Document 3eqGpnJ3r1mGeyx7KqOYbpROy

iPhone: (814) 231-8032 BACK TO MAIN Fax: (814) 231-1.253or (814) 231-1580 Analytical Report Fluorochemical Characterization of Drinking Water, Surface Water, Sediment, POTW Effluent, POTW Sludge and Landfill Leachate Samples Port St. Lucie Resampling (E00-2003) Centre Analytical Laboratory Report No. 0123-014P (Revision 1) Revision Date 3/27/01 Testing Laboratory Centre Analytical Laboratory, Inc. 3048 Research Drive State College, PA 1680'1 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 Ph.D. 3M Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 1 OF5 BACK TO MAIN I lntroduction Results are reported for the analysis of a series of water, leachate, sludge, 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 E00-2003.The Centre study number assigned to the projecl is 023-014. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) and ion chromatography was requested for all samples. A total of 45 samples were receivedfor analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: 0 Table 1:Target Analysis Compound Name Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate Acronvm PFOS PFOSA POAA The analytical methods used for water samples were validated by Centre. The validation protocol and results are on file with Centre. The methods were rnodified for the sediment samples, however the procedures have not been fully validated for this 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. Forty-five individual sample containers were received. Samples were received on 7/25/00. The samples were collected between 7/18/00 and 7/19/00. Chain-of-custody informatiori is presented in Attachment C. 3 Holding Times The analytical method used was validated against a maximiurn holding time of 14 days. 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. PAGEZOFS BACK TO MAIN I 4 Methods -Analytical and Preparatory 4.1 4.1.1 4.1.2 LC/MS/MS Sample Preparationfor LC/MS/MS 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-milliliter portion of sample was transferredto a Cl8SPE 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 and sludge 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. 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 analyzirig 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 quantitatedaga.inststandards. A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed1 using selected reaction monitoring (SRM). Water samples were extracted between 8/15/00 and 8/17/00 and analyzed by MS/MS between 8/18/00 and 8/23/00. Sediment and sludge samples were extracted on 8/18/00 and were analyzed by M S / M S on 8/21/00. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in Attachments D arid E. 5 Analysis 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the a.nalyticalsequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LCIMSNS analysis. The instrument response versus the concentrationwas 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 (1.2 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 concentrations are within +/-20% of the actual value. BACK TO MAIN 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 Surrogatespikes are not a component of the LCNSIMS analytical methods. 5.4 Matrix Spikes Matrix spikes were prepared for every field sample using all compounds of interest. Matrix spike recoveries are given in Attachment B. Field spikes were submitted with the water samples. Field spike recoveries are also included in Attachment 6. The PSLF Leach-C-FMS sample spiked at 200 ng/L appears to have been spiked in error. Spike results are comparable to the 1OOCl ng/L spiking level. 5.5 Duplicates All field samples were analyzed in duplicate. 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 and E. 5.7 Sample Related Comments There are no other sample related comments for this data set. 6 Datasummary Please see Attachment A for a detailed listing of the analytical results. Surface water results are reported in parts per trillion (ppt) (ng/L). Sediment and sludge sample results are reported in parts per billion (ppb) (ug/Kg) on both an as-received i3nd dry-weight basis. 