Document NNN5zrpGvdpoELKekmQ1m3rz8

C e n tre A n a ly tic a l L a b o ra to rie s , Inc. 3048 Research Drive Phone: (814) 231-8032 State College, PA 16801 Fax: (814) 231-1253 or (814) 231-1580 f - 7" Analytical Report Fluorochemical Characterization of Drinking Water Samples Mobile, Alabama (W2151) Centre Analytical Laboratory Report No. 023-007C 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 Kris J. Hansen, Ph.D. 3M Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 10FS 000346 1 Introduction Results are reported for the analysis of a series o f drinking water samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M Environmental Laboratory. The samples were collected from Mobile, Alabama. The Centre study number assigned to the project is 023-007. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 16 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 Acronym PFOS PFOSA POAA I Data generated in support of this study was generated according to USEPA Good Laboratory Practices (GLPs). 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 I time. I 2 Sample Receipt The samples were submitted in individual plastic containers and were not preserved. Sixteen I individual sample containers were received. Samples were received on 02/15/00. The sample collection dates were not supplied. Chain-of-custody information is presented in Attachment A. I 3 Holding Times The analytical method used was validated against a maximum holding time of 14 days. The I stability of the analytes of interest for longer periods has not been determined. I I I 8 C00347 PAGE 2 OPS 8 B 4 Methods - Analytical and Preparatory I 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/WIS/MS Analysis I 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 I LC/MS/MS analysis. A forty-milliliter portion of sample was transferred to a C18 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 I 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 I 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 I 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 I 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 1 (SRM). Samples were extracted on 2/23/00 and analyzed by MS/MS between 2/23/00 and 2/24/00. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in attachment D. a 5 Analysis a 5.1 Calibration a 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 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient o f determination (r2) were determined. A calibration curve is acceptable i f 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. PAGE3 OF5 cooaas 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 ng/L using all compounds of interest. Matrix spike recoveries are given in Attachment C. 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 C. 5.5 Duplicates All samples were analyzed in duplicate. Results are given along with the sample results in Attachment B. 5.6 Laboratory Control Samples Milliq water was spiked with all compound of interest at 25 and 250 ng/L. Initial analysis of the 25 ng/L LCS showed low recovery for PFOS. The standard was reinjected and was found to have acceptable recovery (70-130%). All other recoveries for all compounds were between 70130% 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 Data Summary Please see Attachment B for a detailed listing of the analytical results. 7 Data/Sample 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. PAGE4 OF5 000349 8 Attachments 8.1 Attachment A: Chain-of-Custody 8.2 Attachment B: Results. 8.3 Attachment C: Matrix Spike Recoveries (Field and Laboratory Spikes) 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith PAGE 5 OF5 G00350 aa aaaaaaaaaaaaaaa 3SV3 Envii .mental Laboratory form 38778 - PWO Shipping Address: 3M Bldg 2-3E-09 935 Bush Avenue St. Paul. MN 55106 Telephone: Sample Receiving: (651) 778-494 Alternate: (651) 778-6753 FAX: (651) 778-6176 Chain of Custody /Reque. jr Laboratory Analytical 17129 Project ID/Project Name C & 3 - O D 7 Template # Project Lead & 7 S DepL#(main) L L 3 ll A W H i fin ta l T / l M D k a U / [ c{ U M jU v A v i L f ^ i* - , ' Final Report Due Dat \J Internai Due Date Class/Job/Project # Q O i O S ^ ^ o D6 ! 3M Env ) Project # For Inter, ml Use Only Report Results to: Contact Name ^ Company s$y/\ Date Available Mailing Address U i ' U j / t o ' J3-SS .-< 9 9 POAtHi City. Stale. Zip Qau fan K S IA3 ....................... Telephone # L s ~ f) '7~fy~laPi &__________________ Special Instructions and/or Specific Regulatory Requirements: (method, limit of detection, repotting units, etc.) FM* { ( S l i m * - b i l l * __________ '_______ ` Date Due Contract Lab 1 JU r L A nalysis Requested: QM - o ik W AIT I y / lo b lU ,1 h i - Hem # Client Sample Identification Preservatives: n oz X oiXNn O zoco> k. oJZ 3M Date Time Matrix/ LIMS# Sampled Sampled Media Enter the number of containers of each Total Number of Containers Complete below. Attach any associated Information. (Enter an X In th box below to indicate reauasl) 1. me - M a v U - S t s 1 P 2. yy\ l - 4 3 ^ / 1 - s i t e ) - y f c l / S p t a -$\JO 3. m c^ZOl) - S ',te \~ t d b - S p il e -9/0 AAA UM jtf j ,r / 9 \t l 4. l y x t ' M 3)) H - S - b - P / / / 1 5. m t - H W A S M ________________ ___ \z _ / > 6. - - - - - -7. m l-4 3 3 ---------- - 4 --P id ^^L J iiS ^ -Pl/i>.-..-..-..-..-..-.... _ ... \ J. \ y 8. 9. 10. - - - - - - --- -- - - - - ---- - // z >_ ll Collected by (print): Collector's signature: Item # Relinquished by/Affiliation - ' i -. 1 ` -..Timeiji , ' Dt Shipped Via: Received' by/Affiliation Time Date l~ U ? i i l l u . \j} .u n J L s -- z Jm / d d -" /O JO .- l i '-CZP Chain of Custod Sample Condition Upon Receipt: 0 Acceptable 0 Other: Temperature: 'C Received on Ice O ther Associated CoCs: O l '2.D( |" 7 l Z l , | H U i , l*T 1 1"S, rj'ZS Copies to: 7 ^ -*. n n h >7150. n w , n i 3 3 , n i m K X /J . / A C f Comments: _______________________ Centre Analytical 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 Analytical Results W2151 Mobile, Alabama 3M Sample Identification MC-415H MC-417H MC-420H MC-421H MC-423H MC-426H MC-428H MC-431H NA MC-432H NA MC-433H Sample Description Intake-P/N Intake-P/N duplicate Intake-Field Blank Empty Outflow-P/N Outfiow-P/N duplicate Site 1 P/N Site 1 P/N duplicate Site 2 P/N Site 2 P/N duplicate Site 3 P/N Site 3 P/N duplicate Field Blank-P/N Empty PFOS (ng/L) <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 PFOSA (ng/L) <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 POAA (ng/L) <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 <25 C00353 Piease refer to the reverse side fo r o ur standard terms and conditions.