Document ByM1V7ewgNrYQLN880yKy4J3w

BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Study Title Hydrolysis Reactions of Perfluorooctanesulfonamide (FOSA) Data RequirementBased on OPPTS: 835.2110 Author Thomas L. Hatfield, Ph.D. Study Completion Date April 3, 2001 Performing Laboratory 3M Environmental Laboratory Building 2-3E-09, 935 Bush Avenue St. Paul, MN 55106 Project Identification 3M Laboratory Report No: EL1132 Total Number of Pages 126 Page 1 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 This page has been reserved for specific country requirements. Page 2 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Statement of Non-Compliance Study Title: Hydrolysis Reactions of Perfluorooctanesulfonamide (FOSA) Study Identification Number: EL1132 This study does not fully comply with the requirements of the US EPA Good Laboratory Practices (GLP) Standards at 40 CFR Part 792 (TSCA). However, many GLP standards were used in the development of the analytical method (Appendix A), and the quality assurance procedures followed in this study were based on the practices described in the GLP documentation. Sponsor Representative Date Page 3 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL.1132 Quality Assurance Statement Study Title: Hydrolysis Reactions of Perfluorooctanesulfonamide (FOSA) Study Identification Number: EL1132 The following table provides details of the audits performed by the 3M Environmental Laboratory Quality Assurance Unit (QAU). Inspection Dates 3/20-21/01 3/27/01 Phase Report Tables Report Date Re ported to M anagem ent Study Director 3/21/01 3/21/01 3/27/01 3/27/01 QAU Representative BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Table of Contents Statement of Non-Compliance..............................................................................................3 Quality Assurance Statement................................................................................................4 List of Tables.......................................................................................................................... 6 List of Figures......................................................................................................................... 6 Study Personnel and Contributors.........................................................................................7 Location of Archives............................................................................................................... 7 Summary................................................................................................ 8 Introduction...........................................................................................................................10 Summary of Kinetics Model................................................................................................. 11 Materials and Methods......................................................................................................... 13 Chemical Characterizations............................................................................................13 Sample Preparation........................................................................................................ 13 Sample Analysis.............................................................................................................. 14 Deviations........................................................................................................................ 14 Results and Discussion....................................................................................................... 15 Data Quality Objectives (DQO's)....................................................................................15 Anomalous Analytical Results.........................................................................................15 Statistical Methods and Calculations............................................................................. 16 Data Summary and Discussion.......................................................................................16 Conclusions.......................................................................................................................... 21 References........................................................................................................................... 22 Signatures............................................................................................................................ 23 Appendix A: Analytical Method........................................................................................... 24 Appendix B: Kinetics Model.................................................................................................43 Appendix C: Selected Analytical and Kinetics Results........................................................... 54 Appendix D: Selected Chromatograms.............................................................................. 66 Page 5 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 List of Tables Table 1. Summary of Results Based on FOSA Concentrations.........................................8 Table 2. Summary of Results Based on PFOS Limit of Quantification............................. 8 Table 3. Summary of Results Based on the Estimated PFOS Limit of Detection.............9 Table 4. Summary of Results Based on the Mean and Precision of FOSA M easurem ents........................................................................................................ 9 Table 5. Characterizations of Test and Reference Substances...................................... 13 Table 6. Observed (50 C) Degradation Slopes for FOSA in Aqueous Buffered Solutions and at Various pH Levels..................................................................................... 16 Table 7. Degradation Rate Constant of FOSA in Aqueous Buffered Solutions Using Data Pooled Over pH Levels..................................... ..........................................17 Table 8. Degradation Rate and Half Life of FOSA in Aqueous Buffered Solutions Based on PFOS Limit of Quantification.......................................................................... 19 Table 9. Degradation Rate and Half Life of FOSA in Aqueous Buffered Solutions Based on the Estimated PFOS Limit of Detection..........................................................20 Table 10. Degradation Rate and Half Life of FOSA in Aqueous Buffered Solutions Based on the Concentration Mean and Standard Deviation..............................20 List of Figures Figure 1. Structures of FOSA and the Potassium Salt of PFOS..................................... 10 Figure 2. Observed FOSA Degradation for Various pH levels........................................ 17 Figure 3. Pooled FOSA Data and Slope Regression....................................................... 18 Page 6 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Study Personnel and Contributors Study Director Sponsor Thomas L. Hatfield, Ph.D. 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 (651) 778-7863 3M Corporation 3M Environmental Laboratory and Professional Services Contributing Personnel Kuruppu Dharmasiri, Ph.D Mark T. McCann Anthony E. Scales Joseph J. S. Tokos, Ph.D (Pace Analytical Services, Inc., 1700 Elm St., Minneapolis, MN 55144) Gregory Maisel Jill Maloney (Braun Intertec Corporation, 6875 Washington Ave. South, Minneapolis, MN 55439) Grant M. Plummer, Ph.D. (Rho Squared, P.O. Box 61536, Durham, NC 27715) Location of Archives The 3M Environmental Laboratory will retain the original data documents and digital copies of the original data related to this work for at least 10 years following the effective date of any related final ruling. Information may obtained through written inquiry addressed as follows: 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Page 7 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Summary We report here the results of our study of the hydrolysis of Perfluorooctanesulfonamide (hereafter, FOSA). Our methods are described below and in Appendix A to this work; our results are based on the observed concentrations of FOSA and perfluorooctane sulfonate (PFOS) in buffered aqueous solutions as a function of time. The chosen analytical technique was high performance liquid chromatography with mass spectrometry detection (HPLC/MS). Tables 1 and 2 summarize the results of the study. During this study, we prepared and examined samples at six different pH levels from 1.5 to 11.0 over a period of 42 days. The slopes of the log-concentration ratios, calculated from observations of the FOSA concentrations pooled over the six observed pH levels, are presented in Table 1. Table 1. Summary of Results Based on FOSA Concentrations. Calculated slope (d a y 1) -4.4 x 10'b Calculated slope upper limit (2a) ( d a y '1) 8.6 x 10'4 Calculated slope lower lim it (2a) ( d a y '1) -8.7 x 10'4 We also monitored the concentration of one of the potential hydrolysis products (perfluorooctane sulfonate, PFOS), but never observed this compound at levels above its limit of quantification (LOQ, equal to 52 ng/mL). Assuming PFOS to be the only hydrolysis product of FOSA, this LOQ provides a second estimate of the minimum FOSA half-life, presented in Table 2. T ab le 2. S u m m ary o f R esults B ased on PFO S Limit of Quantification M axim um Possible Rate at 50 C (d a y 1) 2.3 xKT5 M aximum C a lc u la te d Rate at 25 C (d a y 1) 2.3x1 O'4 Calculated Half Life at 25 C (years) >8.3 Page 8 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 We also failed to detect PFOS above Its limit of detection (LOD, with a value estimated to be below 13.0 ng/ml). This LOD value also provides an estimate of the minimum FOSA half-life, presented in Table 3. Table 3. Summary of Results Based on the Estimated PFOS Limit of Detection M axim um Possible Rate at 50 C (d a y 1) 5.7 x1(T M axim um Calculated Rate at 25 C (d a y 1) 5.7 x10a Calculated Half Life at 25 C (years) >33 According to the data available from this study, the half-life estimates of Tables 2 and 3 represent the minimum possible half-life of the compound FOSA under the assumption that it hydrolyzes to form only the compound PFOS. A third half-life estimate (see Equations B 36 and B37) is available from the mean p and standard deviation o of the observed FOSA concentrations, assuming that they were essentially constant over the experimental portion of the study. This estimate is ln(2) _ n A tln (2 ) l * (t ' L = (kp)max 2a Eq. 3 where A t represents the sample incubation period. Table 4 presents the results of the calculation. Table 4. Summary of Results Based on the Mean and Precision of FOSA Measurements Maxim um Possible Rate at 50 C (d a y 1) 1.80 x 10-3 Maxim um C a lc u la te d Rate at 25 C (d a y 1) 1.80 x 10-4 C a lc u la te d Half Life at 25 C (years) > 11 Page 9 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 introduction Three primary chemical routes of environmental degradation are hydrolysis, photolysis, and biodegradation. Studies of these routes provide information on the environmental persistence of both the "parent" compounds and their reaction products, and are ideally carried out over the range of chemical conditions pertinent to both environmental and metabolic processes. The hydrolysis of FOSA (or, more generally, its degradation in the presence of FfeO) is addressed in this report. Structures of the "parent" compound FOSA and the potassium salt of its potential hydrolysis product PFOS are illustrated in Figure 1. Figure 1. Structures of FOSA and the Potassium Salt of PFOS FOSA Potassium Salt of PFOS FFFFFFFFO FFFFFFFFO Page 10 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Summary of Kinetics Model A full mathematical description of the kinetics model employed in this study Is presented in Appendix B. The study data allow two independent estimates of the hydrolytic half-life of FOSA. The first estimate (see Table 1) is based on the observed degradation of the "parent" compound FOSA in dilute, appropriately buffered aqueous solutions. Equation 1 describes the estimated half-life ( f ^ ) in terms of the estimated total parent hydrolysis rate k p (see Appendix B, Equation B10): Eq. 1 We determined the quantity k pfrom the experimental data as described in Appendix B. The data corresponding to "Day 0" (t = 0) were used to determine the relative concentration ratios (see Equations B8 and B9). The measured concentrations of the potential hydrolysis product PFOS (also obtained during the experiments described here) provide a second estimate (see Table 2) of the parent half-life. During the course of this study, we did not detect PFOS above its limit of quantitation (LOQ), and related studies1show that PFOS Is Itself hydrolytically stable. Assuming also that PFOS Is the only hydrolytic product of the parent compound FOSA, these PFOS analyses provide the following estimate (t ^ ) of the minimum FOSA half life (see Appendix B, Equations B32 and B33): Eq. 2 where [P0]= the initial FOSA molar concentration, A t = the time interval over which the study was conducted (42 days), and A pfos = the molar limit of quantitation for the compound PFOS. Equation 2 implies that when the experimental data provide an estimate of the instrumental limit of detection (LOD) for the compound PFOS ( A poS ), a third estimate (T ^p)3 f the Parent half-life is available. This estimate (Equation 3) is identical to that described in Equation 2, with the substitution A poS= A poS (see Appendix B, Equations B38 and B39): Page 11 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 A t [P0] ln(2) A LOD PFOS Eq. 3 All the samples used In this study were maintained at a reaction temperature of 50 C. The quoted results, valid for the reaction temperature of 25 C, were approximated from our experimental results according to methods described in Appendix B (Eq. B40 and B41). Page 12 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Materials and Methods Details of the characteristics of the test materials, sample preparation techniques, and analytical methods are presented in Appendix A (ETS-8-210.0, "Preparation of FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by High Performance Liquid Chromatography with Mass Spectrometry Detection.") A summary of these items is provided below, as well as a description the known deviations from the procedures of Appendix A. 3M prepared and analyzed the samples included in this study between March 13 and October 5, 1999. Chem ical Characterizations Table 5 describes the sources and properties of the materials used in this work. These materials were used to prepare both the samples and the quantitative standards used to quantify them. For this reason, and because Equations 3 and 6 involve only ratios of the parent and product concentrations, the resulting rate and half-life estimates are largely independent of the material purity levels. Table 5. Characterizations of Test and Reference Substances Source Chemical Lot Number Physical Description Molecular Weight (gm mole'1) FOSA 3M Specialty Chemicals TNA-1886 Off-white waxy solid 499 Potassium Salt of PFOS 3M Specialty Chemicals TNA-0844 Light colored powder FBSAa 3M Specialty Chemicals NB 107715-87 TCR-99030-026 White powder 538 299 Aperfluorobutanesulfonamlde Sam ple Preparation W e prepared four 1.0-mL aqueous buffer samples (a sample, a duplicate, a triplicate, and a "matrix spike") at each of six pH levels (1.5, 3, 5, 7, 9 and 11) for analysis at seven time intervals (0, 7,14, 21,28, 35, and 42 days). Buffered solutions containing 499 ng/mL of the analyte FOSA and 225 ng/mL of perfluorobutanesulfonamide (FBSA), the latter serving as the internal standard for the compounds FOSA and PFOS, formed the basis of all these samples. The chosen buffer solutions are described fully in Appendix A. All the samples were prepared simultaneously, and all but the "Day 0" samples were placed in an orbital incubator/shaker maintained at 50 ( 3) C. After at least three minutes of agitation, the "Day 0" samples were spiked (as required) with the FOSA solution, diluted 10:1 with methanol containing the internal standard PFBS, and refrigerated. After the appropriate incubation times, subsets of the sample vials were removed from the incubator and then spiked, diluted, and stored as described Page 13 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 immediately above. Except during the relatively short periods of time required to prepare them, the samples were shielded from light. Five calibration standards containing FOSA (50 to 998 ng/ml) and six standards containing PFOS (13.0 to 1037 ng/ml) served as the fundamental quantitative basis of the study. All other calibration standards were prepared from these fundamental standards, at the appropriate pH levels, using the buffer solutions described above. Sam ple Analysis The equipment we used for the HPLC/ITMS analysis was a Hewlett Packard model 1100 equipped with a Dionex lonPac NG-1 HPLC column (aqueous ammonium acetate/methanol solvent gradient) and an ALS Model G1322A degassing module. An ALS Model G1315A column heater maintained the column temperature at 40 C, a quaternary pump supplied a column flow rate of 0.3 mL/min, and an ALS Model G1313A auto-sampler provided 5 p.L sample injections. The detector was a Hewlett Packard MSD mass spectrometer, operated in negative-mode electrospray ionization mode; anions of the acetate adduct of FOSA, PFOS, and FBSAwere detected at the charge-to mass ratios 498, 499, and 298, respectively. We processed the resulting data using the computer program HP ChemStation forLC (Rev.A.06.0). Further analytical details, including the gradient elution program, instrument and detector parameters, and performance specifications, are presented in Appendix A. Deviations We failed to spike one blank sample at each of the pH levels 3.0, 5.0, 7.0, and 9.0. In each case, the results of additional blank samples performed immediately before the actual sample analyses indicate that the reported data meet the pertinent data quality objectives (see below). Through either human or mechanical error, samples 80399PFOSA-094 through 096 (pH 11.0, "Day 21") were not analyzed, and they have been excluded from the following discussion. Page 14 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Results and Discussion Data Quality Objectives (BOO'S) Below is a brief description of the data quality objectives applied in this study. A full description is presented in Appendix A. With the exceptions of the anomalous results noted below, all the DQO's were met. Appendix C presents the results for each sample set, organized by pH level. Calibrations. The minimum acceptable coefficient of determination (r2) for linear fits to calibration data is 0.990. The acceptance criterion for individual calibration points is that their values fall within 25% of the linear fit value; data outside this range are excluded and the linear fit is recalculated. No more than two points may be rejected from a calibration data set. Data for the high or low calibration standards may be rejected, though this results in a smaller effective calibration range. Continuing Calibration Verification (CCV). Identical calibration samples are examined at the beginning and end of each sample run. Results of the second calibration run may not deviate by more than 25% of the first run for any analyte. The average results of the calibration runs are used to calculate the analyte concentrations. Matrix Spikes. The acceptable percent spike recovery range is 75% to 125%. Analyte specificity is demonstrated by acceptable analyte spike recoveries. Sample Duplicates. Duplicate pairs with relative percent deviation (RSD) greater than 25% may be accepted at the analyst's discretion, but must be noted. Solvent Blanks. Concentration results for solvent blanks may exceed neither 5% of the highest calibration standard nor 25% of the lowest calibration level. System Suitability. Suitability was demonstrated by either an abbreviated mass-tocharge (m/z) check-tune or performance of a full auto-tune routine. Anomalous Analytical Results Calibrations. The PFOS calibration standards at 13.0 ng/ml failed to meet the relevant DQO, so we calculated all the reported concentrations according to the calibration results for the PFOS standard at 52 ng/ml. However, the responses to the 13.0 ng/ml were all non-zero, and were quite consistent, so the instrumental limit of detection (LOD) was clearly below this value. This fact is employed below in the "Data Summary and Discussion" section. Spike Recoveries. As discussed above, the samples 80399PFOSA-094 through 096 failed to meet the related DQO, so we have excluded the "Day 21" data for pH= 11. Other Detected Peaks: Some pH = 9.0 data indicate the presence of peaks at the value m/z = 616, corresponding to the compound 2-(/V-ethylperfluorooctanesulfonamido). No explanation for the appearance of these peaks is apparent. In addition, a very consistent response was noted at m/Z = 499 in all the standards and samples. This response is possibly due to various 13C forms of FOSA. Because the response is consistent, it does not compromise the reported results for the dominant 12C FOSA isotopomer at m/z = 498. Page 15 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 S tatistical Methods and Calculations Using functions provided in Microsoft Excel software, we calculated means, standard deviations, and first-order rate constants (see Appendix B, Equation B8) for various subsets of the acquired data. Our linear regressions included the determination of constant terms, that is, the regression fits were not forced to pass through the origin. As described in Appendix B (Equations B40 and B41), rates measured at 50C were extrapolated to 25C by dividing by a factor of 10; this approximation is valid for reactions with Arrhenius heats of activation near 18 Kcal/mole.2 Data Summary and Discussion The LOQ is defined as the concentration of the lowest (accepted) standard in the calibration set for which the known concentration exceeds 400% of the indicated solvent blank level (see Appendix A). During this study, the LOQ's for FOSA and PFOS were 50 ng/mL and 52 ng/mL, respectively. Results for the internal standard compound (PFBS) were reasonably consistent throughout the study. The percent relative standard deviations of the measured values, calculated for each pH level, ranged from 1.8% to 17%. Table 6 presents the results of the slope determinations (see Appendix B, Equation B8) at six pH levels and 50C. Table 6. Observed (50 C) Degradation Slopes for FOSA in Aqueous Buffered Solutions and at Various pH Levels. PH O b served Slope (d a y 1) Percent (2o) Slope U n certain ty (day1) 1.5 -0.0013 3.0 -0.0009 5.0 -0.0003 7.0 +0.0001 9.0 +0.0012 11 +0.0011 98 261 622 1145 71 115 These slopes are generally only poorly determined; their percent relative 2a (95% confidence) uncertainties range from 71% to 1145%. The data do not indicate any degradation of FOSA. A regression of the slopes vs. pH yields a line with welldetermined slope; however, considering the near-zero values of the slopes, their generally large uncertainties, and the lack of physical meaning of the positive slopes, this trend is not meaningful. We conclude that the data indicate no relationship between the degradation of FOSA and the sample pH level. Page 16 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 In the absence of a clear relationship between the FOSA degradation rate and the sample pH, it is appropriate to "pool" the data over pH level and determine the degradation rate using the entire data set. Figure 3 illustrates the results of this pooled analysis according to Equation 1, and Table 7 summarizes the results of the analysis. Table 7. Degradation Rate Constant of FOSA in Aqueous Buffered Solutions Using Data Pooled Over pH Levels. Observed Rate Constant at 50 C ( d a y '1) 4.43 x 10'B Percent (2a) Rate Constant Uncertainty at 50 C (d a y 1) 19000 The uncertainty in the rate constant presented in Table 7, which is based on direct observations of the compound's concentration in aqueous solution, indicates that FOSA is hydrolytically stable to within the experimental limitations of this study. Figure 2. Observed FOSA Degradation for Various pH levels. Page 17 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Figure 3. Pooled FOSA Data and Slope Regression. 