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 maintained by Centre. PAGE ,4 OF 5 BACK TO MAIN 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 (SurfaceWater Samples) 8.5 Attachment E: LC/MS/MS Raw Analytical Data (Sediment and Sludge Samples) 9 Signatures Kevin J Lloyd, Vice President Date Other Lab Members Contributingto Data Karen Smith CA\ Laboratories. Inc. Centre Analytical 3048 Research Drive, State College PA 16801 814-231-8032 FAX (814-231-7253 BACK TO MAIN 3M Sample Identification MDWPIN-R-0-C MDWPIN-Lime-C MDWPOut -C NPWWTPEff -c wwwTPcc-c FSLF Leach-C TW#2 Fire Dept-C SW#3 SH-C l W # 3 Penpark-C SW#l Penpark-C l W # l Holiday Inn-C SW#2 MCM-C ClSW Palm City-C NPWWTP Sludge-C SED #3 SH-C SED #1 Penpark-C SED #2 MCM-C Sample Description Municipal Drinking Water Plani Intake - Reverse Osmosis Municipal Drinking Water Plant Intake - LIME Municipal Drinking Water Plant Outflow North Port Wastewater Treatm'ent Plant Effluent North Port Wastewater Treatment Plant Chlorine Contact Chamber Port St. Lucie Landfill Leachate Tap Water Site #2 Fire Departrnent Surface Water Site #3 Stuart Harbor Tap Water Site #3 Pendarvis Park Surface Water Site #1 Pendarvis Park Tap Water Site #1 Holiday Inn Surface Water Site #2 Martin Cty Marina Quiet Surface Water Palm City North Port Wastewater Treatment Plant Sludge Sample Sediment Sample #3 Stuart Harbor Sediment Sample #1 Pendarvis Park Sediment Sample #2 Martin Cty Marina 43 Please refer to the reverse side for our standard terms and conditions. BACK TO MAIN .7 . i 4mk!il\ Centre Analytical Laboratories,,Inc. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN Analytical Results E00-2003 Port St. Lucie, FL Resampling (water samples) .3MSample Identification PFOS (ng/L) PFOSA (ng/L) POAA (ng/L) iMDWPIN-R-0-C MDWPIN-R-0-C dup MDWPIN-Lime-C MDWPIN-Lime-C dup MDWPOut -C MDWPOUt-C dup NPWWTPEff -C NPWWTPEff-C dup NPWWTPCC-C NPWWTPCC-C dup PSLF Leach-C PSLF Leach-C dup TW#2 Fire Dept-C TW#2 Fire Dept-C dup SW#3 SH-C SW#3 SH-C dup TW#3 Penpark-C TW#3 Penpark-C dup SW#1 Penpark-C SW#1 Penpark-C dup TW#1 Holiday Inn-C TW#1 Holiday Inn-C dup SW#2 MCM-C SW#2 MCM-C dup QSW Palm City-C QSW Palm City-C dup Blind Dup C l Blind Dup C l dup Blind Dup C2 Blind Dup C2 dup ND ND ND ND ND ND ND ND ND ND ND ND NQ ND NQ ND 85.5 NQ 78.8 NQ 429 NQ 425 NQ ND ND ND ND NQ ND NQ ND ND ND ND ND NQ ND NQ ND ND ND ND ND NQ ND NQ ND 2930 30.0 2850 27.5 ND ND ND ND NQ ND NQ ND ND ND ND ND ND ND NQ NQ 42.9 40.2 1030 1020 ND ND ND ND ND ND ND ND ND ND ND ND 96.9 97.1 ND ND ND ND Limit of Detection (LOD) for the procedure is appoximately 2.5 ng/L for PFOS and PFOSA and 7.5 ngR 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 quantifia'ble. ND c LOD c NQ c LOQ - Please refer to the reverse side for our standard terms and conditions. a\Laboratories. Inc. CEntrE Analytical 3048 Research Drive, State College PA 16801 8 14-231-8032 FAX - 814-231 1253 BACK TO MAIN Analytical Results E00-2003Port St. Lucie, FL Resampling (solids) 3M Sample Identification NPWWTP Sludge-C NPWWTP Sludge-C dup SED #3 SH-C SED #3 SH-C dup SED#l Penpark-C SED#1 Penpark-C dup SED#2 MCM-C SED#2 MCM-C dup PFOS (ug/Kg) (as received) 1.36 1.30 ND ND ND ND ND ND PFOSA (ug/Kg) (as received) ND ND ND ND ND ND ND ND POAA (ug/Kg) (as received) ND ND ND ND ND ND ND ND 3M Sample Identification NPWWTP Sludge-C NPWWTP Sludge-C dup SED #3 SH-C SED #3 SH-C dup SED#1 Penpark-C SED#1 Penpark-C dup SED#2 MCM-C SED#2 MCM-C dup PFOS (ug/Kg) (dry weight) 62.9 60.2 ND ND ND ND ND ND PFOSA (ug/Kg) (dry weight) ND ND ND ND ND ND ND ND POAA (ug/Kg) (dry weight) ND ND ND NO ND ND ND ND Limit of Detection (LOD) for the procedure is appoximately0.08 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 e LOO c NQ e LOQ Yo