8 % [a] > 9 9 % [a] [a] T he co m m e rcially provided m aterial w a s a m ethanol so lu tio n s and la be led w ith a w e ig h t/vo lu m e co n ce n tra tio n purity value. H ow ever, th e co n ce n tra tio n o f fu rth e r dilu tio n s w as based on the certifie d co n ce n tra tio n o f the sto ck m aterial. 5 Test System There was not a test system for this study in the classic sense of a GLP study. This study was conducted for analysis of sediments collected from the Jeffries property that is located in Northern Alabama. Samples for this study are "real world" environmental samples. 6 Method Summary 6.1 Methods The sample extractions and quantitative LC/MS/MS analyses were performed following method ETS-8-053.0. The results reported herein were obtained from analytical run j120507b. Two analytical runs were conducted as o120312a and o120313a, but result not used due to QC results that did not meet method acceptance criteria. 6.2 Sample Receipt On February 21,2012 seven empty 250-mL HDPE NalgeneTM sample bottles, and one travel blank (trip blank) containing approximately 10-25 grams of a control soil TCR-455, were sent from the 3M Environmental Laboratory to W eston Solutions, Inc. field personnel for collection of sediments from the property known as the Jeffries Property, formerly the Bert Jeffries landfill. Following the sample Page 11 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property collections by W eston Solutions, Inc. personnel, five sediment-filled sample bottles and the trip blank were returned in the bottles to the 3M Environmental Laboratory for quantitative analysis of PFOS, PFHS and PFBS. The samples were received with sample chains of custody numbers 15290 on March 02, 2012. Soil samples from Alabama are regulated and the sediments for this study were shipped in accordance with USDA/APHIS soil permit number P330-09-00125. Sample nomenclature follows the form JPAL-SD-ET-xxxx where the first string defines the Jeffries Property Alabama (JPAL), the second string defines the sample media (i.e., SD= sediment, SB -field sample duplicate), the third string defines the site location (ET = eastern tributary), the fourth string defines the field sample (1,2,3... or DB = duplicate field sample) . The fourth string defines the sediment sampling depth (0000 = 0 ft to 0.5 ft interval). 6.3 Sample Preparation Each soil or sediment extraction involved removal of a 1 cubic centimeter (1 cc; 1 mL) aliquot of field sample (typically ~ 1 gram) from each sample bottle using a fixed volume 1 cc spoon, transferring it to a 15 mL conical centrifuge tube, followed by accurate weight determination of the aliquot on a 5-place balance. Then, nominal 3.0 ng of internal standard (IS; nominal 3.0 ng) and 3.0ng of surrogate recovery standard (SRS) was added to each soil aliquot and a known quantity of PFOS (linear isomer), PFHS (linear isomer) and PFBS was added to each LMS. Then each was extracted by addition of 8 mL of a 4:1 acetonitrile:water solution followed by sonication for 1 to 2 hours followed by centrifugation to remove solids. The supernatant from each was then transferred to an autovial for analysis. An accurately measured volume of each supernatant was analyzed by LC/MS/MS. During preparation, each sample and quality control sample received nominal 3.0 ng of a stable isotope labeled 13C4-PFOS surrogate recovery standard (SRS). Although not included as part of the data accuracy assessment for this study, SRS recovery determinations were included as part of an ongoing method validation aspect for SRS behavior in environmental soil and sediment samples for potential future applications. The SRS was quantified from a SRS calibration curve constructed from analysis of calibration standards prepared from the SRS in calibration standards. The SRS recovery was determined based on the calculated concentration of SRS from the analysis and recovery of SRS from each sample is included in Tables 