0.07 0.02 O ' ' "i " O r> 1 1 o1 o -* o ~oQ. -0.03 * * L - -0.08 8o ` ~ " O - - _o Solid Line: o. 1 1 O' y = -4.425E-06x - 1.997E-02 -0.13 R2= 2.751E-06 Dashed Lines: 2a Uncertainties o (slope and intercept) -0.18 ----------- 0 10 20 30 time (days) O8 .Q - m m 0 o o 0o . _o -- -----------------40 50 We also monitored the concentration of the potential hydrolysis product (PFOS), but never observed this compound at levels above its limit of quantification (LOQ, equal to 52 ng/mL). The initial FOSA concentration (499 ng/ml) and the PFOS LOQ provide an estimate of the FOSA half-life (see in Appendix B, Equations B32 and B33). The maximum degradation rate is given by Equation 3: kP (kp L m=l and the minimum half-life is given by Equation 4 A t [P0]ln(2) A^PLFOOQS Eq.3 Eq.4 Page 18 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 We note that in both Equations 3 and 4, the initial FOSA concentration (P0) and the PFOS LOQ ( ApoS) are molar quantities. Table 8 presents the results of the related calculations. Table 8. Degradation Rate and Half Life of FOSA in Aqueous Buffered Solutions Based on PFOS Limit of Quantification At (days) 42 [Pc] (nm/ml) 1.0 a l q ^PFOS (nm/ml) 0.097 Maximum Observed Rate at 50 C (day'1) 2.3 x10`J Maximum Calculated Rate at 25 C (day'1) 2.3 X10"4 Calculated Half Life at 25 C (years) >8.3 Appendix C lists the analytical results for a number of calibration standards containing PFOS at 13.0 ng/ml (e.g. sample 99039-135-02, analyzed just before the initial calibration standard set for pH 1.5). These results failed to meet the relevant data quality objectives for calibration standards, so the test analyte results presented in this report are based on the results for the PFOS standards at 51.9 ng.ml; these latter standards establish the LOQ of 52 ng/ml for PFOS. Using the accepted calibration regressions for PFOS, the instrumental responses to the 13.0 ng/ml standards had an average value of 16 ng/ml and a standard deviation of 4.4 ng/ml. Although these results did fail to meet the relevant data quality objectives for calibration standards, they do firmly establish the fact that the instrumental LOD for PFOS ( Apos) was below 13 ng/ml. The initial FOSA concentration (499 ng/ml) and the PFOS LOD provide an estimate of the FOSA half-life (see in Appendix B, Equations B38 and B39). The maximum degradation rate is given by Equation 5: k p (k p L * = - r ^ 7 X A -0D 0 m=l and the minimum half-life is given by Equation 6 (t " ) , i t [P0]ln ( 2) LOD l PFOS Eq. 5 Eq. 6 Page 19 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 We note that in both Equations 5 and 6, the initial FOSA concentration (P0) and the PFOS LOD (Aps) are molar quantities. Table 9 presents the results of the related calculations. Table 9. Degradation Rate and Half Life of FOSA in Aqueous Buffered Solutions Based on the Estimated PFOS Limit of Detection At (days) 42 [Pol (nm/ml) 1.0 a^-PlFoOdS (nm/ml) 0.024 Maximum Observed Rate at 50 C (day'1) 5.7 x10'4 Maximum Calculated Rate at 25 C (day'1) 5.7 x10'b Calculated Half Life at 25 C (years) >33 The mean and standard deviation of the FOSA concentrations also provide a useful estimate of its half-life. Details of the related calculations are presented in below (see Appendix B, Equations B36 and B37). The maximum degradation rate is given in Equation 7: k p ^ (k p L x 2cP Pp A t Eq.7 and the minimum half-life is given in Equation 4 t !/2 P > (vt *p,,)/r ln(2) _ |ip Atln(2) (k p)max 2cJp Eq. 8 We note that in both Equations 7 and 8, the mean FOSA concentration (jnp) and standard deviation ( o P) can be either molar or mass quantities. Table 10 presents the results of the calculation. Table 10. Degradation Rate and Half Life of FOSA in Aqueous Buffered Solutions Based on the Concentration Mean and Standard Deviation At (days) 42 (ng/ml) 455 aP (ng/ml) 17.2 Maximum Observed Rate at 50 C (day'1) 1.80 x 10-3 Maximum Calculated Rate at 25 C (day'1) 1.80 x 10-4 Calculated Half Life at 25 C (years) > 11 Page 20 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Conclusions We have performed a study of the aqueous hydrolytic degradation of perfluorooctanesulfonamide (FOSA). Six different pH levels were included in the study, which were carried out at 50C and extrapolated to 25C. Our results, based on direct observations of the FOSA concentration and a model of the related first-order kinetics, indicate no hydrolytic degradation of FOSA. We also monitored the concentration of the compound PFOS, a potential hydrolytic product of FOSA. Throughout the study, the PFOS concentration remained below both our limit of quantification (52 ng/mL) and our limit of detection (13.0 ng/ml). Using the LOQ for PFOS and the initial FOSA concentration (499 ng/ml), and assuming PFOS is the only hydrolytic product of FOSA, we estimate that the hydrolytic half-life of FOSA at 25C is greater than or equal to 8.3 years. Using the LOD for PFOS and the same initial FOSA concentration, and assuming PFOS is the only hydrolytic product of FOSA, we estimate that the hydrolytic half-life of FOSA at 25C is greater than or equal to 33 years. Finally, using the mean and standard deviation of the observed FOSA concentrations, we estimate that the hydrolytic half-life of FOSA at 25C is greater than or equal to 11 years. Page 21 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 References 1"Fate, Transport and Transformation Test Guidelines: 835.2110: Hydrolysis as a Function of pH," U.S. EPA Office of Prevention, Pesticides and Toxic Substances, publication number 712-C-98-057, January 1998. 2 "Experimental Physical Chemistry", F. Daniels, et al., McGraw Hill Book Co. (New York), p. 131, 1962. Page 22 of 126 Signatures BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Leader y^bate William K. Reagen, Ph.D., Laboratory Management Date Page 23 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Appendix A: Analytical Method ETS - 8-210.0, "Preparation of FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by High Performance Liquid Chromatography with Mass Spectrometry Detection." This Appendix presents the analytical method employed in this study. Page 24 of 126 I- . . BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 3M Environmental Laboratory M ethod Preparation of FOSA, M eFO SA, or E tFO SA H ydrolysis Sam ples and A nalysis by H igh Performance Liquid Chrom atography w ith M ass Spectrometry Detection Method Number: ETS-8-210.0 Adoption Date: Revision Effective Date: Approved by: Laboratory Manager Team Leader Date ETS-8-210.0 Page 1 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 25 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 I . - . . . ; ......... ............ .. 1.0 Scope and Application_____________________________________________________ 1.1 This procedure defines common steps for sample preparation, hydrolysis, and analysis of perfluorooctanesulfonamide (FOSA, CbF^SOjNH*, sometimes referred to as PFOSA), Nmethylperfluorooctanesulfonamide (MeFOSA, C8F17S 0 2NHCH3, sometimes referred to as FOSMA or PFOSMA), or N-ethylperfluorooctanesulfonamide (EtFOSA, CbFi7S02NHC2H5, sometimes referred to as FOSEA or PFOSEA). Hydrolysis products are identified and quantified by high performance liquid chromatography (HPLC) with mass spectrometry (MS) detection. Each test analyte (FOSA, MeFOSA, or EtFOSA) is studied separately using common, multi-component spike and internal standard solutions. The method is based on EPA OPPTS: 835.2110 (Reference 18.1). FOSA is quantified using FBSA (perfluorobutanesulfonamide, C4F9S 02NH2, sometimes called PFBSA) as an internal standard. MeFOSA and EtFOSA may be quantified using either Nmethylperfluorobutanesulfonamide (N-MeFBSA, C4F9S 0 2NHCH3, sometimes called PFBSMA or MePFBSA) or THPFOS (the anion of 3, 3,4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 8tridecafluorooctane sulfonic acid) as internal standard. Perfluorooctanesulfonate (PFOS anion, a potential hydrolysis product) may be quantified using either FBSA or THPFOS as internal standard. External standard quantification is permitted for all chemical species with appropriate technical justification. Representative structures are shown in Attachment A. 1.2 Compatible analytes. FOSA, MeFOSA, EtFOSA, FBSA, N-MeFBSA, THPFOS, and PFOS. 1.3 Acceptable matrices for analysis. Aqueous solutions at various buffered pH levels. 1.4 This is a performance-based method. Refer to Section 10 for the quality control parameters to be analyzed by this method. Refer to Section 14 for the quality assurance evaluation criteria for this method. 2.0 Summary of Method 2.1 Aliquots of FOSA, MeFOSA, or EtFOSA test-analyte stock solution are added to vials that contain buffers at pH levels 1.5,3.0, 5.0,7.0,9.0, and 11.0. The vials are then placed in an orbital incubator/shaker set at 50 3 C. Sets of vials (sample, duplicate, triplicate, spike, and blank) are rem oved at designated intervals and the date and tim e recorded. A n aliquot of mixed spike solution (containing PFOS, FOSA, MeFOSA, and EtFOSA) is added to the "spike" samples, and all vials are diluted 1:10 with methanol (MeOH) containing an internal standard mixture (e.g. THPFOS, FBSA, and N-MeFBSA). Samples are separated on a reverse phase Dionex IonPac NG-1 HPLC column using an ammonium acetate/MeOH solvent gradient, with detection by electrospray ionization mass spectrometry in the negative mode. 3.0 Definitions 3.1 Solvent Blank. A sample of analyte-free medium (e.g; MeOH) that is not taken through the sample preparation process. This blank is used to evaluate instrument contamination. ETS-8-210.0 Page 2 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 26 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 3.10 3.11 Buffer Blank. A sample of each buffer used in the hydrolysis incubations that is not taken through the sample preparation process. Laboratory Control Sample (LCS). In this method, a sample of each buffer that is spiked with spiking solution and internal standard solution. This sample does not undergo hydrolysis and is prepared prior to analysis. Continuing Calibration Blank (CCB). A sample of analyte-free medium that matches the matrix of the standards used to calibrate the instrument and is run in tandem with the Continuing Calibration Verification (CCV). The CCB is used to evaluate carryover from the standards and instrument baseline, and is run periodically throughout the analytical run (see Section 10 for frequency). Calibration Standard. A stock, intermediate or purchased standard diluted appropriately to achieve standard solutions of test analyte in a concentration range of interest. Continuing Calibration Verification (CCV). Standards analyzed during an analytical run to verify the continued accuracy of the calibration curve. This solution may be prepared from a different source or lot number than the calibration curve standards. Internal Standard: A known amount of a compound similar in analytical behavior to the compound(s) of interest, added to all samples and standards, and carried through the entire measurement process. It provides a reference for evaluating and controlling the precision and bias of the applied analytical method. Matrix Spike (MS). Prepared by adding a known mass of target analyte to a specified amount of a sample matrix exposed to hydrolytic conditions for which an independent estimate of target analyte concentration is available. Matrix spikes are used to determine the effect of the matrix on the method's recovery efficiency. Sample Triplicates. Three samples taken from and representative of the same sample source and carried through all steps of the sampling, treatment and analytical procedures in an identical manner. Sample triplicates are used to assess variance of the total method, including sampling, treatment and analysis. Dilution. A step in the hydrolysis study procedure in which a solvent (e.g. MeOH) is added to the test analyte/buffer solution to prepare it for instrumental analysis. This step occurs after the vials are removed from incubation and before the samples are analyzed. IS(s) may be incorporated into the diluting solvent, if desired. Limit of Quantitation (LOQ). The lowest concentration that can be reliably measured within specified limits of accuracy during routine laboratory operating conditions. The LOQ is generally 5 to 10 times the minimum concentration with a 99% confidence limit that the concentration is greater than zero. However, it may be nominally chosen within these guidelines to simplify data reporting. For many analytes, the LOQ is selected as the lowest non-zero standard in the calibration curve that is greater than 4 times the level of the solvent blanks. Sample LOQs are highly matrix-dependent. 4.0 Warnings and Cautions 4.1 Health and safety warnings ETS-8-210.0 Page 3 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 27 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 I 4.1.1 Wear the proper lab attire for all parts of this procedure. Wear gloves and proper eyewear at all times. 4.1.2 Handle all solvents in a hood for all parts of the described sample preparation procedure. 4.1.3 For potential hazards of each chemical used, refer to material safety data sheets, packing materials, and 3M Environmental Laboratories Chemical Hazard Review. 4.2 Cautions 4.2.1 All glassware in which standards are prepared should be triple-rinsed with 1:1 acetone/MeOH to reduce the possibility of accidental contamination. 4.2.2 Ensure that the mobile phase eluents are freshly prepared and that there is sufficient quantity to complete the run. Do not allow the pump to run dry. 4.2.3 Ensure that before starting the run sequence there is ample hard disk space on the computer to save all run data. 4.2.4 Ensure that there is enough nitrogen in the supply tank to complete sequence runs. 5.0 Interference________________________________________________________ 5.1 Contaminants in solvents, reagents, glassware, and other sample processing or analysis hardware may cause interference. Use the routine analysis of laboratory method blanks to demonstrate that there is no such interference. 5.2 Contamination from columns, HPLC tubing, and detector components may cause interference at low detection levels. The routine analysis of solvent blanks must be used . to demonstrate that there is no such interference. 6.0 Equipment___________________________________________________________ 6.1 Analytical balance sensitive to 0.1 mg 6.2 Shaker, incubator capable of maintaining temperature at 50 3 C 6.3 Hewlett-PackardTM (HP) 1100 HPLC system, or equivalent 6.3.1 Pump, quaternary, Model G1311A, or equivalent 6.3.2 Solvent degasser, Model G1322A or equivalent 6.3.3 Autosampler, ALS Model G1313A, variable injection volume capable 6.3.4 Column heater, Model G l316A 6.4 Dionex IonPacNG-l, 35 mm x 4.0 mm, 10 pm packing, or equivalent 6.5 Mass spectrometer, Hewlett-Packard LC/MSD, or equivalent, capable of operating in the selected-ion-monitoring mode 6.6 Clock, digital 6.7 Centrifuge capable of maintaining 3000 rpm for 5 minutes 6.8 pH meter, ComingTM Model 308 pH/Temperature Meter with 3-in-l gel-filled combination electrode (pH/reference/temperature), or equivalent 6.9 Refrigerator, capable of maintaining 4 3 C ETS-8-210.0 Page 4 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 28 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 i. 6.10 Data system, a personal computer capable of controlling the HPLC system as well as recording and processing signals from the detector 6.11 Data analysis software: Hewlett-Packard - ChemStation, Version A.6.03 or later 7.0 Supplies and Materials 7.1 VOA (volatile organic analysis) vials, 40 mL, I-CHEM or equivalent 7.2 Crimp cap autovials, 1.5 mL 7.3 Labels 7.4 Graduated pipets, glass, disposable, 1 mL-10 mL 7.5 Pasteur pipets, glass, disposable 7.6 Hamilton Gastight syringes (precision 1% of total volume), 10 pL-1000 pL 7.7 Volumetric flasks, various sizes 7.8 Beakers, glass, various sizes 7.9 Automatic pipettor, capable of dispensing 10-5000 pL 8.0 Reagents and Standards 8.1 Methanol (MeOH): HPLC/SPEC/GC grade from EM Science, or equivalent 8.2 Acetone: HPLC/SPEC/GC grade from EM Science, or equivalent 8.3 18.0 MQ water. Water with resistance < 18.0 M fi must not be used. 8.4 Calibration and standard stock solutions 8.5 All weights should be recorded to the nearest 0.0001 g 8.5.1 FOSA prepared in MeOH. (Example: An FOSA stock solution is prepared at a concentration of approximately 14,350 pg/mL by weighing approximately 8.5.2 8.5.3 8.5.4 8.5.5 0.1435 g of FOSA in a 10-mL volumetric flask and bringing to the mark with MeOH. This solution is diluted to make additional, appropriate standards.) MeFOSA prepared in MeOH. (Example: A MeFOSA stock solution is prepared at a concentration of approximately 19,900 pg/mL by weighing approximately 0.1990 g of MeFOSA in a 10-mL volumetric flask and bringing to the mark w ith M eO H . This solution is diluted to m ake additional, appropriate standards.) EtFOSA prepared in MeOH. (Example: An EtFOSA stock solution is prepared at a concentration of approximately 56,580 pg/mL by weighing approximately 0.5658 g of EtFOSA in a 10-mL volumetric flask and bringing to the mark with MeOH. This solution is diluted to make additional, appropriate standards.) PFOS prepared in MeOH. (Example: A PFOS stock solution is prepared at a concentration of approximately 30,520 pg/mL by weighing approximately 0.3052 g of PFOS in a 10-mL volumetric flask and bringing to the mark with acetone. This solution is diluted to make additional, appropriate standards.) Ammonium acetate buffer, approximately 2 mM. This is chromatographic eluent A. See Section 12.3.1. (Example: An acceptable buffer solution is made by weighing out approximately 0.16 g of ammonium acetate into a weigh boat and then quantitatively transferring to a 1-L volumetric flask. Add ETS-8-210.0 Page 5 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 29 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 i approximately 500 mL of 18.0 MO water and 10 mL of MeOH as a preservative. Dilute to the mark with 18.0 MQ water and mix thoroughly.) 8.6 Internal standards 8.6.1 THPFOS prepared in MeOH. (Example: A THPFOS stock solution is prepared at a concentration of approximately 2,000 pg/mL by weighing approximately 0.0200 g of THPFOS in a 10-mL volumetric flask and bringing to the mark with MeOH. This solution is diluted to make additional, appropriate standards.) 8.6.2 FBSA prepared in MeOH. (Example: An FBSA stock solution is prepared at a concentration of approximately 2,000 pg/mL by weighing approximately 0.0200 g of FBSA in a 10-mL volumetric flask and bringing to the mark with MeOH. This solution is diluted to make additional, appropriate standards.) 8.6.3 N-MeFBSA prepared in MeOH. (Example: An N-MEFBSA stock solution is prepared at a concentration of approximately 2,000 pg/mL by weighing approximately 0.0200 g of N-MEFBSA in a 10-mL volumetric flask and bringing to the mark with MeOH. This solution is diluted to make additional, appropriate standards.) 8.7 Buffers for calibration of pH meter Purchased pH calibration standards of pH 4.0, 7.0, and 10.0 (suppliers vary). 8.8 Buffer solutions for hydrolysis study Prepare pH 5.0 buffer solution using guidelines from Fate, Transport and Transformation Test Guidelines (Reference 18.1). Prepare buffer solutions of pH = 1.5, 3.0,7.0, 9.0, and 11.0 at ambient room temperature using guidelines from the CRC Handbook o f Chemistry and Physics (Reference 18.2). Prepare the buffer solutions in 1-L quantities. Calibrate a portable pH/temperature meter using purchased pH calibration standards of pH 4.0, 7.0, and 10.0, and measure the pH of all buffer solutions. The concentrations are presented below. Record final pH measurements of all buffers. Store buffers in sealed glass containers. . 8.8.1 pH 1.5 8.8.1.1 207 mL of 0.2 M HC1 8.8.1.2 250 mL of 0.2 M KC1 8.8.1.3 Adjust pH to 1.5 with additional 1 N HC1 8.8.1.4 Bring to a final volume o f 1 L with 18.0 MO water 8.8.2 pH 3.0 8.8.2.1 500 mL of 0.1 M Potassium Hydrogen Phthalate 8.8.2.2 223 mL of 0.1 M HCL 8.8.3 pH 5.0 8.8.3.1 3.8777 g ammonium acetate added to 250 mL 18.0 MO water 8.8.3.2 Add 250 mL 0.052 M acetic acid 8.8.3.3 Add 18.0 MO water to approximately 900 mL 8.8.3.4 Adjust to pH 5.0 with glacial acetic acid (approximately 0.5 mL) 8.8.3.5 Bring to a final volume of 1 L with 18.0 MO water 8.8.4 pH 7.0 8.8.4.1 500 mL 0.1 M KH2P 0 4buffer 8.8.4.2 291 mL 0.1 N NaOH ETS-8-210.0 Page 6 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 30 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 i 8.8.4.3 Adjust pH to 7.0 with either 1 N HC1 or 1 N NaOH 8.8.4.4 Bring to a final volume of 1 L with 18.0 MQ water. 8.8.5 pH 9.0 8.8.5.1 46 mL of 0.1 N HC1 8.8.5.2 500 mL of 0.1 M borax (Na2B 04H20 ) 8.8.5.3 Adjust pH to 9.0 with either 1N HC1 or 1 N NaOH 8.8.5.4 Bring to a final volume of 1 L with 18.0 MO water. 