Document RJDk1EJzr64OemGxEGb8Epy6B

BACK TO MAIN Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 www.centrelab.com ^P hone: (814) 231 -8032 Fax: (814) 231 -1253 or (814) 231 -1580 Analytical Report Fluorochemical Characterization of Surface Water and Sediment Samples Port St. Lucie Second Resampling (E01-0096) Centre Analytical Laboratory Report No. 023-014EE (Revision 1) Testing Laboratory Centre Analytical Laboratory, Inc. 3048 Research Drive State College, PA 16801 3M Environmental Laboratory Contact Kent R. Lindstrom Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 Phone: (651)778-5352 Requester Dale Bacon 3M Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 10 F 6 BACK TO MAIN 1 Introduction Results are reported for the analysis of a series of quiet surface water (QW) and sediment samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M Environmental Laboratory. The samples were collected from Port St. Lucie, Florida and are part of 3M Project E01-0096. The Centre study number assigned to the project is 023-014. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 23 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1; Target Analysis Compound Name Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate Perfluorohexane Sulfonate Acronym PFOS PFOSA PFOA PFHS The sediment samples were also analyzed for total organic carbon (TOC), % moisture, and % organic matter. The analytical methods used for originally developed for water samples and were validated by Centre. The water sample validation protocol and results are on file with Centre. The methods were modified for the sediment samples. The procedures have not been fully validated for this additional matrix. Data presented here is the highest quality data available at this time. 2 Sample Receipt The samples were submitted in individual plastic containers and were not preserved. Twentythree individual sample containers were received. Samples were received on 1/31/01. Samples were collected on 1/19/01 and 1/24/01. Chain-of-custody information is presented in Attachment C. 3 Holding Times The analytical method used was validated against a maximum holding time of 14 days in water samples. Stability after this time period has not been validated. However, it should be noted that field fortifications in water and other matrices have shown acceptable recoveries at 100 and 1000 ng/L for periods longer than 14 days. PAGE2 OF 6 BACK TO MAIN 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Water samples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliter portion of sample was transferred to a Ci8 SPE cartridge. The cartridge was first eluted with 5 mL of 40% methanol in water solution. The eluate was discarded and the SPE column was then eluted with 100% methanol. A 5 mL portion of methanol was collected for analysis by LC/MS/MS. This treatment resulted in an eight-fold concentration of the samples prior to analysis. For the sediment samples, a representative portion of sample (5 grams) was first extracted into 5 ml of methanol. The extracts were filtered and diluted to a final volume of 40 mL with Type I water. The diluted extracts were then treated in the same manner as the water samples, beginning with the solid phase extraction. 4.1.2 Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted between 2/06/01 and 2/09/01 and analyzed by MS/MS between 2/07/01 and 2/10/01. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in Attachments D. 4.2 Total Organic Carbon (TOC) Sediment samples were analyzed for TOC according to the procedure of Walkley-Black. Organic carbon in the sample was oxidized by dichromate. The heat generated when two volumes of sulfuric acid were mixed with one volume of dichromate solution facilitated the reaction. The excess dichromate was determined by titration with standard ferrous sulfate solution. The quantity of organic carbon was calculated from the amount of dichromate reduced. The method can be found in "Methods of Soil Analysis - Part 2 Chemical and Microbiological Properties" American Society of Agronomy, Number 9, Part 2 - 1982. Raw analytical data is given in Attachment E. 4.3 Percent Moisture / Organic Matter Sediment samples were analyzed for percent moisture and percent organic matter. The percent moisture was determined by drying the samples at 105C and determining the weight loss. The PAGE3 OF6 BACK TO MAIN percentage organic matter was determined by treating the dried sample with hydrochloric acid to remove carbonates, followed by ashing at 750C. The percentage organic matter was calculated from the weight loss after taking into account the carbonate concentration. Raw analytical data is given in Attachment F. 5 Analysis 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r >.0.985 (r2> 0.970). Calibration standards are prepared using the same SPE procedure used for samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. For the results reported here, calibration criteria were met. 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant. Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical methods. 5.4 Matrix Spikes Matrix spikes were prepared for every sample using all compounds of interest. Field matrix spikes were also performed on selected samples. Matrix spike recoveries are given in Attachment B. 5.5 Duplicates All field samples were analyzed in duplicate. Field duplicates were also collected at selected locations. Results are given along with the sample results in Attachment A. 5.6 Laboratory Control Samples For LC/MS/MS analyses, Milliq water was spiked with all compounds of interest at 25 and 250 ng/L during each extraction set. All recoveries for all compounds were between 70-130% in each LCS. Results are given along with the raw data in Attachments D. PAGE4 OF6 BACK TO MAIN 5.7 Sample Related Comments There are no other sample related comments for this data set. 6 Data Summary Please see Attachment A for a detailed listing of the analytical results. Water results are reported in parts per trillion (ppt) (ng/L). Sediment results are reported in parts per billion (ppb) (ug/Kg) on both an as-received and dry-weight basis. TOC results are reported as parts per million (ug/g) and organic matter data is reported as % by weight. 7 Data/Sampie Retention Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Centre. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 8.5 Attachment E: TOC Raw Analytical Data 8.6 Attachment F: %Solids / Organic Matter Raw Analytical Data PAGE 5 OF 6 9 Signatures Other Lab Members Contributing to Data Karen Smith G. Ronald Ripper BACK TO MAIN PAGE 6 OF6 ANALY Centre Analytical Laboratories, Inc. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 Analytical Results Port St. Lucie Resampling (water samples) 3M Sample Identification PFOS (ng/L) PFOA (ng/L) PFHS (ng/L) PFOSA (ng/L) QWI East-C QWI East-C (lab duplicate) QWI East-C (field duplicate) QWI South-C QWI South-C (lab duplicate) QWI West-C QWI West-C (lab duplicate) QWI North-C QWI North-C (lab duplicate) QWI Culvert Discharge-C QWI Culvert Discharge-C (lab duplicate) QWII-C QWII-C (lab duplicate) QWII-C (field duplicate) QWIII-C QWIII-C (lab duplicate) Blind-C Blind-C (lab duplicate) 1970 2220 2310 2120 2090 2200 2340 2080 2010 1840 1980 NQ NQ 25.1 25.5 NQ 2367 2230 79.6 72.7 79.4 84.8 79.6 82.8 93.7 93.5 81.4 70.1 76.1 NQ ND NQ 33.0 NQ 75.5 82.0 459 31.9 442 30.2 479 30.5 470 44.1 437 35.4 455 37.5 458 38.2 468 43.0 480 41.8 628 45.5 695 51.9 NQ ND NQ ND NQ ND NQ ND NQ ND 446 34.6 450 39.7 Limit of Detection (LOD) for the procedure is approximately 2.5 ng/L for PFOS, PFHS and PFOSA and 7.5 ng/L for POAA Limit of Quantitation (LOQ) for the procedure is 25 ng/L for all compounds ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ Please refer to the reverse side for our standard terms and conditions. ANALY ! flr riT"*w k Centre Analytical Laboratories. Inc. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 Organic 3M CENTRE TOCS Matter ID ID (Mg/g) Dry Wt. (%) Dry Wt. QWI East-C Sediment 0100677 5260 1.97 QWI East-C Sediment 0100677 4690 1.77 QWI South-C Sediment 0100679 2100 0.950 QWI South-C Sediment 0100679 1940 0.920 QWI West-C Sediment 0100681 284 0.750 QWI West-C Sediment 0100681 277 0.760 QWI North-C Sediment 0100683 6480 0.910 QWI North-C Sediment 0100683 6230 0.890 QWII - C Sediment 0100689 6350 1.03 QWII - C Sediment 0100689 6720 1.06 QWI 11 - C Sediment 0100691 2070 0.290 QWI 11- C Sediment 0100691 2100 0.430 Blind - C Sediment 0100693 3660 0.460 Blind - C Sediment 0100693 3530 0.500 Moisture (%) 36.6 35.1 34.6 34.5 38.4 38.3 41.2 41.0 35.7 34.4 31.3 30.3 31.5 32.9 TOCS Analysis Date: 02/09/01 Organic Matter Analysis Date: 02/07/00 % Moisture Analysis Date: 02/06/01 Please refer to the reverse side for our standard terms and conditions. Centre Analytical Laboratories, Inc. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 Analytical Results Port St. Lucie Resampling (sediments as received) 3M Sample Identification PFOS (ug/Kg) PFOA (ug/Kg) PFHS (ug/Kg) PFOSA (ug/Kg) % Solids QWI East-C QWI East-C (lab duplicate) QWI South-C QWI South-C (lab duplicate) QWI West-C QWI West-C (lab duplicate) QWI North-C QWI North-C (lab duplicate) QWII-C QWII-C (lab duplicate) QWIII-C QWIII-C (lab duplicate) Blind-C Blind-C (lab duplicate) 6.11 5.93 7.83 9.36 6.67 6.47 5.46 5.77 NQ NQ NQ NQ 5.68 5.73 NQ ND NQ ND NQ 0.330 NQ 0.252 NQ 0.227 NQ 0.209 NQ ND NQ ND ND ND ND ND NQ ND NQ ND NQ 0.320 NQ 0.216 Limit of Detection (LOD) for the procedure is approximately 0.08 ug/Kg for all compounds (as received) Limit of Quantitation (LOQ) for the procedure is 0.20 ug/Kg for all compounds (as received) ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ 0.295 0.279 0.654 0.964 0.375 0.355 0.319 0.740 ND ND ND ND 0.327 0.292 63.4 63.4 65.4 65.4 61.6 61.6 58.8 58.8 64.3 64.3 68.7 68.7 68.5 68.5 Please refer to the reverse side for our standard terms and conditions. ANALYTi Centre Analytical Laboratories, Inc. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 Analytical Results Port St. Lucie Resampling (sediments dry weight) 3M Sample Identification PFOS (ug/Kg) PFOA (ug/Kg) PFHS (ug/Kg) PFOSA (ug/Kg) % Solids QWI East-C QWI East-C (lab duplicate) QWI South-C QWI South-C (lab duplicate) QWI West-C QWI West-C (lab duplicate) QWI North-C QWI North-C (lab duplicate) QWII-C QWII-C (lab duplicate) QWIII-C QWIII-C (lab duplicate) Blind-C Blind-C (lab duplicate) 9.64 9.34 12.0 14.3 10.8 10.5 9.28 9.80 NQ NQ NQ NQ 8.29 8.37 NQ ND NQ ND NQ 0.504 NQ 0.385 NQ 0.369 NQ 0.340 NQ ND NQ ND ND ND ND ND NQ ND NQ ND NQ 0.467 NQ 0.315 Jmit of Detection (LOD) for the procedure is approximately 0.08 ug/Kg for all compounds (as received) Limit of Quantitation (LOQ) for the procedure is 0.20 ug/Kg for all compounds (as received) ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ 0.465 0.440 1.00 1.47 0.609 0.575 0.543 1.26 ND ND ND ND 0.477 0.426 63.4 63.4 65.4 65.4 61.6 61.6 58.8 58.8 64.3 64.3 68.7 68.7 68.5 68.5 Please refer to the reverse side for our standard terms and conditions. 