15, 16 and 17 but was not used for evaluation of data accuracy for this study and is otherwise excluded from the discussions in the report. Each analytical sample was prepared in duplicate for analysis of PFOS, PFHS and PFBS in the sample. Additionally, a third and/or fourth replicate was weighed out and used to prepare LMSs. The LMS results were used for determination of data accuracy. RPD of duplicate samples results was used for determination of data precision. Appropriate LMS levels are considered those that are within 0.5-times to 10-times the measured endogenous analyte level in the equivalent non-fortified soil/sediment sample, and the fortification of 20 ng and 200 ng was sufficient in at least one of the LMSs to be considered appropriate for determination of the data accuracy for PFOS, but was greater than 10-times the PFBS and PFHS endogenous levels which were less than the LLOQ (BLQ) in all samples. Calibration standards were prepared by spiking known quantities of PFOS (linear isomer), PFHS (linear isomer), PFBS and 13C4-PFOS into 1-cubic centimeter (1 cc, 1 mL) aliquots of 3M Environmental Laboratory control soil TCR-455. The nominal mass of 1 cc of control soil TCR-455 is 1.0 gram (dry), therefore, the nominal calibration standard range prepared and analyzed was 0.200 ng/g to 500 ng/g. Laboratory control spike (LCS) samples were prepared with each sample preparation batch; prepared at three levels (nominal 3.00 ng/g, 30.0 ng/g and 300 ng/g) and each level in triplicate. The LCSs were prepared using control soil TCR-455, same as calibration standards, and were fortified with PFOS (mixed linear + branched isomers), PFHS (mixed linear + branched isomers) and PFBS. The LCS results were used to estimate the analytical method uncertainty. Page 12 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property 6.4 Percent Soil Moisture Determination The percent moisture of sediment samples was determined by gravimetric analysis. Dry weights were determined from separate weighings than the sample aliquot weighings used for extractions. To determine the percent moisture, duplicate aliquots of each soil sample were removed and the accurate "wet" weight determined for each. Each aliquot was then dried at > 100C until no further mass loss occurred from water evaporation, at which time the accurate dry sample weights were determined. The difference in mass, attributed to water evaporation, was used to calculate the percent moisture of the original sample. The averaged percent moisture result for each was then used to report the PFOS, PFHS and PFBS concentration on a dry weight basis. 6.5 LC/MS/MS Analysis The analysis of sample extracts for PFOS, PFHS and PFBS was performed by LC/MS/MS as described in method ETS-8-053.0. The relative percent difference (RPD) of duplicate prepared sample results was used as a measure of the analytical precision. The determined recovery of fortified PFOS, PFHS and PFBS from LMS samples was used as a measure of analytical accuracy. Surrogate recoveries are reported in Tables 15, 16 and 17, but were not used for evaluating analyte recovery for this study. The surrogate data was collected as part of an on-going evaluation of surrogate recovery from environmental field samples for supporting a method validation of ETS-8-053. Details of the specific instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are detailed in the raw data, and are briefly described below in Table 4 , Table 5 and Table 6. Table 4. Instrument Information Instrum ent Nam e A n a ly tic a l M e th o d ID Liquid C h rom ato grap h G uard colum n E xtraction colum n A na lytica l colum n Injection V olum e M ass S pectrom eter Ion S ource P olarity S oftw are E T S -J o n a s () E T S -8 -0 5 3 .0 A g ile n t 1100 w ith B inary P um p P re -A u to sa m p le r; P rism RP (2.1 x 50 m m , 5 mm) O a s is H L B (3 x 2 0 m m , 2 5 m); 30C B e ta s il C 1 8 (2.1 x 1 0 0 m m , 5m) 2 5 mL API 5000 T