Document NRax1y2ybEzKDrGXE37ajExw

/W .S i6-067S Centre Analytical Laboratories, Inc 3 04 8 Research Drive Phone: (814) 231-8032 State C ollege, PA 16801 Fax: (814) 231-1253 or (814) 231-1580 Analytical Report Fluorocheraicai Characterization of Surface Water Samples Port St. Lucie, FI (W2363) Centre Analytical Laboratory Report No. 023-014F 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 1 0 F 5 000986 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 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/M S/M S) was requested for all samples. A total of 8 samples were received for analysis. The samples were prepared and analyzed by LC/M S/M S for the following list of fluorochemicals: Table 1: Target Analysis ComDound Nam e Perfluorooctane Sulfonate -Perfluorooctane Sulfonvlamide Perfiuorooctanoate 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. Eight individual sample containers were received. Samples were received on 05/03/00. T h e sample collection dates were not supplied. Chain-of-custody information is presented in Attachment A . 3 Holding Times The analytical method used was validated against a maximum holding time o f 14 days. T h e stability of the analytes o f interest for longer periods has not been determined. PAGE 2 OF 5 0009S7 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sam ple Preparation fo r LC /M S/M S A nalysis 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/M S analysis. A forty-milliliter portion of sample was transferred to a C 18 SPE cartridge. The cartridge was first eluted with 5 m L of 40% methanol in w ater 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 /M S/M S. This treatm ent resulted in an eight-fold concentration of the samples prior to analysis. 4.1.2 Sam ple Analysis by LC /M S/M S 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 am ount of time. Following HPLC separation, ES/M S provides a rapid and accurate m eans 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-Packard H P1100 HPLC system coupled to a Micromass Ultima M S/M S was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM ). Samples were extracted on 5/19/00 and analyzed by M S/M S between 5/22/00 and 5/23/00. An initial analysis was performed on 5/21/00, however, the data was rejected because of unacceptable standard curves. The data is included in Attachment D for informational purposes only. The HPLC and M S/M S 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 o f 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) w ere determ ined. A calibration ' curve is acceptable if r > 0 .9 8 5 (r2 > 0.970). Calibration standards are prepared using the sam e SPE procedure used for samples. Calibration check standards were analyzed periodically (every three to five sam ple injections) throughout the analysis sequence. Com pliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. For the results reported here, calibration criteria were met. PACE3 O f 5 0009S8 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/M S/M S 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 C. Sam ple M C-684H had PFO S at levels significantly greater than 10 times the spiking level, therefore accurate matrix spike recoveries could not be determined. All other compounds in all samples showed matrix spike recoveries between 70-130% . . Field spikes were also prepared on sample M C-601H for all compounds at a concentration of 100 ng/L using all compounds of interest. Field spike recoveries are also given in Attachment C. All compounds showed recoveries between 70-130% in the field spikes. 5.5 Duplicates All field samples (excluding blanks) 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 ail compound of interest at 25 and 250 ng/L. PFO S showed a recovery of 133% in the 25 ng/L spike. All recoveries for all other compounds were between 70-130% in each LCS. Results are given along 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 sam e m anner as the other samples. The field blank for this sample did show PFO S above the reporting lim it 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 m edia and hard copy reports are stored in data folders maintained by Centre. PAGE 4 OF 5 000959 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/M S/M S Raw Analytical Data 9 Signatures aLnj fLlLz ^ /J o h n M. Raherty,/M anager- Operations M anager D a te Kevin J Uoyd, Vice President D a te Other Lab Mem bers Contributing to Data Enaksha Wickremesinhe Karen Smith David Bell Tiffany Proctor PAGE 5 OF 5 000930 ANALYTICAL REPORT Centre Analytical Inc. 3048 Research Drive, State Cotiege PA 16801 814-231-8032 FAX 814-231-1253 Analytical Results W2363 Port St. Lucie, FI 3M Sample Identification Sample Description PFOS (ng/L) MC-601H MC-603H MC-606H NA MC-607H NA MC-608H MC-684H NA Site 1 Surface Water Site 1 Surface Water Duplicate Site 2 Surface Water Site 2 Surface Water (Duplicate Site 3 Surface-Weter Site 3 Surface Water Duplicate Field Blank-P/N Empty Quiet Surface Water Quiet Surface Water Duplicate <25 <25 138 137 18.8 J 23.2 J 43.1 45300 51100 J - Compound is present, but below the reporting limit of 25 ng/L. The result is an estimated value. Method Detection Limits are approximately 2.5 ng/L for PFOS and PFOSA and 7.5 ng/L for POAA. PFOSA (ng/L) <25 <25 <25 <25 < 25 <25 <25 83.6 95.2 POAA (n <25 < 25 18.4 J 18.8 J <25 <25 <25 737 760 Please refer to he reverse side for our standard terme and conditions. 000991