0 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: QWI East-C Spiked Amount (ng/L): | 1000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 1970 79.6 459 31.9 Matrix Spike Result (ng/L) 3120 1110 1410 1320 Matrix Spike Result (% Recovery) 115.0 103.0 95.1 128.8 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWI South-C 1000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 2120 84.8 470 44.1 Matrix Spike Result (ng/L) 3170 1182 1450 1450 Matrix Spike Result (% Recovery) 105.0 109.7 98.0 140.6 Criteria (Pass / Fail) PASS PASS PASS FAIL L.ower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWI West-C 1000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 2200 82.8 455 37.5 Matrix Spike Result (ng/L) 3200 1087 1410 1330 Matrix Spike Result (% Recovery) 100.0 100.4 95.5 129.3 Criteria (Pass / Fail) PASS PASS PASS PASS L.ower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWI North-C 1000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 2080 93.5 468 43.0 Matrix Spike Result (ng/L) 2910 1086 1450 1370 Matrix Spike Result (% Recovery) 83.0 99.3 98.2 132.7 Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: QWI Culvert-C Spiked Amount (ng/L): | 100(3 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 1840 70.1 628 45.5 Matrix Spike Result (ng/L) 2710 1088 1610 1360 Matrix Spike Result (% Recovery) 87.0 101.8 98.2 131.5 Criteria (Pass / Fail) PASS PASS PASS FAIL L.ower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWII-C 1000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 24.4 9.82 6.53 0 Matrix Spike Result (ng/L) 1080 961 998 1280 Matrix Spike Result (% Recovery) 105.6 95.1 99.1 128.0 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWIII-C 1000 PFOS F'FOA F'FHS F'FOSA Sample Concentration (ng/L) 25.5 33.0 8.16 0 Matrix Spike Result (ng/L) 1150 1010 863 1310 Matrix Spike Result (% Recovery) 112.5 97.7 85.5 131.0 Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recovery Limit: 70 Upper Recovery Limit: 130 Mote: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): Blind-C 1000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 2367 75.5 446 34.6 Matrix Spike Result (ng/L) 3368 955 1250 1500 Matrix Spike Result (% Recovery) 100.1 88.0 80.4 146.5 Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: QWI East-C (sediment) Spiked Amount (ng/L): | 500 F'FOS F'FOA F'FHS F'FOSA Sample Concentration (ng/L) 806 12.3 0 36.9 Matrix Spike Result (ng/L) 1400 376 567 624 Matrix Spike Result (% Recovery) 118.8 72.7 113.4 117.4 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Concentrations represent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: QWI South-C (sediment) Spiked Amount (ng/L): 500 F'FOS F'FOA F'FHS F'FOSA Sample Concentration (ng/L) 979 13.3 41.2 81.8 Matrix Spike Result (ng/L) 1270 364 533 666 Matrix Spike Result (% Recovery) 58.2 70.1 98.4 116.8 Criteria (Pass / Fail) FAIL PASS PASS PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Concentrations represent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: QWI West-C (sediment) Spiked Amount (ng/L): 500 3FOS PFOA PFHS PFOSA Sample Concentration (ng/L) 802 14.6 28.4 46.9 Matrix Spike Result (ng/L) 1270 368 516 679 Matrix Spike Result (% Recovery) 93.6 70.7 97.5 126.4 Criteria (Pass / Fail) PASS PASS PASS PASS L.ower Recovery Limit: 70 Upper Recovery Limit: 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Concentrations represent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: QWI North-C (sediment) Spiked Amount (ng/L): 500 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 744 12.6 0 39.9 Matrix Spike Result (ng/L) 1340 382 610 686 Matrix Spike Result (% Recovery) 119.2 73.9 122.0 129.2 Criteria (Pass / Fail) PASS PASS PASS PASS L.ower Recovery Limit: 70 Upper Recovery Limit: 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Concentrations represent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWII-C (sediment) 500 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 24.0 0 0 0 Matrix Spike Result (ng/L) 474 361 567 645 Matrix Spike Result (% Recovery) 90.0 72.2 113.4 129.0 Criteria (Pass / Fail) PASS PASS PASS PASS L.ower Recovery Limit: 70 Upper Recovery Limit: 130 Mote: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Concentrations represent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWIII-C (sediment) 500 F' FOS F' FOA F' FHS F' FOSA Sample Concentration (ng/L) 19.3 9.2 0 0 Matrix Spike Result (ng/L) 428 350 410 450 Matrix Spike Result (% Recovery) 81.7 . 