urbo lo n Spray N egative A n a lyst 1.4.2 Page 13 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053) Step N um ber Total Time [m in] 1 0.0 2 3.0 3 3.5 4 17.0 5 17.5 6 19.5 7 20.0 8 23.0 Flow Rate [m L/m in] 0 .4 0 0 0 .4 0 0 0 .4 0 0 0 .4 0 0 0 .4 0 0 0 .4 0 0 0 .4 0 0 0 .4 0 0 Percent A [2 mm Aqueous Am m onium A cetate] 97.0 97.0 7 0 .0 4 0 .0 10.0 10.0 97.0 97.0 Percent B [ A cetonitrile] 3.0 3.0 3 0 .0 6 0 .0 9 0 .0 9 0 .0 3.0 3.0 Table 6. Mass Transitions A n a ly te M ass Transitions M onitored PFBS 299>99, 299>80 18O 2-P F B S (IS) 303>84 PFHS 399>99, 399>80 13C a -P F H S (IS ) 402>80 PFOS 499>130, 499>99, 499>80 13C 8 -P F O S (IS ) 507>80 13C 4-P F O S (S u rro g a te ) 503>80 Note: Multiple m ass transitions are sum m ed to give the instrum ent response fo r that analyte. 7 Analytical Results Concentration values are rounded to three significant figures according to EPA rounding rules. Because of rounding some calculated values may vary slightly from those found in the raw data. Samples with RPDs for duplicate results of less than 50% and LMS results meeting the method criterion of within 100 30% demonstrated that the method was appropriate for those samples and were reported without footnotes in results tables. The nominal 20.0 ng and 200 ng fortified quantities of PFOS, PFHS and PFBS into LMSs for field samples were at an appropriate level for evaluating sample-specific analyte recoveries for PFOS. Results for PFHS and PFBS were all less than the LLOQ (BLQ) and therefore LMS fortifications were greater than 10-times the endogenous level measured in the samples. 7.1 Calibration A set of calibration standards were prepared by spiking varying known quantities of PFOS (linear), PFHS (linear), PFBS and surrogate (13C4-PFOS), and a fixed quantity of stable isotope labeled internal standards, into one cubic centimeter (1 cc, 1 mL) aliquots of 3M Environmental Laboratory control soil TCR-455 (nominal soil mass of 1.0 g/mL). A total of twelve (12) calibration standards were prepared as a set. The prepared standards were fortified from nominal 0.200 ng to 500 ng in 1 cubic centimeter of Page 14 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property control soil TCR-455; equivalent to nominal 0.200 ng/g to 500 ng/g in soil TCR-455. Following analysis of the calibration standards, the concentration of each standard was plotted against the measured analyte /IS peak area ratio. A quadratic equation with 1/x weighting was used to fit the data for each analyte. Calibration curves were not forced through zero. Determining the standard concentration using the resultant calibration curve and comparing to the known concentration confirmed accuracy of each curve point at within 100 30% (+ 35% at the LLOQ). The correlation coefficient (r) was greater than 0.999 for all calibration curves, and the coefficient of determination (r2) was greater than 0.990. Calibration results for PFOS, PFHS and PFBS are summarized in Table 7, Table 8 and Table 9, respectively. Because soil and sediment weights can vary significantly for a 1 cc (1 mL) field sample, depending on composition and moisture content, the instrument response was calibrated for the known concentrations of target analytes based on the mass quantity of reference substance added to a 1 cc soil (1 mL) calibration standard prior to extraction (e .g . calibrated in this study for a range of 0.500 ng to 500 ng PFOS, PFHS and PFBS; the 0.200 ng standard was excluded). Because a 1cc aliquot of control soil TCR-455 weighs nominally 1.0 gram (dry weight) and has less than 5% moisture content, the nominal concentration range of the calibration was essentially 0.200 ng/g to 500 ng/g. However, because sample soil aliquots may weigh more than 1.0 gram and contain significant moisture, the determined concentrations during the analysis on an ng per sample aliquot basis from the calibration curve and then adjusted for the accurate determined weight