8.8.6 pH 11.0 8.8.6.1 500 mL 0.05M NaHC02 8.8.6.2 227 mL 0. IN NaOH 8.8.6.3 Add water to 950 mL 8.8.6.4 Adjust pH to 11.0 with 1 N NaOH 8.8.6.5 Bring to a final volume of 1 L with 18.0 MO water 8.9 Test Analyte, Spike, and Diluting solutions: 8.9.1 FOSA test analyte solution. [Example: Approximately 150 pL of solution 8.5.1 is diluted in 10 mL MeOH, yielding a concentration of approximately 215 pg/mL FOSA. A 10-pL aliquot of this solution is then added to 1.0 mL of buffer before hydrolysis testing. After hydrolysis, dilution with 9.0 mL MeOH containing internal standards (step performed in Section 12.1.12) results in concentrations before analysis of approximately 215 ng/mL FOSA. 8.9.2 MeFOSA test analyte solution. Follow the procedures in Section 8.9.1, but use the MeFOSA test analyte solution prepared in Section 8.5.2. 8.9.3 EtFOSA test analyte solution. Follow the procedures in Section 8.9.1, but use the EtFOSA test analyte solution prepared in Section 8.5.3. 8.9.4 Spiking solution. [Example: A common post-hydrolysis spiking solution is used for the analysis of FOSA, MeFOSA or EtFOSA hydrolysis samples. This solution contains approximately 50 pg/mL FOSA, 50 pg/mL MeFOSA, 50 pg/mL EtFOSA, and 50 pg/mL PFOS in MeOH. It is made by first preparing intermediate solutions of approximately 500 pg/mL of each compound by MeOH dilution of the solutions prepared in Sections 8.5.1, 8.5.2, 8.5.3, and 8.5.4, respectively. The combined 50 pg/mL FOSA, 50 pg/mL MeFOSA, 50 pg/mL EtFOSA, and 50 pg/mL PFOS solution is made by adding 1.0-mL aliquots o f each o f the intermediate solutions to a 10-mL volumetric flask and diluted to the mark with MeOH. After the hydrolysis period is complete, 50 pL of the mixed solution is added to each of the "spike" samples. After dilution with 9.0 mL MeOH solution containing internal standard (step performed in Section 12.1.12), the final concentrations of the added spikes in the sample are approximately 250 ng/mL FOSA, MeFOSA, EtFOSA and PFOS]. 8.9.5 Diluting Solution Containing THPFOS, FBSA, and N-MeFBSA Internal Standards. A common, mixed-stock solution is first prepared in MeOH. This solution is used for the analysis of FOSA, MeFOSA, or EtFOSA hydrolysis samples. [Example: A solution containing approximately 250 pg/mL each THPFOS, FBSA, and N-MeFBSA is prepared by adding appropriate volumes of THPFOS stock (Section 8.6.1), FBSA stock (Section 8.6.2), and MeFBSA stock ETS-8-210.0 Page 7 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 31 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 (Section 8.6.3) to a 10-mL volumetric flask and diluting to the mark with MeOH. A working dilution solution is prepared by adding 2 mL of the 250 pg/mL mixed THPFOS, FBSA, and N-MeFBSA stock solution to a 2 L volumetric and diluting to the mark with MeOH (final concentration of 250 ng/mL of each compound). After the hydrolysis period is complete, 9 mL o f the working solution is added to the sample. The final concentrations of the added internal standards in the sample are approximately 225 ng/mL THPFOS, 225 ng/mL FBSA, and 225 ng/mL N-MeFBSA]. 9.0 Sample Handling 9.1 Handle samples and standards in a well-ventilated area. Wear gloves and eyewear whenever handling any solutions. 9.2 Record times of initial preparation and quenching additions on the fluorochemical degradation (hydrolysis) Analysis Sample Preparation Data Sheet (Attachment B). 9.3 Once the 9.0 mL of final diluting solvent has been added, analyze the samples. Alternatively, aliquots of the methanol-diluted samples should be refrigerated at 4 3 C or frozen until analysis can be performed. 10.0 Quality Control (Frequency of Performance) 10.1 Solvent Blank. Solvent blanks should be run before and after every calibration curve, before and after every CCV (where it is called a CCB), and after no more than 20 sample injections. 10.2 Buffer Blank. A buffer blank should be analyzed once per run (30 samples or less). 10.3 Laboratory Control Sample (LCS). An LCS should be analyzed once per run (30 samples or less). . 10.4 Continuing Calibration Blank (CCB). A CCB (solvent blank) is run before and after every CCV. 10.5 Continuing Calibration Verification (CCV). A mid-range CCV standard, flanked by solvent blanks (CCBs), is run after every 20 samples (or less) to verify the calibration stability. This solution may be prepared from a different source or lot number than the calibration curve standards. 10.6 Internal Standards. IS(s) are added in a constant concentration to all standards, samples, and matrix spikes. In this method, internal standards are added to the diluting solvent (Section 8.9.5). 10.7 M atrix Spikes. Prepare a post-hydrolysis matrix spike solution along with each set of triplicate samples at each of the pH levels used in the study (refer to Section 8.9.4). Concentrations of the spike should be approximately equal to the mid-range calibration standard. 10.8 Triplicate Samples. All samples are prepared in triplicate incubation mixtures for each pH and time point. 11.0 Calibration and Standardization ETS-8-210.0 Page 8 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 32 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 11.1 Standard preparation. Prepare six calibration standards of FOSA, MeFOSA or EtFOSA in. MeOH, depending on the choice of test analyte for the analysis. Standards from approximately 10-1000 ng/mL are suggested. This solution should also contain appropriate concentrations of the internal standard. 11.2 Calibration standards. Analyze the calibration standards at the beginning and end of the run. Use the data reduction software program for linear regression calculations to relate the analyte peak area ratio versus the amount ratio from the internal standard. External standard calibration may be used if data review shows a problem with the internal standard analysis. Consult with the group leader for direction prior to performing the external calibration methodology. Note on the standard curve and in the report why a decision was made to perform external standard calibration on the raw data. 12.0 Procedures 12.1 Sample and spike preparation 12.1.1 Before spiking with any of the stock standards, transfer approximately 1 mL of the solution to an autovial and cap it. Use this smaller volume for spiking to minimize the effects of evaporation from stock solutions. 12.1.2 Determine the number of time points that will be analyzed. Each time point will have four vials for each pH, multiplied by the number o f pH levels analyzed. One vial at each level will be labeled as "sample", "duplicate", "triplicate", or "spike." 12.1.3 Obtain the appropriate number of 40-mL I-CHEM vials with caps and cardboard boxes. Prepare appropriate sample preparation worksheets and create labels and affix to the vials. The labels should include the sample number, pH, time point, and initials of the analyst. Record the pH of each buffer solution. 12.1.4 Remove the cap of the I-Chem vial and add 1 mL of the appropriate buffer solution to all of the prelabeled vials. Always replace the cap immediately after any addition to minimize evaporation. 12.1.5 To all of the vials, add 10 pL of the appropriate FOSA, MeFOSA, or EtFOSA test analyte solution (prepared in Section 8.9.1, 8.9.2, or 8.9.3) with a 10-pL Gastight syringe. Record the time of addition for each vial. 12.1.6 For "Time Zero" samples only, proceed to section 12.1.11. For all other samples, continue on to section 12.1.7. 12.1.7 Make sure that the cap has been firmly tightened and place the samples back in the cardboard case. 12.1.8 Place the case into a pre-warmed incubator/shaker for the appropriate time. Record the time, temperature, and rate of shaking. The temperature is determined by the conditions of the experiment. Continue to monitor the incubator temperature daily during the entire incubation. Record the temperature on the sample preparation sheet. 12.1.9 Remove the case from the incubator at the designated preset time. ETS-8-210.0 Page 9 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 33 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 12.1.10 Remove the vials from the case and place in racks. Allow the vials to cool for 15 minutes to room temperature. Alternatively, freeze the vials if solutions are to be diluted and analyzed at a later date. 12.1.11 Using a 10-p.L gas tight syringe, add 10 pL of mixed-spike solution (Section 8.9.4) to the "spike" vials. Invert each vial several times to mix the contents. 12.1.12 Using a 10-mL graduated pipet, add 9.0 mL o f the MeOH diluting solution prepared in Section 8.9.5 to each vial. Invert each vial several times to mix the contents. 12.1.13 Aliquot approximately 1 mL of each sample to the appropriately labeled autovial. Cap the vials and mark the bottom of the meniscus. 12.1.14 Place the vials in the HPLC autosampler. 12.2 Instrument setup 12.2.1 Check that the appropriate HPLC column is in the instrument for each analysis. 12.2.2 Check that the correct eluent solutions are in bottles to be used and that enough is available to complete the sequence run. 12.2.3 Place the samples in the autosampler tray and construct a sequence table with appropriate calibration standards, calibration check standards and solvent blanks. 12.2.4 Verify that all samples and standards are positioned correctly. Enter sequence information: (sample or standard ID, method name) use one injection per sample. 12.2.5 Save sequence as analysis date (e.g. on March 14,1999, save sequence table as 031499.s). Save all data to a subdirectory labeled with analysis date (e.g., 031499). 12.2.6 Set post-sequence command macro to shut down system (Example: "STANDBY" on HP systems). 12.3 HPLC set up: 12.3.1 Analysis of FOSA, MeFOSA, or EtFOSA samples from pH levels 1.5, 3.0, 5.0, . 7.0, 9.0, and 11.0: Install the column: Dionex IonPacNG-l, 4.0 x 35 mm, 10-pm packing, or equivalent. Solvent A: 2 mM ammonium acetate including 1% MeOH Solvent B: MeOH Solvent Gradient (may vary slightly from study to study: T im e (m in ) 0.0 0.5 2.5 6.0 - 7.0 %A %B Fl o w Ra te 60 40 0.5 mL/min 60 40 0.5 mL/min 5 95 0.5 mL/min 5 95 0.5 mL/min ETS-8-210.0 Page 10 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 34 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 12.4 Post time: 2 .0 -3 .0 minutes; column temperature: 40C. Recommended Mass Spectrometer set up:* 12.4.1 Analysis of FOSA, MeFOSA, or EtFOSA at pH 1.5,3.0, 5.0,7.0,9.0, and 11.0: Identifiable ions: Acquisition Mode Selected Ion (SIM) Ionization Mode Electrospray Polarity Negative Drying Gas Flow 8 L/min Nebulizer Pressure 30 psig Drying Gas Temp 300 C Capillary Voltage 3500 V ' Example conditions ate applicable to Hewlett Packard H P1100 equipment only. Name FBSA (M-H+) PFBS (M-H+) N-MeFBSA (M-H+) THPFOS (M-H+) *FOSA (M-H+) **PFOS (M-H+) MeFOSA (M-H+) EtFOSA (M-H+) N-MeFOSE-OH (M-H+) N-EtFOSE-OH (M -H +) ''Quant" ion for FOSA ** "Quant" ion for PFOS 12.5 Autosampler set-up* SIM Io n s 298.00 299.00 312.00 427.00 498.00 499.00 512.00 526.00 616.00 630.00 G ain (EMV) 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Fr ag m ento r (V) 70 70 70 70 70 70 70 70 70 70 Dw ell (m s e c ) 97 97 97 97 97 97 97 97 97 97 12.6 Autosam pler: ALS Model G1313A AUTOSAMPLER PROGRAM: None In j e c t io n v o l u m e : 5.0 pL ` Example conditions are applicable to Hewlett Packard HP 1100 equipment only. Sample analysis 12.6.1 Enter the standard, sample and QC information into the sequence table. Analyze solvent blanks and calibration standards first, then up to 20 sample injections, followed by solvent blanks and calibration standards. If more than 20 sample ETS-8-210.0 Page 11 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 35 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 12.6.2 12.6.3 12.6.4 12.6.5 injections are to be run, analyze a continuing calibration standard (CCV) after every 20 and run the calibration standards again at the end of the sequence. Run solvent blanks before and after each standard curve, before and after the CCV, and after the set of samples to check for any analyte carryover. Identify the electronic acquisition files with an appropriate prefix. Do not exceed five characters if the sequence contains more than 99 lines. Place the standards, samples, and QC (matrix spikes and sample blanks) into the autosampler tray according to the order they are listed in the sequence. Save the sequence table with a name corresponding to today's date. (e.g. if today is December 1, 1998, save the sequence as 120198.S) Start the sequence. 13.0 Data Analysis and Calculations___________________________ ____________ 13.1 Peak evaluation: Peaks must be symmetric in shape and identified by extracting compound specific ions. Peaks considered for calibration must have peak heights greater than 5 (five) times the baseline noise for that region of the chromatogram. Peak integration is from baseline to baseline through a peak using automatic or manual integration. Compounds with isomers present as a shoulder or as a discrete second peak should be integrated with the parent compound unless otherwise noted. Quantitation data are calculated using THPFOS, FBSA, or N-MEFBSA as the internal standards, as appropriate. However, external standard calibration may be acceptable when sample integrity is intact. Consult with the team leader for direction prior to performing the external calibration methodology. Document change in raw data and final report. 13.2 Calculation of k: Calculate the FOSA, MeFOSA, or EtFOSA concentrations in each of the pH matrices using the curves obtained from the calibrations and the internal standard. Assinning first-order kinetics, a rate constant (k) can be determined by plotting the natural logarithm of the ratio (concentration of FOSA at any given time / initial concentration of FOSA) versus the time (-t). The slope of the resultant line is k. Half-life of the test analyte (t1/2, in the units of t) is obtained from the relation: Ln 2.0/k = 0.693/k. 13.3 Matrix spikes. Calculate the percent recovery for each o f the matrix spikes. Using the observed matrix spike recoveries, calculate the average spike recovery. Calculate the matrix spike percent recoveries using the following equation: % Recovery = (observed spiked sample result - average sample result) x 100 actual amount spiked 13.4 Sample triplicates. Calculate the relative standard deviation (RSD) for the triplicate samples. STDEV (A. B, Cl x 100 % AVERAGE (A, B, C} ETS-8-210.0 Page 12 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 36 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Where: A = the concentration measured in the sample, and B = the concentration measured in the duplicate, and C= the concentration measured in the triplicate 14.0 Method Performance______________________________ ___________ _ 14.1 Solvent Blanks, Buffer Blanks, and Continuing Calibration Blanks. The measured value for these blanks should be less than 25% of the limit of quantitation (LOQ) of the method. Solvent blanks should show no more than a 5% carry over from a high standard or calibration check standard. If so, two solvent blanks may be necessary to rule out instrumental contamination. If peaks with greater than 50% of the peak area of a low standard value are observed in sequential solvent blanks, the run should be stopped. This is indicative of instrument contamination. The instrument shall be brought into compliance by thoroughly cleaning the electrospray source, and replacing or cleaning columns, tubing, etc. 14.2 Coefficient of Determination (r2). The coefficient of determination (r2) for linear calibration curves should be 0.990 or greater. The curves should be examined closely for linearity and intercept, particularly for accuracy of quantitation at the low and high ends of the curve. On occasion it may be necessary to utilize exponential or quadratic fits of the data, usually when broad range curves (greater than 3 orders of magnitude between the low and high concentration standards) are used. Record in the raw data the reasons for using quadratic equations, and get approval from QAU. If a point is 20 % of the nominal value the point is used for quantitation. If the value exceeds 20 %, the curve is out of range and the curve is rerun until all points pass the criteria. 14.3 Continuing Calibration Verification (CCV). If the relative percent difference for the amount of measured analyte is > 15 % of the true value, relative to the initial standard curve, stop the run. Only those samples analyzed before the last acceptable CCV will be used. Appropriate steps must be taken to correct the problem before analysis is allowed to proceed (consult the project lead for guidance). Reanalyze the remaining samples with a new calibration curve. 14.4 Internal Standards. Peak-area ratios of samples (relative to the IS) are used for quantification. The %RSD of the internal standards in calibration curves should be < 10 %, or the project lead should be consulted. The area response of an IS in a sample must be between 50% and 150% of the mean area response of the IS in an acceptable calibration curve. Samples having area response outside this range should be reanalyzed or prepared again, at the discretion of the project lead. 14.5 Matrix Spikes. The analyst shall accept percent spike recovery values of 100 25%. Spike recoveries of 70 - 75% or 125 - 130% of nominal may be used at the discretion of the project lead. Spike recoveries < 70% or > 130% place the analysis out of control. Appropriate steps (e.g. cleaning, blank tests, install a new column) must be taken to correct the problem before the analysis is allowed to proceed. 14.6 Sample Triplicates. The analyst shall accept RPD values of < 25%. RPD values > 25% place the analysis out of control. Appropriate steps must be taken to correct the problem before analysis is allowed to proceed; consult the group leader for direction. ETS-8-210.0 Page 13 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 37 of 126 I ! BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 14.7 Limit of Quantitation (LOQ). The limit of quantitation is equal to the lowest standard in the calibration curve that is < 5 times the blank level or the S/N, whichever is greater. 14.8 System Suitability. System suitability is demonstrated by acceptable instrumental checks (e.g. abbreviated m/z check-tune, or full auto-tune routines). Acceptable checks should be documented in instrument run logs. 15.0 Pollution Prevention and Waste Management__________________________ 15.1 Dispose of sample waste by placing in high or low BTU containers as appropriate. Use broken glass containers to dispose of glass pipettes. 15.2 Collect HPLC solvent waste in the satellite accumulation can. Empty into the flammable storage drum in the hazardous waste collection area on the 2nd floor. 15.3 Use smaller bore columns when possible to minimize waste generation. 16.0 Records_________________________________________________________ 16.1 Print out hard copies of all graphics and data analysis summaries for archiving. 16.2 Sign and date all graphics and label with instrument ID. 16.3 Fill out the hydrolysis sample preparation worksheet completely, making sure to include all initials and dates. 16.4 Print out the sample sequence table, photocopy a reduced-size duplicate, and tape the photocopy to the instrument log. Keep the original copy for the raw data files package. 16.5 Print chromatograms and internal standard reports for all analyses. 16.6 Print calibration tables and curve information and store in the raw data file. 16.7 Store hydrolysis sample preparation worksheets in the raw data file. 16.8 Enter all standard preparation information in the standards preparation logbook. Make a photocopy of the logbook page and include the copy in the raw data file. 16.9 Archive electronic data to appropriate media when necessary. 17.0 Attachments 17.1 Attachment A: Representative Chemical Structures 17.2 Attachment B: Hydrolysis Sample Logsheet ' 18.0 Bibliography_________________________________________ _______________ 18.1 Fate, Transport and Transformation Test Guidelines Office of Prevention, Pesticides and Toxic Substances (OPPTS) 835.2110 Hydrolysis as a Function of pH, EPA 712-C-98057, January 1998. 18.2 CRC Handbook o f Chemistry and Physics, 1st Student Edition, "Buffer Solutions Operational Definitions of pH," Robert C. Weast, Ph.D., 1988, p. D-87. ETS-8-210.0 Page 14 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 38 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 19.0 Affected Documents None. 20.0 Revisions Revision Number Reason for revision Date ETS-8-210.0 Page 15 o f 18 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 39 of 126 l t - BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Attachment A: Representative Chemical Structures FOSA (MW = 499) MeFOSA (MW = 513) EtFOSA (MW = 527) PFOS (MW of anion = 499) THPFOS (MW o f anion = 427) FFFFFFHHO 1 - - - - -t ETS-8-210.0 Prep, o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 16 o f 18 Page 40 of 126 FBSA (MW = 299) I* BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 N-MeFBSA (MW = 313) ETS-8-210.0 Prep, o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 17 o f 18 Page 41 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Attachment B: Hydrolysis Sample Logsheet TEST ANALYTE: HOURS: Fluorochemical Degradation (Hydrolysis) Analysis Time of Initial ISTD Spike Buffer Volume Test Analyte Solution Solution Time of Quenching ______-_____ -_____ Sample__________________________ V5__________ VO___________________________________________________________ ______-_____ -_____ Duplicate________________________ V5__________ 1L0______ ____________________________________________________________ - - Spike I I______________________ V5___________1.0 ___________________________________________________________ Sample__________________________ 5 _ _________ 1.0 Duplicate_________________________ 5____________1.0 Spike I I______________________ 5____________VO Sample__________________________ 7____________VO Duplicate_________________________7____________1.0 Spike I I_________ '____________ 7___________ VO Sample___________________________ 9___________ VO Duplicate__________________________9___________ VO Spike I I_______________________ 9___________ VO Sample___________________________ 11__________ 1.0 Duplicate_________________________ 11__________ 1.0 Spike I I_______________________ 11__________ VO Date o f Initial Prep:______________________ Test Analyte Quenching Solution ISTD Solution Spike Solution Solution Standardlyraceability No.