68.2 82.0 90.0 Criteria (Pass / Fail) PASS FAIL PASS PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Mote: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Concentrations represent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): Blind-C (sediment) 500 F'FOS F'FOA F'FHS FFOSA Sample Concentration (ng/L) 646 15.0 40.0 40.9 Matrix Spike Result (ng/L) 1170 368 497 687 Matrix Spike Result (% Recovery) 104.8 70.6 91.4 129.2 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Concentrations represent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWI East-C 1A 1000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 1970 79.6 459 31.9 Matrix Spike Result (ng/L) 3040 975 1470 1130 Matrix Spike Result (% Recovery) 107.0 89.5 101.1 109.8 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWI East-C 1B 1000 F'FOS F'FOA F'FHS F'FOSA Sample Concentration (ng/L) 1970 79.6 459 31.9 Matrix Spike Result (ng/L) 3650 1130 1570 1330 Matrix Spike Result (% Recovery) 168.0 105.0 111.1 129.8 Criteria (Pass / Fail) FAIL PASS PASS PASS Lower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWI East-C 25A 25000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 1970 79.6 459 31.9 Matrix Spike Result (ng/L) 32500 23300 24100 29800 Matrix Spike Result (% Recovery) 122.1 92.9 94.6 119.1 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: f QWlEast-C25B ~ Spiked Amount (ng/L): | 25000 PFOS PFOA PFHS PFOSA Sample Concentration (ng/L) 1970 79.6 459 31.9 Matrix Spike Result (ng/L) 32100 24000 26600 32900 Matrix Spike Result (% Recovery) 120.5 95.7 104.6 131.5 Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recovery Limit: Upper Recovery Limit: 70 130 BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWII-C 200 F'FOS F'FOA F'FHS PFOSA Sample Concentration (ng/L) 24.4 9.8 6.5 0 Matrix Spike Result (ng/L) 240 206 211 244 Matrix Spike Result (% Recovery) 107.8 98.1 102.3 122.0 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Mote: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BCkT MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: Spiked Amount (ng/L): QWII-C 1000 PFOS F'FOA F'FHS F'FOSA Sample Concentration (ng/L) 24.4 9.8 6.5 0 Matrix Spike Result (ng/L) 1080 1020 1030 1160 Matrix Spike Result (% Recovery) 105.6 101.0 102.4 116.0 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Environmental Form 30778 - PWO Laboratoor5rkfty, Shipping Address: 3M Bldg. 2-3E-09 935 Bush Avenue S t Paul, MN 55106 Telephone: Sample Receiving: (651) 776-4948 Alternate: (651) 778-6753 BACK TO MAIN Chain of Custody /Request for Laboratory Analytical 1 o 1 n 1 ., 1V & Uu pie - fi\ iteri ---------------------------------------=** 'Project ID/Project Name -- y--i ________- .y X O J. U X Template # Final Report Due Date Y ~ (l J 0 )_______ Project Lead Inntfearmneall DHuuea DHantte *' 3M Env. Lab Project # For Internal Use Only b O l - od}, -------------------------r ~ > iA 5 Contact Name \ . faft - ::i- - Company tt.Q t. i` Mailing Address : Q. City, State, Zip C Telephone # ------------------- r - ? - = ---------- ' r? ^ opeciei in stru ctio n s ano/or opecm c Regulatory Requirem ents: (method, limit o f detection, reporting units, etc.) T ffr o r - & =M o so V - - - - - - - - - T \ < r i \ _______________________ _ L ^ la s s / J O D /r r je c tff t j U l - p n Date Available ^ Date Due ^ FAX # Contract Lab / P re s e rv a tiv e s : om z X * o (N/) X O O > oc z L. -C O ^ ___ \ --? J (\ &v \ /, Anal)rsis Reqilesteid : Com plete below . / attach m y as sodated