and percent moisture so they could be reported on a ng/g (dry weight) basis. Table 7. PFOS Calibration Summary Analytical Run Actual STD 1 0.199 STD 2 0.499 STD 3 0.748 STD 4 0.997 s111007a excluded 0.478 0.791 0.888 Recovery N/A 95.8% 106% 89.1% STD 5 2.49 2.51 101% PFOS (ng) STD 6 STD 7 STD 8 4.99 9.97 24.9 5.42 10.1 24.5 109% 101% 98.4% STD 9 49.9 STD 10 99.7 STD 11 199 STD 12 499 r N/A 50.6 98.9 199 499 0.9999 101% 99.2% 100% 100% N/A Table 8. PFHS Calibration Summary Analytical Run Actual STD 1 0.200 STD 2 0.500 STD 3 0.750 STD 4 1.00 STD 5 2.50 s111007a excluded 0.473 0.801 0.908 2.41 Recovery N/A 94.6% 107% 90.8% 96.4% PFHS (ng) STD 6 STD 7 STD 8 5.00 10.0 25.0 5.57 9.95 26.2 111% 99.5% 105% STD 9 50.0 STD 10 STD 11 STD 12 100 200 500 r N/A 47.5 99.9 201 500 0.9998 95.0% 99.9% 101% 100% N/A Table 9. PFBS Calibration Summary Analytical Run Actual STD 1 0.200 STD 2 0.500 s111007a excluded 0.415 Recovery N/A 83.0% STD 3 0.750 STD 4 1.00 0.773 0.944 103% 94.4% STD 5 2.50 2.54 102% PFBS(ng) STD 6 STD 7 STD 8 5.00 10.0 25.0 STD 9 STD 10 STD 11 STD 12 50.0 100 200 500 r N/A 5.90 9.76 25.5 51.5 97.7 199 501 0.9998 118% 97.6% 102% 103% 97.7% 99.5% 100% N/A Page 15 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property 7.2 Limits of Quantitation (LOQs) The lower limit of quantitation (LLOQ) was the lowest non-zero calibration standard in the curve that met the linearity and accuracy requirement for a low standard (100 + 35%) and for which the area counts were at least twice that of the average response determined for the method blank injected just prior to the calibration standards . The LLOQ for this study was the nominal 0.500 ng calibration standard (nominal 0.500 ng/g in soil TCR-455) for PFOS, PFHS and PFBS. All sample analyte responses less than the response of the 0.500 ng calibration standard were reported as BLQ (below the limits of quantitation). The upper limit of quantitation (ULOQ) was the nominal 500 ng calibration standard. 7.3 Continuing Calibration During the course of each analysis, continuing calibration verifications (CCVs) were performed by regular injection of a mid-level calibration standard after approximately every 15th sample injected in the analytical run. The back calculated concentration results were used to confirm that the instrument response and the initial calibration curve were still in control. All CCVs flanking reported data met the method criteria of 100% 30% accuracy. 7.4 Blanks Three types of blanks were analyzed during this analysis: method blanks were prepared with blank matrix soil TCR-455 and were spiked with IS and surrogate; travel blanks (trip blanks) prepared from aliquots of soil TCR-455 sealed in s ample bottle that accompanied the bottle order to and from the sampling site; and solvent blanks containing extraction solvent. The different blank results were reviewed to evaluate potential contamination during shipment, and to evaluate method performance parameters such as injector carry over and to establish the LLOQ. All blanks were below the LLOQ (BLQ) 7.5 Laboratory Control Spikes (LCSs) Laboratory control spikes were prepared by spiking know quantities of PFOS (linear + branched), PFHS (linear + branched) and PFBS into 1 cc aliquots of soil TCR-455, fortified at nominal 3.0 ng and 30 ng and 300 ng levels, with each level prepared in triplicate. The results of the LCS analyses and calculation of analyte measurement accuracies (percent recovery) for PFOS, PFHS and PFBS are shown in Table 10, Table 11 and Table 12 respectively. The analytical method uncertainty calculated from LCS results is shown in Table 13. LCS Recovery -(-D--e-t-e--r-m--i-n-e--d--C--o--n-c--e-n--t-r-a-t-i-o-n--o--f--L--C--S--) *_1,00% Spike Concentration Page 16 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 10. LCS Results (PFOS, linear + branched isomer) Sample ID PFOS Recovery 3.00 LCS 30.0 LCS 300 LCS 114% 109% 118% LCSs (j120507b) 112% 109% 117% 108% 114% 