__________________________________________________ Component_____________________________________________________________ Concentration (pg/mL)_______________________________________________NA Buffer Addition by: ISTD Addition by:______ Test Analyte Addition fay. Quenching by:_______ _ Spike Addition by:_____ Autovial Aliquoting by: Centrifugation Yes l No Centrifuge: RPM:________________ Time: min By;___________________ Date o f Quenching: Temperature of Incubator (C): Incubation Start (Date and Time): Incubation Stop (Date and Time): Total Incubation Time: Filtration: Yes / No By: Pore Size: urn, Brand: Reviewed by: ETS-8-210.0 Preparation o f FOSA, MeFOSA, or EtFOSA Hydrolysis Samples and Analysis by HPLC/MS Page 18 o f 18 Page 42 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Appendix B: Kinetics Model This Appendix includes a mathematical description of the kinetics model employed in the study. Page 43 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Kinetics Model B1. Reaction Components and Rates The arguments below are based on the following Idealized set of reactions representing the hydrolysis of a parent compound P and its hydrolysis products A m, which number N. The actual hydrolysis reactions that occur under neutral, acidic, and basic conditions are subsumed in these equations, and are assumed to proceed with pseudo-first order rates k Pm(forthe parent) and k Am(forthe parent's hydrolysis products). P + H 20 o n m A m+ Y m] (m = l to N) (B1) A m+ H 20 Ym2 (m = 1 to N) (B2) where the general symbols Y ml and Yra2 represent all the other hydrolysis products. B2. Parent Compound Concentrations Equation B1 indicates that the pseudo-first order differential change in the parent concentration P is given by (B3) which is equivalent to the separable differential equation (B4) Equation B4 may be directly integrated to obtain the general solution With the initial condition P(t = 0 ) s P 0, the specific solution to Equation B4 is using the additional definition of the total parent hydrolysis rate (B5) (B6) Page 44 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 N kp = n m k Pm m=l (B7) Equation B6 can be re-written in a form that allows a least-squares estimate of the total parent hydrolysis rate: k pt = -In (B8) Using the initial (t = 0) measured value of the parent concentration P0and later values P measured at later times t , one can calculate and plot the (linear) quantity [- in (P/P0)] versus time and obtain a least -squares estimate of the slope of the line. The resulting slope is the least-squares estimate k p of the total parent hydrolysis rate. Equation B6 indicates that over a period of time T 1^ (the parent hydrolysis half-life) the parent concentration P is reduced through hydrolysis by a factor of two, where (B9) A least squares estimate T ^ of the parent hydrolysis half-life is therefore available from ,= i, (B10) B3. Product Compound Concentrations The pseudo-first order differential changes in the product concentrations An (using Equations B2 and B6) are d A m= ( n mk PmP - k AmAm) dt = ( n mk PmP0 e"kp ` - k AmA m)d t (B11) and the (first order, non-separable) differential equation governing the product concentrations is dA* + k AmAm= nmk PmP0 e-kpt dt The "standard form" of Equation B12 is (B12) Page 45 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 A m+ S ( t)A m = Q (t) where the "function" S (t) is actually a constant: S(t) = k Am and Q(t) = nmk PmP0 e_ltpt . The general solution A mto Equation B12 Is contained In (B13) (B14) (B15) A e 's(t)dt = j Q ( t ) ^ s(,')4' dt + C (B16) where e JS(t)dt _ e |S (t')d t' __ gkA nJdt _ gltArat (B17) and jQ ( t) e ^ s(t')dt' dt + C = nmk PmP0J e ^ e ' ^ d t + C (B18) There are two cases of Equation B18 to consider. In the circumstance that k Am = k P, which occurs only when the hydrolysis rate of the mth product Is identical to the total parent hydrolysis rate, the general solution to Equation B18 is ( fo r k ^ = k P) A mekP' = n mk PmPOt + C (B19) and, using the initial condition A m(t = 0) = A ^ , the specific solution to Equatlon18 Is (f o r k Am = k p ) A m = (nmkpraP0 t + A m0) e `kpt . (B20) We note that when k ^ = k p = 0 (that is, when both the parent and potential product are hydrolytically stable), Equation B7 requires (also) that k Pm= 0 , so Equation B20 becomes Page 46 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 A,, =A,, (B21) indicating, as required, that the product concentration does not change with time. The circumstance k Am = k p is highly improbable, and is neglected in the remainder of this discussion. However, the reader should bear in mind that the expressions derived below do not hold when the parent hydrolysis rate k pand the product hydrolysis rate k ^ approach each other. In the more probable case, for which k Am * k p (i.e. that the hydrolysis rate of the m,h product is different from the total parent hydrolysis rate), the general solution to Equation B18 is A e k Amt -- n P m | o _ e ( kA,, --k P ) t + q m k Am- k P , and the specific solution to Equation B18 with the initial condition A m(t = o) = A m0 is A,, = A m0 + n mkpmfil kp --km n m k p mP() e -kP t k p - k Am (B23) Of greatest interest here is the case in which the product compounds are known to be hydrolytically stable, that is, when k ^ = 0 for all m. In this case, Equation B23 becomes (for hydrolytically stable products) A m = A m0+ (!_,,*,.) . Kp (B24) B4. Relationships Between the Parent and Compound Concentrations Equations B7 and B24 can be combined to obtain (for hydrolytically stable products) N k P X n">^ m=l k p y 1(A m- A m0) ( l - e ' "' ' ) p (B25) Page 47 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 so that or (for hydrolytically stable products) c- K p ) _ ^ (A m - A m0) n=l Po (for hydrolytically stable products) (B26) k pt = - In J ^ (A n , ~ A m0) -, p0 (B27) If the changes in the product concentrations are all small compared to the original parent concentration, that is, If ^ A m - A m0 1, m-1 P0 we may use the expression (valid for -1 < X < 1 ) (B28) ln(l + X ) = X - --X 2 + - X 3 - --X 4 + . 234 and Equation B23 becomes (for hydrolytically stable products and /N _ ^ r Am ^rnO v m=i 0y <<P0) (B29) (B30) Page 48 of 126 or (for hydrolytically stable products and BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Po) (B31) B5. Parent Half-Life Estimates Based on Limits of Quantification of the Products In every experimental determination of k p, there is some set of values A ^00 (the "limits of quantitation") below which the product concentrations A mcannot be reliably measured. If during an experiment carried out over the period of timeA t all the product concentrations A mremain below their limits of quantitation, then the maximum possible value of the rate k P is obtained by assuming (for all the products) that 1) A m0 = 0 and 2) at time t = A t , the product concentrations have increased to the values A m= A[;0Q. With these assumptions, the experimental data indicate that the reaction rate k Pis less than some maximum value (kP^ as follows: (for hydrolytically stable products at concentrations below the limits of quantitation) kp ^ (k p L x iN -- y a ^o q . , A t A ra (B32) Under the same circumstances and assumptions, the experimental data indicate that the parent half-life T 1^ (see Equation B9) is greater than the value ( T ^ ) . as follows: (for hydrolytically stable products at concentrations below the limits of quantitation) T^2 > t ^2 --_M__2 L = A t P0 ln(2) a l q r " 1 p L " " (k p), . m=I (B33) The reader should note that Equations B32 and B33 are valid only when both 1) the products are hydrolytically stable and 2) the concentrations of all the potential products are measured. Otherwise, the quantity ( k p ) ^ in Equation B32 may not actually represent the maximum possible value of the rate constant k p, and the related result in Equation B33 for (t vp) is also questionable. Page 49 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B6. Parent Half-Life Estimates Based on Limits of Quantification and Experimental Precision of Product Concentrations In certain experiments, some hydrolysis products are present at quantifiable but essentially constant concentrations over the time (A t ) of the experiment. In this case, it is the experimental precision of the measured product concentrations, rather than the limits of quantitation, which contribute to the estimate of the maximum value of the parent hydrolysis rate k p. If the set of concentrations measured for the mth product have the mean value p mand standard deviation a m, the data do not exclude the possibility that the product concentration increased from the initial value o m- p mto the value c m+ at time t = A t . Taking this possibility to be the actual case for the measured products, the maximum value of the quantity (A m- A m0) is 2c m. This reasoning suggests that the following estimate of the maximum parent hydrolysis rate is appropriate: (for hydrolytically stable products at either 1) constant measured concentrations with standard deviation cm or 2) concentrations below the limits of quantitation) k r ^ (kpLx l ^ T 2 > " Q+ X 2m Below LOQ Cons tan t (B34) Under these circumstances and assumptions, the experimental data indicate that the parent half-life T 1^ P is greater than the value (T x ^ P 7)min as follows: (for hydrolytically stable products at either 1) constant measured concentrations with standard deviation om or 2) concentrations below the limits of quantitation) n > (t i/2\ _ h (2 ) _ A t P0 ln(2) p 1 p' min (k p ) X Ar+ Below LOQ Constan t -1-1 (B35) The reader should note that Equations B34 and B35 are valid only when both 1) the products are hydrolytically stable and 2) the concentrations of all the potential products are measured. B6. Parent Half-Life Estimates Based on the Experimental Precision of Parent Concentrations In certain experiments, the hydrolytic parent remains at an essentially constant concentration over the time ( A t) of the experiment. In this case, it is the experimental precision of the measured parent concentrations that determines the maximum value of the parent hydrolysis rate k P. If the set of concentrations measured for the parent have the mean value p pand standard deviation a p, the data do not exclude the possibility Page 50 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 that the product concentration increased from the initial value | iP- ctp to the value p p + a p at time t = A t . This reasoning suggests that the following estimate of the maximum parent hydrolysis rate is appropriate: (for essentially constant parent concentrations with mean value p pand standard deviation Op ) k Pp < (VkPP/)max 2op Up A t ' (B36) Under these circumstances and assumptions, the experimental data indicate that the parent half-life T 1^ is greater than the value (t ^ ) as follows: (for essentially constant parent concentrations with mean value p pand standard deviation Op) T |/2 P > (T yj) \ pA ln(2) _ Up A tln (2 ) (^p)max 2oP (B37) B5. Parent Half-Life Estimates Based on Limits of Detection of the Products In every experimental determination of k p, there is some set of values A ^0D (the "limits of detection") below which the product concentrations A mcannot be reliably detected. If during an experiment carried out over the period of timeA t all the product concentrations A mremain below their limits of detection, then the maximum possible value of the rate k P is obtained by assuming (for all the products) that 1) A m0 = 0 and 2) at time t = A t , the product concentrations have increased to the values A m= A^;0D. With these assumptions, the experimental data indicate that the reaction rate k Pis less than some maximum value (vkrp)/max as follows: (for hydrolytically stable products at concentrations below the limits of detection) kp - (kP)raK= 0 m=l (B38) Page 51 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Under the same circumstances and assumptions, the experimental data indicate that the parent half-life T 1^ (see Equation B9) is greater than the value (t 1/2) as follows: (for hydrolytically stable products at concentrations below the limits of detection) V 'l > (t 1'2) = P ' P 'm in l- \ (K)n = A t P, H2) ' . m=l LOD (B39) The reader should note that Equations B38 and B39 are valid only when both 1) the products are hydrolytically stable and 2) the concentrations of all the potential products are measured. Otherwise, the quantity ( k p ) ^ in Equation B38 may not actually represent the maximum possible value of the rate constant k p, and the related result in Equation B39 for (t 1/2) is also questionable. B9. Temperature Dependence of the Reaction Rate and Half-Life In order to increase the speed of the reactions of interest, we conducted this experimental study using samples maintained at the temperature 50C = 323 K. Of greater interest are the corresponding results for the environmentally important temperature 25C = 298 K. When the Arrhenius activation energy for a reaction is A H a, Equation B38 81 provides the following relationship between the hydrolysis rates (Iq and k2) for that reaction at two different absolute temperatures (T, and T2): (B40) where R = 1.99 x 10'3 Kcal mole'1K'1is the ideal gas constant. Using the value82 A H a=18 Kcal/mole, the rate ratio k , / k 2at the corresponding temperatures T, =298 K and T2=323 K is k, 18 ' 1 1 = exp(-2.35) = 0.095 k ! " rapl 1.99X10'3 .323 298 (B41) Equation B39 indicates that the hydrolysis reactions of interest proceed approximately ten times more slowly at 25C than at the chosen experimental temperature of 50C. Accordingly, the rate reactions reported here for the temperature 25C are ten times lower than those measured at 50C, and the hydrolysis half-life estimates reported here Page 52 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 for 25C samples are ten times longer than those calculated from the 50C experimental data. References to Appendix B: 61 I. N Levine, "Physical Chemistry," McGraw-Hill (New York), pp. 498-501 (1978). 62 F. Daniels, et al., "Experimental Physical Chemistry", McGraw Hill (New York), p.131 (1962). Page 53 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Appendix C: Selected Analytical and Kinetics Results This Appendix includes selected sample data and their related kinetics results. Page 54 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 FOSA Buffer Hydrolysis Study at 50 C. All concentrations in ng/ml. pH Time (Days) 1.5 0 1.5 7 1.5 14 1.5 21 1.5 28 1.5 35 1.5 42 Cone. 475 464 443 450 441 458 441 In(rP M P lo ) 0.000 -0.024 -0.069 -0.054 -0.075 -0.036 -0.073 FOSA @ 50 C pH 1.5, Rate constant graph pH Time (Days) Cone. ln (rP M P ]o ) 3.0 0 484 0.000 3.0 7 481 -0.006 3.0 14 457 -0.057 3.0 21 429 -0.121 3.0 28 457 -0.057 3.0 35 467 -0.035 3.0 42 466 -0.037 FOSA @ 50 C 0.05 -, 0.00 i : -0.05 5, -0.10 T -0.15 -0.20 J -0.25 0 -------* -------- =y - 8 . 6 7 E - 0 4 X - 2 .6 6 E -0 2 ........R2= l 05R-m .. 1 10 2 0 3 0 40 50 __ Time (days) ______ SUMMARY OUTPUT Regression Statistics Multiple R R Square Adjusted R Square Standard Error Observations 0.67379 0.45399 0.34479 0.02299 7 ANOVA Regression Residual Total df 1 5 6 SS 0.00220 0.00264 0.00484 Intercept X Variable 1 Coefficients -0.02072 -0.00127 Standard Error 0.01567 0.00062 % 2c Slope Uncertainty 98% SUMMARY OUTPUT Regression Statistics Multiple R R Square Adjusted R Square Standard Error Observations 0.32433 0.10519 -0.07377 0.04187 7 ANOVA Regression Residual Total df 1 5 6 SS 0.00103 O.OU77 0.00980 Intercept X Variable 1 Coefficients -0.02664 -0.00087 Standard Error 0.02853 0.00113 % 2 c Slope Uncertainty 261% Page 55 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 FOSA Buffer Hydrolysis Study at 50 C. All concentrations in ng/ml. pH Time (Days) 5.0 0 5.0 7 5.0 14 5.0 21 5.0 28 5.0 35 5.0 42 Cone. 470 455 440 435 442 461 457 ln([P]t/[P1o) 0.000 -0.032 -0.066 -0.076 -0.061 -0.019 -0.027 FOSA @ 50 C pH 5.0 - Rate constant graph 0.05 -, 0.00 - !-- * _________________ ST -0.05 - a. -o to - 1 -0.15 " -0.20 - =y - 2 .6 4 E - 0 4 x - 3 . 4 7 E - 0 2 R2 =2 .0 3 E - 0 2 10 20 30 40 Time (days) 50 pH Time (Days) Cone. ln([P]t/[P]o) 7.0 0 481 0.000 7.0 7 474 -0.015 7.0 14 465 -0.034 7.0 21 484 0.007 7.0 28 456 -0.055 7.0 35 488 0.014 7.0 42 479 -0.004 0.05 n 0.00 - S' -0.05 -0.10 ^ -0.15 -0.20 -0.25 0 FOSA @ 50 C pH 7.0 - Rate constant graph , ' y= 1.25E-04x-1.51E-02 R2= 6.06E-03 - --- T 10 -, - .... T- - - r- 20 30 40 Time (days) -----1 50 SUMMARY OUTPUT Repression Statistics Multiple R R Square Adjusted R Square Standard Error Observations 0.14235 0.02026 -0.17568 0.03036 7 ANOVA Regression Residual Total df 1 5 6 SS 0.00010 0.00461 0.00470 Intercept X Variable 1 Coefficients -0.03470 -0.00026 Standard Error 0.02069 0.00082 % 2a Slope Uncertainty 622% SUMMARY OUTPUT Repression Statistics Multiple R R Square Adjusted R Square Standard Error Observations 0.07787 0.00606 -0.19272 0.02653 7 ANOVA Regression Residual Total df 1 5 6 SS 0.00002 0.00352 0.00354 Intercept X Variable 1 Coefficients -0.01505 0.00013 Standard Error 0.01807 0.00072 % 2o Slope Uncertainty 1145% Page 56 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 FOSA Buffer Hydrolysis Study at 50 C. All concentrations in ng/ml. pH Time (Days) 9.0 0 9.0 7 9.0 14 9.0 21 9.0 28 9.0 35 9.0 42 Cone. 429 430 437 438 428 451 452 ln(rPM Pjo) 0.000 0.003 0.018 0.022 -0.002 0.050 0.052 SUMMARY OUTPUT Regression Statistics Multiple R R Square Adjusted R Square Standard Error Observations 0.78210 0.61167 0.53401 0.01555 7 0.10 FOSA @ 50 C pH 7.0 - Rate constant graph o.oo I -0.10 - 0.20 0 10 20 30 40 Time (days) 50 ANOVA Regression Residual Total Intercept X Variable 1 % 2a Slope Uncertainty 71% df 1 5 6 SS 0.00190 0.00121 0.00311 Coefficients -0.00410 0.00118 Standard Error 0.01060 0.00042 pH Time (Days) Cone. ln(fPM P]o) 11.0 21 445 11.0 0 446 0.000 11.0 7 445 -0.001 11.0 14 439 -0.017 11.0 28 438 -0.018 11.0 35 463 0.038 11.0 42 466 0.044 SUMMARY OUTPUT Regression Statistics Multiple R R Square Adjusted R Square Standard Error Observations 0.65519 0.42927 0.28659 0.02276 6 FOSA @ 50 C pH 11 - Rate constant graph 0.10 g 0.05 0.00 __ r- 5. -0.05 2 - 0.10 " -0.15 y = 1.07E-03X-1.47E-02 R1=4.29E-01 - 0.20 0 10 ' 20 30 40 Time (days) 50 ANOVA Regression Residual Total Intercept X Variable 1 % 2c Slope Uncertainty 115% df 1 4 5 SS 0.00156 0.00207 0.00363 Coefficients -0.01467 0.00107 Standard Error 0.01590 0.00061 Data in Italics excluded on the basis of data quality objectives; see text. Page 57 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 FOSA (Perfluorooctanesulfonamide) Hydrolysis Study 50C; pH 1.5 All concentrations in ng/ml. All areas x 10`3 FOSA MeOH Blank Data m e PFOSA003.D Time Point Ret Time 4.5 MeOH Blank 99039-135-02 99039-135-03 99039-135-04 PFOSA001.D PFOSA005.D PFOSA006.D PFOSA007.D 4,5 4.5 4.5 99039-135-05 99039-135-06 PFOSA008.D PFOSA009.D 4.5 4.5 Area 200 412 1060 2091 3951 Cone. < 12.5 53 101 252 513 1018 %Standard or %RSD 106% 102% 101% 103% 102% % Spike Recovery MeOH Blank MeOH Blank PFOSA014.D PFOSA015.D 4.5 < 12.5 4.5 < 12.5 80399PFOSA-001 80399PFOSA-002 80399PFOSA-003 80399PFOSA-004 80399PFOSA-025 80399PFOSA-026 8 0 3 9 9 P F O SA -0 27 80399PFOSA-028 80399PFOSA-049 80399PFOSA-050 80399PFOSA-Q51 80399PFOSA-052 80399PFOSA-073 80399PFOSA-074 80399PFOSA-075 80399PFOSA-076 PFOSA016.D PFOSA017.D PFOSA018.D PFOSA019.D PFOSA020.D PFOSA021.D PFOSA022.D PFOSA023.D PFOSA024.D PFOSA025.D PFOSA026.D PFOSA027.D PFOSA028.D PFOSA029.D PFOSA030.D PFOSA031.D Day 0 Day 0 Day 0 Day 0 Day 7 Day 7 Day 7 Day 7 Day 14 Day 14 Day 14 Day 14 Day 21 Day 21 Day 21 Day 21 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 1958 2005 1949 2789 1915 1940 1945 2911 1885 1881 1957 2850 1864 1931 1976 2810 474 481 469 689 459 465 467 703 447 438 443 684 439 447 463 652 1% 1% 1% 3% 86% 96% 97% 81% MeOH Blank MeOH Blank PFOSAG35.Q PFOSA036.D 4.5 <1 2 .5 4.5 < 12.5 80399PFOSA-097 80399PFOSA-098 80399PFOSA-099 80399PFOSA-100 80399PFOSA-121 80399PFOSA-122 80399PFOSA-123 80399PFOSA-124 8 0 3 9 9 P F O S A -1 45 80399PFOSA-146 8 0 3 9 9 P F O S A -1 47 8 0 3 9 9 P F O S A -148 PFOSA037.D PFOSA038.D PFOSA039.D PFOSA040.D PFOSA041.D PFOSA042.D PFOSA043.D PFOSA044.D PFOSA045.D PFOSA046.D PFOSA047.D PFOSA048.D Day 28 Day 28 Day 28 Day 28 Day 35 Day 35 Day 35 Day 35 Day 42 Day 42 Day 42 Day 42 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 1850 1840 1914 2905 1898 1896 1974 2682 1927 1871 1854 2898 437 441 444 699 448 455 470 651 451 434 439 700 1% 2% 2% 104% 77% 103% MeOH Blank MeOH Blank PFOSA049.D PFOSA050.D 4.5 < 12.5 4.5 < 12.5 99039-135-01 PFOSA051.D 99039-135-02 PFOSA052.D 4.5 195 50 101% 99039-135-03 PFOSA053.D 4.5 405 96 96% 99039-135-04 PFOSA054.D 4.5 1037 243 97% 99039-135-05 PFOSA055.D 4.5 2067 489 98% 99039-135-06 PFOSA056.D 4.5 3935 979 98% Method ID: 030 9J5 A .M Internal Standard quant: ^=0.999 Curve Averaged, Quadratic, Origin ignored Cai. range min. and max = 49.9 998 Original conc.= 499.4 Spike conc,= 249.7________________ (A) The relative standard deviation (RSD) is not defined when the mean concentration is zero. Ret Time 3.7 3.7 3.7 3.7 3.7 3.7 3.7 Area 25 119 238 611 1173 2154 Cone. < 13.0 15 54 104 264 531 1050 `/Standard or %RSD 104% 100% 102% 102% 101% 3.7 < 13.0 3.7 < 13.0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 593 255 3.7 0 0 3.7 0 0 3.7 0 0 3.7 596 250 3.7 0 0 3.7 0 0 3.7 0 0 3.7 590 246 3.7 0 0 3.7 0 0 3.7 0 0 3.7 597 242 (A) (A) (A) (A) 3.7 < 13.0 3.7 < 13.0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 589 246 3.7 0 0 3.7 0 0 3.7 0 0 3.7 587 249 3.7 0 0 3.7 0 0 3.7 0 0 3.7 592 248 (A) (A) (A) 3.7 < 13.0 3.7 < 13.0 3.7 28 16 3.7 115 51 98% 3.7 240 101 3.7 604 257 3.7 1160 506 97% 99% 98% 3.7 2177 1026 99% Internal Standard quant: ^=0.999 Cal. range min. and max = 51.9 ___________ Spike conc.