Info matlor . l Total Number of Containers Item # Client Sample Identification 3M Date LIMS# Sampled 1. \*S > 3 y ,r /n //o i 2. I b V T K p f - C I - / ilti& L 3. - t ^ - 9 0 6 p p h V -2 L 'M i i L k4. - P ^ Q S r i p f b __________________ 5. Time Sampled Ib g Z ). X tL A u 0 X . R i A t - - O ________________________________________ 7. Q u iH ___________________________ >4 \2 L 9. Q u i t 10. ppb ftu p # - , 5)0 -U l -V 3>> y / Matrix/ Media Enter the number o f containers of each t(j 1 I * 10 / in l 1 L(xiJl 11 \ -- 41-------- \4 l Ii \ Vy 1/ _L_ 1 K Sample Condition Upon Receipt: ^JZ^Acceptable O Other: Temperature: oC?: 'C ^ R e c e iv e d on Ice 1 \7U)Litflo * m oh IT U 5 <_ |Page Originel - Accompanying Samples f [ // ff L -A t C tr K fc / -- U Last Page - Originator Comments: 15 \h CcvtK jU SttUrkiu^- 1 Vn ( a /.X -'N J __________________________ m___ i t ) rey ^R U s- See R everse Side for Instructions Form 38770 - PWO Shipping Address: 3M Bldg. 2-3E-09 935 Bush Avenue Telephone: Sample Receiving: (651) 778-4948 Alternate: (651) 778-6753 BACK TO MAIN ca e Z 7Chain of Custody /Request for Laboratory Analytical 1 8 1 0 6 aProject ID/Project IName teh im J -Z I ! 0 \Template # _____________________________ Final Report 006*0316 Project Lead Internal Due Date 1 l- 3M Env. Lab Project # For Internal Use Only & i' c t\( p Report Results to: Contact Name & A t^ > rv J Company Mailing Address City, State, Zip Telephone # Special Instructions and/or Specific Regulatory Requirements: (method, Rmit of detection, reporting units, etc.) FAX # Date Available Date Due Contract Lab Preservatives: ^f S ^ t r -/ (U i Analysis Requested: Complete below. Attach any associated information. Total Number of Containers o z X * <10N0 m oo > 0) Co z k0. o i N'N n vC X Item Client Sample Identification # 3M LIMS# Date Time Sampled Sampled Matrix/ Media Enter the number of containers of each 3 {Enter an 'X in the box below to indicate request) \Y * 1p p b I^ J L p I1 J 5 o fli- K LO l) lX 3- 4. k i DuA t - t r p M - 1 pjpb p ft / \# \^ _ L J ___ t \ 1* ! 1X t\\X fC ^^S ^r~ 'C rf'K L S -' p h >u> B XJi f -t te J - R u s - Dl t i >. f i T ^ C >/ / fY ? m if K u r C t V l i S - K - 1 6 - ' \ '/>4 5 i K l ' 1 1A t i f c F l a e r - C ) d im d r ^ r \9. 8 i K rxjt *zfZ--CjCollected by (print): o > ____________ :_______ U` v40> L HV i/p g jo i 0 4 3 /1 03 \ i/ ^ l _ l z __ 1 1 Collector's signature: C* 1 _L 1 ( l 1 i1 tiflr7*x ^ X X, F* X. X -------- ----------- > Chain of Custody f7Zi /J ^Item # Relinqujsbfidjby/Affilation Time . Dat_e_ Shipped Via: ReceivedTSy/Affiliation i. . Wf " bt Z i# yt t/*P e tto j <i/Spom/l < ^ r _ ^ 'A .5 A -------t^= ^ /f i c l -OL _ Time Date 13/t. --Xl-j2--3///--t Vfc) /S/-0/ Sample Condition Upon Receiipptt:: A(cceptable 0 Other: Temperature: 'C Received on Ice Other Associated CoCs: I Copies to: 1 s m o i, iJ io i, irroHinos I K J ^ U tc, Comments. i j i vyv cCSn ) H ^ /iH -l i t 7 ~ 0 <^ & y ^ r r i (^ ' Page _ 2 = - or _ j L Original - Accompanying Samples Last Page - Originator See Reverse Side for Instructions 3M Environmental Labora Form 38778 - PWO Shipping Address: 3M Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Telephone: Sample Receiving: (651) 778-4948 Alternate: (651)778-6753 FAX: (651)778-6176 BACK TO MAIN Chain of Custody /Request for Laboratory Analytical 1 8 1 0 5 Project ID/Project Name 3M Env. Lab Project # For Internal Use Only Sample Condition Upon Receipt: Temperature: 'C nn ik?.r a T r~ rffo \ / O Acceptable 0 Other: # Received c n ic e f f lttf r iV U U W S IU. , Page Original - Accompanying Samples X \S. / , ^ _ LM( kito Last Page - Originator djui "H l Y i^mftcrrhu t> J/ ,, s _______________ J V ' C C - ^ T fL c ^ - See Reverse Side for Instructions Environmental Labor BACK TO MAIN U4Chain of Custody /Request for Laboratory Analytical 1 8 1 Form 38778 - PWO Shipping Address: 3M BIdg. 2-3E-09 Telephone: Sample Receiving: (651) 778-4948 \ Project ID/Project Name Template # 1 Final Report Due Date m i o \ JtJ 935 Bush Avenue Alternate: (651)778-8753 Project Lead Internal Due Date 3M Env. Lab Project # > For Internal Use Only E D !' 