Document ypEoVyqjLbvZmj8gMDmjdg49E

LPhone: (814)231-8032 BACK TO MAIN Fax:(814)231-1253 or (814)231-1 580 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 1 OF6 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 requestedfor all samples. A total of 23 samples were receivedfor analysis. The samples were preparedand analyzedby LCIMSIMS for the following list of fluorochemicals: ComDound Name Perfluorooctane Sulfonate I Perfluorooctane Sulfonvlamide Perf luorooctanoate . Perfluorohexane Sulfonate Acronvm 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 presentedhere 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 individualsample containers were received. Samples were received on 1/31/01.Samples were collectedon 1/19/01and 1/24/01C.hain-of-custodyinformationis 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 nglL for periods longer than 14 days. PAGEZOFG BACK TO MAIN 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LClMSlMS Analysis Water samples were initially treated with 200 UL of 250 mgR sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliterportion of sample was transferredto a CI8SPE 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 LCNSIMS. 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, beginningwith the solid phase extraction. 4.1.2 Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injectedand passed through a liquid-phasechromatographic 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-PackardHP1100 HPLC system coupled to a Micromass Ultima MS/MS was usedto 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 105OC and determining the weight loss. The PAGE 3OF6 BACK TO MAIN percentage organic matter was determined by treating the dried sample with hydrochloric acid to remove carbonates, followed by ashing at 75OOC. The percentage organic matter was calculated from the weight loss after taking into account the carbonateconcentration. 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 ngR (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plottedfor each point. Using linear regressionwith l/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (?) were determined. A calibration curve is acceptable if r 20.985 (?2 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 concentrationsare 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-levelcalibrationstandard. For these samples, the extractionblanks 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 presentedhere 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 ngL 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. PAGE 4 OF 6 BACK TO MAIN 5.7 Sample Related Comments There are no other sample relatedcomments for this data set. 6 Datasummary Please see Attachment A for a detailed listing of the analytical results. Water results are reported in parts per trillion (ppt) (ngR-). 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 "Lo by weight. 7 DatdSample 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 maintainedby 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 OF6 9 Signatures Kevin J Lloyd, Vice President Other Lab Members Contributingto Data Karen Smith G. Ronald Ripper BACK TO MAIN Date PAGE 6 OF 6 (W\ Laboratories. Inc. Centre Analytical 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN 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 201 0 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 < NO < LOQ - Please refer to the reverse side for our standard terms and conditions. BACK TO MAIN Centre Analytical - Laboratories, Inc. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 3M ID QWI East-C Sediment QWI East-C Sediment QWI South-C Sediment QWl South-C Sediment QWl West-C Sediment QWl West-C Sediment QWl North-C Sediment QWI North-C Sediment QWll - C Sediment QWll - C Sediment QWlll - C Sediment QWIll - C Sediment CENTRE ID 01 00677 01 00677 01 00679 01 00679 01 00681 0100681 01 00683 01 00683 01 00689 01 00689 0100691 01 00691 TOCS (l-JS/S) Dry Wt. 1 5260 1 4690 1 2100 Organic Matter (W Dry Wt. 1.97 1.77 0.950 1940 I 0.920 284 I 0.750 277 I 0.760 6480 1 0.910 6230 I 0.890 6350 I 1.03 I 6720 I 2070 1 2100 1.06 0.290 0.430 Blind - C Sediment 01 00693 0.460 Blind - C Sediment 01 00693 0.500 Moisture (Yo) 1 - I I 36.6 I 35.1 I 34.6 I II 34.5 I 38.4 I 1 38.3 I 1 41.2 1 I1 41.0 I 35.7 I 1 34.4 I 1 I 31.3 I 1 30.3 TOCS Analysis Date: 02/09/01 Organic Matter Analysis Date: 02/07/00 ?LOMoisture Analysis Date: 02/06/01 Please refer to the reverse side for our standard terms and conditions. (W\ Laboratories. Inc. CEntre Analytical 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN Analytical Results Port St. Lucie Resampling (sediments as received) 3M Sample Identification PFOS (ug/Kg) PFOA (ug/Kg) PFHS (ug/Kg) PFOSA (ug/Kg) QWI East-C 6.1 1 QWI East-C (lab duplicate) 5.93 QWI South-C 7.83 QWI South-C (lab duplicate) 9.36 QWI West-C 6.67 QWI West-C (lab duplicate) 6.47 QWI North-C 5.46 QWI North-C (lab duplicate) 5.77 QWII-C NQ QWII-C (lab duplicate) NQ QWIII-C NQ QWIII-C (lab duplicate) NQ Blind-C 5.68 Blind-C (lab duplicate) 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 0.21 6 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 % Solids 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. 