= 259.40 % Spike Recovery 98% 96% 95% 97% 95% 96% 96% Ret Time Area 3.8 0 3.8 1008 3.8 1012 3.8 1022 3.8 1012 3.8 1029 3.8 1021 3.8 1031 3.8 1027 3.8 1026 3.8 1029 3.8 1032 3.8 1030 3.8 1051 3.8 1039 3.8 1058 3.8 1088 3.8 1056 3.8 1044 3.8 1065 3.8 1055 3.8 1088 3.8 1043 3.8 1028 3.8 1063 3.8 1054 3.8 1044 3.8 1027 3.8 1038 3.8 1039 3.8 1055 3.8 1060 3.8 1040 3.8 1051 3.8 3.8 3.8 3.8 3.8 Cone. mean S.D. %S.D. 1038 1053 1036 1046 1059 225 1042 18 1.8 % Page 58 of 126 BACK TO MAIN 3M hnvironmental Laboratory Report No. EL1132 FOSA (Perfluorooctanesulfonamide) Hydrolysis Study 50C; pH 3.0 All concentrations in ng/ml. All areas x 103 FOSA Time Sample Data PH* Point Ret Time MeOH Blank PFOSA058.D 4.5 99039-136-01 PFOSA059.D 99039-136-02 PFOSA060.D 4.5 99039-136-03 PFOSA061.D 4.5 99039-136-04 PFOSA062.D 4.5 99039-136-05 PFOSA063.D 4.5 99039-136-06 PFOSA064.D 4.5 __________ Area Cone. < 12.5 195 403 1059 2041 3909 48 99 262 516 1022 "/.Standard or %RSD 95% 99% 105% 103% 102% % Spike Recovery MeOH Blank MeOH Blank PFOSA069.D PFOSA070.D 4.5 0 < 12.5 4.5 0 < 12.5 80399PFOSA-005 80399 PFOSA-006 80399PFOSA-007 80399PFOSA-008 80399PFOSA-029 80399PFOSA-030 80399PFOSA-031 80399PFOSA-032 80399PFOSA-053 80399PFOSA-054 80399PFOSA-055 80399PFOSA-056 80399PFOSA-077 80399PFOSA-078 80399PFOSA-079 80399P FOSA-080 PFOSA071.D PFOSA072.D PFOSA073.D PFOSA074.D PFOSA075.D PFOSA076.D PFOSAQ77.D PFOSA078.D PFOSA079.D PFOSA080.D PFOSA081.D PFOSA082.D PFOSA083.D PFOSA084.D PFOSA085.D PFOSAOB6.D Day 0 Day 0 Day 0 Day 0 Day 7 Day 7 Day 7 Day 7 Day 14 Day 14 Day 14 Day 14 Day 21 Day 21 Day 21 Day 21 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 1972 1971 1984 2931 1919 1917 1981 2953 1908 1952 1890 3050 3565 1880 1805 2874 484 481 486 734 484 476 482 732 448 468 455 721 421 446 419 690 1% 1% 2% 3% 100% 100% 106% 105% MeOH Blank MeOH Blank PFOSA090.0 PFOSA091.D 4.5 < 12.5 4.5 < 12.5 80399PFOSA-101 80399PFOSA-102 80399PFOSA-103 80399PFOSA-104 80399PFOSA-125 80399PFOSA-126 80399PFOSA-127 80399PFOSA-128 80399PFOSA-149 80399PFOSA-150 80399PFOSA-151 80399PFOSA-152 PFOSA092.O PFOSA093.D PFOSA094.D PFOSA095.D PFOSA096.D PFOSA097.D PFOSA098.D PFOSA099.D PFOSA100.D PFOSA101.D PFOSA102.D PFOSA103.D Day 28 Day 28 Day 28 Day 28 Day 35 Day 35 Day 35 Day 35 Day 42 Day 42 Day 42 Day 42 4.5 1871 4.5 1857 4.5 1883 4.5 2873 4.5 1933 4.5 1953 4.5 1898 4.5 2962 4.5 1958 4.5 1984 4.5 1867 4.5 2911900 458 455 458 700 467 471 464 730 471 479 448 695 0% 1% 3% 98% 105% 92% MeOH Blank PFOSA104.D 4.5 < 12.5 MeOH Blank PFOSA105.D 4.5 < 12.5 99039-136-01 PFOSA106.D 99039-136-02 99039-136-03 PFOSA107.D PFOSA108.D 4.5 201 4.5 411 48 98 96% 98% 99039-136-04 PFOSA109.D 4.5 1056 254 102% 99039-136-05 PFOSA110.D 4.5 2108 472 94% 99039-136-06 PFOSA111.D 4.5 3986 977 98% Method ID: 0309_15A.M Internal Standard quant: ^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min. and max = 49.9 998 Original conc.= 499.4 Spike conc.= 249.7 (A) The relative percent deviation (RPD) is not defined when the mean concentration is zero. PFOS _____________ ________________________ Ret Time 3.7 Area Cone. < 13.0 "/Standard or %RSD % Spike Recovery 3.7 25 11 3.7 117 51 3.7 232 101 3.7 614 273 3.7 1171 540 3.7 2160 1064 98% 98% 105% 104% 103% 3.7 0 < 13.0 3.7 0 <1 3 .0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 593 256 3.7 0 0 3.7 0 0 3.7 0 0 3.7 593 253 3.7 0 0 3.7 0 0 3.7 0 0 3.7 621 253 3.7 0 0 3.7 0 0 3.7 0 0 3.7 585 242 (A) (A) (A) (A) 99% 98% 98% 97% 3.7 < 13.0 3.7 < 13.0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 589 248 3.7 0 0 3.7 0 0 3.7 0 0 3.7 601 255 3.7 0 0 3.7 0 0 3.7 0 0 3.7 598 246 (A) (A) (A) 96% 98% 95% 3.7 <1 3 .0 3.7 < 13.0 0.0 27 12 3.7 115 49 94% 3.7 239 101 98% 3.7 615 265 102% 3.7 1191 484 93% 3.7 2205 1014 98% Internal Standard quant: 1^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min. and max = 51.9 1038 Spike co ne .- 259.40 FBSA Ret Time 3.8 3.8 3.8 3.8 3.8 3.8 Area 0 0 1041 1041 1044 1045 1054 3.8 0 3.8 0 3.8 1073 3.8 1080 3.8 1076 3.8 1075 3.8 1045 3.8 1060 3.8 1082 3.8 1086 3.8 1118 3.8 1098 3.8 1092 3.8 1137 3.8 2222 3.8 1108 3.8 1128 3.8 1116 3.8 0 3.8 0 3.8 1074 3.8 1074 3.8 1081 3.8 1101 3.8 1089 3.8 1091 3.8 1077 3.8 1091 3.8 1095 3.8 1091 3.8 1094 3.8 1123 3.8 0 3.8 0 3.8 3.8 3.8 3.8 3.8 Cone. mean S.D. % S .D . 1067 1072 1076 1176 1120 225 1116 186 16.7% Page 59 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 FOSA {Perfluorooctanesulfonamide) Hydrolysis Study 50C; pH 5.0 All concentrations in ng/ml. All areas x 10"3 FOSA Sample ID . MeOH Blank 99039-137-01 99039-137-02 99039-137-03 99039-137-04 99039-137-05 99039-137-06 - Data Fit PFOSA003.D PFOSA004.D PFOSA005.D PFOSA006.D PFOSAO7.D PFOSA008.D PFOSA009.D ' > Time Ret Time 4.5 4.5 4.5 4.5 4.5 4.5 Area 194 419 1026 2059 4043 Cone. < 12.5 51 101 246 495 986 %Standard or %RSD 102% 101% 98% 99% 99% % Spike Recovery MeOH Blank MeOH Blank PFOSA014.D PFOSA015.D 4.5 < 12.5 4.5 <1 2 .5 80399PF OSA-009 PFOSA016.D Day 0 4.5 2010 80399PFOSA-010 PFOSA017.D Day 0 4.5 2039 80399PFOSA-011 PFOSA018.D Day 0 4.5 2003 80399PFOSA-012 PFOSA019.D Day 0 4.5 3010 80399PFOSA-033 PFOSA020.D Day 7 4.5 1934 80399PFOSA-034 PFOSA021.D Day 7 4.5 1956 80399PFOSA-035 PFOSA022.D Day 7 4.5 1935 80399PFOSA-036 PFOSA023.D Day 7 4.5 3030 80399PFOSA-057 PFOSA024.D Day 14 4.5 2285 80399PFOSA-058 PFOSA025.D Day 14 4.5 1964 80399PFOSA-059 PFOSA026.D Day 14 4.5 1942 80399PFOSA-060 PFOSA027.D Day 14 4.5 3055 80399PFOSA-081 PFOSA028.D Day 21 4.5 1966 80399PFOSA-082 PFOSA029.D Day 21 4.5 1980 80399PFOSA-083 PFOSA030.D Day 21 4.5 1853 80399PFOSA-084 PFOSA031.D Day 21 4.5 2945 472 470 468 705 446 461 458 716 436 441 443 684 443 450 413 703 0% 2% 1% 5% 94% 96% 97% 81% MeOH Blank MeOH Blank PFOSA035.D PFOSA036.D 4.5 < 12.5 4.5 < 12.5 80399PFOSA-105 80399PFOSA-106 80399PFOSA-17 8 0 3 9 9 P F O S A -1 08 80399PFOSA-129 80399PFOSA-130 80399PFOSA-131 8 0 3 9 9 P F O S A -1 32 8 0 3 9 9 P F O S A -1 53 8 0 3 9 9 P F O S A -154 80399PFOSA-155 80399PFOSA-156 PFOSA037.D PFOSA038.D PFOSA039.D PFOSA040.D PFOSA041.D PFOSA042.D PFOSA043.D PFOSA044.D PFOSA045.D PFOSA046.D PFOSA047.D PFOSA048.D Day 28 Day 28 Day 28 Day 28 Day 35 Day 35 Day 35 Day 35 Day 42 Day 42 Day 42 Day 42 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 1873 1888 1869 2863 1949 1926 2007 2957 1926 1947 1887 2963 444 446 437 692 461 453 468 705 459 461 452 705 1% 2% 1% 104% 77% 103% MeOH Blank MeOH Blank PFOSA049.D PFOSA050.D 4.5 < 12.5 4.5 < 12.5 99039-137-01 PFOSA051.D 99039-137-02 99039-137-03 99039-137-04 PFOSA052.D PFOSA053.D PFOSA054.D 4.5 197 4.5 404 4.5 1015 52 100 246 103% 100% 98% 99039-137-05 99039-137-06 PFOSA055.D PFOSA056.D 4.5 2083 4.5 4003 510 1011 102% 101% Method ID: 0309 15B.M Internal Standard quant: ^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min and max = 49.9 998 Original conc.= 499.4 Spike conc.= 249.7 (A) The relative percent deviation (RPD) is not defined when the mean concentration is zero. Ret Time 3.7 3.7 3.7 3.7 3.7 3.7 3.7 Area 26 118 236 579 1171 2218 Cone. < 13.0 15 54 103 254 523 1028 %Standard or %RSD 104% 99% 98% 101% 99% % Spike Recovery 3.7 0 < 13.0 3.7 0 < 13.0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 596 249 3.7 0 0 3.7 0 0 3.7 0 0 3.7 598 252 3.7 0 0 3.7 0 0 3.7 0 0 3.7 634 253 3.7 0 0 3.7 0 0 3.7 0 0 3.7 598 254 (A) (A) (A) (A) 96% 97% 98% 102% 3.7 < 13.0 3.7 < 13.0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 575 248 3.7 0 0 3.7 0 0 3.7 0 0 3.7 571 243 3.7 0 0 3.7 0 0 3.7 0 0 3.7 592 251 (A) (A) (A) 95% 94% 97% 3.7 < 13.0 3.7 < 13.0 3.7 26 3.7 118 15 54 104% 3.7 236 105 101% 3.7 576 255 98% 3.7 1147 521 100% 3.7 2179 1046 101% Internal Standard quant: ^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min. and max = 51.9 1038 Spike conc.= 259.40 Ret Time Area 3.8 0 3.8 1054 3.8 1075 3.8 1062 3.8 1070 3.8 1099 3.8 0 3.8 0 3.8 1092 3.8 1113 3.8 1098 3.8 1115 3.8 1110 3.8 1087 3.8 1082 3.8 1106 3.8 1341 3.8 1141 3.8 1124 3.8 1165 3.8 1137 3.8 1127 3.8 1147 3.8 1094 3.8 0 3.8 0 3.8 1081 3.8 1086 3.8 1095 3.8 1081 3.8 1083 3.8 1088 3.8 1100 3.8 1095 3.8 1076 3.8 1082 3.8 1070 3.8 1098 3.8 0 3.8 0 3.8 3.8 3.8 3.8 3.8 Cone. mean S.D. %S.D. 1050 1054 1051 1051 1063 225 1099 49 4.5% Page 60 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 FOSA (Perfluorooctanesulfonamide) Hydrolysis Study 50C; pH 7.0 All concentrations in ng/ml. All areas x 10'3 FOSA Time Sample ID. Data Fite Point Ret Time MeOH Blank PFOSA057.D 4.5 99039-138-01 PFOSA059.D 99039-138-02 99039-138-03 PFOSA06.D PFOSA061.D 4.5 4.5 99039-138-04 PFOSA062.D 4.5 99039-138-05 PFOSA063.D 4.5 99039-138-06 PFOSA064.D 4.5 Area 203 412 1050 2035 3978 Cone. < 12.5 48 97 258 496 1003 ________ ____________P F O S ___________________________________________________ FBSA /.Standard or % Spike /Standard or % Spike %RSD Recovery Ret Time Area Cone. %RSD Recovery Ret Time 3.7 < 13.0 3.8 3.7 26 11 3.8 97% 3.7 122 52 101% 3.8 97% 3.7 238 101 97% 3.8 103% 3.7 597 264 102% 3.8 99% 3.7 1155 516 100% 3.8 100% 3.7 2162 1044 101% 3.8 Area 0 0 1043 1060 1030 1050 1040 MeOH Blank MeOH Blank PFOSA069.D PFOSA070.D 4.5 < 12.5 4.5 < 12.5 3.7 < 13.0 3.7 <1 3 .0 3.8 0 3.8 0 80399PFOSA-013 PFOSA071.D Day 0 4.5 1974 80399PFOSA-014 PFOSA072.D Day 0 4.5 1992 80399PFOSA-015 PFOSA073.D Day 0 4.5 1977 80399PFOSA-016 PFOSA074.D Day 0 4.5 2979 80399PFOSA-037 PFOSA075.D Day 7 4.5 1936 80399PFOSA-038 PFOSA076.D Day 7 4.5 1899 80399PFOSA-039 PFOSA077.D Day 7 4.5 1968 80399PFOSA-040 PFOSA078.D Day 7 4.5 3004 80399PFOSA-061 PFOSA079.D Day 14 4.5 2006 80399PFOSA-062 PFOSA080.D Day 14 4.5 1921 8Q399PFOSA-Q63 PFOSA081.D Day 14 4.5 2131 80399 PFOSA-064 PFOSA082.D Day 14 4.5 2955 80399PFOSA-085 PFOSA083.D Day 21 4.5 1943 80399PFOSA-086 PFOSA084.D Day 21 4.5 2000 80399PFOSA-087 PFOSA085.D Day 21 4.5 2109 8 0 3 9 9 P F O SA -0 88 PFOSA086.D Day 21 4.5 3153 486 476 482 733 469 474 480 737 457 469 470 710 479 484 490 738 1% 1% 2% 1% 101% 105% 98% 101% 3.7 0 0 3.7 0 0 3.7 0 0 3.7 583 252 3.7 0 0 3.7 0 0 3.7 0 0 3.7 593 256 3.7 0 0 3.7 0 0 3.7 0 0 3.7 603 255 3.7 0 0 3.7 0 0 3.7 0 0 3.7 613 252 (A) (A) (A) (A) 97% 98% 98% 101% 3.8 1039 3.8 1070 3.8 1048 3.8 1051 3.8 1055 3.8 1025 3.8 1048 3.8 1056 3.8 1121 3.8 1046 3.8 1159 3.8 1076 3.8 1037 3.8 1056 3.8 1100 3.8 1106 MeOH Blank MeOH Blank PFOSA090.D PFOSA091.D 4.5 <12.5 4.5 < 12.5 3.7 < 13.0 3.7 < 13.0 3.8 0 3.8 0 8399PFOSA-110 PFOSA092.D Day 28 4.5 1813 8Q399PFOSA-111 PFOSA093.D Day 28 4.5 1884 8 0 3 9 9 P F O S A -1 12 PFOSA094.D Day 28 4.5 1876 8 0 3 9 9 P F O S A -1 13 PFOSA095.D Day 28 4.5 2876 8 0 3 9 9 P F O S A -1 33 PFOSA096.D Day 35 4.5 1935 8 0 3 9 9 P F O S A -134 PFOSA097.D Day 35 4.5 2089 80399PFOSA-135 PFOSA098.D Day 35 4.5 2009 80399PFOSA-136 PFOSA099.D Day 35 4.5 2918 80399P FOSA-157 PFOSA100.D Day 42 4.5 1993 8399PFOSA-158 PFOSA101.D Day 42 4.5 1939 80399PFOSA-159 PFOSA102.D Day 42 4,5 1932 80399PFOSA-160 PFOSA103.D Day 42 4.5 2980 446 458 463 711 474 497 493 721 487 480 471 723 2% 3% 2% 102% 93% 98% 3.7 0 0 3.7 0 0 3.7 0 0 3.7 574 250 3.7 0 0 3.7 0 0 3.7 0 0 3.7 583 253 3.7 0 0 3.7 0 0 3.7 0 0 3.7 585 250 (A) (A) (A) 96% 98% 96% 3.8 1038 3.8 1050 3.8 1037 3.8 1045 3.8 1044 3.8 1075 3.8 1043 3.8 1047 3.8 1047 3.8 1032 3.8 1049 3.8 1066 MeOH Blank PFOSA104.D 4.5 < 12.5 MeOH Blank PFOSA105.D 4.5 <12.5 99039-138-01 PFOSA106.D 99039-138-02 PFOSA107.D 4.5 200 49 97% 99039-138-03 PFOSA108.D 4.5 413 101 101% 99039-138-04 PFOSA109.D 4.5 1023 253 101% 99039-138-05 PFOSA110.D 4.5 2017 496 99% 99039-138-06 PFOSA111.D 4.5 3998 996 100% Method ID: 0309 15B.M Internal Standard quant: 1^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min and max = 49.9 998 Original conc.= 499.4 ___ _______ Spike conc.= 249.7 (A) The relative percent deviation (RPD) is not defined when the mean concentration is zero. 3.7 < 13.0 3.7 < 13.0 3.7 26 12 3.7 116 51 98% 3.7 237 103 100% 3.7 589 262 3.7 1144 517 3.7 2166 1032 101% 100% 99% Internal Standard quant: ^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min. and max = 51.9 1038 Spike cone.- 259.40 3.8 3.8 3.8 3.8 3.8 3.8 3.8 Cone. mean S.D. %S.D. 0 0 1023 1026 1023 1040 1052 225 1054 28 2.6% Page 61 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 FOSA (Perfluorooctanesulfonamide) Hydrolysis Study 50C; pH 9.0 All concentrations in ng/ml. All areas x 10`3 - Sample 1.0. MeOH Blank 99039-139-01 99039-139-02 99039-139-03 99039-139-04 99039-139-05 99039-139-06 Data Fila PFOSA003.D PFOSA004.D PFOSA005.D PFOSA006.D PFOSA007.D PFOSA008.D PFOSA009.D Tma Point Ret Time 4.5 Area 4.5 196 4.5 420 4.5 1056 4.5 2258 4.5 3943 Cone. < 12.5 56 98 229 498 953 "/Standard or %RSD 111% 98% 92% 100% 95% % Spike Recovery MeOH Blank MeOH Blank PFOSA014.D PFOSA015.D 4.5 < 12.5 4.5 < 12.5 80399PFOSA-017 PFOSA016.D Day 0 4.5 1948 80399PFOSA-018 PFOSA017.D Day 0 4.5 1921 80399PFOSA-019 PFOSA018.D Day 0 4.5 1948 80399PFOSA-020 PFOSA019.D Day 0 4.5 2936 80399PFOSA-041 PFOSA020.D Day 7 4.5 1947 80399PFOSA-042 PFOSA021.D Day 7 4.5 1945 80399PFOSA-043 PFOSA022.D Day 7 4.5 1894 80399PFOSA-044 PFOSA023.D Day 7 4.5 2760 80399PFOSA-065 PFOSA024.D Day 14 4.5 2054 80399PFOSA-066 PFOSA025.D Day 14 4.5 1931 80399PFOSA-067 PFOSA026.D Day 14 4.5 1982 80399PFOSA-068 PFOSA027.D Day 14 4.5 2872 80399PFOSA-089 PFOSA028.D Day 21 4.5 1893 80399PFOSA-090 PFOSA029.D Day 21 4.5 1970 80399PFOSA-091 PFOSA030.D Day 21 4.5 1985 80399PFOSA-092 PFOSA031.D Day 21 4.5 2960 434 425 427 683 431 435 423 628 435 431 443 669 430 440 444 691 1% 1% 1% 2% 102% 79% 93% 101% MeOH Blank MeOH Blank PFOSA035.D PFOSA036.D 4.5 < 12.5 4.5 < 12.5 8 0 3 9 9 P F O S A -1 13 8 0 3 9 9 P F O S A -1 14 8 0 3 9 9 P F O S A -1 15 8 0 3 9 9 P F O S A -1 16 8 0 3 9 9 P F O S A -1 37 80399PFOSA-138 80399PFOS A-139 80399PFOSA-140 80399PFOSA-161 8 0 3 9 9 P F O S A -1 62 8 0 3 9 9 P F O S A -1 63 80399PFOSA-164 PFOSA037.D PFOSA038.D PFOSA039.D PFOSA040.D PFOSA041.D PFOSA042.D PFOSA043.D PFOSA044.D PFOSA045.D PFOSA046.D PFOSA047.D PFOSA048.D Day 28 Day 28 Day 28 Day 28 Day 35 Day 35 Day 35 Day 35 Day 42 Day 42 Day 42 Day 42 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 1883 1849 1850 2813 1948 1936 1917 2933 1872 1929 1951 2831 431 422 430 686 450 452 450 711 444 452 459 697 1% 0% 2% 103% 104% 98% MeOH Blank PFOSA049.D 4.5 < 12.5 MeOH Blank PFOSA050.D 4.5 < 12.5 99039-139-01 PFOSA051.D 99039-139-02 PFOSA052.D 4.5 190 57 113% 99039-139-03 PFOSA053.D 4.5 408 99 100% 99039-139-04 PFOSA054.D 4.5 1050 245 98% 99039-139-05 PFOSA055.D 4.5 2165 521 104% 99039-139-06 PFOSA056.D 4.5 3835 1042 104% Method ID: 0309 15C.M Internal Standard quant: 1^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min. and max = 49.9 998 Original conc,= 499.4 Spike conc.= 249.7 (A) The relative percent deviation (RPD) is not defined when the mean concentration is zero. Ret Time 3.7 3.7 3.7 3.7 3.7 3.7 3.7 Area 26 114 248 612 1232 2172 Cone. < 13.0 22 55 102 244 505 985 %Standard or %RSD 106% 99% 94% 97% 95% % Spike Recovery 3.7 < 13.0 3.7 < 13.0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 572 230 3.7 0 0 3.7 0 0 3.7 0 0 3.7 577 230 3.7 0 0 3.7 0 0 3.7 0 0 3.7 581 235 3.7 0 0 3.7 0 0 3.7 0 0 3.7 584 235 (A) (A) (A) (A) 89% 89% 90% 94% 3.7 < 13.0 3.7 < 13.0 3.7 0 0 3.7 0 0 3.7 0 0 3.7 557 235 3.7 0 0 3.7 0 0 3.7 0 0 3.7 579 241 3.7 0 0 3.7 0 0 3.7 0 0 3.7 559 237 (A) (A) (A) 90% 93% 91% 3.7 < 13.0 3.7 < 13.0 3.7 26 23 3.7 112 57 3.7 242 105 3.7 597 256 3.7 1218 547 109% 101% 99% 105% 3.7 2127 1089 105% Internal Standard quant: 1^=0.999 Curve Averaged, Quadratic, Origin ignored Cal. range min. and max = 51.9 1038 Spike conc.= 259.40 Ret Time Area 3.8 0 3.8 997 3.8 1029 3.8 1016 3.8 1022 3.8 1038 3.8 0 3.8 0 3.8 1002 3.8 1008 3.8 1016 3.8 1007 3.8 1006 3.8 997 3.8 996 3.8 1018 3.8 1052 3.8 1000 3.8 998 3.8 1003 3.8 981 3.8 999 3.8 998 3.8 1005 3.8 0 3.8 0 3.8 974 3.8 975 3.8 958 3.8 962 3.8 968 3.8 958 3.8 953 3.8 974 3.8 941 3.8 955 3.8 952 3.8 955 3.8 0 3.8 0 3.8 3.8 3.8 3.8 3.8 Cone. mean S.D. % S .D . 941 981 942 942 946 225 986 30 3.0% Page 62 of 126 BACK TO MAIN <3M bnvironmental Laboratory Report No. EL1132 FOSA (Perfluorooctanesulfonamide) Hydrolysis Study 500; pH 11 All concentrations in ng/ml. All areas x 10'3 FOSA ... = , S am ple J.D. ; *& DataPIte TNne ?Point Ret Time MeOH Blank PFOSA058.D 4.5 99039-140-01 PFOSA059.D 99039-140-02 PFOSA060.D 4.5 99039-140-03 99039-140-04 PFOSA061.D PFOSA062.D 4.5 4.5 99039-140-05 99039-140-06 PFOSA063.D PFOSA064.D 4.5 4.5 Area 196 393 1031 1995 3844 Cone. < 12.5 53 96 242 475 998 "/.Standard or %RSD 107% 96% 97% 95% 100% % Spike Recovery Ret Time 3.7 3.7 3.7 3.7 3.7 3.7 3.7 Area 27 115 227 596 1126 2139 Cone. < 13.0 20 54 99 255 491 1026 /.Standard or %RSD 104% 95% 98% 95% 99% % Spike Recovery MeOH Blank MeOH Blank PFOSA069.D PFOSA070.D 4.5 < 12.5 4.5 < 12.5 3.7 < 13.0 3.7 < 13.0 80399PFOSA-021 80399PFOSA-022 80399PFOSA-023 80399PFOSA-024 80399 PFOSA-045 80399PFOSA-046 80399P FOSA-047 80399PFOSA-048 80399PFOSA-069 80399PFOSA-070 80399PFOSA-071 80399PFOSA-072 80399PFOSA-093 80399PFOSA-094 80399PFOSA-095 80399PF OSA-096 PFOSA071.D PFOSA072.D PFOSA073.D PFOSA074.D PFOSA075.D PFOSA076.D PFOSA077.D PFOSA078.D PFOSA079.D PFOSA080.D PFOSA081.D PFOSA082.D PFOSA083.D PFOSA084.D PFOSA085.D PFOSA086.D Day 0 Day 0 Day 0 Day 0 Day 7 Day 7 Day 7 Day 7 Day 14 Day 14 Day 14 Day 14 Day 21 Day 21 Day 21 Day 21 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 1906 1884 1856 2893 1852 1884 1906 2810 1933 1782 1855 2845 1871 1913 447 450 440 707 437 446 453 692 459 427 430 692 446 445 445 445 1% 2% 4% (B) 105% 99% 101% (B) 3.7 0 0 3.7 0 0 3.7 0 0 3.7 568 236 3.7 0 0 3.7 0 0 3.7 0 0 3.7 570 239 3.7 0 0 3.7 0 0 3.7 0 0 3.7 584 242 3.7 0 0 3.7 0 0 3.7 0 0 3.7 0 0 (A) (A) (A) (A) 91% 92% 93% 0% MeOH Blank MeOH Blank PFOSA09Q.D PFOSA091.D 4.5 < 12.5 4.5 < 12.5 3.7 < 13.0 3.7 < 13.0 8 0 3 9 9 P F O S A -1 17 8 0 3 9 9 P F O S A -1 18 8 0 3 9 9 P F O S A -1 19 80399PFOSA-120 80399PFOSA-141 80399PFOSA-142 80399PFOSA-143 80399P FO SA -144 80399PFOSA-165 8 0 3 9 9 P F O S A -1 66 80399PFOSA-167 80399 PFOSA-168 PFOSA092.D PFOSA093.D PFOSA094.D PFOSA095.D PFOSA096.D PFOSA097.D PFOSA098.D PFOSA099.D PFOSA1Q0.D PFOSA101.D PFOSA102.D PFOSA103.D Day 28 Day 28 Day 28 Day 28 Day 35 Day 35 Day 35 Day 35 Day 42 Day 42 Day 42 Day 42 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 1829 1886 1853 2800 1949 1921 1911 2819 1955 1831 1956 2793 435 436 444 697 461 464 464 704 473 444 482 703 1% 0% 4% 104% 96% 95% 3.7 0 0 3.7 0 0 3.7 0 0 3.7 558 237 3.7 0 0 3.7 0 0 3.7 0 0 3.7 567 241 3.7 0 0 3.7 0 0 3.7 0 0 3.7 550 236 (A) (A) (A) 91% 93% 91% MeOH Blank PFOSA104.D 4.5 < 12.5 3.7 <1 3 .0 MeOH Blank PFOSA105.D 4.5 < 12.5 3.7 < 13.0 99039-140-01 PFOSA106.D 3.7 25 19 99039-140-02 99039-140-03 PFOSA107.D PFOSA108.D 4.5 187 4.5 406 53 101 107% 101% 3.7 109 54 3.7 234 104 105% 100% 99039-140-04 PFOSA109.D 4.5 998 247 99% 3.7 583 262 101% 99039-140-05 PFOSA110.D 4.5 2105 533 107% 3.7 1185 549 106% 99039-140-06 P F O S A 1 1 1.D 4.5 3653 998 100% 3.7 2068 1049 101% Method ID: 03Q9_15C.M Internal Standard quant: 1^=0.999 Internal Standard quant: ^=0.999 Curve Averaged, Quadratic, Origin ignored Curve Averaged, Quadratic, Origin ignored Cal. range min and max = 49.9 998 Cal. range min and max = 51.9 1038 Original conc.= 499.4 Spike conc.= 249.7 Spike conc.= 259.40 (A) The relative standard deviation (RSD) is not defined when the mean concentration is zero. (B) Excuided; samples 80399PFOSA-094 and -095 not analyzed, due to human o r mechanical error; no spike added to sample 80399PFOSA-096. Ret Time 3.8 Area 0 3.8 932 3.8 934 3.8 927 3.8 936 3.8 951 3.8 0 3.8 0 3.8 946 3.8 929 3.8 935 3.8 951 3.8 938 3.8 936 3.8 935 3.8 941 3.8 937 3.8 923 3.8 956 3.8 953 3.8 932 3.8 953 3.8 953 3.8 953 3.8 0 3.8 0 3.8 932 3.8 959 3.8 927 3.8 931 3.8 940 3.8 921 3.8 916 3.8 930 3.8 922 3.8 916 3.8 905 3.8 922 3.8 0 3.8 0 3.8 3.8 3.8 3.8 3.8 Cone. mean S.D. %S.D. 882 913 880 890 903 225 930 19 2.1% Page 63 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Pooled FOSA Data and Slope Regression 0.10 0.05 0.00 Ji>-1 O _Q _ O (L -0.05 -I c .................... --- . . Solid Line: - 0.10 y = -4.425E-06X - 1.997E-02 R2 = 2.751 E-06 _o. "o o O o o o _o_ .............. -0.15 -i - 0.20 Dashed Lines: 2a Uncertainty Limits (Slope and Intercept) 10 20 30 time (days) oo o o 40 50 SUMMARY OUTPUT Regression Statistics Multiple R 0.001658616 R Square 2.75101E-06 Adjusted R Squa Standard Error -0.025638204 0.038763091 O b s e rv a tio n s 41 % 2o slope uncertainty 19309 ANOVA Regression Residual Total df SS 1 1.61211E-07 39 0.058600511 40 0.058600673 MS 1.61211E-07 0.001502577 F Significance F 0.00010729 0.991788409 Intercept X Variable 1 Coefficients Standard Error -0.019972663 0.010823282 -4.42532E-06 0.000427234 t Stat -1.84534255 -0.01035807 P-value 0.072590288 0.991788409 Lower 95% -0.041864795 -0.000868587 Upper 95% 0.00191947 0.000859736 Lower 95.0% -0.041864795 -0.000868587 Upper 95.0% 0.00191947 0.000859736 Page 64 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 EL11320.xls 4/2/2001 5:46 PM Rate and T1/2Calculations Author: GMP Shaded results included in the report.________________________________ Incubation time (days)_____________________4.200E+01________ Parent FOSA Analyte (LOQ) PFOS Analyte (LOD) PFOS Rates and Half-Lives from LOQ (Eq's B32, B33, and B41) Rates and Half-Lives from LOD (Eq's B38, B39, and B41) Parent Mass (gm/mole) 4.990E+02 Analyte Mass (gm/mole) 5.379E+02 Analyte Mass (gm/mole) 5.379E+02 Max Rate @50C (day-1) 2.300E-03 Max Rate @50C (day-1) 5.749E-04 Parent P0 (ng/ml) 4.994E+02 Analyte LOQ (ng/ml) 5.200E+01 Analyte LOD (ng/ml) 1.300E+01 Max Rate @25C (day-1) 2.300E-04 Max Rate @25C (day-1) 5.749E-05 Rates and Half-Lives from mean (p.) and standard deviation (2o) concentrations: (Eq's B36, B37, and B41) Max Rate @50C (day-1) Max Rate @25C (day-1) 1.802E-03 1.802E-04 mean = 4.5 5 1 E + 0 2 s td e v = 1.7 2 2E + 0 1 Date: 4102101 Parent P0 (nm/ml) 1.001E+00 Analyte LOQ (nm/ml) 9.667E-02 Analyte LOD (nm/ml) 2.417E-02 M ihHal^Llfe @25C (year) 8.3 : ' : Min Half-Life@25C (year) 33 ' Min Half-Life @25C (year) 11 Pooled Data Regression Slope 2c Minimum (day-1) Regression Slope Value (day-1) Regression Slope 2c Maximum (day-1) (Eq's B8, B9, and B41) Slopes @50C (day-1) -8.686E-04 -4.425E-06 8.597E-04 Max. H-Life @25C (year) (N/A - slope positive) Slopes @25C (day-1) -8.686E-05 -4.425E-07 8.597E-05 Calc. H-Life @25C (year) 4291 Min. Half-Life @25C (year) 22 Page 65 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Appendix D: Selected Chromatograms A representative set of chromatograms from the present study is included in this Appendix. Page 66 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 3 o f 57 D a ta F i l e C :\H P C H E M \l\D A T A \012400\P F Q S A 003.D M S D `1 4 9 9 r E IC = 4 9 8 :6 :4 9 9 :r( 0 1 2 4 0 0 \P F O S A 0 0 3 :D r~ A P r-E S rN e g rs iM " 450 400 350 300 12 34 M S D r2 9 8 rE IC = 2 9 7 :7 :2 9 8 ^ 7 7 0 1 2 4 0 0 \P F O S A 0 0 3 ;D ) A P F E S , N e g7 S IM ------------ 600 400 ^ S a m p l e N a m e : MeOH B l a n k FOSA Hydrolysis pH 1.5 MeOH Blank 12 34 - M S D r 3 1 2 r E IC = 3 r r .7 :'3 1 2 ` 7"f0 12 40 0 \P F O `S A 0 0 3.D ) APr-ES7fsTeg7SIM ----------- 1000- i 500 12 34 ' M S D T 4 9 8 7 E lC "= 4 9 7 :5 :4 9 8 :5 _(O i2 4 0 0 \P F O S A 0 0 3 :D ) A Pr*ES7 N e g T S IM ------------ 400 -j 3 5 0 : 300 1 1 52 ' ' ' ' ' ' ' 4~ M S D T5 1 2rE IC = 51 'T7 7:5 12 ".7 '(0 12 4 00 \P FO S A 00 3TD ) A P I: E S 7 N e g T S lM ------------ 350 300- ' - v/" ' - _1 ' ' ' ' 5 "" 4 M S D r 3 6 9 , E [C = 3 68.7;36977~ (012400\P FO S A 003:D ) A P F E S 7 N e g , S IM ----------- 5 0 0 -I 400 _ _ T i ' ' ' ' 5 ' ' ' ' 5 ' ' ' ' 3T M S D 1 T 0 8 , E IC 5 1 0 7 .7 ri0 8 :r(0 1 2 4 0 0 \P F O S A 0 0 3 :D 7 ~ `A P r E S ;N e g 7 S IM ------------ 350 3 0 0 - \_/\ Ny \ / 1 .2 34 - M S D `r6 1 6 rE IC = 6 1 5 I7 :6 1 6 7 7 '(0 f2 4 0 0 V P F O S A 0 0 3 T D l- A P tE S , N e g T S IM '.... -- 350 325 300 / Y 275 1 --. f'. 