113% Average Recovery 111% 111% 116% Std Dev. 2.9% 3.1% 2.8% RSD 2.6% 2.8% 2.4% Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/g and 300 ng/g of PFOS (linear + branched isomers), each prepared and analyzed in triplicate. Table 11. LCS Results (PFHS, linear + branched isomer) Sample ID 3.00 LCS PFHS Recovery 30.0 LCS 300 LCS 118% 109% 108% LCSs (j120507b) 116% 107% 113% 103% 107% 105% Average Recovery 113% 108% 109% Std Dev. 8.3% 1.1% 3.9% RSD 7.4% 0.99% 3.5% Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/g and 300 ng/g of PFHS (linear + branched isomers), each prepared and analyzed in triplicate. Table 12. LCS Results (PFBS) Sample ID LCSs (j120507b) 3.00 LCS 116% 117% 113% PFBS Recovery 30.0 LCS 106% 114% 109% 300 LCS 98.3% 112% 106% Average Recovery Std Dev. RSD 116% 2.1% 1.8% 110% 4.2% 3.8% 106% 7.0% 6.6% Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/g and 300 ng/g of PFBS, each prepared and analyzed in triplicate. Page 17 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 13. Analytical Method Uncertainties Sample ID 3.00 LCSs 30.0 LCSs 300 LCSs Average Recovery Std Dev. RSD Method Uncertainty (2 x Std. Dev.); 95% CI PFOS 114% 112% 109% 109% 109% 115% 119% 118% 113% 113% 3.7% 3.3% 7.3% LCS Results PFHS 118% 116% 103% 109% 107% 107% 108% 113% 105% 110% 5.1% 4.7% 10% PFBS 116% 117% 113% 106% 114% 109% 98.3% 112% 106% 110% 6.1% 5.5% 12% 7.6 Laboratory Matrix Spikes (LMSs) Laboratory matrix spikes (LMSs) were generated by adding a known quantity of PFOS (linear), PFHS (linear) and PFBS to an aliquot of sediment sample, and then preparing the sample the same as non spiked samples. Spikes for this study, LMSs were spiked at levels that were appropriate for the endogenous analyte levels in the soils, determined from screening analysis and fortified with the target analytes from 0.5-times to 10-times the endogenous analyte levels determined in the soil/sediment samples during the range finding analysis. The LMS method acceptance criterion of within 100 30% were met for all LMS recoveries. The LMS recovery results are summarized in Table 2. The nominal 20.0 ng and 200 ng fortified quantities of PFOS, PFHS and PFBS into LMSs for field samples were at an appropriate level for evaluating sample-specific analyte recoveries for PFOS. Results for PFHS and PFBS were all less than the LLOQ (BLQ) and therefore LMS fortifications were greater than 10-times the endogenous level measured in the samples. The PFOS, PFHS and PFBS recovery calculations for LMSs used the following equation: LMS Recovery - (Determined Concentration of LMS - Determined Concentration of Field Sample) * 1 0 0 % Spike Concentration 7.7 Percent Moisture Determinations The percent moisture was determined for each soil sample. Duplicate aliquots of each were taken and accurately weighed to determine the "wet" weight. Then each aliquot was dried at > 100C until no further loss in mass occurred due to water evaporation, after which the dry weight was accurately determined. The average percent moisture and RPD of the duplicate determinations for each soil are reported in Table 14. The percent moisture was calculated by the following equation: ,,Percent,M,oi.sture - -(O--rig-i-n--a-l-S--o-i-l--W--e--t-M---a-s-s-----D--r-i-e-d--S--o-i-l--M--a--s-s-) *100%. Original Soil Wet Mass Page 18 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 14. Percent Moistures for Jeffries Property Sediments LIMS ID Sample ID Average Percent Moisture (w/w) [a] GLP10-01-01-26-001 JPAL SD TRIP1 0 0000 2.7% GLP10-01-01-26-002 JPAL SD ET01 0 0000 28% GLP10-01-01-26-003 JPAL SD ET02 0 0000 30% GLP10-01-01-26-004 JPAL SD ET02 DB 0000 30% GLP10-01-01-26-005 JPAL SD ET03 0 0000 40% GLP10-01-01-26-006 JPAL SD ET04 0 0000 61% [a] Percent moisture determined for duplicate sample aliquots taken from each sample bottle Relative Percent Difference [a] 2.5% 0.78% 1.5% 0.78% 3.6% 0.096% 7.8 Individual Analytical Sample Results The individual analytical sample