Document ka4OBrwk2kQvjao2Dyyg4OOLb

BACK TO MAIN Centre Analytical Laboratories, Inc. 3048 Research Drive State C a ? g e ,PA 16801 www.centrelab.com (814)231-8032 Fax: (814)231-1253or (814)231-1580 Analytical Report Fluorochemical Characterizationof Surface Water Samples Decatur, Alabama (W1979) Centre Analytical Laboratory Report No. 023-014 8 (Revision 1) Revision Date 3/21/01 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 Kris J. Hansen, Ph.D. 3M Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 1 OF 5 BACK TO MAIN 1 Introduction Results are reported for the analysis of a series of surface water samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M EnvironmentalLaboratory. The samples were collectedfrom Decatur, Alabama. The Centrestudy 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 9 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: I Table 1:Target Analysis ComDoundName Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate ;1;E 1 The analytical method used was validated by Centre. The validation protocol and results are on file with Centre. 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. Nine individual sample containers were received. Sample hAC-202H was not analyzed as per client request. (E-mail communication from Kris Hansen on 5/16/00). Samples were received on 05/03/00. The sample collection dates were not supplied. 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. 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 ngR for periods longer than 14 days. PAGE 2 OF 5 BACK TO MAIN 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparationfor LC/MS/MS Analysis Samples were initially treated with 200 ULof 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-milliliterportion of sample was transferredto a C18SPE cartridge. The cartridge was first eluted with 5 mL of 40% methariol 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 concentrationof the samples prior to analysis. 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-PackardHPl1 00 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 on 5/16/00and analyzed by MS/MS between 5/19/00and 5/20/00. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in attachment D. 5 Analysis 5.1 Calibration A -/-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) The response of the quantita1:ion 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 (?) 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. PAGE3OF5 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-levelcalibrationstandard. 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 sa,mples. 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 compliiant. 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 field sample (excluding blanks) at a concentration of 100 ng/L using all compounds of interest. Matrix spike recoveries are given in Attachment 6. All laboratory matrix spikes showed recoveries of all compounds between70-130% Field spikes were prepared on sample MC-201H at a concentration of 100 ng/L using all compounds of interest. The field spike is identified as FdC-204H. Field spike recoveries are also given in Attachment B. PFOS showed high recovery in the field spike. All other compounds showed recoveries between 70-130%. 5.5 Duplicates All field samples (excluding blanks) 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 ;!5 and 250 ngR. All recoveries for all compounds were between 70-130% in each LCS. Recoveries are given with the raw data in Attachment D. 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 Data Summary 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 i:;sued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Centre. PAGE4OF5 BACK TO MAIN 8 Attachments 8.1 Attachment A: Results 8.2 Attachment 6:Matrix Spike Recoveries(Fieldand Laboratory Spikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures . 6 Kevin J Lloyd, Vice President Other Lab Members Contributingto Data Enaksha Wickremesinhe Karen Smith David Bell 27 mMw I Date PAGE 5 OF5 \ 4 laboratories,,Inc. CEntre Analytical 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN ,Analytical Results W1979 Decatur, Alabama :3MSample Identification MC-201H MC-203H MC-206H NA MC-207H NA MC-208H MC-284H NA Sample Description Site 1 P/N Surface Water Site 1 PIN Surface Water Duplicate Site 2 P/N Surface Water Site 2 P/N Surface Water Duplicate Site 3 P/N Surface Water Site 3 PIN Surface Water Duplicate Field Blank P/N Empty Quiet P/N Surface Water Quiet PIN Surface Water Duplicate PFOS (ng/L.) NQ NQ NQ NQ ND ND ND 108 114 PFOSA (ng/L) ND ND ND ND ND ND ND NQ NQ 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 e LOD c NQ e LOQ POAA (ng/L) NQ ND ND NQ ND ND ND 63.1 57.3 - 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-205H !Spiked Amount (ng/L): I 100 1 PFOS PFOSA Sample Concentration (ng/L) 23.1 0 9.2 Matrix Spike Result (nQ/L) 128 107 106 Lower Recovery Limit: I 70 1 Upper Recovery Limit: I 130 Matrix Spike Result (% Recovery) 104.9 107.0 96.8 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. Also note that sample MC205-H is a laboratory spike of sample MC-201H BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I MC-206H Spiked Amount (ng/L): I 100 1 Lower Recovery Limit: IJpper Recovery Limit: Sample Concentration 14.5 0 0 I 70 I 130 Matrix Spike Result (ng/L) 117 103 113 I Matrix Spike Result I:% Recovery) 102.5 103.0 1 13.0 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 I)elow 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 Spiked Amount (ng/L): I MC-207H 100 Lower Recovery Limit: lJpper Recovery Limit: Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 100 101 105 I 70 1 130 I Matrix Spike Result ([% Recovery) 100.0 101.o 105.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Rlecovery !Sample ID: I !Spiked Amount (ng/L): I MC-284H 100 Lower Recovery Limit: IJpper Recovery Limit: . Sample Concentration (ng/L) 108 18.9 63.1 I 70 1 130 Matrix Spike Result (ng/L) 200 110 161 Matrix Spike Result (% Recovery) 92.0 91.1 97.9 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: 1 MC-204H I !SpikedAmount (ng/L): I 100 I [ E A POAA Sample Concentration (ng/L) 23.1 0 9.2 Matrix Spike Result (ng/L) 169 85.6 111 Matrix Spike Result -(% Recovery) 145.9 85.6 101.8 Criteria (Pass / Fail) FAIL PASS PASS 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. Also note that sample MC-204H is a field spike of sample MC-201ti 3M Environmental Laboratory FM 38776 - PWO Shlpplna Addrass: 3 M B 4 2-3509 935BushAvenue it. Paul. MN 55106 T:!:;hs.?o: Sample Recolving: (651)n 8 4 w Alternate: (651)7786751 F A X (651)7786176 BACK TO MAIN Chain of Custody /Request for Laboratory Analytical - -IProject ID-lP~roject Name &EA)0\4/11b, b1(% Template # Project Lead -4 e Dept. # (main) 42Q\ ur?Afifi&h~+ ",- Final Report Due Date Internal Due Date ClasslJoblProject # 001 1 4266 3M Env. Lab Project # For Internal Use Only - -. Analysis Requested: Original - Acmmpanyhg Samples Last Page - Originator See Reverse Side for lnstruclions