Sollds 2.16 2.16 76.68 76.68 76.10 76.10 65.74 65.74 Please refer to the reverse side for our standard terms and conditions. BACK TO MAIN BACK TO MAIN ,Attachment B: LC/MS/MS Laboratory Spike Recovery !sample ID: I MDWPIN-ROC 1 Spiked Amount (ng/L): [ 100 1 Lower Recovery Limit: IJpper Recovery Limit: Sample Concentration 0 70 130 1 Result (ng/L) 90.3 l1o157 Result (% Recovery) Criteria (Pass / Fail) I I 90.3 105.0 117.0 PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: 1 MDWPIN-LimeC I !SpikedAmount (ng/L): [ 100 I Sample Concentration (ng/L) 0 0 0 Matrix Spike Result 101 98.8 111 Lower Recovery Limit: I Upper Recovery Limit: 1 70 1 130 1 Matrix Spike Result (% Recovery) 101.o 98.8 111.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I MDWPIN-OutC I Spiked Amount (ng/L): I 100 J [F'FOS F'FOSA F'OAA Sample Concentration (w-1 0 0 0 Matrix Spike Result (ng/L) 102 103 103 Matrix Spike Result (% Recovery) 102.0 103.0 103.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I NPWWTP Eff-C I Spiked Amount (ng/L): I 100 Sample Concentration (ng/L) 14.7 0 15.1 Matrix Spike Result (ngU 112 85.0 127 Matrix Spike Result (% Recovery) 97.3 85.0 111.9 Criteria (Pass I Fail) PASS PASS PASS Lower Recovery Limit: I 70 llpper Recovery Limit: 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 recove#rycalculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I NPWWTPCC-C ] Spiked Amount (ng/L): I 100 I Sample Concentration Matrix Spike Result ~ PFOSA 4.4 POAA 42.9 I-ower Recovery Limit: [ 70 'Upper Recovery Limit: 1 130 88.5 149 1 1 Matrix Spike Result 84.1 106.1 =I Criteria (Pass / Fail) I IVote: Sample results less than 25 ng/L are reported as NQ in the results section as they are Ibelow the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I PSLFLeach-C 1 SDiked Amount fna/U: I 100 1 Sample Concentration (n!m 429 7.0 1030 Matrix Spike Result (ng/L) 554 102 1125 Matrix Spike Result (% Recovery) 125.0 95.0 95.0 Criteria (Pass / Fail) PASS PASS PASS Lower Recovery Limit: I 70 Upper Recovery Limit: 1 130 I Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are lbelow the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I TW#2 Fire Dept-C 1 Spiked Amount (ng/L): 100 POAA Sample Concentration 0 0 0 Matrix Spike Result (ng/L) 101 102 110 Lower Recovery Limit: 1 70 1 Upper Recovery Limit: I 130 Matrix Spike Result ("A Recovery) 101.o 102.0 110.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): I SW#3SH-C 1 100 I PFOS PFOSA rPOAA Sample Concentration (ng/L) 7.8 0 0 Matrix Spike Result (ng/L) 103 98.5 117 Matrix Spike Result (% Recovery) 95.2 98.5 117.0 Criteria (Pass / Fail) PASS PASS PASS Lower Recovery Limit: I 70 1 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. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I TW#3 Penpark-C 1 Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 96.0 107 110 Lower Recovery Limit: 70 Upper Recovery Limit: I 130 I Matrix Spike Result (% Recovery) 96.0 107.0 110.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I SW#1 Penpark-C I Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 5.2 0 0 1 70 1 130 Matrix Spike Result (ng/L) 114 109 126 I Matrix Spike Result (% Recovery) 108.8 109.0 126.0 Criteria (Pass / Fail) PASS PASS PASS 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 Spike Recovery Sample ID: ITW#l Holiday Inn-C] Spiked Amount (ng/L): 100 I PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 108 119 117 I 70 1 I 130 Matrix Spike Result (% Recovery) 108.0 1 1 9.0 117.