results for PFOS, PFHS and PFBS concentrations are shown in Table 15, Table 16 and Table 17, respectively. Table 15. Individual PFOS Results for Jeffries Property Sediments Sam ple Description GLP10-01-01-21-001 GLP10-01-01-21-001 Dup GLP10-01-01-21-001 LMS GLP 1 0 - 0 1 - 0 1 - 2 1 - 0 0 2 GLP 10-01-01-21-002 Dup GLP10-01-01-21-002 Low LMS GLP 10-01-01-21-002 High LMS GLP 1 0 - 0 1 - 0 1 - 2 1 - 0 0 3 GLP 10-01-01-21-003 Dup GLP10-01-01-21-003 Low LMS GLP 10-01-01-21-003 High LMS GLP10-01-01-26-004 GLP10-01-01-26-004 Dup Surrogate (13C4-PFO S) Recovery 109% 110% 105% 101% 103% 102% 104% 106% 110% 107% 103% 106% 104% LMS Spike Concentration (ng/g; dry w e ig h t) N/A 1.04 N/A 14.6 143 N/A 15.0 151 N/A Measured PFOS Concentration (ng/g; dry w e ig h t) BLQ BLQ LMS Recovery N/A Average PFOS Concentration (ng/g; dry wt.) and RPD (%) BLQ 1.35 130% N/A 3.81 4.09 N /A 3.95 18.8 152 102% 103% [a] 7.0% 8.99 8.20 N/A 8.59 24.1 166 104% 104% [a] 9.1% 9.8 N /A 10.0 10.2 Page 19 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 15. Individual PFOS Results for Jeffries Property Sediments Sam ple Description GLP10-01-01-26-004 Low LMS GLP10-01-01-26-004 High LMS Surrogate (13C4-PFO S) Recovery 105% 105% LMS Spike Concentration (ng/g; dry w e ig h t) 16.6 152 Measured PFOS Concentration (ng/g; dry w e ig h t) 27.5 168 LMS Recovery 105% 104% [a] Average PFOS Concentration (ng/g; dry wt.) and RPD (%) 3.6% GLP10-01-01-21-005 GLP10-01-01-21-005 Dup 104% 106% N/A 11.9 N /A 12.1 12.2 GLP10-01-01-21-005 Low LMS GLP10-01-01-21-005 High LMS 104% 104% 19.6 198 33.8 227 111% 108% [a] 2.9% GLP 1 0 -0 1 - 0 1 - 2 1 - 0 0 6 GLP10-01-01-21-006 Dup 104% 102% N/A 23.5 24.1 N/A 23.8 GLP10-01-01-21-006 Low LMS GLP10-01-01-21-006 High LMS 106% 104% 35.8 380 61.4 418 105% 104% 2.5% N/A; not applicable BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.500 ng/g low standard. [a] LMS fortification level was greater than 10-times the endogenous analyte level. Table 16. Individual PFHS Results for Jeffries Property Sediments Sam ple Description GLP 1 0 -0 1 - 0 1 - 2 1 - 0 0 1 GLP10-01-01-21-001 Dup GLP10-01-01-21-001 LMS GLP 1 0 - 0 1 - 0 1 - 2 1 - 0 0 2 GLP10-01-01-21-002 Dup GLP10-01-01-21-002 Low LMS GLP10-01-01-21-002 High LMS GLP 1 0 - 0 1 - 0 1 - 2 1 - 0 0 3 GLP10-01-01-21-003 Dup GLP10-01-01-21-003 Low LMS GLP10-01-01-21-003 High LMS Surrogate (13C4-PFO S) Recovery 109% 110% 105% 101% 103% 102% 104% 106% 110% 107% 103% LMS Spike Concentration (ng/g; dry w e ig h t) N/A 1.04 N/A 14.6 144 N/A 15.1 151 Measured PFHS Concentration (ng/g; dry w e ig h t) BLQ BLQ LMS Recovery N/A Average PFHS Concentration (ng/g; dry wt.) and RPD (%) BLQ 1.30 125% N/A BLQ N /A BLQ BLQ 15.3 105% [a] N/A 148 103% [a] BLQ N /A BLQ BLQ 15.4 158 102% [a] 105% [a] N/A Page 20 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 16. Individual PFHS Results for Jeffries Property Sediments Sample Description GLP10-01-01-26-004 GLP10-01-01-26-004 Dup Surrogate (13C4-PFOS) Recovery 106% 104% LMS Spike Concentration (ng/g; dry weight) N/A Measured PFHS Concentration (ng/g; dry weight) BLQ BLQ LMS Recovery N/A Average PFHS Concentration (ng/g; dry wt.) and RPD (%) BLQ GLP10-01-01-26-004 Low LMS GLP10-01-01-26-004 High LMS 105% 105% 16.7 153 16.7 157 100% [a] 103% [a] N/A GLP10-01-01-21-005 GLP10-01-01-21-005 Dup 104% 106% N/A BLQ N /A BLQ BLQ GLP10-01-01-21-005 Low LMS GLP10-01-01-21-005 High LMS 104% 104% 19.7 199 20.7 212 105% [a] 107% [a] N/A GLP 1 0 -0 1 - 0 1 - 2 1 - 0 0 6 GLP10-01-01-21-006 Dup 104% 102% N/A BLQ N /A BLQ BLQ GLP10-01-01-21-006 Low LMS GLP10-01-01-21-006 High LMS 106% 104% 36.0 382 38.7 371 108% [a] 97.0% [a] N/A N/A; not applicable BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.500 ng/g low standard. [a] LMS fortification level was too low relative to the endogenous analyte level to make an accurate determination of recovery. Table 17. Individual PFBS Results for Jeffries Property Sediments Sample Description