0 0 % Report Results to: VOCs Other Total Number of Containers Contact Name Company D /Y U / 'Y ftC O N ) Mailing Address City, State, Zip Telephone # Special Instructions and/or Specific Regulatory Requirements: (method, limit of detection, reporting units, etc.) FAX # Date Available Date Due Contract Lab Preservatives: o z X * O {/) X 0) c0 z ^ ,o L / ^ b*V $ i\ <7 cc 0^ Analysis Requested: ^ CBTtyjlete below. Attach any associated information. L v\ Item # 1. Client Sample Identification (tm tV T ^ - C j t o e v k 3. Q \ j T - l > ^ \y 5. Y i i j i P ^ L ' K P L 6/ u ) l < t2 . 7. f t ' u r D - l6 - f i U S 1- ^ D p p t 8. t X v YlU -PAAS " a u J T E ' C '. - i -AAS - p o lo _____________ s->o* Collected by (print): .;m3 Item # .o -4-1 fijo I J(ZV. Relinquished by/Affiliation fk A 3M LIMS# Date Sampled \H M .G L r & 'i i/p q l ) \ Jf i1 5A WO ii Y VA . \!/ Time il. Time Sampled Matrix/ Media Enter the number of containers of each LO l 1 / LO _ L ___ _L JL \ ] 1 _JU \ 1 > IX /. y Collector's signature; 1 11 _L 1 JL 1 _L Date Shipped Via: a 3 (Enter an X in the box below to indicate request) X X L X < X X XJL / * 3 o /-? / *( Sample Condition Upon Receipt: ^jy'A cceptable O Other: Temperature: liioi a m , irm i iOther Associated CoCs: ^ Received on Ice 7c KArt. Ltf-t / k^dL o u im iicm a , O L U -b 'V v k \M P / rt r\ . ^ J7> c a ^ T T i ? ^P a g e or _ T Original - Accompanying Sam ples Last Page - Originator See Reverse Side for Instructions 1 Report Results to: VOCs None Other Total Number of Containers Environmental Laboratory. Form 38776 - PWO Shipping Address: 3M Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Telephone: Sample Receiving: (6S1) 778-4948 Alternate: (651) 7784753 FAX: (651) 778-8176 \ \ \ \ Contact Name Company j )P t U & Mailing Address City. State, Zip Telephone # Special Instructions and/or Spectflc Regulatory Requirements: (method, limit of detection, reporting units, etc.) BACK TO MAIN 1 8 1 0 3Chain of Custody /Request for Laboratory Analytical Project ID/Project Name D V + " ^ Template # Project Lead Dept. # (main) j LA / "' * \ \ \ L 0 QsO>uuCT\J> Il W - L r 4^ -inai Report bue Date f i t ( 01 nternal Due Date # /VC/3lass/Job/Project VJ\\-- A Date Available ^ $ -9 3M Env. Lab Project# D l- O C ^ f, FAX # Date Due Contract Lab Preservatives: ^ sVi* } `d:Analysis Requeste / Complete below. Attach any associate d Info m atter . #Item Client Sample Identification 3M Date Time LIMS# SampJed Sampled 1. ScSrrmY M \ .m \________________________ z z a V ixZL\ \ & 0 fe w y iY' _______________________ L 3. S uiter- A j a )Mlol m i QtirtE-' C> 5. ------ JJL 73UDl mu i t t n " - l<c o teWLTftseAJiYwnv 7. /nfc S l'n d -% ____ :_____ 4-U2 La - J L ' M JA J/ W D\ b 9. , ' Phwi - )CshzU1 v_yv_z_x/iIiP^___ :_______ L3d jL r)i)vyi - S&dj nk^rt, ' \J Matrix/ Media 5 Vo Ln 3 S VJQ to 9 O o 0 z X (N0 1 S1 Enter the number of containers of each \ 1 is --11v-- /I~i-----/ T i \ 1/ 1 1i l ( }C 1J t 11 _L t Item # j a3 o Sw': 3 (p, Relinquished by/Affiliation ------- / 3 r~v Time Date 7 3 2 l W Q l l 60 i p e j i l ___fo v e z Sample Condition Upon Receipt: ^^O'Acceptable 0 Other: Temperature: n iK n - A e en rlo tarf n ^ m - 'C Received on Ice rvs/_v_p_ i o o u . f . i m . if ltK , ( f t 66, lii O t , /C 5 H r/ /fc . >_ Page Original - Accompanying Sam ples Last Page - Originator Comments: , O jU L + n v e -Jp i\AiayPu ^ > / ir \ O e n k & l 5 y ___ ____________________________ * y k ]~Q Sea Reverse Side for Instructions