4w\ Centre Analytical Laboratories, Inc. 3048 Research Drive, State College PA 76807 874-237-8032 FAX 874-237-1253 BACK TO MAIN Analytical Results Port St. Lucie Resampling (sediments dry weight) 3M Sample Identification PFOS (ug/Kg) PFOA (ug/Kg) PFHS (uglKg) PFOSA (uglKg) o/' Solids QWI East-C QWI East-C (lab duplicate) QWI South-C QWI South-C (lab duplicate) QWI West-C QWI West-C (tab duplicate) QWl 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 0.31 5 -imit of Detection (LOD) for the procedure is approximately 0.08 ug/Kg for all compounds (as received) I-imit of Quantitation (LOQ) for the procedure is 0.20ug/Kg for all compounds (as received) IJD - Compound not detected IJQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. lrlD c LOD < NQ < LOQ 0.465 0.440 1 .oo 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. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery !Sample ID: I QWI East-C 1 !Spiked Amount (ng/L): I 1000 F'FOS F'FOA I-F'FHSF'FOSA Sample Concentration (ng/L) 1970 79.6 459 31.9 Matrix Spike Result (ng/L) 3120 1110 1410 1320 Matrix Spike Result (% Recovery) 1 15.0 103.0 95.1 128.8 Criteria (Pass / Fail) PASS PASS PASS PASS L.ower Recovery Limit: I 70 Upper Recovery Limit: 1 130 BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: 1 QWI South-C !Spiked Amount (nglL): I 1000 I bFOS f'FOA PFHS F'FOSA Sample Concentration (ng/L) 21 20 84.8 470 44.1 Matrix Spike Result (ng/L) 31 70 1182 1450 1450 Matrix Spike Result (% Recovery) 105.0 109.7 98.0 140.6 Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recovery Limit: I 70 Upper Recovery Limit: 1 130 I BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: I QWI West-C 1 :SpikedAmount (ng/L): [ 1000 I II'FOS PFOA f>FHS PFOSA Sample Concentration (ng/L) 2200 82.8 455 37.5 Matrix Spike Result (ngU 3200 1087 1410 1330 Lower Recovery Limit: I Upper Recovery Limit: I 70 1 130 I Matrix Spike Result (% Recovery) 100.0 100.4 95.5 129.3 Criteria (Pass / Fail) PASS PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: I QWI North-C 1 Spiked Amount (ng/L): I 1000 PFOS PFOSA Sample Concentration (ng/L) 2080 93.5 468 43.0 Matrix Spike Result (ng/L) 291 0 1086 1450 1370 Matrix Spike Result (% Recovery) 83.0 99.3 98.2 132.7 Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recoverv Limit: I 70 I I I lJmer Recoverv Limit: I 130 I BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery !Sample ID: I QWl Culvert-C 1 !SpikedAmount (ng/L): I 1000 1 Sample Concentration (ng/L) 1840 70.1 628 45.5 Matrix Spike Result (ng/L) 271 0 1088 1610 1360 Matrix Spike Result (% Recovery) 87.0 101.8 98.2 131.5 Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recovery Limit: I 70 Upper Recovery Limit: [ 130 I BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Samde ID: I QWII-C 1 Spiked Amount (ng/L): [ 1000 I PFOS PFOA PFHS 'FOSA Sample Concentration (ng/L) 24.4 9.82 6.53 0 Matrix Spike Result (ng/L) 1080 961 998 1280 Matrix Spike Result (YORecovery) 105.6 95.1 99.1 128.0 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: [ lJpper Recovery Limit: I 70 1 130 1 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 !;ample ID: I QWIII-C Spiked Amount (ng/L): 1 1000 I 1F'FOS F'FOA F'FHS ~~FOSA Sample Concentration (ng/L) 25.5 33.0 8.1 6 0 Matrix Spike Result (ng/L) 1150 1010 863 1310 Matrix Spike Result (% Recovery) 112.5 97.7 85.5 131.O Criteria (Pass / Fail) PASS PASS PASS FAIL Lower Recovery Limit: 1 70 I Upper Recovery Limit: I 130 1 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: Blind-C 1 hFOS F'FOA -~ F'FHS F'FOSA Sample Concentration 0-w) 2367 75.5 446 34.6 Matrix Spike Result (ng/L) 3368 955 1250 1500 Lower Recovery Limit: [ Upper Recovery Limit: r 70 1 130 1 Matrix Spike Result ("A Recovery) 100.1 88.0 80.4 146.5 Criteria (Pass / Fail) PASS PASS PASS FAIL BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery !;ample ID: I QWI East-C (sediment) I Spiked Amount (ng/L): I 500 I 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 1 13.4 117.4 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: I 70 I Upper Recovery Limit: I 130 1 Note: Sample