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I SW#2MCM-C j Spiked Amount (ng/L): I 100 1 PFOS PFOSA POAA Sample Concentration (ngJL) 7.7 0 0 Matrix Spike Result (ng/L) 125 119 135 Matrix Spike Result (% Recovery) 1 17.3 119.0 135.0 Criteria (Pass / Fail) PASS PASS FAIL m Lower Recovery Limit: I Upper Recovery Limit: I 70 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 Spike Recovery Sample ID: I QSW Palm City-C I Spiked Amount (ng/L): I 100 i PFOS PFOSA POAA Sample Concentration (ng/L) 2930 30.0 96.9 Matrix Spike Result 3260 160 249 Matrix Spike Result ("A Recovery) 330.0 130.0 152.1 Lower Recovery Limit: [ 70 I Upper Recovery Limit: I 130 I PFOS sample concentration exceeds spiking concentration by greater than 1OX Criteria (Pass / Fail) FAIL PASS FAIL BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I Blind Dup 1 I Spiked Amount (ng/L): I 100 PFOS PFOSA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 101 93.5 99.4 Matrix Spike Result (% Recovery) 101.o 93.5 99.4 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I Blind Dup 2 1 Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA k Sample Concentration (ng/L) 8.0 0 0 Matrix Spike Result (ng/L) 109 103 112 Matrix Spike Result (% Recovery) 101.0 103.0 112.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: 1 NPWWTPSludge-C ] Spiked Amount (ng/L): I 250 1 PFOS PFOSA POAA Lower Recovery Limit: I Upper Recovery Limit: 1 Sample Concentration (ng/L) 170 16.7 12.3 70 130 Matrix Spike Result WL) 377 193 256 I 1 Matrix Spike Result (% Recovery) 82.8 70.5 97.5 Criteria (Pass / Fail) PASS PASS PASS Concentrations indicate amount of material in the sample extract 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: l,C/MS/MS Laboratory Spike Recovery Sample ID: I Sed#3 SH-C Spiked Amount (ng/L): I 250 I PFOS PFOSA Sample Concentration (ng/L) 0 0 Matrix Spike Result (ng/L) 227 21 0 Lower Recovery Limit: I 70 j Upper Recovery Limit: 1 130 I Concentrations indicate amount of material in the sample extract Matrix Spike Result (% Recovery) 90.8 84.0 , Criteria (Pass / Fail) PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: 1 Sed#l Penpark-C I Spiked Amount (ng/L): 1 250 1 Sample Concentration (ng/L) 3.3 0 0 Matrix Spike Result (ng/L) 215 21 6 236 Matrix Spike Result (% Recovery) 84.7 86.4 94.4 Criteria (Pass / Fail) PASS PASS PASS Lower Recovery Limit: [ 70 lJpper Recovery Limit: I 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 indicate amount of material in the sample extract BACK TO MAIN .Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: I Sed#2 MCM-C 1 !Spiked Amount (ng/L): 250 I Lower Recovery Limit: 1 lJpper Recovery Limit: I Sample Concentration (ng/L) 2.9 0 0 70 130 EMatrix Spike Result 240 220 246 I I Matrix Spike Result (% Recovery) 94.8 88.0 98.4 Criteria (Pass / Fail) PASS PASS PASS 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. Concentrationsindicate amount of material in the sample extract BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MDWPIN-RO-C FMS ] Spiked Amount (ng/L): I 200 1 'PFOS PFOSA Sample Concentration (ng/L) 0 0 Matrix Spike Result (ng/L) 197 177 Lower Recovery Limit: [ Upper Recovery Limit: 1 70 130 I Matrix Spike Result ( O h Recovery) 98.5 88.5 Criteria (Pass / Fail) PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MDWPIN-RO-C FMS I Spiked Amount (ng/L): I 1000 PI=os PFOSA POAA Lower Recovery Limit: I Upper Recovery Limit: I Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 954 857 768 ~ ~ 70 130 I Matrix Spike Result (YORecovery) 95.4 85.7 76.8 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MDWPIN-Lime-CF M S ] ~~~~ Spiked Amount (ng/L): [ ~~~~ 200 I Lower Recovery Limit: I lJpper Recovery Limit: I Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 179 173 189 1 Matrix Spike Result (% Recovery) 89.5 86.5 94.5 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MDWPIN-Lime-C FMS I Spiked Amount (ndL): I 1000 I PFOS PFOSA POAA Lower Recovery Limit: [ Upper Recovery Limit: I Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 844 a44 793 1 I Matrix Spike Result (% Recovery) 84.4 84.4 79.3 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: 1 MDWPOut-CFMS ] Spiked Amount (ng/L): [ 200 I PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: I Sample Concentration (ngW 0 0 0 70 130 Matrix Spike Result (ng/L) 201 190 172 Matrix Spike Result (% Recovery) 100.5 95.0 