Document ZOVd9NBqj3vNKMaONko80ov8

BACK TO MAIN CEntrtz Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 www.centrelab.com (814) 231-8032 Fax: (814) 231-1253 or (814) 231-1580 Analytical Report Fluorochemical Characterization of Drinking Water Samples Port St. Lucie, FI (W2363) Centre Analytical Laboratory Report No. 023-007E (Revision 1) Revision Date 3/20/01 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 Kris J. Hansen, Ph.D. 3M EnvironmentalTechnology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 1 OF5 BACK TO MAIN 1 Introduction Results are reported for the analysis of a series of drinking water samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M Environmental Laboratory. The samples were collected from Port St. Lucie, FI. The Centre study number assigned to the project is 023-007. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requestedfor all samples. A total of 16 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 - ComDound Name Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate Acronvm PFOS PFOSA POAA The analytical method used was validated by Centre. The validation protocol and results are on file with Centre. 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. Sixteen individual sample containers were received. Samples were received on 02/15/00. The sample collection dates were not supplied. Chain-of-custodyinformationis presentedin Attachment C. 3 Holding Times The analytical method used was validated against a maximum holding time of 14 days. The stability of the analytes of interest for longer periods has not been determined. 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 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis 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 Cla 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 1OOoh 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. 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-PackardHPl100 HPLC system coupledto a Micromass Ultima MS/MS was usedto analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 2/25/00 and analyzed by MS/MS on 2/26/00. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in attachment D. 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) The response of the quantitation ion versus the concentration was plotted for each point. Using linear regression with l/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (P) 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 concentrations are within +/-20% of the actual value. For the results reported here, calibration criteria were met. PAGE 3 OF 5 BACK TO MAIN 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 method. 5.4 Matrix Spikes Matrix spikes were prepared for every sample at a concentration of 100 ngR using all compounds of interest. Matrix spike recoveries are given in Attachment B. Field spikes were also prepared on several samples at a concentration of 100 ng/L using all compounds of interest. Field spike recoveries are also given in Attachment B. 5.5 Duplicates All samples were analyzed in duplicate. Results are given along with the sample results in Attachment A. 5.6 Laboratory Control Samples Milliq water was spiked with all compound of interest at 25 and 250 ngR. All recoveries for all compounds were between 70-130% in each LCS. 5.7 Sample Related Comments Field blank samples consisted of empty containers. Forty milliliters of type I water filtered through a hypercarb cartridge was added to the empty container and analyzed in the same manner as the other samples. 6 Datasummary Please see Attachment A for a detailed listing of the analytical results. 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 OF5 BACK TO MAIN 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: MatrixSpike Recoveries(Fieldand LaboratorySpikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Kevin J Lloid, Vicd President Date Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith PAGE 5OF5 a\Laboratories, Inc. CEntrE Analytical 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN Analytical Results W2363 Port St. Lucie, FI 3M Sample Identification MC-615H MC-617H MC-620H MC-621H MC-623H MC-626H MC-628H MC-631H NA MC-632H NA MC-633H Sample Description Intake-PIN Intake-P/N duplicate Intake-FieldBlank Empty Outflow-PIN Outflow-PIN duplicate Site 1 PIN Site 1 PIN duplicate Site 2 P/N Site 2 PIN duplicate Site 3 P/N Site 3 P/N duplicate Field Blank-PIN Empty PFOS (ng/L) ND ND ND ND ND ND ND ND ND ND ND ND PFOSA (ng/L) ND ND ND ND ND ND ND ND ND ND ND ND POAA (ng/L) ND ND ND ND ND ND ND ND ND ND ND ND Limit of Detection (LOD) for the procedure is appoximately 2.5 ng/L for PFOS 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 e NQ < LOQ 43 Please refer to the reverse side for our standard terms and conditions. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I MC-619H 1 Spiked Amount (ng/L): [ 100 PFOS PFOSA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 87.1 90.4 96.2 Matrix Spike Result (% Recovery) 87.1 90.4 96.2 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I MC-625H 1 Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 I 70 I 130 Matrix Spike Result (ng/L) 83.6 89.5 93.2 I Matrix Spike Result (% Recovery) 83.6 89.5 93.2 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: MC-630H 1 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 87.4 81 .O 98.3 1 70 J 1 130 I Matrix Spike Result (% Recovery) 87.4 81 .O 98.3 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): MC-631H I 100 PFOS PFOSA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 95.0 87.0 104 Lower Recovery Limit: ~ 70 I Upper Recovery Limit: I 130 Matrix Spike Result (% Recovery) 95.0 87.0 104.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment 9: LC/MS/MS Laboratory Spike Recovery Sample ID: I MC-632H I Spiked Amount (ng/L): I 100 1 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 1 70 1 130 Matrix Spike Result (ng/L) 94.0 97.1 95.8 Matrix Spike Result (% Recovery) 94.0 97.1 95.8 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: Spiked Amount (ng/L): I MC-618H 100 I PFOS PFOSA POAA Sample Concentration (m-1 0 0 0 Matrix Spike Result (ng/L) 125 128 125 Lower Recovery Limit: I 70 Upper Recovery Limit: I 130 1 Matrix Spike Result (% Recovery) 125.0 128.0 125.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MC-624H Spiked Amount (ng/L): 100 I PFOS PFOSA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 128 109 126 Lower Recovery Limit: I 70 I Upper Recovery Limit: I 130 1 Matrix Spike Result (% Recovery) 128.0 109.0 126.0 - Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment 9: LC/MS/MS Field Spike Recovery Sample ID: I MC-629H I Spiked Amount (ng/L): I 100 1 PFOS PFOSA POAA Sample Concentration (WL) 0 0 0 Matrix Spike Result (ng/L) 130 107 126 Matrix Spike Result (% Recovery) 130.0 107.0 126.0 Criteria (Pass / Fail) PASS PASS PASS Upper Recovery Limit: I 130 I Envii .mental Laboratory Form 30770 - PWO Shipping Address: 3M Bldg 2-3E09 Telephone: Sample Recelvlng: (651) 7784948 BACK TO MAIN 1 7133 Chain of Custody/Reque,,,,>r LaboratoryAnalytical . - Project IDlProject Name 023-077 mL,I.+& Template # 935 Bush Avenue SI Paul, MN 55106 Alternate: (651) 778-6753 FAX: (651) 778-6176 Project Lead )L,,-&~Q Dept. # (main) I 124/ Internal Due Date ClasslJoblProject # (9QlQs3sm 3 Contact Name &+3 Company 3;w\' Date Available - Po kqL m331 Date Due 3M Env -I Project # For I n t e t d Use Only ,pedalInstructions andlor Specific Regulaloiy Requlrements: nethod. limit of detedion. repoiling units. etc ) GLU-014 ua3c03 '30ft- 541 b L i q J'L Item # Client Sample identification 1. __ - 2. - 3. - 4. - 5. - 6. - 7. - 8. - 3. - 10. FAX# /&TI) Contract Lab I Preservatives: && LIMW Time Sampled Sampled Matrix/ . od Analysis Requested: Complete below. Attach any associated Information. SamDle Condition UDon Receipt: e Acceptable 0 Other: Shippinu Address: 3M Bldg 2-3E09 .. Telephone: Sample Rccslvlng: (651) 7784948 - Company 3m A P)' 3 #,- E MailingAddress g city, State, ZIP Telepho:<:n,,e,#,f, - (QOlri peclal Inslrucllons rndlor Specific Regulatory Requlremenls: nelhod. limilof deledim. reportingunils. eIc ) DlProject Name f)a2,-cQ7 ' m ~ FAX# (bg)ixc bl7b BACK TO MAIN 9-5 J Date Available Date Due Contract Lab II I Analysis Requested: Item ~~ ~ # Client Sample Identification 3M LIMS# Date Sampled Time Matrix/ E Media 7. 8. 3. IO. Collected by (print): A ] 8 I' 3 \I Relinquished bylAffiliation .-C I U c m I 0 I SamDle Condition UDon Receipt: 0 Acceptable 0 Other: c I I ~~ I I -57 Date I I I Page I Original- Accompanying Sampler I Lasl Page - Origmalor See Reverse Side for lnslruclions