2 ' 'i 4 M S D 1 '6 3 0 7 E IC = 6 2 9 i7 :6 3 0 .7 7 0 1 2 4 0 0 \P F O S A 0 0 3 .D y 'A P r -E S , N e gT S IM ------------ / ' .. /\ ,, 400 350 300- 12 34 M S D T 5 2 67 E IC = 52 5 17 :'52 6 :7 `(0 1 2 4 0 0 \P F O S A 0 0 3 .D )' ' A P I-E S ; N e g V S IM ----------- 400 : 3 5 0 -i 300 -i- 12 _ M SD4'427rE[C=426:7:427:7"(0T2400\PFO SA003:D) 34 A P F E S 7 N e g 7 S IM ------------ 600 400- Data4 9/21/00 12:38:00 PM AES/ALS Page 2 of 6 Page 67 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 5 o f 57 D a ta F i l e C :\H P C H E M \l\D A T A \012400\P F O S A 005.D " M SD1 4 99 7E 1C=498:61499:7"(0T2400\P FO S A005:d j A PP E S 7N gTS IM ~ 10000-j 5000 3 nL ^so= 12 34 M S D T 2 9 8 7 E 1 C = 2 9 7 7 :2 9 8 7 7 _(0 T Z 4 00 \P F O S A 00 5 'D ) 100000 -1 A P P E S 7 N e g 7 S lM ------------ < CO m. ! 50000 ~ : 04 12 34 _ M S D T3T27H rC =31T.7f312T'(0T2400\P FO SA '005D )" A Pr:ES7Neg7SIM 150000 - 100000 50000 - 04 12 3 ~M S D i'498rE IC =497.5r498:5T 0T 2400\P F O S A 005:D )"_ A P rE S 7 N e grS IW _ ~ 4 " 20000- 1QQ00- 0 12 3 ''M S D r5127E IC =51177T5T2.7C ai2400\P FO S A005.D )''"A P r-E S 7N eg7S IM 4 20000 10000^ 0 "" T - j ' ' ' j ' T 1 ' 5 ' T ' T V _ M S D T3697 E !C = 36 8 77 y3 69 r7 _{0 T 2 4 0 0 \P F O S A 0 0 5 D l A P f; E S 7 N g7 S IM S am ple Nam e: 9 9 0 3 9 -1 3 5 -0 2 FOSA Hydrolysis pH 1.5 Std 2 -1 st inj /u.\ /(pO'\ / 0- 400 -j 350 300 -] . 250 -i .A '1' 2 11 3 ' M SD1 6 30 ,` E IC = 6 2 9 7 :6 3 0 :7 'f0 T 2 4 0 0 \P F O S A 0 0 5 .D r "API-E S 7N egT S IM 4 400 300 1' ' ' 1 ' ' ' ' 2 ' ' ' ' 3 ' ' 'F M SD1 5 2 6 rE IC = 5 2 5 :7 :5 2 6 :7 "(0 1 2 4 0 0 \P F O S A 0 0 5 :D ) A P I-E S 7 N e g 7 S IM 20000 10000i 0-U 1 2 3 ____4 - M S D i-4 2 7 7 E IC = 4 2 6 :7 r4 2 7 :7 _(012400\PFOSA'O O 5 ;D r ~ A P I-ES7 N egT S IM " 10 0 0 0 0-i4 l(OuL_,\ /f\ Data4 9/21/00 12:38:21 PM AES/ALS :o&c/>>. 5____ __6 Page 2 of 4 Page 68 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 12 o f 57 D a ta F i l e C :\H P C H E M \1\D A T A \012400\P F O S A 012.D ~ M S D T 4 9 97 E IC = 49 8 .6:499.7 (0 1 2 4 0 0 \P F O S A 0 T 2 :D r'A P I-E S 7 N e g 7 S IM ' 1000 : 750 1 o . u. ' 0. 500 i 250 C 1 ~ M S D r29 87E [C = 297T :'2987 r(0124 00\P F O S A 0 12;D P ~ A P r-E S ;~ N e g7S IM ~ i 600 a I 500 4 i -too \ i 300 V // ~MSDr3127ErC=3T177`:3127" (012400\PFOSA012iD) APFES7Neg7SIFiT 1000-, 500 4 123 4 - MSD1"4987EIC=497:5r49ir5` (0't2400\PFOSA"0rT2:Dr" API-ES7Neg7SlM -------~ S am ple Nam e: 0 8 1 3 9 9 -B L K -1 .5 FOSA Hydrolysis pH 1.5 Matrix Blank 4000 2000 - bata4 9/21/00 12:39:27 PM AES/A _________ 6 Page 2 of 4 min Page 69 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 13 of 57 Data File C:\HPCHEM\l\DATA\012400\PFOSA013.D M S D 1 493TEIC =498137499:7_(0 1 2 4 0 0 \F F O S A 0 1 3 :D ) R P I-E S 7 N e g T S IM " 60000 7 40000 20000 J 04= 12 ~M S D T 29 8 7E !C =2 97 7 7f2 98 7 7~ (0 T 24 00 \P F O S A 0T 3T J) 3 APP:E S 7 N e g 7 S IM 4 " 100000 i 50000 -i 0-tr 12 3 "M S D r3 1 2 rE IC = 3 1 T 7 :3 1 2 7 7 "(0T2400\P FO S A 013;D )'~ A P i;E S 7N eg7S IM -- 4 150000 - 100000 50000 O-*1 ' * ' .. i ' ' ' 5 T' ' f 5 ' ' ' ' MS D T 4 9 8 ,"E IC =4971549875 (0"12400\P FOSOT3ID) APPES7NeflTS1M i~ 1 00000 -j J50000 4 o -L 1 ''' 'TWSDT5T2TEiC=5TT77T5T277^0i2i00\PFOSA0T3TD) 3 APFESTNegTSIM 4 100000 - 50000 0 ' J1 ' ' ' ' ' ' 3 ~ ' ' ' 4~~ 'M S D r 3 6 9 ;E IC = 3 6 8 :7 :3 6 9 :7 '(0 1 2 4 0 0 \P F O S A 0 1 3 7 D r" A P r E S 7 N e g /S lM ------------ S am p le Nam e: 0 8 1 3 9 9 -L C S -1 .5 FOSA Hydrolysis pH 1.5 Lab Control !K\ /M0. 100000-! 50000 12 3 ~ M S D 1 _4 2 7 rE lC = 4 2 6 '.7 r4 2 7 :7 '(0 1 2 4 0 0 \P F O S A 0 1 3 :D } A PI:ES7Neg7SIM Oc/) I 10000-j 4 Data4 9/21/00 12:39:36 PM AES/ALS S(P/) Page 2 of 4 Page 70 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 18 of 57 Data File C:\HPCHEM\l\DATA\012400\PFOSA018.D ~M S D T499rE rC =498:6I49977"(012400\PFOSA0T8:D) A P!-ES7N egTSlM ~ 10000- S am ple Nam e: 80399PFO SA -003 FOSA Hydrolysis pH 1.5 Day 0 - Sample Trip 123 ~MSD1 2 98 7E 1 0 = 2 9 7 :7 :2 9 8 ^ ( 0 1 2 4 0 0 \P F O S A 0 T 8 X )p "A P ^ E S r;N e g , SIM 4 100000 50000 <GO CO Li a 0 '' ' 1 1 ' i. 1 3 MSD1 312, EIC =311,7:312.7 (O lZ400\P FO $A 018.D ) AHI-tb, Neg, bIM 150000J 100000 - 50000 - 0 1^ ' 2' M S m 498, E l0=49775:498:5 {012400\PFOSA0'187Dy 3 A PI-E S i'N egTSIM 200000 - 4 4 100000 0 - . - ............ ..................... . - .............................................. - 11 i 3 ~ M S D T 5 1 2 7 EIC=5T177:5T277"fO12`40Q \P F O S A 0 18 .D ) A P r-E S , N e g T S IM " 4 1000 750 500 250 - _ __________________ _____________________ J \_ 123 -M S D r3 6 9 ;E IC = 3 6 8 :7 :3 6 9 :7 '(0 1 2 4 a 0 \P F a S A 0 1 8 .D J "--A P I-E S , N eg, S IM 800 600 400- A /V _____ ... 1 1 ' ' '2 ' ' 3 "M S O 1 T 0 8 , E IC =107;71108.7TD 'T2400\P FO S A 018:D ) A P I-E S , NegTSTM 4 1000 500- A 12 3 M S D l 616, E IC =615,7:616.7 (012400\PFOSA018.D ) A P l-E b, Neg, bIM 4 - PFOSA 5 5 ,1 / E> 5 6 min 6 min 6 min 5 '6 min .j 6 ' ' min 5 6 min ---- 1------ ) ---1------ r- '---------5 6' ' m in 300 250 v / ' x 1 '2 ~5 ' MSD1 630, ElC =629.7:630.7 (0124UU\HFOSAO18.D) A P l-h b , Neg, bIM 400 300- ! 23 MSD1 526, tlC = 5 2 5 .7:526V (0124U0\PKJSA018.L>) A P I-tb , Neg, bIM 400 300 i ' ___ --------- -- - " 10000 0 12 MSD1 427rE lC =4267:4277'(012400\P FO S A 0T8TD ) 12 3 APPESV N eg.'SIM 01 o s t. > 3 Data4 9/21/00 12:40:24 PM AES/ALS 4 4 - 4 4 5 - . -- - 5 6 min ." .- 6 min 5 6 min 5 6 __ m in Page 2 of 4 Page 71 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL 1132 B a tc h R un # 19 o f 57 D a ta F i l e C :\H P C H E M \l\D A T A \012400\P F O S A 019.D 'MSm49g7EIC=498T6r499;770T2400\PFOSA0T91D5 APPES7N5g7SlM_ 6 0 0 0 0 -; 40000 - 20000 oU_ /CL. o4 =CL=n=rr 12 34 MSDT'2S3rEIC=297T:298:r(0T2'400\PFOSA0T 9 X ))~ A P FES',' NgTSIM----- j 100000 4 w< ' 50000 \ /.U00_:, ,D-\ 04; 12 34 "WSD1 ~3127EIC=31Y.7:312.7`(012400\PFOSA019.D)' API-ES, NegTSIM--------- 150000 : 1 0 0 0 0 0 -j ' 50000 I oi= 12 34 ~MSDT4987EIC=497:5r49875"X0T2400\PFOSA019ID) API-ES7Neg7'SIM--------- ! 200000 3 I 100000^ 0-fe MSDT512, EIC=i511.7:5T2.7'(01240i0\PFOSA0ig.Dr' APiI-ES, NegTSIM--1---4-' 100000 : 50000 ' o' ' ' ' ' ' ' '2 ' '' '3 ' 4 M S D 1 3 69 7E IC = 36 87 7 369771012 4 0 0 \P F O S A 0 1 9 ;D )'" A P I-E S : N e gT S IM ------------ 750 500 2501 i 3 MSDri087E1C=107:7;108:7'(012'400\PFOSA019:DpAPr-ES:Neg7SIM"' 4 S am ple Nam e: 80399PFO SA -004 FOSA Hydrolysis pH 1.5 Day 0 - Sample Spike la>\ ,&o\ < ;fot 500 400 300- "' 1 ' ' ' '2 ' ' ' '3 4 - MSD1'5267EIC=525r7T52677"(0T2400\PFOSA0'197D) API-ES7 NegTSIM--------- 10000011 50000 4 0-L 12 - MSDr4277EIC=426'.7i427;7~(012400\PFOSA019:D) 34 APPESTNegTSIM--------- 15000 10000 d 5000 -j 04=: Data4 9/21/00 12:40:33 PM AES/ALS :oW ' u. . i CL 5 Page 2 of 4 Page 72 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 47 of 57 Data File C:\HPCHEM\l\DATA\012400\PFOSA047.D I _M S D 1 - 490TE IC =498:6r49977XC rT2400\P FO SA 047:D )` ~~API-ESl N e g 7 S iM r' 10000^ 0i - 12 MSD1 2987E !C=297;7:298:7-(02400\PFO SA047.D) 100000- 3 API-ES7N g7SlM ; 5 00 00 -i I 0-1 12 3 ~M S D r3T27E IC =3TT7:3i27T(0'12400\P FO S A 047TD ) API-ES7N eg7SIM 100000 7 50000 \ 0V T " M S D T 4 9 8 7 E IC=497:5749875~(0T2400\PFOSA047:D)" ~AP FES7Ng7S 4 4 : 100000 t '0 1000 . t 11' j ' ' 1' j 1' ' ' 27ErC=5TT7T5`1 2 7 7 0 1 2 i0 0 \P F O S A I3 4 7 :D y ^A P IiS 7 N e g ,S IM ----------- 500 "" . t ' 1 ' ' j ' ' ~ r " 5 ' ' 1 ' V ~ M S D r 3 6 9 7 E lC = 3 6 B :7 :3 6 g ;r(0 1 2 4 0 0 \P F O S A W X )r~ A P rE S 7 N e g , S IM ------------ S am p le Nam e: 8 0 3 99PFO SA -147 FOSA Hydrolysis pH 1,5 Day 42 - Sample Trip //k0n.-'' < /A<M 4001 350 \ 300 -f 250 !. ' '1 2 MSD1 '4277EIC=42B'.7r427;7"(0f2400\PFOSA047TD) 3 A P F E S 7 N e g 7 S IM ------------ 150001 10000i 5000 \ o4 Data4 9/21/00 12:44:55 PM AES/ALS Page 2 of 4 Page 73 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL.1132 B a tc h R un # 48 o f 57 D a ta F i l e C :\H P C H E M \1\D A T A \012400\P F O S A 048.D - M S D 'T 4997E ie= 49876:4997`(0T24001PFOSA048:D) 6 0 0 0 0 = 4 0 0 0 0 -j 20000 i 04= API-E S 7N eg7SlM ~ w .ou. 12 34 ~MSD1 29a7EIC=2977:2987(012400\PFO SA048.D J--API-ES7Neg7SIM---------- 1000004 $ 50000 - 0L 12 34 M S D 1 3 1 2 , E IC =31 177:312:71012 40 0\P FO S A 0 48 :D >-- A P l-E S 7 N e g . S IM ---------- I 100000 j I 50000 4 i 04 - t ' j ' ' 1 1 3 ' ' 1 ' J~ M S D 1 -4987E 1 C =4 9 7.5 :4 9 8:5 ` (0 1 2 4 0 0 \P F O S A 0 4 8 .D A P I-E 5 ,7 4 ig 7 S IW ----------- 200000 -j 1000001 0-L ~1 ' ' '2' ' ~3 ' ' ' ' i M SD1 5127EICH5T177:5127 (0TZ400\PFO SA0487DJ A P I-E S 7 N e g 7 S IM ----------- 100000] 50000 0 '\ 1 3 .......................... i ' ~MSD1~3697EIC=3687:369.7 (012400\PFOSA048:D) API: ES7Neg7SIM---------- 1000 750 500 250 TT THSD1 1087EIC=T07.7:108.71012400\PFOSA048:D) APFES7Neg7SIM~ 800 600 400- 200 -t- 1 '3' ' ' ' 3' ' T W S 01 6 1 6 7 E IC = 6 1 5 7 :6 1 6 7 (0 1 2 4 0 0 V P F O S A 0 4 8 :D } A P I-E S 7 N e g 7 S IM ---------- 500 400 300 _y\_. T '5 3 ' ' ' i~ "B IS D T 6 3 0 7 E rC 5 6 2 9 7 :6 3 0 :r( 0 1 2 4 0 0 \P F O S A 0 4 8 :D r" A P F E S 7 N S g 7 S H r--------- 5 0 0 -j 400 j 300 i 12 34 'M S O r5 2 6 7 E IC = 5 2 5 7 T 5 2 6 7 (0 1 2 4 0 C \P F O S A 0 4 8 7 D r~ A P F E S 7 N e g .S IM ---------- 100000 -j 50000 -j 0-1= 12 ' M S D r427rE IC =426'.7:427T'(0'12400\P F O S A 048;D ) 3 A PI-ES7N eg7SlM ' 15000 \ 10000 5000 0->= a. 1; Hx . ' 4 S am p le Name: 80399PF O S A -148 FOSA Hydrolysis pH 1.5 Day 42 - Sample Spike < mQ\\ i\ :0 : u. a. Data4 9/21/00 12:45:03 PM AES/ALS Page 2 of 4 Page 74 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 50 of 57 Data File C:\HPCHEM\l\DATA\012400\PFOSA050.D M SD T 499; EIC=498.6y499.7'(012400\PFOSA050T>) APFES7NigTSIM ' 450 400 350 1 M S D ~ rZ 9 87 E rC = 2 9 7:7 :2 9 8 ` 7 X 0 1 2 4 0 0 \P F O S A 0 5 0 :D r ~API: E S 7 N e g,~ S lM -------------- 500 J 400 /' J S a m p le N a m e : MeOH B l a n k FOSA Hydrolysis pH 1.5 MeOH Blank M SD r3'127EIC =31'i:7:3'12;r(0`12400\P FO SA050:D r_APFES7Neg. SIM ` 1000- 500- __________ i 23 MSU1 498, EIC=497.5:498.5 (U12400\PFOSA50.D) AP-ES, Neg, SIM 600 500- 4 3 m s u i 512, ElC=5t1.7:512.7 (l2400\PFOSA050.D) API-fcS, Neg, SIM 400 i 350- 1 300 - r i ii 'WSD1 369. EIC=368.7:369.7 (012400\PFOSA050'D) API-ES, Neg,S IM 4 800 600- A 400- ,__ -------------- _--------_ _ - .. ' 1 ' ' ' ' ' ' ' ........................... MSD1 106, ElC=107.7:108.7 (12400\PFOSA050X)) API-ES, Neg, SlM 300 280 / - . ^ _____ . /- 260- 1 i 3 "MSD1 616, EIC*615.7:616.7 (0l2400\PFOSA050TD) API-fcS, Neg, SIM 350- 325 - 300 v ~ -____ ^ \ 7 \ / - - V A - __ A ___ 4 r\ j i ' 3 4 'M S m 6307EIC=62977:630T710'12400\PFOSA0507D} API:ES, Neg. SlM------ [' ooo oo l- 1 2 3 4 M SD I 526, c 1C=525.7526,7 (01Z400\PF05A050X>) API-ES, NegTSIM 400 -j 350 -] ^ / 123 M5U1 427, EIC=426.77427.7 (012400\PFOSA0507D) API-ES, NgTSIM 4 600 ^ 400-' Data4 9/21/00 12:45:23 PM AES/ALS 56 5 56 56 56 5 - - 5 5 6 6 -- 6 -------- 5 ____ ________ 6 Page 2 of 6 Page 75 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 52 o f 57 D a ta F i l e C :\H P C H E M \1\D A T A \012400\P F O S A 052.D S am p le Nam e: 9 9 0 3 9 -1 3 5 -0 2 M S D 499, E IC =498:6:4997r(012400\PFO S A 052.D ) 10000 5000 0 12 M S D T 2 9 8 , EIC=297.7:298E7 (012400\P F O S A 052:D ) 100000 50000 012 MSD1 312, E IC = 3 i 1.7:312.7 (012400\PFO S A 052.D ) A PI-E S , Neg,' SIM " V) o u. Q. .. 3 A P I-E S T N e g T S IM 4 t<o .CD. ,U_. 1.__ 3 API-ES, Neg, S M 4 100000i 50000 n j ... '^ 2 MSD1 498, E IC =497.5:498.5 (012400\PFOSA052.D ) 20000 3 A P I-tS , Neg, SIM 10000 0- 12 M S01 512, E IC -5 1 1 .7:512.7 (012400\PFUSA052.DJ 3 A PI-E S , Neg, SIM 4' 4 20000 10000 0- t2 ~M SD1'369, E rC =368.7T369.7l012400\P FO S A 052.D ] 800 600 - 400 - 3 A PI-ES.NegTSIM 4' / 123 'MSCT1 T08, E IC = 1 0 7 .7 :1 0 8 T '(0 1 2 4 0 0 \P F O S A 0 5 2 :0 ) A'Pr-ES, N eg, SIM 4' 1000 - 750 f\ 500 250-U V - ___________________________ 1 MSD1 616, E lC = 6 l5 .7 :S l6 ,7 (0l2400\P F O S A 052.U ) 3 A P I-h S , Neg, SIM A 350 /\ . _ _^ ------. -- 250- \y ... . . . ,^ _. i ' ' ' ' ' MSDT630, EIC=629i7:630T7~(012400\PFOSA052^Dj API-ES7Ng, SIM 4 4 ' FOSA Hydrolysis pH 1.5 Std 2 - 2nd inj 5 6 min 5 < ,to / " . 5 < to ,o\ 6 '1 6 5' ' ' '6 /tot /S\ ! o- ' . 5 ' ' ------------ ............ 5 ' ' ' m in m in .m in . 5' ' 6 ' min; 5 6 min 400 300- - 2' 3' '4 5 6 min MSD1 526, E IC =525.7 :525.7 (0 1 2 4 0 0 \P F O S A 0 5 2 0 ) A PI-ES, Neg, SIM -| 20000 -i 10000 1 n j ___________________________ -- s GO - OLL CL 123 M S D T 427, E iC = 42 6.7:427.7 (012400\P F Q S A 052.D ) A P I-E S , Neg, SIM 4' 6 min 1 10000 4 - a !F V 1 2 3 4 5 6 m in Data4 9/21/00 12:45:43 PM AES/ALS Page 2 of 4 Page 76 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 2 o f 55 D a ta F i l e C :\H P C H E M \l\D A T A \012400\P F O S A 058.D MSD1 499, EIC=498:6:499.7~(0124a0\PFOSA05B:Dr_APr-ES7NegrSIM~ 450 A 4 0 0 -j 3 5 0 -! 12 34 M S D 1"2987EIC =297:7:298r7"(0124001PF O S A 058TD J A P F E S 7 N e g 7 S IM ------------ 500 400 300 12 34 M S D 1 3 1 2 , E IC = 3 1 1 .7 :3 1 2 .7 `(0 1 24 00 \P F O S A 05 8 :D ) A P I: E S 7 N e g 7 S IM ----------- 1000 4 500 J 1' 'Y ' 3 '~ T M S D 1 4 9 8 7 E IC = 4 9 7 :5 T 4 9 8 .5 (0 1 2 4 0 0 \P F O S A 0 5 8 .D ) A P I: E S7N eg7`S IM ------------ S a m p l e N a m e : MeOH B l a n k FOSA Hydrolysis pH 3 MeOH Blank 500 1 1.___ _ --y -.y / ,'- 12 34 'M S D 1 5 1 2 , E IC = 5 1 t7 ;5 1 2 T 7 f0 1 2 4 0 0 \P F O S A 0 5 8 .D ) A P I-E S 7 N e g 7 S IM ------------ 400 300 t' i" 'M S D 1 369,EIC =368.7:369:7f012400\P FO S A058.D ) A A P l-E S 7 N e g 7 S IM ------------ 800 6 0 0 -] 40 . ^ 1J ' 1 ' " 3 /\ ( ' ' '5 ' MSD'1 108, E tC = 1 0 7 :7 f1 0 8 ;7 '(0 1 2 4 0 0 \P F O S A 0 5 8 :D J ~ A P I-E S 7 N e g 7 S IM ------------------------- 320 J 300 280 260 ^ - 1' t / -A - -- j 1 t t ' j " T T 1 37 M S D T O 6 . E[C=657T6T6.7'(0'12400\PF05A058.D) API-ES; Neg7S[M 350 325 j 300 -L ~T~' ' 1 1 MSD1'630,"EIC=629i7:63CT7l012400\PFOSA05&D] 3 "4 APrES7Neg7SlM-- ..... ' V- ' "5 ' / ......... ' ; 400 j 350 : 300 ! 12 34 'M S D T5267E 1C =525'.7:526.7(012400\P FO S A 058:D ) API-ES7N eg7SIM 600 ' 400 - 12 3 "M SD 1""4277EIC=:426.7:4277~(012400\PFO SAD58.D) A P 7 E S !`Neg7SIM 4 600 500 400 5_____________ 6 ............... Data4 9/26/00 1:04:37 PM AES/ALS Page 2 of 6 Page 77 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run I 4 of 55 Data File C:\HPCHEM\1\DATA\012400\PFOSA060.D M S D 1'499, EIC =49876749971012400\PFO SA060;D} A PFE S 7N eg7SIM ~ 10000 5000 0 _ 12 34 M S D T 2 9 8 , E IC ='2 9 7 ;7 :2 9 8 T X a T 2 4 0 0 \P F O S A 0 6 0 :D )-- A P I-E S ;N e g T S IM ---------- 100000- 50000 0-^ ] h\ 5 TT' ' 5 TTr 4 " MS D 1 3 1 2 rE IC = 3 1 T 7 :3 1 2 .7 '(O r12400\P F O S A 060. D )-- A P I: E S T N e gTS IM 100000 -1 50000 0 4= 1 " M SD 14987EIC =497:5749B.5(012400\PFO SA060.D ) A PI-E S 7N eg7SIM _ : 20000 ; ! 10000 4 0-L 12 34 M S D T 512 7 E IC = 5 1 1 7 :5 1 2 7 1 0 1 2400\P FO S A0607D ) A P I: ES7"Neg7SIM------------ 20000 10000 0 ' 1 1 ' j ' 1 ' 13 1 ~T M S D r369 7E IC =3 68:7 :36 97' {01240mPFOSA060:DT--AP FES 7N ig7SIM ----------- 4000 2000- M 1T MSD1 1087E !C =107:7:10871012400\P FO SA 060:D ) APFES7Neg7S!M S am ple Nam e: 9 9 0 3 9 -1 3 6 -0 2 FOSA Hydrolysis pH 3 Std 2 -1st inj 5< </) icQ /' fi /fOuw_'.-, . Q5 500 ] 2' ' ' 3 T ' J~~ M S D T 6 '1 6 7 E IC = 6 1 5 7:6 *1 6 :7 1 0 1 2 40 0 \P F O S A 0 6 0 X f) A P I-E S 7 N e g 7 S IM ------------ . 1I 350 I \ / - ' VI 300 -I : 250-] '' ' 'r - V V '-" x ' 1 ' $ ' 1 1 T5 TTr ' 4 MSD1 630 r E IC =629~7:630T~(0T2400\P FO S A0607D ] A P I-E S T N e g T S lM ------------ 400 1 350, ' 300- j 250 1 2 T 1 ' ' T ' i~ M S D 5267EIC=525:7:526^7 (012400\PFOSA060TD) API-ES7 NegTSIM 20000 4 10000 J 0-U 12 "~ M S D T 4 27 7 E [C = 42 6 ?7 r4 27 7 7T 0 T 2 40 0\P F O S A 0 60 7 D ) 34 API-ES7 NegTSIM- "" 1150000000 5000 0 Data4 9 / 2 6 / 0 0 1:04:57 PM AES/ALS s /O' 5_________ 6......... Page 2 of 4 Page 78 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL 1132 B a tc h Run # 11 o f 55 D a ta F i l e C :\H P C H E M \1\D A T A \012400\P F O S A 067.D ~M S01 4 9 9 ; e IC =4 9 8 :6 :4 9 9 .7 (0 1 24 00 \P F O S A '06 7 .'D )--A P rE S T N e g T S IM 1000 750 500 4 250 12 3 "M SDT2987Erc=297:7:29fl77"(0'12400\PFOSA067;D] API-ES7Neg7 SIM 600 400 - 4 12 3 'M S D T3T27E IC ^31T7:312^7'(0T2400\P FO S A 0677D ) AP-ES7N g7SIM 1500 , 1000- 500 4 " 1 1 ' T ' ' ..... 7 ' T T 3 T ' r T 4 ~ "M 5 D 1 4987E IC =497:5:498:5" C012400\PFOSA067:D)-- A PI-ES7N eg7SIM 1705000 .;1\ 5000 4 250 . ^ 1 ' T ' T2 " T T' 3 T 7 ^ " 1 MSDTTT27EIC=5'1T7:5'12T1(0T2400\PFOSA067X)r_APr-ES7Neg7SIM S am p le Name: 0 8 1 3 9 9 -B L K -3 .0 FOSA Hydrolysis pH 3 Matrix Blank A 400 12 3 'M SD1'5267EIC=525:7;526:7{012400\PFOSA067.T))" ~API-ESrNeg7SIM 1000 -I 750 J 500 - 250 ----------V - 12 "M SD 1 4277E lC 426:7f427'7(012400\P FO S A 067.D ) 3 A PI-ESrNeg7SIM 3000 - 2000 1000 4 4 Data4 9/26/00 1:05:59 PM AES/ALS Page 2 of 4 Page 79 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 12 o f 55 D a ta F i l e C :\H P C H E M \1\D A T A \012400\P F O S A 068.D MSDr49grEIC=4983r499:r{0'12400\PFOSA068:D r`APr-ES:NegrSIM" 450 400 350 S am p le Name: 0 8 1 3 9 9 -L C S -3 .0 POSA Hydrolysis pH 3 Lab Control 12 34 ~M$Dr298rElC=297.y:298TTOT24O0\PFOSA068;D) API-ES7NegT$IM-------- 600 500 400 300 12 34 MSDr3T2THlC^31177:3iZr(012400\PFOSA068;D)"`APr-ESrNeg7SlM -------- i 1000 I I 500 /\ - ' ' T ' ' ' 1 T ' ' J 1 ' ' ' J" M S D 'P f98 7 P fC = 49 7 :5 T4 98 :5~ {0 12 4 00 O 3F O S A 0 68 :D ) A P rE S 7 N e g 7 S IM ------------ 400J 350-j 300-'ML SDr5T27EIC515Ti:7:512TT[0T2400\PFOSA068X)r_ATPreS7NegrSIM- / 350 300 l--_ / 1 1 1 ] 1 1 ' ' 2 ' ' ' ' 5 ' ' ' ' 4~ M S D 1 3 6 9 7 E IC = 3 6 8 ;7 :3 6 9 :r(0 1 2 4 0 0 \P F O S A 0 6 8 :D )^ A P I-E S 7 N e g 7 S IM ------------ 500 400 ' ' ' 1' ' ' ' ' M S D 4 _T 0 8 7 E IC = 1 0 7 :7 :1 0 87 7'(012400\P FO S A 068'.D ) 3' Y A P P E S 7 N 0 7 S lM ----------- 325 300 r \ 2757 \ J --y\. ~MSDin516rEICT=515yr6T6:7T01240T0\PFOSA068:D)~"API-ESrNeg7S1Kr \/ 340 320 300 --j -- s -- y ~MSDr6307EIO629'.7:6307'(012'400\PF0SA06B:D) APr-ES7Neg7SIM-------- 4004 350i / V,- _ 300 ! T i ' r~~' T i T " ' T 5 ' tr _ M S D 1 `5 26 7 E rC = 5 2 5 ;7 :5 2 6 ;7 "(0124 00 \P F O S A 06 8 ^D ) A P I: E S 7 N e gT S lM ----------- 400 i 350 300 12 34 ~ M S D 1 `4 2 7 ; E iC -4 2 6 .7 :4 2 7 .7 (0 1 2 4 0 0 \P F O S A 0 6 8 T ))^ 'A P F E S 7 N e ff7 S lM ------------ 600 500 400 Data4 9 / 2 6 / 0 0 1 :0 6 : 0 8 PM AES/ALS Page 2 of 6 Page 80 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 17 o f 55 l F i l e C :\H P C H E M \1\D A T A \012400\P F O S A 073.D S am p le Name: 80399PF O S A -007 M S D 1 4 99 ; E IC = 4 9 8 .6 :4 9 9 .7 (0 1 2 4 0 0 \P F O S A 0 7 3 ID ) A P I-E S . Neg, SIMTM~ : 10000- ! i' 1 2 3 4 'M S D T 2 9 8 7 E IC = 2 9 7 7 7 :2 9 8 7 r(0 i2 4 '0 0 \P F O S A 0 7 3 .'DJ A P I^E S T N eg T S lM ' 100000 31 ,Scoi 15 00 00 3 0 ------------- _ / .' --------------_ ------------------------------------ ------------------------------------ -- o 23 MSD1 312, E IC =31T 7:312.7 (012400\P F O S A 073.D )~A P I-E S , Neg, SIM 4 100000^ 50000 H 'i 24 M S D T 4 9 8 , EIC=49775f498.5 (012400\PFOSA0737D) A PI-E S , NegTSIM 200000 - 100000 - 4` 1 in ;CO 1 u_ \ ! Q- s A i' 2'' 4 M S O T 51 2 rE IC = 5 1T .7 :51 2:7 (012400\PFO S A 073,D ) A P i: ES, Neg, SIM 4 1000 750 500, 250 J .. ! A / L_ 2 3' ~MS D T 3 6 9 ^ E fC = 3 6S773369.7-(0T2 4 00\P FO SA0737D) API-ES,* N eg, SIM 4' FOSA Hydrolysis pH 3 Day 0 - Sample Trip 5 6 m jn 5 6 m in 5 6 min 5 6 min 5 '' m in 3000 2000 1000- A. ' 1234 M S D T 1 0 8, EIC=1O7.7:10er7 (0 1 2400\P F O S A 073:D r~A P I-E S , Neg, S IM - ' ; 1000 A 500 _ jv . ___________________________ I \ 2 3 4' j ~MSD1 6 TB, E IC = 6 1 5 I7 :6 1 6 .7 (012 4 0 0 \P F O S A 0 7 3 ID r A P F E S , N eg, S IM j 300 250 / -- j . i 234 ! MSD1 630, E 1C =629.7:630!77012400\PFO SA073:D) APEES,' Neg, SIM 400 ' /' i 300 P - - 1 ,. .., - ........ ............' ^ 4 M SDr5267EIC =525.7:526(7~(0T2400\PFO SA073ID] A PI:ES7NegTSIM 43500014 .. _ _ / _\ / 300 -1 ,, ________----------------------------- ~ - " ~ ' r ..... 5 ' ' '6 min 5* 6 56 m in ,i min. 5 6 ......... m in 2 3 4 5 6 . min -------------- M S D r 4 2 7 - E (C E 4 26 :7 ;4 2 7 i7 ^ 0 i 2 4 0 0 \P F O SA 07 3 .D )" A P l:E S , Ne g ( S IM 3 V) 15000 O 5000 : in \ h- . 1 2' 3 4 5 6 min Data4 9/26/00 1:06:54 PM AES/ALS Page 2 of 4 Page 81 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL 1132 B a tc h Run # 18 o f 55 D a ta F i l e C :\H P C H E M \l\D A T A \012400\P F O S A 074.D " 'M S D 1 `4 9 9 7 S C = 4 9 8 7 6 :4 9 9 X (0 1 2 4 0 0 \P F O S 0 7 4 X )J 16 0 0 0 0 40000 20000 0 APFES7W eg7SIM~" GO o, ,,l l . /CL. 12 34 ~ M S D `1` 2 98 rE IC = 2 9 7 7 7 :2 9 8 ` 7 -(0'12400\P FO S A 074*D J A P I-E S T N e g T S lM ------------ ; 100000- j 50000 - : o- 12 34 'M S D '1 '3 1 2 7 E IC = 3 1 1 7 7 :3 i2 7 7 '{O T 2 4 0 0 \P F S 0 7 4 7 D ) A P F E S T N e g T S IM ------------ 100000 -i 5 00 00 -i 0-L *' ' 1 ' ' ' ' '' '3 4 M SD1 4987E !C = 49 77 5 :4 9 87 57 0 12 4 00 \P F O S A 07 4.D ) ' A P I-E S 7N eg 7 S 1 M ------------ Ij ! 2000001 j 100000 J : 04= 5 ' 'J ' ' ' '3 ' ' ' '\ 'MSDT5127EIC=5T177:51277~i0T2i00\PFOSA0747DJ PFES7Neg7SIM--------- 100000J 5 00 00 -j 0-W 12 ~ M S D T 3 6 9 7 E lC = 3 6 8 7 7 7 3 6 9 7 "(042400\P F O S 0747D ) 4000 4 Ja 34 A P I: E S 7 N e g T S IM ------------ 2000- S am p le Nam e: 80399PF O S A -008 FOSA Hydrolysis pH 3 Day 0 - Sample Spike /u. ' I aS m\ IO i 't 234 " M S D 1 108. E !C = 1 07:77108777012 4 0 0 \P F O S A 0 7 4 .D ) A P 0 E S 7 N e d 7 S IM ------------ 1000 500- A 12 3 M S D 1 6 1 e r E IC = 6 1 5 :7 :6 1 6 T T 0 12400VPFO SA074.DJ A P I-E S , N g ? S IM 350 i - .300 7j ~ \ . 250il V_,/ r " .... -- --i - 1 i ............ M SD r6307E lC =62977:630T`(0T2400\PFOSA0747D] API: ES7Ng7SIH 4 / h 400 300- 1 ' ' ' '2 ' ' ' '3' 4 ~ M S D T 52 6 7H lC = 5 2 5 i7 :5 2 6 .7 "(0 1 2 4 0 0 \P F O S 0 7 4 7 D ) A P I-E S 7 N e g 7 S IM ----------- :, 1000001j I 5 00 00 -j ! . o4= 12 34 - M S D T4277ElC=426.7T42777'i(0T2400\PFO SA074:D) A P i: ES7N 7SIM ' 15000 10000 J 5000 0 /' Data4 9/26/00 1:07:01 PM AES/ALS m ia OU-'-\ n. 5____ _ 6 ________ Page 2 of 4 Page 82 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 46 of 55 Data File C:\HPCHEM\l\DATA\012400\PFOSA102.D ~ M S D T 4 9 9 7 E IC = 4 9 8 7 6 :4 9 9 I7 ~(012400\PFOSA'102'.D) A P I-E S 7 N e g 7 S IM ~ 10000 0- 12 34 M 5 D r 2 9 8 ;` E | C 2 9 7 ;7 :2 9 8 T 3 0 2 4 0 0 \P F O S A 1 0 2 .D ) A P I; E S |N e g 7 S IM ------------ : 100000 $ 50000 S am ple Nam e: 80399PFO SA -151 FOSA Hydrolysis pH 3 Day 42 - Sample Trip 1 ' ' ' '2 ' ' ' '3 ' ' MSD1 312, E IC -3 1 1,7:312.7 (012400\PFO SA102.D ) API-ES, N6g, SlM 4' 100000 50000 0- ' 1' ' '3 1' MSD1 4 98 ,'E IC = 49 7 .'5:498.5 C012400\PFOSA102.DJ_ A PI-E S , Neg, SIM 4 , //I8L.