GLP10-01-01-21-001 GLP10-01-01-21-001 Dup GLP10-01-01-21-001 LMS G LP 1 0 -0 1 - 0 1 - 2 1 -0 0 2 GLP10-01-01-21-002 Dup GLP10-01-01-21-002 Low LMS GLP10-01-01-21-002 High LMS G LP 1 0 -0 1 - 0 1 - 2 1 -0 0 3 GLP10-01-01-21-003 Dup GLP10-01-01-21-003 Low LMS Surrogate (13C4-PFOS) Recovery 109% 110% 105% 101% 103% 102% 104% 106% 110% 107% LMS Spike Concentration (ng/g; dry weight) N/A 1.04 N/A 14.6 144 N/A 15.1 Measured PFBS Concentration (ng/g; dry weight) BLQ BLQ LMS Recovery N/A Average PFBS Concentration (ng/g; dry wt.) and RPD (%) BLQ 1.09 105% N/A BLQ BLQ 16.6 148 N/A 114% [a] 103% [a] BLQ N/A BLQ BLQ 16.6 N/A 110% [a] BLQ N/A Page 21 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Table 17. Individual PFBS Results for Jeffries Property Sediments Sample Description GLP10-01-01-21-003 High LMS Surrogate (13C4-PFOS) Recovery 103% LMS Spike Concentration (ng/g; dry weight) 151 Measured PFBS Concentration (ng/g; dry weight) 148 LMS Recovery 103% [a] Average PFBS Concentration (ng/g; dry wt.) and RPD (%) GLP10-01-01-26-004 GLP10-01-01-26-004 Dup GLP10-01-01-26-004 Low LMS GLP10-01-01-26-004 High LMS 106% 104% 105% 105% N/A 16.7 153 BLQ BLQ 17.4 150 N/A 105% [a] 98.5% [a] BLQ N/A G LP 1 0 -0 1 - 0 1 - 2 1 -0 0 5 GLP10-01-01-21-005 Dup 104% 106% N/A BLQ N /A BLQ BLQ GLP10-01-01-21-005 Low LMS GLP10-01-01-21-005 High LMS 104% 104% 19.7 199 21.2 206 108% [a] 104% [a] N/A G LP 1 0 -0 1 - 0 1 - 2 1 - 0 0 6 GLP10-01-01-21-006 Dup 104% 102% N/A BLQ N /A BLQ BLQ GLP10-01-01-21-006 Low LMS GLP10-01-01-21-006 High LMS 106% 104% 36.0 382 41.4 384 115% [a] 101% [a] N/A N/A; not applicable BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.500 ng/g low standard. 8 Conclusion Sediments collected from the Jeffries Property in March 2012 were successfully analyzed for PFOS, PFHS and PFBS following 3M Environmental Laboratory method ETS-8-053.0 and conducted as 3M study GLP10-01-02-25. The average PFOS, PFHS and PFBS concentration results for the soil samples are summarized in Table 1 and the LMS recoveries are summarized in Table 2. The individual analytical sample results are shown in Table 15, Table 16, and Table 17 for PFOS, PFHS and PFBS, respectively. The soil trip blank that accompanied the sample bottles to the site and then accompanied samples back to the laboratory was sufficiently devoid of PFOS, PFHS and PFBS, indicating that no contamination of the samples occurred during sample shipment or sample to the laboratory. The PFHS and PFBS levels in the samples were all less than the 0.5 ng/g calibration standard that defined the lower limit of quantitation. The PFOS concentrations in the sediment samples ranged from 3.95 ng/g to 23.8 ng/g. The data accuracy was within 100 + 30% and the data precision was excellent with RPDs less than 10%. The analytical method uncertainties (95% CI) were determined by statistical examination of the LCS results for PFOS, PFHS and PFBS and were + 7.3% for PFOS, + 10% for PFHS and + 12% for PFBS, respectively, at the 95% confidence interval (95% CI). Page 22 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFFIS & PFBS in Sediments Collected from the Jeffries Property 9 Data/Sample Retention All associated project data (hardcopy and electronic) will be archived as project GLP10-01 -02-25 according to 3M Environmental Laboratory standard operating procedures. The percent moisture raw data was determined for the samples as part of study GLP10-01-01-26 and that raw data are archived with that interim study data packet and report. 10 List of Attachments Attachment A: Preparation Forms, Raw Data and Chromatograms 11 Signatures Report Approval: Cleston C. Lange, Ph.D., Principal Analytical Investigator Date William K. Reagen, Ph.D., 3M Environmental Laboratory Management Date Date 24l2-- Date Page 23 of 24 Study: GLP10-01-02, Interim Report 25 Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property Attachment A Preparation Forms, Raw Data and Chromatograms Page 24 of 24