results less than 25 ng/L are reportedas NQ in the results section as they are bmslow the limit of quantitation. Results are given in this table for recovery calculations only. Concentrationsrepresent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: I QWI South-C (sediment) ] Spiked Amount (ng/L): I 500 -F'FOS F'FOA -F'FHS F'FOSA Sample Concentration v (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: I 70 1 Upper Recovery Limit: I 130 I hlote: 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 9: LC/MS/MS Laboratory Matrix Spike Recovery Sample ID: [ QWI West-C (sediment) 1 Spiked Amount (ng/L): I 500 J =FOS IPFOA 'IDFHS I'FOSA Sample Concentration (ng/L) 802 14.6 28.4 46.9 Matrix Spike Result (ng/L) 1270 368 51 6 679 Matrix Spike Result (% Recovery) 93.6 70.7 97.5 126.4 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: I 70 I Upper Recovery Limit: I 130 I Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are tielow 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: 7 Spiked Amount (ng/L): I 1 500 1 ,?FOS IPFOA PFHS PFOSA Sample Concentration 744 12.6 0 39.9 Matrix Spike Result (ng/L) 1340 382 61 0 686 Matrix Spike Result (% Recovery) 119.2 73.9 122.0 129.2 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: [ Upper Recovery Limit: I 70 I 130 I Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are tselow 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: [ QWII-C (sediment) I Spiked Amount (nglL): I 500 I Sample Concentration (ng/L) 24.0 0 0 0 Matrix Spike Result (ng/L) 474 36 1 567 645 Matrix Spike Result (% Recovery) 90.0 72.2 113.4 129.0 Criteria (Pass / Fail) PASS PASS PASS PASS L.ower Recovery Limit: I llpper Recovery Limit: I 70 1 130 I 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. C:oncentrationsrepresent amounts of material in the sample extracts BACK TO MAIN Attachment B: LC/MS/MS Laboratory Matrix Spike Recovery !Sample ID: 1 QWIII-C (sediment) 1 !$pikedAmount (ng/L): I 500 I Sample Concentration 19.3 9.2 0 0 Matrix Spike Result OWL) 428 350 41 0 450 Matrix Spike Result (% Recovery) 81.7 . 68.2 82.0 90.0 Criteria (Pass / Fail) PASS FAIL PASS PASS I Lower Recoverv Limit: 70 1 I I Upper Recovery Limit: I 130 I 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: I Spiked Amount (ng/L): 1 Blind-C (sediment) 500 Sample Concentration (ng/L) 646 15.0 40.0 40.9 Matrix Spike Result 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: I 70 I Upper Recovery Limit: [ 130 1 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are b'slowthe 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: I QWI East-C 1A I Spiked Amount (ng/L): 1 1000 I 'PFOS IPFOA 'PFHS IPFOSA 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 Recoverv Limit: I 70 I IJpper Recovery Limit: I 130 I BACK TO MAIN Attachment 9: LC/MS/MS Field Matrix Spike Recovery !;ample ID: r !;piked Amount (ng/L): 1 QWI East-C 1B 1000 F'FOS F'FOA `F'FHS F'FOSA I 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 Lower Recovery Limit: I Upper Recovery Limit: [ 70 130 I Criteria (Pass / Fail) FA1L PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: I QWI East-C 25A I Spiked Amount (ng/L): 1 25000 I 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 I-ower Recovery Limit: I ~~ ~~~~ 70 IJpper Recovery Limit: I 130 I BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery Sample ID: I QWI East-C 25B I Spiked Amount (ng/L): 1 25000 I PFOS PFOA PFHS PFOSA L Sample Concentration (ng/L) 1970 79.6 459 31.9 Matrix Spike Result (ng/L) 321 00 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: I lJpper Recovery Limit: I 70 J 130 1 BACK TO MAIN Attachment B: LC/MS/MS Field Matrix Spike Recovery !;ample ID: I QWII-C I Spiked Amount (ng/L): I 200 I -F'FOS F'FOA F'FHS Sample Concentration (ng/L) 24.4 9.8 6.5 Matrix Spike Result (ng/L) 240 206 21 1 Matrix Spike Result (% Recovery) 107.8 98.1 102.3 Criteria (Pass / Fail) PASS PASS PASS Lower Recovery Limit: I 70 I Upper Recovery Limit: [ 130 1 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 Field Matrix Spike Recovery !Sample ID: 1 QWII-C I !Spiked Amount (ng/L): I 1000 I 1F'FOS F'FOA F'FHS rFOSA Sample Concentration (ng/L) 24.4 9.8 6.5 0 Matrix Spike Result 1080 1020 1030 1160 Matrix Spike Result (% Recovery) 105.6 101.o 102.4 116.0 Criteria (Pass / Fail) PASS PASS PASS PASS Lower Recovery Limit: 1 L'pper Recovery Limit: I 70 I 130 I Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are bm31ow the limit of quantitation. Results are given in this table for recovery calculations only. 3M Environmental Laborat Form - 38778 pwo Shipping Address: 3M Bldg 23E-09 935 Bush Avenue St Paul. 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