\ . ' 0. 5 5 ' 6 6 min. min 100000 0- - - ... 12 M SD1 5121 E IC = 5 T 1 T :5 1 2 .7 "(0 't2 4 0 0 \P F O S A '1 0 2 :0 ) ....... - 3 A PFE S , N eg, SIM 1000 'A Ol oo /\_ 4000 2000 12 MSU1 369, bl(J= 368.7 :3 6 9 ./ {12400\PFOSA102.U) A 3 A Pl-ES, Neg, SlM 1\ ) ` , '5 . . Tg ' ^' ...m n r^ __ ____ -- - __ ................. .................... ........ ' ' 6 min i .. . . . . MSCT1 1 08 , E l C = 1 0 7 X 1 0 8 .7 (0 1 2 4 0 0 \P F O S A T 0 2 :D ) 2000 - o ... . APICES, NegTSIM i 1000- K 1i 3 MSD1 616, E IC =615:7:616,7 (012400\PFO SA102.D ) A PFES, Neg, S lM i 350 300 - 250- 12 MSD1 630, EIC =629.7:630.7 (01240\PFO SA102.D) AP-ES, Neg, SlM 400 r 300 ........ . /v - .. - . - / i '' " ' 'i i ' 'i ' 'M S D 1 5267EIC=525T7!526rr(012400\PFO SA`0 2 :D ] APFESTNg, SlM 4 400 ' ' '6 min. r ---5 ' ~' 6 ' min ( 5 -- 5 6 ..m in . " . - / 6 min 300 oo o oo o :I oin oo mo 2 " M S D f "4 27 , EIC =42(T7:42777~(012'400\PFO SAT02:D) 3 APICES, Neg, SIM c0 O IL!(L\ x. / 1 - . 123 ... I j Data4 9/26/00 1:10:54 PM AES/ALS 4 4 5 6 min 5 6 min Page 2 of 4 Page 83 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 47 of 55 Data File C:\HPCHEM\1\DATA\012400\PFOSA103.D MSD1 499, EIC=498:6r499T7~(012400\PFOSA103.D)~~APPES7Ng7S IM" 60000 ^ 4 0 0 0 0 ; 20000 3 0 12 _MSDT2987ElC'=297r7r298T*(012400\PFOSAT0XD) o 0u_ .. 34 API:ES7Neg7SlM--------- 10 0 0 0 0 7 50000 7 /u.-, I 04^ H 12 34 MSDr3'12, EIC=3 1T7;3'T2T_(012400\PFOSAT03:D1 API-ES7Neg7SIM--------- 150000 100000 50000 0 12 34 'MSD1 4987ElC=497.5:498:51012400\P FOSA10 3 :D]T~APl-ES7TJeg7SIM--------- 1 S am ple Nam e: 8 0 3 99PFO SA -152 FOSA Hydrolysis pH 3 Day 42 - Sample Spike 200000 4 \ 100000 7 ! 04 1234 "M S D 1 5 12 , E lC = 5 T i7 :5 1 2 7 7 _(0T2400\P FO S AT037D ) A P I-E S 7 N e g T S IM ------------ 100000 50000 ' ' 'i 34 " M S D1 "3 69 7 E IC ^ 3 6 6 :7 :3 6 9 '.7 (0 1 2 4 0 0 \P F O S A 1 0 3 .D )~ ~ A P l-E S 7 N e g 7 S IM ------------- 2000 /$ \\ ^$ /w\ //uo_\\' 12 34 'M S D n 0 8 r E I C = 1 0 7 : 7 r i0 8 . 7 _{0124001PFO SA'103:D )-- A P r-E S T N eg ."S IM ------------ 2000 1 S 1000 ^i i : 'i ' '' 'i 'M S D T 6 1 6T E IC = 6 5 ^ 7 :6 1 6 ^ 7 "(0 'T 2 4 0 0 \P F O S A "0 3 X )J A P F E S ^ N e g T S lM ------------ 500 -I I 4 0 0 -j i 300 -v I- " '' ' ' " ' '3' ' ' '4 " MSD1'630, EIC=6297:6307'(012400\PFOSAi03;D) API-ESlNegTSIM ..... 400 300 12 34 _ M SD1 5 2 6 rE [C = 5 2 5 `.7 :5 2 6 .7 (0 1 2 4 0 0 \P F O S A 1 0 3 ;D ) ' A PF E S ;~N e g 7S IM ------------ 100000 -j 5 0 0 0 0 -1 O-U 12 ~MS D1~4277E10=42677:427771012400\PFOSA103:D) 15000 7 ioooo4 5000 4 0-7= 3 A P I-E S 7 N e g 7 *S IM o10 ;CILL.' 4 Data4 9/26/00 1:11:02 PM AES/ALS /\ V o LL . 0. 5 ___________ 6 ...... Page 2 of 4 Page 84 o f 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 49 o f 55 D a ta F i l e C :\H P C H E M \l\D A T A \012400\P F O S A 105.D 1M SD 499,E IC =498.6:499.7 (012400\PFOSA105:D) API-ESrNeg,"SIM " 500 400 ' ! 300 i- I T . , ------' - .- ~- '' *" 12 34 ~MSD1"2987EIC=297'.7:29877~(OT24001PFOSAT05:DJ API;ES7Neg7SIM----------- 500 400 1 3 0 0 -L 12 34 A S O T 312;EIC=311;7:312:7`(012400\PFOSA105.D)-- APFESTNegTS'M ---------- 1000 500 4 12 34 "M S D 1 4 9 8 7 E lC = 4 9 7 ;5 r4 9 8 .5 (0 ~ 1 2 4 0 0 \P F O S A 1 0 5 ;D r7 A P 7 E S 7 N e g 7 S IM ------------ 600 -j 500 j 4001 '- / 2 " ' ............ i M S D r5 1 2 rE rC = 5 ^ fT 7 :5 1 2 T 7 `(0 i2 4 0 0 \P F O S A "105.D ) "A P I-E S rN e g , S IM ------------ S a m p l e N a m e : MeOH B l a n k FOSA Hydrolysis pH 3 MeOH Blank / -, 350 300 - i 2 T5 TTTTV "M S D T 3 6 9 rE !C = 3 6 8 T 7 ;3 6 9 '.7 '{0 1 2 4 0 0 \P F O S A T 0 5 ^ D ) A P F E S ^ N e g T S IM -------- -- 800 600 - A /\ 400 ! i' ~ T" - " ' 1 ! M S 0 1 '1 0 8 7 E IC = W .7 f1 0 8 .7 (0 1 2 4 0 0 \P F O S A 1 0 5 X ir_ A P re S 7 N e g 7 S IM ------------ 350 * 300 7 LI. . 4 --j- "MSD1 6 16 7E IC = 61 5:7 :61 6 .7 (012400\PFaSA105:D]T_APPES7Neg7SIM--------- 350 300- _/ __,.N / v . V," ~ 2 " ' ' 13 ' 1 ' ' MSDr630rEIC=629:7:630:7 (0i2400\PFOSAT05D) 'APr-ES. MejTSlM--------- 4 0 0 -j 350-3 3 0 0 4- - . -- " ' ' ' ' ' ' ' ' 5 ' ' ' -M S D 1 5261`E IC =525:7:5 26 :7'(01 2 40 0\P F O S A 1 05 1 D J A P I; E S 7 N e g 7 S IM ------------ 400 - 350 1 300 : . 12 34 "'WSD1 427, EIC=426:7:427.7 (012400\PFQSA105.D)' "AP1-ES; Neg, SIM----------- 600 -1 400 - Data4 9/26/00 1:11:20 PM AES/ALS Page 2 of 6 Page 85 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 51 of 55 Data File C:\HPCHEM\l\DATA\012400\PFOSA107.D " M S D T '4997T:IC =498:6T499.7"(012400\P F O S A 1Q 7;D ) A P I-E S .N e g T S IM - 10000 2 w O, 5000 /*' 0 12 34 -M S D r2 9 8 7 E lC = 2 9 7 :7 :2 9 S .r(0 T 2 4 0 0 \P F O S A `1 0 7 D r ~ A P r e S r N e g r S IM ------------ 100000- 50000-1 / ' ! oi . , - ,-- ' 12 3 4 i---------------------M S D 1 3 1 2 , E IC = 3 1 1.71312:7 (0 1 2 4 0 0 \P F O S A T 0 7 X > r'A P I: E S 7 N 5 g 7 S IM ------------ 100000 1 ; 50000 1 o l---------- ---- 1 ^ t ' T5 ' " $ T ' T J~ M S D t"4 9 8 7 E IC = 4 9 7 .5 :4 9 8 ;5 "(0 1 2 4 0 0 \P F O S A T 0 7 :D )~ A P I-E S rN e g T S IM ` 20000 10000 0 ... r ' ............t -- ..... i ....... .... ..r MSDT51Z7EIC=51t.7;.5127?7012400'iPFOSA1071D)'_ APr-ES7Neg7SIM^------- 20000 10000 0 ' ' ' ' ' ' ' ' \ ' ' ' ' ~3 ' ' ' ' M SDT3697EIC=368:7!369T710T2400\PFO SA1071D ) A PI; ES7Neg7S1ST S am ple Nam e: 9 9 0 3 9 -1 3 6 -0 2 F O S A H y d ro ly s is S td 2 - 2 nd in j pH 3 iWJi / on \ /&' IAnCL \ / /8\ ; 350 4 I 300 -h \ y r -> \ , \ ' ' i " " _ i ......................r ~ M S D `n >3 07 E rC = 6 2 97 :B 3 0 ?7 '(0 T 2 40 0iP F O S A ~ 1 0A D ) A P I-E S 7 N e g 7 S IH ------------ 400 300 ^ 1 1 ' 1 j ' ' ' ' 5 ' ' ' ' i~ M S D 1 "5267E IC =52517:52617`'(O T2400\PFO SA'107:D) A P I: E S 7 N e g 7 S IM ------------ 20000 ; 1000000J 0L . -, j ' ' ' 3 ' 1 ' ' X M S D T 4 2 7 7 E IC '=42617:42777"(0T240 0\P F O S A 1 07 .'D ) 15000J 1 00 00 -j 5000 i 0-L A P I; E S 7 N e g 7 S IM ------------ </) Sa.i\ /E Data4 9/26/00 1:11:40 PM AES/ALS mi n IS 8 Page 2 of 4 Page 86 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 3 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \0l2500\P F O S A 003.D _M S D T 4 g g rE rC " 498T6T499T^012500\PFO SA003T3) A PFE S TTTegTS lN r 500 -' 400 : 1 M S D T2987ET C =29777:298 77 {0 1 25 0 0\P F 05 A 00 3 ;D ) ~A P I-E S 7N eg7S 1M " S a m p l e N a m e: MeOH B l a n k FOSA Hydrolysis pH 5 MeOH Blank 600 1 400- 1 ~ M S D T 3 i2 7 E ic = 3 ri:7 :3 i2 :r(o i2 5 o o \p F o s A o o 3 :D r~ A p re s rN e g 7 s iM _ 1000 500 j 234 - M S D 1 "4 9 8 T E IC = 4 9 7 ^ r4 9 8 7 5 _(0T25O 0\P FO S A 003.D ) A P F E S 7 N e fl7 'S IM ------- 450 400 350 / / \ 'M S D 1 5 1 2 ;E IC = 5 T r7 :5 1 ? .r(0 T 2 5 0 0 \P F O S A 0 0 3 X fr^P re s rN e g 7 S IM 350 300- ^ / /' ./ \2 M 5D1 369. EKJ=36o.7:369.7 (012500\PF05A0037U ) 800 - 3 A PI-ES, NegTSlNl A' ` 5' '6 600 - 400- ' ' ' -l ' 4 ......................... A ' M S D 1 108. E IC = 1 0 7 J :1 0 8 :7 (0T250 0\P F O S A 0 03 .'D ; "APr-ESTNegT^Sira 340 320 300 280-3 - - . ^ / \ / " \ j \ r --A _/ 1 2 3' ' MSD1 616, E IC -6 1 5 .7 :b 1 6 ./ (01250\PFOSAo03.U) A P re S 7 N e g T S IM " i -- - - - -- ....... ' '5' 6 . ... min, ' _ / \ . ' \ , . - , 15 ' 6' 350 300- _____ -- / v --- ~ __v - , / " J 4 4 '' MSD1 630. E IC =629.7:630.7 (012500\PF O S A 003.D ) API-ESTNeg, SIM 4 400 350 3 0 0 - ___ _____ ___ ' ^ _ . _ ____ \ 2 3'' M b U l 526. fc lU = 0 2 5 .r.5 2 6 ./ (U 125U U\PhUSA003.U) A P I-E S , Neg, SIM 4 - . / " " '- 5 ' -- - - 5 '' 6 6 min min 350 300 1 _ ' , . y ~ / \ -, / ' / - ----- .... ! .- . ~ . 42 3 5 6 min 600 400- Data4 9/26/00 2:25:05 PM AES/ALS _5____________ 6 ___ _______ Page 2 of 6 Page 87 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 5 of 56 Data File C:\HPCHEM\l\DATA\012500\PFOSA005.D M SD1"499rEIC=498r5:499I7~(0T2500\PFO SA00iTD) APtE S 7N g7"SIM ~ 10000 5000 0 M S O rr2 9 S rE IC i29 77 7 :2 9 8:r(01 25 0 0\P F O S 'A O U 5 X IO -- R P F E S T N eg T S IM ----- 100000-i < : m. 50000 J I" -'. S am ple Nam e: 9 9 0 3 9 -1 3 7 -0 2 FOSA Hydrolysis pH 5 Std 2 -1st inj i2 _M S O T 3T 27E IC = 31'r7:31277"(012500\P F O S A 005;D ) 1 1000004 50000 - 0 4= 12 _ M S U r4987E IC =497.~5:498.5(0'i2500\P FO S A 005T)] 20000- i4 A P [: E S 7 N e g 7 S IM ------------ 34 AP7ES7 NegTSIM--------- ~ 10000 0-V T~ T M S D r5'127ElC=5T1.7:512.7'(0125C!0\PFOSA`005^D) APICES, Neg, SIM " 20000 -j 10000-j 04 . T ' ' J 1 ' ' ' ~ 4 M S D 1 ~ 3 69 rE IC = 3 6 87 7 :3 6 9l7 "(0T2500\P FO `S A 0 0 5 iD ) A P F E S rN e g T S IM ------------ 4 0 0 0 -1 /\ /3 \ ~' 1 i ' ' ' ' 2 ' 1 ' ' 5 1 ' ' r " M S D 1 "1 0 B rE rC = 'i0 7 .7 ri0 8 .7 '(0 '1 2 5 0 0 \P F O S A 0 0 5 :D ) A P I-E S 7 N e g . SIM ------------ < 5CmO ! ua .. ' < Au_\ n\ ///Cou5<O.\'\ 20000^ ! 10000- : 0-L 12 34 'MSDT4277EIC=426:7f427:7'(012500\PFOS"A005:D) API-ES7Neg7SlM----------- 10000- 0 eCO. -. Data4 9/26/00 2:25:24 PM AES/ALS /o(0\ 1a. ' _5____ 6 Page 2 of Page 88 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 12 of 56 Data File C:\HPCHEM\1\DATA\012500\PFOSA012.D M SDr499,E!C=49876i499.7~(012500\PFO SA012.D ) 1000 750 A P I-E S T R eg/S lM - #> p 500 250 12 34 ~ M S D r2 9 6 7 E !C = 2 9 7 :7 :2 9 8 :7 (0 1 2 5 0 0 \P F O S A 0 1 2 ;D ) ~ A P r-E S .N e g T S IM ------------ S am ple Nam e: 0 8 1 3 9 9 -B L K -5 .0 FOSA Hydrolysis pH 5 Matrix Blank 400- 1 - MSDr3T2rErC=3TT7rr3T2:7-(0125001PFOSAOT2;D)-- APPESTNegTSIM- 1000s 500 ~F ~M SD 1 4987 E[C =497.5:498.51012500\P FO S AU 1ZD ) 1000 APFES7N g7SIM ~ 500- ~ 1 1i ' ' ' ' J ' ' ' ' 5 ' ' ' ' _MSDY5T2rEIC=51TT:5'12.7`(0T2500\PFOSA0T2TD) APrESTNegTSlM--------- 750 500 - 250- TT M S D r 3 6 9 7 E IC = 3 6 8 ^ 7 !3 6 9 n 0 `1 2 5 0 0 \P F O S A 0 1 Z D J T APFESTNegTSiM - 4000 2000 /i\ ' ''i ' ` ^` `' MSD"1" 1 0 8 rE IC = T 0 7 7rrT 08 T r[0 T 2 50 0\P F O S A 0 i2 T )} A P F E S 7N g7S lM ~ 350 -i 300 250 T _ M S D r616rE rC =615;7616r7'(012500\P FO S A 012.U ) 1000 APl-ES," NegTSIM- 500- ~1 T ' T 2 ' ' ' ' 3 ' T ' ' V - M S D r6 3 0 7 E IC = 6 2 9 '.7 :6 3 0 :7 "(0 1 2 5 0 0 \P F O S A 0 i2 :D J A P I-E S T N e gT S IM -------- 400 J 300 J 1T 'M S D 1 526 ,' E IC =525.7:526.7~0~12 500\P FOSAOT233J- A P r-ES7N eg7S I 1000- 750 500 250 -c MSDr427rEIC^1426:7r427:2r(aT2500\PFOSA0i 2:D)" 3 APr-ESVNgTSIM 4 2000J .... min; Data4 9/26/00 2:26:27 PM AES/ALS Page 2 of 4 Page 89 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 13 o f 56 D a ta F i l e C :\H P C H E M \1\D A T A \012500\P F O S A 013.D I MSD1 499. E IC =498.6:499'7 (Q 1 2 5 0 0 \P F O S A 0 1 3 :D )^A P tE S rN e g 7 S IM : 60000 40000 20000 0 ,LoL_ a. 12 M S 01 2987610=297.7:298.7 (012500\PFO S A fff3.D ) 1000001 5 0 0 0 0 -, 34 A P F E S , N e g rS IM ------------ <m m. 0-4= 12 34 ~ K 1 S D t3 1 2 rE IC = 3 1 1 7 7 :3 1 2 7 "(0 1 2 5 0 0 \P F O S A 0 1 3 .`D ) A P I-E S 7 N e g rS [M ------------ 150000 4 100000 4 50000 -j 04 12 34 "M S D r4 9 8 rE IC = 4 9 7 .5 .- 4 9 8 ;5 (0 1 2 5 0 0 \P F O S A 0 1 3 :D J ~ ~ A P re S .N e g 7 S !M ----------- 100000^ 50000 0 12 _ M S D T 5 1 2 7 E r C = 5 T r7 :5 i2 T l0 1 2 5 0 0 \P F O S A 0 `f X D l 3 APFE S rN egTSIM - 4 S am ple Nam e: 0 8 1 3 9 9 -L C S -5 .0 FOSA Hydrolysis pH 5 Lab Control < f&\ lr -3 100000 5 0 0 0 0 -j 5o 4 ^ 1} ' ' ' 2 ' 1 ' ' ' 4 M S D 1"4 2 7 rE IC = 4 2 6 7 7 r4 2 7 T '(0 1 2 5 0 0 \P F O S A 0 T 3 iD ] A P I-E S 7 N e g 7 S lM ----------- 10000- OU_. 0- Data4 9/26/00 2:26:35 PM AES/ALS 5 ________________ 6 Page 2 of 4 Page 90 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 18 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \012500\P F O S A 018.D S am ple Nam e: 80399PFO SA -011 MSD1 4 9 9 ;e C = 4 9 8 ;6 r4 9 r7 {012500\P FO S A 018:D )"~ A P |.E S l Neg. SIM 10000 0 123 M s u i 298, El 0 =2 97 77 :29 8 7 {012500\P FG S A 018.D ) A PI-ES, Neg, SIM 4 100000 - 50000 - 0i2 MSD1 312, E!C =311.7:312.7 (012500\PFOSAOT8;D) 5CD U_' /CL . APPESTNeg, SIM 4 100000 -j 5 00 00 ~j o 4 -- _.____--_--_--_-_'-_--_-_--_1-_--_-_--_--_-_--_--__--_--_-_--_-_-_--_-'_--_-_--_1-_-_--_--_-_--_--_-_- '_--_--_-_--_-_---_- _- __---_-_--_--_--_-_'-_--_-_--__-_--_-_!-_---_- ___________ 1 2 3' MSU1 49a, b lU = 4 9 7 .5:496.5 (0125Q\PFU5AU18,D) A PI-E S , Neg, SIM 200000 - 4 100000 0 ., 2 1\ MSU1 512, fclU =511.7:512.7 (012500\PFO SA018.D ) AP1-ES, Neg, SIM 1000 4 J5 0 /\ y\ F O S A H y d ro ly s is p H 5 D a y 0 - S a m p le T rip 5 6 . m in 5 I to *CQ ilL / CL '5 6 -. k '' m in m in ' i2 MSD1 369, E lC =368.7:369.7 {012500\P FO S A 018.D ) 1000 * 800 600 400- .. 3' A PI-ES, Neg, SlM i A \ ' '2 ' ' ' '3 ' ' 'k MSD1 108, E IC =10777:08.7'(012500\P FO S A T 8.D ) A PI-E S , TJegTSIM ,/\6 0 0 4 00 ____ , / _____ _________ . __ ____ _______________________ 12 MSD1 616, E1C=61577:6T6.7 (012500\PFOSA018.D ) f\ 3 '' A PI-E S , Neg, SIM i 300 -- \ f J -- -v , . ^ - " \ / ~ " \ J i3 M S D r6307E IC =62917:630.7l012500V PF O S A 018D ) API-ES, NegTSIM " 4 400 350 300 /" ~ ' i 3 M 5U1 526, c lU = 5 2 5 .7 :5 2 6 .7 (012500\PP O S A018.D ) APFE S TN eg, SIM i 350 3 300 i _ .... x' \ ______ 7 - j- ........ " 12 MSD1 427, EIC =426.7:427:7 (0T2500\PFOSA018:D) .. . 3 API-ES, Neg, S IM ' CO 10000 - fi ,'Q.i 4 4 - 0 1234 '5 '6 `5 . , . ' ' min 5 /' A / V '' /' 5 6 - 6 -' 5 '' 6 - . ... 56 min. m in 5 6 min Data4 9/26/00 2:27:21 PM AES/ALS Page 2 of 4 Page 91 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 19 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \012500\P F O S A 019.D M S0T499, EIC=498.6:499;r(012500\PFOSA019.DJ-- APr-ESTNegTSIW 60000 - in :4 00 00 : 20000 //O,. S a m p l e N a m e : 80399PFOSA-012 FOSA Hydrolysis pH 5 Day 0 - Sample Spike o ooo--ooooM ooooW 2 P F B S A- 123 H SD r298TEIC=29777T298:7 (0 i2 50 0 \P F O S A 0 1 9;D ) "A P I-E S , N eg, SIM 100000 50000 0 123 M SDT3T27E!C -3'T1.7:312.7~(012500\P FO S A019.D )` API-ES, Neg, S IM 4' 5 m in 6 100000 50000 0 ---------------------------------------- ----- ---- 1i 3 M S D r 4 9 8 iE IC - 4 9 7 .5 :4 9 8 .5 (0 1 25 00 \P F O S A 0 r1 9 U ] A P N E S TN eg, S IM 4 I 5 6 . .min. 123 ~MSD1 51 2 7E IC = 5T1?7;512.7 (0 1 2500\PFOSA01'XTDJ A P I-E S ^N e g, SIM ir ' 5 ' ' 100000 50000 - 0 l-- - - - - ..................... 123 T tfS 0 T ~ 3 6 9,E rc= 3 6 8.7 :36 9.7 (012500\PFOSA019TD) APPES, Neg, SIM - 4 ' l\ 5 1000 -7 5 0 .-500 A, --------- , ' ' 3 ' ' ' ' MSD1 108, E IC -1 7.7 .10 8.7 (012500\PFOSAT9TD) A PI-E S , Neg, SIM 4' ' /\ 5' '' 6 ' . min -- -r--j 6' ' 600- 40Q- A ________ ii MbUl 6 1 6 , fc iu = 6 1 5 .7 :e i6 .7 (0 1 2500\P F O S A 019X )J i API-E S TN eg, SIM k' 325 300 275- i '3 ' ~MSD1 630, E IC =629.7:630.7T0T2500\P FO S A019.D ) API-ES, Neg, SIM 4 500 - 400 300- 2 ' ''3 ' '' ' M SD1 5 2 6 7 E IC = 5 2 5 .7 :5 2 6 .7 _(0`1 25 00 \P F O S A 01 9 :D ) A PI-EST N e g .'S IM -- 4 ... 100000 50000 0 2 MSD1 427. E IC =426.7:427:r(012500\P FO S A 0i9:D ) 15000 10000 5000 0 1 2 3 APFES, NegTSIM C/3 ;,HIL` 3 4 4 5 '6 '5 ' ' / '6 / v _ ----- 5 s :(0\ /' 5 6 ~ ~6 ; ... min .. min. . min. 5 6 min Data4 9/26/00 2:27:29 PM AES/ALS Page 2 of 4 Page 92 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL.1132 Batch Run # 47 of 56 Data File C:\HPCHEM\l\DATA\012500\PFOSA047.D M S D 1 4 9 g rE rC = 4 9 8 :B r4 9 9 7 '(0 1 2 5 0 0 \P F O S A 0 4 7 .D )~ A P re S rN e g rS IR r 1 10000J 04= 12 ' 'M S D r29 87 E IC =2 97 l7 :29 8'.7 "(01 2 50 0\P F O S A 0 47 !3J 100000 50000 4 04 _1 2 M S D T 3 T 2 , EIC =31T7^3T2!7- (012500\PFOSA047:D ) 34 A P F E S T N e gT S IM ------------ 0\ 1/L0i-.' 34 A P F E S 7 N e g T S IM ------------ 100000 50000 - 04 ' ' ' ' 1' ' ' ' 5 ' ' ' 3' 1' ' r W SD1 4 9 8 ;"E IC = 4 9 7 :5 i4 9 8 :5 (0 1 2 5 0 0 \P F O S A 0 4 7 .D ) A P I-E S rN e g T S IM ------------ Sample Name: 80399PFOSA-155 FOSA Hydrolysis pH 5 Day 42 - Sample Trip 10000 1 o -!= Data4 9/26/00 2:31:39 PM AES/ALS Page 2 of 4 Page 93 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 48 of 56 Data File C:\HPCHEM\l\DATA\012500\PFOSA048.D MSDV499, EIC=498.6:499'.710T2500\PFOSA048X)) APFESTNegTSIRT . 60000 j 400001 j 20000 J ! 0-v 12 ~M SD T2937EiC=29t7I29877~(0T2500VPFO SA048XtJ 100000 34 A P I: E S 7 N e g 7 S IM ------------ < 50000 - 0 1 23 " M S D i 3 1 2 7 E IC = 3 1 1 7 7 :3 1 2 7 1 0 1 2 5 0 0 \P F O S A 0 4 8 :D r_ A P I`-E S 7 M e g rS IM ~ i: 150000 5 100000 -j -j! 50000 04= 12 34 - M S D T 4 9 87 E lC = 4 9 7T 5 i4 98 T 5 70 T 2 50 0\P F O S A 0 48 X 5] A P F E S 7 N e g T S IM ------------ 300000 200000 100000 0 1 ' ' ' ' ' " ' 2 ' ' ' ' 5 1 ' ' ' i MSD`1_5T2TErC=51T7T51277"(0"12500\PFOSA048X3) APFESTNegTSIM--------- 100000 J -j5 0 0 0 0 ol i2 _MSDT369TElC=368r7T369rr(0i2500\PFOSA048iDl 3 4~ APFESTNegrSIM--------- S am ple Nam e: 80399PF O S A -156 FOSA Hydrolysis pH 5 Day 42 - Sample Spike /Unat.\\x 5 A M o\ 800 600 400 - . | ' ' ' ' 1 1J /X ' ' ' J~ M SD1 1 0 8 rE IC = 10777TT067T(0r2500\PFOSAO48.Dl A P F E S 7N eg;"S lM ' t ' ' ' ' 2 ' ' ' ' 5~ _ MSD1 6307EIC=629.7:63077 (0T2500\PFOSA048X)) API-ES,Neg7SIM 4 5 0 0 -i 4 0 0 -j 300 1 - 1 ' ' ' '3 4 - M S D r52 67 E IC =5 25 T 7 :5 2 67 7"(0 1 25 00 \P F S A 0 48 ~D } A P I-E S 7 N g 7 S IM ------------ 1000001 50000 i 04= 1 MSD1 4277EIC=426:7:4277r(012500\PFO SA048.Dy " A P F E S rN eg7S lM ~ 15000 10000 - 5000 0 1 V) , /i\ Data4 9/26/00 2:31:47 PM AES/ALS /&0/>\. IL . / Q. 5 ......... 6 ________ Page 2 of 4 Page 94 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL.1132 B a tc h R un # 50 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \012500\P F O S A 050.D ` W SD1U997ElC=498".6f499`7(012500\P F O S A 050:D ) A P I: E S7Neg7SIM ~ 500 400- 12 ~M S D T2987E IC =297;7:29S ;7- (OT2500\PFOSA050:D) -i 600 J 400 J 34 A P !-E S 7 N e g T S IM ------------ A- 12 3 " M S D 1_3 '1 2 rE IC = 3 n :7 :3 T 2 X f0 T 2 5 0 0 \P F O S A 0 5 0 T D r~ A P I-E S rN e g rS IM i 4 1000 A 500 J1 1 T Tr 5 TT' 7J 77' " MSD1 4987E rC=49775r4983*(at2500\PFOSA050TJr~APr-ESrNegrS 7V S a m p l e N a m e : MeOH B l a n k FOSA Hydrolysis pH 5 MeOH Blank min. / J 1............... i ' ' ' ' ' ' ' I ~ M S D T 5 1 2 7 E IC = 5 1 T T r5 T 2 T 7 "(0 1 2 5 0 0 \P F O S A 0 5 0 :D ) A P I: ES," N e g 7 S IM ----------- 350 4 300 -j - r r ' T ' J T ^ T5 ' ' TTV _ M S D r36 9T E IC = 36 8^7 r3 i6 97 7 (0 1 25 00 \P F O S 'A 0 E 0 D ) A P H E S TN egTS IM A.600 400 - ^ 1' J ' ' ' ' 5' ' ' ' f M S D r lO B r E IC = T 0 7 .7 n 0 8 .7 (0 1 2 5 00 \P F O S A 05 0 X IJ_ 'A P r-E S ','N e rS lM ------------ 1 300 4 \ J 2 5 0 -11---------~~T~ " " 1 1 1 i....... ........ 4 M S D r 6 1 6 ." E IC = 6 1 5.7:616774CT12500\PFO SA050U) A P I-E S ,N e g 7 S IM ------------ 320 300 W y v A / ^ v 280 1' ' ' '2 ' ' ' '3' ' ' ' MSD'1"630TEIC=629;7:63017 (0T2500\PFOSA0501D) APFES7NegTSIM A ./\ - " 400 3 50 -j 300 4 - ^ ' 'j TT' J T' 3 TT ' " MS D T 5 26TE !C =52577[526.7"(0125Q0\PFO SAO507D) 4PI:ES7 Ng7 SIM 400 J 350 \ 300 123 " M S D 1'4277E IC =426:7f4277'(012500\P FO S A 050;D )" 'A P I-E S 7 N e g ;S IM 4 4 600 400 Data4 9/26/00 2:32:06 PM AES/ALS __________ 6_______________ m in Page 2 of 6 Page 95 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 52 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \012500\P F O S A 052.D S am ple Nam e: 9 9 0 3 9 -1 3 7 -0 2 tn o oO o oo oo MSD1 499, EI0 = 4 9 8 .6 :4 9 9 .r(0 1 2 5 0 0 \P F O S A 0 5 2 :D r A PI-E S , Neg, SIM </) O . &\ / ,\ 1 o> ' 12 M SD1 2 9 8 7 E IC = 2 9 7 .7:2 9 8 7 T (0 12 500\P F O S A '0 5 2X )) 100000 50000 - 3 APF-ES, Neg, slM 4 1</3 D F O S A H y d ro ly s is S td 2 - 2 n d in j pH 5 5 6 min oi ^ i ' ' ' '2 ' ' ' M $1 312, E lC = 3 1 1.7:312.7 ( 12500\PFO SA052.D) 3 'l API-ES, Neg, SIM 4 ' 5 6 min 1 100000 . 50000 0- i ... 2 MS1 498, EIC =497.5:498.5 {012500\PFOSA052. ) i '' A PI-ES, Neg, SIM 20000 10000 - t 23 ` M S D T 5 1 2 , E IC = 5 r i. 7 :5 1 2 7 " ( t 2 5 0 0 \P F O S A 0 5 2 X ) P `A P re S 7 N e g 7 S IM 20000 - 10000 - 0. ,. i ' ' ' '3 ' "M S D T 36 9 , E1C =3687:369TT012500\PFO S A 052X 1) APEES, NgTSIM ! /m \ /u. \ y a. y 4` ' 6 JA. k5 ' 6' < /w \ o\ LL \ j a\ . . .^ . 5' m in min I m in' 4000 2000 - / ' \ 4 MSU1 108, E IC =107,7:108.7 (012500\PFOSA052.D ) . A P l-E S , Neg, SIM i' 350 300 250 - .1 2 M 51 616, E IC =615.7:616.7 (012500\PFOSA052.D ) 3 A P l-tS , Neg, SIM k' 1000- : seo- A 5 '' 6 -- -, 5' '6 min ! __ ,. , .j min' ii3 MSD1 b3U, E IC =629.7:630.7 (0125\PFOSA052.D) A P l-E S , Neg, SIM i1 l 400 y \^ /' I 300- I i . - i ' ' 2 1 ` 13 ' ' k MSU1 526, E IU = 5 25 .7:5 Z 6.7 (QTT2500\PFOSA05Z.DJ~~ A P I-E S , N eg, SIM 6 v - ' .... - - . ' 56 m in min 20000 10000 s / ISu_\ Cl i 3 4 5 6 m in MSD1 4 2 7 , EIC=426.7T42777 (0 1 2 5 0 0 \P F O S A 0 5 2 X )) A P I-E S , Neg, 51M 1 10000 ] 8 ioi\ ' oj . /iEv- - ---- ------ --- --------- - __________________________ _1____________________2___________________3___________________4___________________ 5______________ ____ 6_____________ m in Data4 9/26/00 2:32:25 PM AES/ALS Page 2 of 4 Page 96 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 2 of 55 Data File C:\HPCHEM\l\DATA\012500\PFOSA058.D ~M SDr499rEIC=498:6r499.7T0T2500\PFOSA058;Dr" APPES7Neg7S!M" 5 00 -i 400- S a m p l e N a m e: MeOH B l a n k FOSA Hydrolysis pH 7 MeOH Blank 12 34 _ M S O T 2 9 8 7 E IC = 2 9 7 7 :2 9 8 7 "(0 1 2 5 0 0 \P F O S A 0 5 8 iD ) A P P E S T N e g T S IM " .... 600 400 _ __ _ ____________________________ _ _____ ___ _____ 23 M S u r 31Z7E !C =311.7:312,r<012S 00\P FO S A 058.D ) A P I-E 5, Neg, SIM i1 500 "i 23 MSD1 4987EIC=497T5i49875"(01250Q \PFO SA058!D) A P I S N e g T S I K T -------- - 4 r\ J\ 4 --5 5 6 min, 6 min 500 400 ' ' ' '\ 4 4 ' M S D'1" 5127ErC=51TT755T2777012500\P FO SA 058'.D) A P ^ E S , N e gT S IM a' * 350 : _ .----. ----s ^ ., '2 '' " MSD1 369, E IC = 3 68 7 :3 6 97 7(01 2 50 0\P F 0 5A 0 58 7D ) A P f-E S , Neg. SIM 4 600 400 , _ ____ y .__________ ___________ _ ., .^ i .__^ ^ "M S D 1 087ETC =107.7:108.7 (012500\PF SA058.DJ 3' A P FES7 N eg. SIM / 'V , \ 325 300 ' ' ..... - 56 _ /x . 56 .. m i n| m in -..... - `' -- '6 f ' min /\. ' j . ., 24 M SD1 6 16 , "E !C = 6 1 5 .7 :6 1 6 7 T 0 f2 5 0 0 \P F O S A `058. D) A P I-E S , Neg, SIM 4 _yw ^A ... ., . 4' ' '4 M S D V 6 3 0 , El 0 = 6 2 9 7 :6 3 0 7 (01250D\PFUoAQ58.D) API-ESTNegTSIIw 5 f\ /J \ V A - 'A 5 \ \ . 400 1350 300 _ /V _ / ' 3' ' ' \ "2 4 M S D T 5 2 6 , E l0 = 5 2 5 7 : 5 2 6 7 1 0 T 2 5 0 0 \P F O S A 0 58 D) 'A P H E S , N eg, S IM ' 4 " / x 5 6 6 6 min min m in .3 1 2 H S D 1 4 2 7 rE lC = 4 2 6 `.7:4 27 `.7~(0T2500\PFO SA058^D) 3' API-ES, Ng, SIM ;*\ 4 400 1 2 Data4 9/27/00 11:10:45 AM AES/ALS 3 4 _ ' 5 T m in . _ ...___ 5 6 min Page 2 of 6 Page 97 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 4 of 55 Data File C:\HPCHEM\1\DATA\012500\PFOSA060.D ~ M S D r4 9 9 ;E IC = 4 9 8 :6 :4 9 9 :7 (0 i2 5 0 0 \P F O S A 0 6 0 .D r'A P i:E S 7 N e g rS IM _ 10000 5000 J 04^ 12 " M S D T2987E IC = 297:7:29877` (0't2500\PFO SA060TD) 50000 A l;\ 34 A P I-E S T N e gT S IM ------------ 3 04 12 *W SD r3127E IC =311.7:312` 7l01 2 50 0 \P F O S A 0 6 0.D ) 34 A P F -E S 7 N e g7 S !M ----------- : 100000A j 50000 \ ! 