86.0 Criteria (Pass I Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery SamDle ID: I MDWPO- ut--CFMS I L I Spiked Amount (ng/L): I 1000 1 PFOS PFOSA POAA Lower Recovery Limit: 1 Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ngN 83 1 787 708 1 I Matrix Spike Result (% Recovery) 83.1 78.7 70.8 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I NPWWTPEff-CFMS I Spiked Amount (ng/L): I 200 I PFOS PFOSA POAA ? Lower Recovery Limit: I Upper Recovery Limit: I Sample Concentration OWL) 14.7 0 15.1 70 130 Matrix Spike Result (ng/L) 203 106 223 I Matrix Spike Result (% Recovery) 94.2 53.0 104.0 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. Criteria (Pass / Fail) PASS FAIL PASS J BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I NPWWTPEff-CFMS ] Spiked Amount (ng/L): I 1000 I PFOS PFOSA POAA Lower Recovery Limit: I Upper Recovery Limit: I Sample Concentration (ng/L) 14.7 0 15.1 70 130 Matrix Spike Result (ng/L) 81 6 538 1290 Matrix Spike Result (% Recovery) 80.1 53.8 127.5 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. Criteria (Pass / Fail) PASS FAIL PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: [ NPWWTPCC-C FMS I Spiked Amount (ng/L): 200 I PFOS PFOSA POAA Sample Concentration (ng/L) 85.5 4.4 42.9 Matrix Spike Result (ng/L) 302 162 252 Matrix Spike Result ("I!. Recovery) 108.3 78.8 104.6 Criteria (Pass / Fail) PASS PASS PASS 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 Spike Recovery Sample ID: I NPWWTPCC-CFMS I Spiked Amount (ng/L): I ~~ 1000 PFOS PFOSA POAA Sample Concentration (ng/L) 85.5 4.4 42.9 Matrix Spike Result 946 775 972 Matrix Spike Result (% Recovery) 86.1 77.1 92.9 Lower Recovery Limit: I Upper Recovery Limit: 1 70 130 ~ ~~ 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. Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I PSLFLeach-C FMS I Spiked Amount (ng/L): I 200 I . PFOS PFOSA POAA Lower Recovery Limit: I Upper Recovery Limit: I Sample Concentration 429 7.0 1030 70 130 Matrix Spike Result (ng/L) 1066 a97 1790 1 1 Matrix Spike Result (% Recovery) 318.5 445.0 380.0 Note: Sample results less than 25 ng/L are reported as N Q in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Criteria (Pass / Fail) FAIL FAIL FAIL Data indicates that this sample was spiked at 1000 ng/L rather than the 200 ng/L given in the field data BACK TO MAIN Attachment 6: LC/MS/MS Field Spike Recovery Sample ID: I PSLF Leach-C FMS 1 Spiked Amount (ng/L): I 1000 1 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: I Sample Concentration (nW 429 7.0 1030 70 130 Matrix Spike Result (ng/L) 1100 829 1870 I 1 Matrix Spike Result (% Recovery) 67.1 82.2 84.0 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. Criteria (Pass / Fail) FAIL PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: [ PSLF Leach4 FMS 1 Spiked Amount (ng/L): 25000 1 L PFOS PFOSA POAA L Sample - Concentration (ng/L) 429 7.0 1030 Matrix Spike Result (m-) 20900 21800 22800 Matrix Spike Result (% Recovery) 81.9 87.2 87.1 Lower Recovery Limit: [ Upper Recovery Limit: 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. Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: [ PSLF Leach-C FMS B 1 Spiked Amount (ng/L): I 200 I PFOS PFOSA POAA L Sample Concentration 429 7.0 1030 Matrix Spike Result (ng/L) 630 179 1270 Matrix Spike Result (% Recovery) 100.5 86.0 120.0 ~ Criteria (Pass / Fail) PASS PASS PASS 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 Spike Recovery Sample ID: I PSLF Leach-C FMS B I Spiked Amount (ng/L): I 1000 I PFOS PFOSA POAA Sample Concentration 0-m) 429 7.0 1030 Matrix Spike Result (ng/L) 1170 877 1980 Matrix Spike Result (% Recovery) 74.1 87.0 95.0 Lower Recovery Limit: 1 70 1 Upper Recovery Limit: 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 calculationsonly. Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I PSLF Leach-C FMS B I Spiked Amount (ng/L): I 25000 PFOS PFOSA POAA Sample Concentration (ng/L) 429 7.0 1030 Matrix Spike Result (ng/L) 21 900 19800 20500 Matrix Spike Result (% Recovery) 85.9 79.2 77.9 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. Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I Penpark-C FMS I Spiked Amount (ng/L): I 200 I PFOS I PFOSA POAA Lower Recovery Limit: I U.p.per Recoverv Limit: I, Sample Concentration OWL) 0 0 0 70 130 Matrix Spike Result (n!m 200 I I 139 194 I I 1 Matrix Spike Result (% Recovery) 100.0 69.5 97.0 I Criteria (Pass / Fail) PASS I FAIL PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I Penpark-C FMS 1 Spiked Amount (ng/L): [ 1000 J PFOS PFOSA POAA Lower Recovery Limit: [ Upper Recovery Limit: I Sample Concentration OWL) 0 0 0 70 130 Matrix Spike Result (ng/L) 83 1 678 794 1 I Matrix Spike Result (YORecovery) 83.1 67.8 79.4 Criteria (Pass / Fail) PASS FAIL PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I I, Holidav Inn-C FMS I [ I Spiked Amount (ng/L): I 200 1 PFOS PFOSA POAA Lower Recovery Limit: I Upper Recovery Limit: I Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 21 2 193 200 1 I Matrix Spike Result (% Recovery) 106.0 96.5 100.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I Spiked Amount (ng/L): I Holiday Inn-C FMS 1 1000 1 IPFOS PFOSA POAA Lower Recovery Limit: I Upper Recovery Limit: 1 Sample Concentration (WL) 0 0 0 70 130 Matrix Spike Result (ng/L) 1060 865 866 1 I Matrix Spike Result (% Recovery) 106.0 86.5 86.6 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: 1 QSW Palm City-C FMS I Spiked Amount (ng/L): 1 200 1 PFOS PFOSA zPOAA Sample Concentration 2930 30.0 96.9 Matrix Spike Result (ng/L) 3360 248 325 Matrix Spike Result (% Recovery) 21 5.0 109.0 114.1 Lower Recovery Limit: I 70 1 Upper Recovery Limit: I 130 I PFOS sample concentration exceeds the spiking level by greater than 1OX I Criteria I (Pass / Fail) FAIL PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I QSW Palm Citv-C FMS 1 Spiked Amount (ng/L): I 1000 I PFOS PFOSA ?POAA Lower Recovery Limit: I Upper Recovery Limit: I Sample Concentration (ng/L) 2930 30.0 96.9 70 130 Matrix Spike Result (ng/L) 381 0 76 1 899 I Matrix Spike Result (% Recovery) 88.0 73.1 80.2 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: 1 QSW Palm Citv-C FMS I I I Spiked Amount (na/Lk f 25000 I PFOS PFOSA POAA L Sample Concentration (ng/L) 2930 30.0 96.9 Matrix Spike Result 23300 20700 20900 Upper Recovery Limit: 1 130 I Matrix Spike Result (% Recovery) a i .5 82.7 83.2 Criteria (Pass / Fail) PASS - PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I QSW Palm City-C FMS 131 Spiked Amount (ng/L): I 200 I PFOS PFOSA POAA Sample Concentration (ng/L) 2930 30.0 96.9 Matrix Spike Result (ng/L) 3590 240 340 Matrix Spike Result (% Recovery) 330.0 105.0 121.6 Lower Recovery Limit: I Upper Recovery Limit: I 70 130 I PFOS sample concentrationexceeds the spiking amount by greater than 1OX Criteria (Pass / Fail) FAIL PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I QSW Palm City-c FMS B I Spiked Amount (ng/L): I 1000 I PFOS PFOSA POAA Lower Recovery Limit: 1 Umer Recoverv Limit: I I. I Sample Concentration (ng/L) 2930 30.0 96.9 70 1. _3_0 Matrix Spike Result (ng/L) 4000 819 955 1 I Matrix Spike Result ("10Recovery) 107.0 78.9 85.8 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: [ QSW Palm City-C FMS B 1 Spiked Amount (ng/L): I 25000 PFOS PFOSA POAA Lower Recovery Limit: I Upper Recovery Limit: I Sample Concentration WL) 2930 30.0 96.9 70 130 (ng/L) 24500 26200 20100 I Matrix Spike Result ("A Recovery) 86.3 104.7 80.0 I Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN tLi BACK TO MAIN a2 ln a 2 'OSZH 2 + 0 "H 2 n 0 , 'Tllim m 0 co 0 Ln 4 -2Q 5.m- m Q e d BACK TO MAIN IA E a m a ,BACK TO MAIN 9 s t- il 'I I- - f a - C .- - m POSH ? l I CONH i ? .E 0 1 4 cz1 Ea(0 0 0 BACK TO MAIN Ir) E m 0 e I t i Ir BACK TO MAIN I f T 1 - 8 C 0 U .-m> 0 a B 0 -. . 2 e s 0 I- BACK TO MAIN ,. 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