04= 12 3 ` M SDr4987EIC =49775":498.5 (012500\PFO SA060Tl)` " A P [-E S ,'N egrS IM 20000 A 10000 J o-l 1 "* 2 ~ M S D T5127ErC =5H '.7:527770T2500\P FO S A06C rD ) 3 A P I-E S T N e g T S IM 4 4 20000 J 10000 0 '... - \..................r ...... 4 ........... M S D r3 6 9 7 E IC = 3 6 8 T :3 6 9 :7 `(012500\PFO S A 060:D )"_APFES7NegTSIM 4.A-600 400 T M S D 1 T 0 B 7 E V C = i 0777:1 0 8 .r(0 1 2 5 0 0 \P F O S A 0 6 0 :D r~ A P |:E S 7 N g 7 S [M _ S am p le Nam e: 9 9 0 3 9 -1 3 8 -0 2 FOSA Hydrolysis pH 7 Std 2 -1st inj fi\ / Q- H - J \250 j \ y " T " M S a in B T 6 7 E iC ^ 1 5 :7 :6 1 6 :7 (0 1 2 5 0 0 \P F O S A 0 6 0 X ))_^ P r - E S 7 N e g 7 S I M ' 800 36 0 0 A 400 ; ., 2 ' ' ' "5 ' ' ' ' MSD1'6307EIC=6297i63Cf.710T2500\PFOSA050iC() AP7ES~Nig" SIM <T 400 / V350 300 4 ' ' ' ' ' i MSD1 5267EIC=525.7!526:77012500\PFOSA060:D) APFES7Neg7SIM Y~" r-- 20000 10000 0 12 " MSDT4277EIC=4267:427:7T012500\PFOSA060:D)" 3 AP reS7N esrS lM 4 10000 0 ,(4H\\ < III oV ) mm: _________ __m m Data4 9/27/00 11:11:04 AM AES/ALS Page 2 of 4 Page 98 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a t c h R un # IX o f 55 D a ta F i l e C :\H P C H E M \l\D A T A \012500\P F O S A 067.D "M S D 1 4 9 9 7 E IC = 4 9878749977 (0 1 2 5 0 0 \P F O S A 0 6 7 .o r~ A P r-E S 7 N e g 7 S IM _ 1000 i 500 O LL ID. / S am p le Nam e: 0 8 1 3 9 9 -B L K -7 .0 F O S A H y d ro ly s is p H 7 MatrixBlank " M SDT2987EIC=297T7T298T~(0T2500\PFOSA067X>) API-ES7Neg7SIM~~ 600 400 12 34 M S D T 3 1 2 , E IC = 3 1 T 7 ;3 1 2 :7 '(C ri2 5 0 0 \P F O S A 0 6 7 :D r'`A P F E S 7 N e g rS IM ------------ 1500 A 1000 500 " t ' ' ' ' ' 3 ' ' ' 4 "M S D 1"49 8 7E IC =4 9 7T 5 i4 98 T 5 "(0 T 2 50 0 \P F O S A 0 6 7X fJ~~ A P F E S 7 N e grS IK 1 ------------ 600 400 X - A _ i _ ' T T2" TTT5 T ' r4 SCJ1 5T2, E IC = ^rr7 J5T 2^-(0T 2 500\P F O S A 067.D r_API-ES7NegrS)M _--------- 600 400. "" -- } ' 1 2 ' ' ' ` 5 1 ' r ' J- " M S D T 3 6 9 , E !C = 3 6 8 .7 :3 6 9 ;7 (0 1 2 5 O 0 \P F O S A 0 6 7 :D r~ A P F E S 7 N e g 7 S ira ------------ Ai 6 0 0 400 A ~ . ^j ' ' ' ' 2 ' 3 4 H S D 1 1 08 , E IC = 1 0 7 7 :10 8 .7 1 0 1 2 5 0 0 \P F O S A 0 6 7 .D ) A P I-E S 7 N ig 7 S IM ----------- 300 250- ~\ / - t 11' ' J ' 1' ' 5 ' 1' ' MSD1~6167EIC=615^7:61B77y012500\PFOSA067:D]-- APFESTNegTSIM------------ 800 j 600 4 0 0 -1 / 'V __ _1 2 3 4 MSDT6307EIC=629T:63077~(012500\PFOSA067T>J API^ES7Neg7S!M---------- 400 I .. / v350 300 1 T ~V /\ T X 'M S 0 1 5267EIC=525.7:526.7"(012500\PFOSA067,DJ A PFES7N g7SIM _ 6 0 0 -j 5 0 0 = 4 0 0 -j 300 i 12 34 - MSD'1"4 2 7 7 E rC = 4 2 6 :7 i4 2 7 :7 '(0 1 2 5 0 0 \P F O S A 0 6 7 :D l A P I-E S 7 N e g 7 S lM ----------- 1000J 5 0 0 ; I\ l\ /\ Data4 9/27/00 11:12:07 AM AES/ALS Page 2 of 4 Page 99 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 12 of 55 Data File C:\HPCHEM\l\DATA\012500\PFOSA068.D ~M SDr4997EIC=4987(ir4997"(0T2500\PFO SA068TDJ APFESTNegTSIM - 6 00 00 -i 4 0 0 0 0 -j 20000 4 0 12 MSD1 298, E IC =29777:298.T(012500\PFO SA068:0) I, 3 3 A PFES, Ng, SIM 4 45 : : / . Q .1 S am p le Name: 0 8 1 3 9 9 -L C S -7 .0 FOSA Hydrolysis pH 7 L ab C o n tro l 56 i 23 MSD1 312, E IC -311T7:312.r(012500\P FO SA 068TD ) A PFE S , Ng. SIM 150000 100000 l1 23 M S D 1 498, E IC =497.5:498.5"(012500\PFOSA0681D) API-ES, Ng, SfM 100000 50000 1 2 3' '` MSD1 512, E IC -5 1 1 ,7 :5 1 2 .7 (012500\PF O S A 068.D ) A P I-E S , Neg, SIM 4 < 4' ja . A< / \ 4 5 5 5 6 6 6 100000 50000 0 'i 23 M S D 1 369, E rC = 35 8T :3 6 9.T (012500\PFOSA068.DJ ~ A P F E S , N eg,'S IM 1800 600 400 . /i _ /\^ w A. i '1 5 ^ ...A 6 1 i ' ' '3 ' ' ' MSD1 108, E IC =107.7/108.7 (012500\PFO SA068.D) APFESTNegTSIM 4 '' 5' ' '6 / \ .. . . ........... ...... ....... ............. ........ ' ,, ' 3 MSD1 616, EIC =615.7:61677~t012500\P FO S A 068.D j A P I-E S , Neg, SIM i. A600 400 . 123 ' MSDT630rElC=629T.7;63077'(0T2500\PFOSA068:D)~API-ESrNg; SIM" 400 ' \ .-V . 300 ' ' ' '1' ' ' ' ' '3' '' ' MSD1 526,E!C =52577T526.7{012500\P FO SA 068.O ) A PI-E S , N g /SIM 150 00 0 -i 100000J 50000 J oi 12 3 " MSD1 427, EIC=426.7:427'.7 (0 1 2 5 0 0 \P F O S A 0 6 8 :D r_ A PI-E S , Neg/ SIM 4~ 4 10000- 0-1= /f\ .......... . 5 !VOS).\ u. . CL 5' '6 ' ' Data4 9/27/00 11:12:16 AM AES/ALS Page 2 of 4 Page 100 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 17 of 55 Data File C:\HPCHEM\1\DATA\012500\PFOSA073.D WSDT499, E!C=498.6:499:7~(012500IPFOSA073`D) API:ES`'Neg7SIM~ 10000 0 : , MSDT2987E1C=1297:7T298727'(OT2500\PFOSA073:D) 34 API-ESrNegTStM-------- ! 1 0 0 0 0 0 < 50000-4 0-U /a\ -10-- 12 34 " M S D T 3 1 27 E fC = 3 1177:31277~C012500\PFOSA0737D)-- A P r-'E S 7 N e g 7S IM ------------ S am p le Nam e: 80399PF O S A -015 FOSA Hydrolysis pH 7 D ay 0 - Sample Trip 100000-j 50000-j .to 1, /CD. /IL. ' l a . 12 _ M SD1'4987E IC =49775r498:5"(0T2500\P FO S A073:D) 200000 - 3 A PI: ES7Neg7SIM 4 100000 - o4' ' T T ' 7 ' T 2 T T 7 7 5 7 7 1 7 4~ M SD T T O T E IC S S I T77r512:7` (012500\P F O S A 073:D )" AP[-ES7Neg7STM /Q.\ -Ai A 300 - '' MSD 5267EIC= 525.7:526.7'(012500\PFOSA073'D) 3 API-ESTNegTSIM ? /\ 400 - 4 300- "MSD1"427rElC=1426T.7r427.7'(012T5002\PFO7SAT0737'Dr~*AP3I-EST7Ne'g7S'lM ' V) o, 10000- u_. a. x 0 A Data4 9/27/00 11:13:02 AM AES/ALS 5___ __ 6 Page 2 of 4 Page 101 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 18 of 55 Data File C:\HPCHEM\1\DATA\012500\PFOSA074.D M8DFT499. E IC =498:6:499;7(012500\P FO SA 074.D )' ' API-ES, N e gi'S IN T 60000 40000 20000 0- ! M S D T 2 9 8 7 E lC = 2 9 7 :7 :2 9 8 i7 - (0"12500\PFO SA074iD J A P F E S T N g T S IM ------ ; 100000 1 < ' 50000 j \ 0 12 34 -M S D r3 2 iE IC = 3 1 T .7 :3 1 2 i7 "(0 '1 2 5 0 0 \P F O S A 0 7 4 7 D )' A P I: E S 7 N e gT S IM ------------ 100000J 50000 \ 04= _ MSDT4987ErC=497.5r49875~(0i2500\PFOSA0747DJ API; ES7N eg7S lM _ j 200000 100000h Io \_ 1 2 f - MSDT527EIC=51T7T5127770T2500\PFOSA074.D) ~\ I 100000 34 APl:ES7NegTSfM--------- j 500 00 -j . 0 '. I-- , . -- t t f "" t t 5 1 " t t r WSD1 3697E IC =36B.7-.369;7 (0 1 25 00 \P F O S A 07 4 .D )" A P r-E S ';N g i'S lM ------------ 1000 750 500 /V 250 4; 12 " M S D 1"10 8 7 E 10= 10777:108.7(012500\PFO SA0747U) 34 AP l-E S ; N e g7 S IM ------------ 300 275 : 250 -] .A 'j - 1" ' ' ' 2 ' ' ' ' 5 " ~J ~ M S D r6 1 6 rE IC = 6 1 5 .7 :6 T 6 .7 `'(0T2500\PFOSA"0747D) A P I-E S 7 N e g T S IM ------------ S am p le Name: 8 0 3 99PFO SA -016 FOSA Hydrolysis pH 7 Day 0 - Sample Spike /co /tv s<a /co\ ! 100000 : | 50000 J o 4= "MSDr4277EIC=426;7r427:74ai2500\PFOSA074:Dr'APreS7Neg7SIRr 10000 0 Data4 9/27/00 11:13:10 AM AES/ALS 2 CO o Page 2 of 4 Page 102 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 46 of 55 Data File C:\HPCHEM\1\DATA\012500\PFOSA102.D MSD1'4997EIC=498:6r499:7T012500\PFOSA102;D) API-ES, N eg7S IM _ 10000 : 0 123 4 'M S D T 2 9 8 rE IC = 2 9 7 T 2 9 8 7 7 "(0'12500\PFOSAT 027D) A P I-E S , Neg, SIM ! 100000]] < 1! CwD. ; 50000 -i : /u./- ! o4 J: 2 ' ' '3` ' ' MSD1 3127E IC = 31t7:312.7"(0T2500\P FO S A 102;D ] A PFESTNeg, SIM 4 100000 50000 0 1 ' 2' M S D 498, E IC =497.5.498.5 (0T2500\PFOSA102.D) 3' A PI-ES, Neg, SIM 4 S am p le Nam e: 80399PF O S A -159 FOSA Hydrolysis pH 7 Day 42 - Sample Trip 56 5 W, lea , LL . CL M 6 6 12 ' ' ' i~~ ~ "M S D 1 '3 6 9 7 E IC = 3 6 8 :7 ;3 6 g X 7 C n 2 5 0 0 \P F O S A 1 0 2 :D )_ "A P F E S , NegV S IM ------------ 600 400 ; ./V - , __ _ yv_ \ 2 3 M S D T 1 0 8 , E IC = 1 0 7 .7 1 0877*(0T2500\PFOSAT027DJ A P I-E S , Neg, STM 300250 ; A !\ / - ~' ... - ... '" t 2 3''1 MSD1 61b, E IC -6 1 5.7:616,7 (012500\PFO S A 102.D ) A PI-ES, Neg, SIM _ /\ . . . .^ . 4 .--------. , ^ /- 4 ' '5' 6' 800 600 400- .A i 23 ~MSD1 630, E tC =629.7:630.7 (012500\PFOSA'102'.D)" 7 A P rH S 7 N e g. SIM 4 ` 5' ' 400 350 A- . . . - ... - " ; 300 .. i 3 MSD1 526, E lC = 0 2 6 ,/:5 2 b .7 (012500\PF O S A 102.D ) A PI-E S , Neg, SlM 4 '5 6 6 1 m in m in m in | 400 /\ ! 300 - 10000 i2 MSD1 427, E IC =426.7:427.7 (012500\PFO S A 102.D ) 3 A PI-E S , Neg, SIM <0 UO..i 0. - XI - ' 123 -- .. . . 4 4 5 5 Data4 9/27/00 11:17:11 AM AES/ALS 6 min 6 Page 2 of 4 m in Page 103 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL 1132 Batch Run # 47 of 55 Data File C:\HPCHEM\l\DATA\012500\PFOSA103.D S am p le Nam e: 80399PFO SA -160 MSD1 499, E IC =4 98 :6:4 99 7 r(0 i2 5O 0 \P F O S A 1 0 3X 0 "A Pr-ES; N eg; SIM 60000 -j 40000 3 20000 3 V , ............. ....... ; ----- : ..... ; -- -00---- 123 mjlh yo, t t o = ^ y / . / : y o . / ( i)UO\p p u 5AT03X)) a p i-e s , Neg, SIM 100000 4 50000 -i / . 0 j ____________________________________________________ _____-- 2 '3 M SD1 3 1 2 T E IC = 3 1 1.7 3 1 2 `.7"(0 1 2 5 0 0 \P F O S A T 0 3 .D ) APICES, N eg, SIM 4 FOSA Hydrolysis pH 7 Day 42 - Sample Spike 56 56 100000 I, 50000 0 ______ i 2 ' '41 ~MS1 4 y d , E IU =4 97 '.5 :4 9 8 .5 ( 1 2 5 0 0 \P F 0 5 A 1 0 3 .D ) A P I-E S , Neg, SIM y i\ I a- 300000 200000 100000 0 !ACL\ / v ii3 M S D T 5 1 2, E IC = 5 ir7 :5 2 T 7 0 2 5 0 0 \P F O S "A 1 0 3 T D ) A PFES, Neg, SIM 4 5 5 6 6' 100000 50000 0i ' ^ ' ' i ....................... 4 "M S 0 1 3 6 9 , E IC = 3 6 e r7 :3 6 9 7 7 7 0 1 2 5 0 0 \P F O S A l0 3 ;D ) A P I-E S T N e g , S IM ----- ' 1000 750 500 250- A ___ _ 123 M SD1 1 08 7 E lC = 1 0 7 .7 :1 0 8 .7 r*(0 12 5 00 \P F O S A 10 3 .D ) A P^E S TN eg, SIM 4 | f Q\. - 5 . ___ ___ 5 6 300 / ' ^ 250i M S D T 6 1 671=10=615.7:616.7 (012500\PFOSA103;D ) ^. A P I: E S 7N 6gT S IM ----- 600 600 400- .A 1i 34 MSD1 63CrEC=629`7:630X(012500\PFOSA103D) API-ES, Neg, SIM ` -- - 5 ' ` ` '6 ' 56 'I mtn, 400 3 0 0 - . . . . . / V ........ . . . .___________ . 2 ' ' '3 '' (U iZO U O V rrU S A 103.U ) A P I-E S , Neg, SIM 1000001 500 00 T " "~ __ ,/\ '5 ` V) O lCiL. ... / \ 6 O oooO ; 1234 5 6 "M S D 1 4 27 , E IC = 4 2 6 !7 4 2 7 T "(0`f2 5 0 0 \P F O S A 1 0 3 :D ) A P I-E S , N eg, SIM V) S\ ,/! F \ , 1234 5 6 Data4 9/27/00 11:17:20 AM AES/ALS Page 2 of 4 Page 104 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 49 of 55 Data File C:\HPCHEM\l\DATA\012500\PFOSA105.D M SD T 4 9 9 7 E IC =49876;499'.7'(0 1 2500\P FO S A Q 57D ) 600 \ i5 0 0 400 __ __ ___ 300 i;-" ' T ' "7 12 M S D 2987EIC=297;7;29877'(012500\PFOSA105.'D) A P F E S 7N eg 7 S IM ~ ; ; ^ 34 APEES7Neg7SIM ----------- 600 A 400 - ,, -- 1, - ' ' J ' ' ' ' 3 ' ' ' ' MSD1 312, EIC311.7:312.7 (012500\PFOSA15.D) API-ES, Neg, 5IM '' 4 ' 1 S a m p l e N a m e: MeOH B l a n k F O S A H y d ro ly s is p H 7 M e O H B la n k ~------- ------ - 5 " " '`-- 6 min cuoo ooo _______________ - _ 42 MSD1 498, E1C=497.5:498.5 (012500\PFOSA105.D ) -- 3 A PI-E S , Neg, SIM J 4 600500- 1 2 '' 3 ~MSD1 512 , E IC -5 1 1,7:512.7 {Q12500VPFOSA105.U) A P I-E S , Neg, SIM 4 ____ ______ '- 5 -- --------- .... '6 \ '' 5 '6 ' m in m in 350 300- , . . /. - i ' 2 ' ' 3 M 51 369, E IC =3 68 .7:369.7 (0l25 0\P FO SA 1 5.D ) A PI-ES, Neg, SlM 4 \. - 5 6' 500- _ 400 . . . . . ., _______ _ . ................. " 2 j - MSD1 108, EIC =107.7:18.7 (01250 \P FO S A105.D ) A P I-E b, Neg, SlM 320 300 ; 280 _ 260- \ ,-.a 1 r~ -^ \ M S D 1 6 16 , E IC = 6 1 5 .7 :6 1 6 .7 (0125O'vPFOSA15.D) ^ 3' API-ES, Neg, SlM 320 300 280- V t J i' 4' '5 ., N" " ' / 4 -V \ / A ' V 5 v -v ' v- 45 ^ 6 6 ^ ' / m in min mi n m in 400 - 350 - 300 -4- - .. 12 3 " M SDr5267EIC=525;7:5267`(0T2500\PFOSA105.Dr" API.ES7NgTSIM" 400 -1 T 350 300 -} 12 3 " M S D 1 4 2 7 7 E IC = 4 2 5 :7 :4 2 7 .7 (0 1 2 50 0\P F Q S A 1 05 .D )" APi-`E S 7 N e g 7 S IM 4 600 400- 5 ______ ____6 Data4 9/27/00 11:17:38 AM AES/ALS Page 2 of 6 Page 105 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 51 of 55 Data File C:\HPCHEM\1\DATA\012500\PFQSA107.D ~M S D 1 499. E IC -498;6:499:r(0T2500\P FO S A '107;D ) 1 : 5000 : 0i m s l ji 2 ao. 1 2 i u i 2duu\p f u s a iu 7. ) 100000 -; 50000 J J. 0 12 M S D T 312, E IC =31T 7:312.7 (0125001PFOSA107JD) A PI-E S 7R eg, SIM w o li. . 3 a p i-e s , Neg. SIM 4 < wm iU .i / - -, J' - 3 A P I-E S rN e g T S IM 4 100000 50000 0 12 MSD1 498, E C =497.5:498.5 (012500\PFOSA107.D ) 3 API-ES, Neg, S1V 20000 -1 10000 I 01 , ^ 23 MSD1 512, E lC = 5 1 T ,7 ;5 1 Z 7 l0 i2 5 0 0 \P F O S A 1 0 7 ^D ) 'A P P E S IN e g , SIM 4 4 S a m p le N a m e : 9 9 0 3 9 - 1 3 8 - 0 2 F O S A H y d ro ly s is S td 2 - 2 n d in j 56 PFBSMA I 5 5 A 5 6 6 k -.. j PFOSMA 10000 0 i 2' MSD1 3t>9, E lC -3 S b .7 :3 6 9 .7 ( 12500\P FUS A 1Q 7,DJ API-ES, Neg, SlM 4 1 /8 \ I 2000j / d ' - L ------------- ^-- -- --------------------- ...................................... -- ----------------------------------- -- 1 2' 3 ' '4 " MSD1 1087E C =107.7:108.7 (0 1 2 5 0 0 \P F O S A W ;D r'A P F E S , Neg, S lM 350 300 250 '! ` 3 MSLJ1 616, E IC = t1 5 .7 :6 1 6 .7 (0 1 2 5 0 0 \P F O S A 1 0 7 .U ) A P I-E S , Neg, S lM 4 56 '` ' '6 ' ' -- '5 ` ' ' '6 ' 1750 500 250 A 1i MSD1 630, E IC =629.7:630.7 (0125OO\PFOSA1O7.D) i A Pl-ES, Neg, SlM 4 5 400 --- -- ~- 300 6' 123 MSD1 526, 10=525.7:526.7 (Q12500\PFO SA107.D) API-ES, Neg, SlM 4 10000 0 '1 '2 ' '3 ` M S D T 4 2 7, E IC =426.7:427.7 (012500\PFO SAT07.D) API-ES, Neg, SlM -< ' 10000 10 o /t'. i ,/f\ 12 3 4 4 5 5 00 ou_. Q- 5 6 6 56 Data4 9/27/00 11:17:57 AM AES/ALS Page 2 of 4 Page 106 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 3 o f 56 D a ta F i l e C :\H P C H E M \1\D A T A \012600\P F O S A 003.D ~ M S D 'T 4 9 9 rE lC -4 9 8 .6 .r4 9 9 .7 (0 1 2 6 0 0 \P F O S A 0 0 3 .D ) ~ A P r e S ,T r e g 7 S I& T 500 400 S a m p l e N am e : MeOH B l a n k FOSA Hydrolysis pH 9 MeOH Blank 12 34 _ M S D 1 '2 9 8 rE IC s 29777l29877"(0T2600\P FO S A003TD ] A P F E S T N e g T S lM ------- 500 - 400- XT ~ M S D T 3 1 2 , E T C = 3 T -n 7 :3 1 2 T (0 1 2 6 0 0 lP F O S A 0 0 3 .u r'A P I-E S . Neg, SIM 1500- 1000- 500- J ........... i 1 1 1 i " M S D T 4 9 5 , EIC=497:5T4g8 `(0T 2 60 0\P F O S A 0 03 .D )` A P I-H S /N e g T S IM ------------ \ 500 450 400 350 \ i' '3 MSDT5`12TErC=5'1 T 7 i5 '12 77 7 0T 2 6 00 \P F O S A 00 3.D r API-ES7 Neg. S IM 4 350 325- 300 .y"--'-'-_/- T 2' ' ' " MSD1 369. EIC -358:7:36977~(012600\PFOSA003:D) \,a 5 ' ' ' ' I" A P l-E S 7 N e g 7 S lM ------------ / ' ' \,J 500 -j A 400 i 5. -- - J ' ' ' ' 2 ' T ' ' ' ' ' ' 4~ _ M S D 'f_1 0 8 7 B C -1 0 7 ^7 .r4 0 8 ;7 `(O T2500\P FO S A O 0X D ) A P I-E S , N e gT S IM ------------ 325 - / '\ / X-~' \ 300 - 'J 275 \, .................... i 234 ~ M S D V 6 1 5 T E rC = 6 t 5 .7 :6 1 6 .7 (0126001PFO S A 003:D )-- A P P E S I N a flT S IM ------------ 6 __ rom 3201 3001- / *\ A ,, 2 8 0 - j ___ ____ X-- X -.. /V -X /x / v / J MSDr630;`EICT=629r7:6307i:012600\PFOSA003:D)--ATPrESrNegTSIM^ 400 4 350 \ 300 Ir--~ --.-- ' T T " MSD1 526,ElC=52577T526rr{0T2600\PFO SA003X)y f T API: ES7N eg, SIM - 400 350 300 t 1 T 1r ' ' ' r ' ~ M S D 1 4 2 7 rE lC = 4 2 6 .7:427.7 {0 i2 6 0 O \P F O S A 0 0 3 :D r" API-ES7N egTSIM 700 t 600 J 500 400 A -- _________ 6___________ . . . m in Data4 9/27/00 3:46:28 PM AES/ALS Page 2 of 6 Page 107 of 126 to o Hi QT)J CaQ> o co o ro CD Page D a t a 4 9 / 2 7 / 0 0 3 : 4 6 : 4 7 PM A E S /A L S a to pj p> pr r of t HI0-- C3 Ott ^ oi XX 0 n hi X 3M Ui H O tcon o o >OCO o oin b COO' < 301 3(D V1O0 owID (jJ VO oM 3M Environmental Laboratory Report No. EL1132 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 12 of 56 Data File C:\HPCHEM\l\DATA\012600\PFOSA012.D S am ple Nam e: 0 8 1 3 99-B L K -9 .0 " M S D "1'4997E I0=498:6^499:77012600\PFOSA0'12.DJ 'A P I-E S 7 N eg T S IM " 600 400- /\ FOSA Hydrolysis pH 9 Matrix Blank 12 ^SDT2987HIC=297.7:298'7`(012600\PFOSAaT2:D) 600 400 A 34 A P F E S 7 N e g T S lM ------------ f\ /\ i ' 'i ' ' M S D T "3 f2 7 E IC = 3 1 T 7 :3 1 277 (0 1 26 00 \P F O S A 01 2 '.D ) A P I-E S , N eg, S IM 1500 1000 500- i MSD1 498, b lC =4 9 7.5 :4 9 8.5 (0126\PFO$A012.D) A P I-b S , Neg, SlM 4 A j\ i 5' 6' min 5 6 .. m in 600 500 400 ^ \' 1 i ' "M S D rS 1 2 T E rC = 5 1 T 7 :5 1 2 7 r(0 T 2 6 0 0 \P F O S A 0 1 2 :D ) A P i - t s , Meg. S IM 500 - 40 300 ^ 1 2' '' ' ' M S D T3697ElC =368.7T369T7 (0 1 2 6 0 0 \P F O S A 0 T Z D rA P F E S T N e g , SIM 4 A_ __ 5 /\ 45 1 6 min --'6 ' ; min, 800 600 J \ _ 400. , . . j * 1' ' ' 1 MSD1 108. blC=1Q 7.7; 108.7 (012600\P F 05A 012.D J 3' ' 1 API-ES, Neg, SIM 600 ----- 1------'------T --'----- T 5' 6' . .j m in 400- 1i '' _ MSD1 61S7EIC=6T5r7:61677 (012600\P F O S A 0T2:D T A F I-bS , Neg. SIM ------ -- ------------------------ -- ----------------------- --- ............ 45 6 min 400 - JY _ _ 300 - ---- -- '-- --' --- - 12i MSDr6307ElC=629.7:63077012600\PFOSA012Dr'A P I- E S , N e g.'S IM \ 400 350 300 ...... ! . T 1 J ' ~~ 3 4 ` MSDT1 "526, E rC = 5 2 5 7 7 :5 2 6 7 "(0 T 2 6 0 0 \P F O S A 0 1 2 .D )' A P I-E S , Neg, SIM ! 600 ; 500- | 400 300. . , 1 ' ' MSD1 4 27 7E IC =:4 26 .7 :4 2 7 .7 (0 1 26 00 \P F O S A 01 Z ;D ) 3 API-ES7Neg, a lM 4 4000 -i ~ -- 5 / -- ' 5 /\ 5 6 6 6 m in min min 2000 1 . /\ ,, /\ 1 '2 '3 ' ' '4 5 6 min Data4 9/27/00 3:47:50 PM AES/ALS Page 2 of 6 Page 109 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 13 of 56 Data File C:\HPCHEM\1\DATA\012600\PFOSA013.D S am ple Name: 0 8 1 3 9 9-L C S - 9 .0 MSD1 4997EIC=49876:49977~(012600\P FO SAO1 T D J ~ A P PESTNegTSl M------ 60000 40000 00 Q ,U-' 20000 0 A 1 2 3' '4 M SDr2987EC=297.7:29877T012600\PFOSAai37D} APPESTNeg, SIM 1 50000 <to Cll_D, . 0. 0 - ............ .............................................................................. - J p 123 MSU1 312, E iC -3 1 1.7:312.7 (0l260O\PFGSA013.D) API-bS, Neg, SIM 4 " 100000* 50000 - 0 i 2 '' 'M SD1~4g8;EIC^197:5r495;5_{012600\PFOSA0'13:D) ' ' ' ' APP-ESTNeg, SIM 4 100000 50000 0H 4 "M SDT512rElC=511.7:5T27n0T2600\PFO SA(IT3D ) fiP tE S , N eg.S IM ------ ' j - pfOsa < s. .V)\ /E \ FOSA H y d ro ly s is p H 9 Lab C o n tro l 56 5 6 min 5 '6 5' 6 100000 50000 0- MSD1 369, EIC=368.7:369.7 (012600\PFGSA013.D) APl-ES, Neg, SlM i' lw \ oU. \\ /' 5 6 min 800 600 - 400 A .. . _____________________ / ^ ^ ^. U- "M SD 1T08. EIC=107:7riD8777012600\PFOSQT3:Dl API^ESTReaTSIM , _______ _______ _ 5' 6 ........... min 1000001 50000 o4: 12 3 M S D T 4 2 7rE IC = 42 6:7 r4 27 .77 0 T 26 00 \P F O S A 0'13 :D r'A P i:E S rN eg rS IM 15000 10000-' 5000 0 /l\ 4 Data4 9/27/00 3:48:01 PM AES/ALS s ,to, .O ' U_ . / CL 5________ 6 ......... Page 2 of 4 Page 110 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 18 o f 56 D a ta F i l e C :\H P C H E M \1\D A T A \012600\P F O S A 018.D MSDr4997EIC=498~6:'49Sr7(012600\PFOSA0f8~D) APr-ES7Neg7SINT 10000-j 0-1= 12 34 _ M S D r298 rE IC =297.T :298.7`(0 2 6 0 0 \P F O S A 0 1 D r_APr-"ESrNeg. SIM----------- "50000 - ,1 /-\ TT - M S D T 3'127"ErC=3Tr7:3"T27_(0T2600\PFOSA0T8.D) ' "APFESTNegTSIM- I 10000011 I 500010o04I - 1 T " M S D 1" 4 9 8 7 E C=497.'5i4'98T5"((T2600\PFCrSA01 S U f " A P I-E S T N e g, S tfJT S am ple Nam e: 80399PF O S A -019 FOSA Hydrolysis pH 9 Day 0-Sample Trip /;uCD. \v CL 350 325 300 w ' " '2 ' ' ' '5 ' ' ' _MSDr4277EIC=426:7r427r7(012600\PFOSA018.D`) A P I: E S 7N eg7S lM 1 10000-j / `\ 4 Data4 9/27/00 3:48:47 PM AES/ALS 5 _________ ____ 6_____ ____ Page 2 of 4 Page 111 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 19 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \012600\P F O S A 019.D " MSDT~499`~EIC=49B.6:499.7"(0"12600\PFOSA019"DJ 40000 - 20000 3 0 12 SD T2987EIC=2977:29877~(012600\PFO SA0T9XJ APf^S7Ne07S1M~ w A 34 PI-E S T N e oT S IW ------------ S am p le N am e: 8 0 3 99PFO SA -020 FOSA Hydrolysis pH 9 Day 0 - Sample Spike . i ' ' ' j ' 5 1 ' ' 4~ ~MSD1 4277EI C=426.7 :427.7(012600\PFOS019:D) 1 : 10000 4 04i= P rE S T N e g T S IM ------------ w o, Data4 9/27/00 3:48:55 PM AES/ALS _ 5 ___________________6 _____ __ _ Page 2 of 4 Page 112 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 47 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \012600\P F O S A 047.D " MSDr4997E[C=4 AP-ES, Neg, SIM 10000^ 1 _MSDT2987ErC=297:7T29877~(0T2600\PFOSA`0r47X)) APFES7 Neg, SW T | 50000 :CD\ " MSd1~3'127HrC=3TT7:312:7"(OT2600\PFOSA047,D} API-ESrN eg7SlM "" 100000-j 50000 j T' ' ' 1T 13 ' ' ' 1 W S D T 4 9 8 7 E IC = '49775749?5TOT2600\PFOSAO"47:D) A PI-E S 7 Neg, S IM " S am ple Nam e: 80399PFO SA -163 FOSA Hydrolysis pH 9 Day 42 - Sample Trip 65 min 65 min. 1 2 ________ 3 Data4 9/27/00 3:52:59 PM AES/ALS ______ 4___________ 5 _______________ 6 ......m in Page 2 of 4 Page 113 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 48 o f 56 D a ta F i l e C :\H P C H E M \1\D A T A \012600\P F O S A 048.D S am p le N am e: 80399PFO SA -164 ~"M S D f'4 9 9 ," E l C =49B 76I4997~(0T2 6 0 0 \P F O S A W B T D T ^ P F E S . Neg, S IK /T I WO ! 40000 -j I 20000 4 /Q-` FOSA Hydrolysis pH 9 Day 42 - Sample Spike 12 3 _ M S D T 2 9 8 rE IC = 2 9 7 .7 T 2 9 8 7 n O T 2 6 0 0 \P F O S A 0 4 8 .D r_A P P E S T N e g T S lM 4 5 00 00 -] oi 12 " WSD1 3 1 2;'E !C = 3T 1 T 7 T 31 2 .T (0T 2 6 00 \P F O S A 04 8:D ) hitia-\\ Av 34 A P F E S T N e g T S IM ------------ 100000- 50000 0- "MSDTi ~5 S'TNeTgTSTlM--'---4-~ /IfSr\\ 200000 - 100000 0 - 1 1 T 1 ] ' 1 r-- 1 \ ' " _1 T 5 T 1 1 ' W S D T 5 T 2 7 E r 0 5 1 1 .7 :5 1 2 7 (012 60 0\P F O S A G 4 8.D ) ~ A P I-E S 7 N g T S !M 100000 50000 0 T- ^4SD T369rEIC=3687T36977T012600\PFO SA048TD) T~ API^ESTTegrSIM " k /8\ 100000- 50000 0 1 T~ " M S D 1 _4277E IC = 42 6:7 r4 27 T 7 "(0 T 2 60 0 \P F O S A 0 4 8 `.D ] - 10000J oi ' A PrESTN egTSIM - w a li\ Data4 9/27/00 3:53:08 PM AES/ALS 5. /:OV)\, . 1 Li. \ Q. Page 2 of 4 Page 114 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 50 o f 56 D a ta F i l e C :\H P C H E M \1\D A T A \012600\P F O S A 050.D MSD1 4997~E(C=49876:4997T(0T2600\PF0 SA0507D)'~A P FESTNegTSIM~ 5004 400 i 300X S a m p l e N a m e : MeOH B l a n k FOSA Hydrolysis pH 9 MeOH Blank 400! 3501 300 12 3 "M S D r427TE rC =426T^27TT0T 2600\P F O S A 05C TD r"A P reS 7N egrS !M _ 600A 5004 A 4004 V'-' Data4 9/27/00 3:53:27 PM AES/ALS Page 2 of 6 Page 115 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 52 o f 56 D a ta F i l e C :\H P C H E M \l\D A T A \012600\P F O S A 052.D M S D T 4 9 9 7 B C = 4 9 8 :6 :4 9 9 .7 `f01260 0\P F O S A 0 52 ~D ) APSES', N e g rS IM ---------- 10000 1 : 5000 : oJ. , - V - , rT- , . , 12 M S D T 298;E [C =29777T298;r(012600\P FO S A 052.D ) p Al.\ ! ' 34 APr-ES7NeQ,- SIM--------- 1 50000 4 ;E\ h-\ 04 . T I j ' ' ' ' 5 ' ' ' F 4 S 0 1 3 1 2 rE IC = 3 T 1 7 T 3 `1 27 7 0 T 2 6 0 0 \P F O S A 0 5 2 X J) A P I: E S ,N e g 7 S lM _ 100000 50000 4 04= T T " M SDT498rETC=497i5T49875'{O ri2600\PFOSA052iD) APPES7Negi~SlM - S am ple Nam e: 9 9 0 3 9 -1 3 9 -0 2 FOSA Hydrolysis pH 9 Std 2 - 2nd inj m in Data4 9/27/00 3:53:50 PM AES/ALS Page 2 of 4 Page 116 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 2 o f 55 D a ta F i l e C :\H P C H E M \1\D A T A \012600\P F O S A 058.D 'MSD1 499/EIC=498:6r499'.7~(012600\PFOSA058:D) APl-ES,'Neg7SlM~ 500 400- . ,1 2 MSD1 298, E lC = 297.7:290./ (012600\PFOSA058TDJ 3 A P l-E S , Neg, SIM -6 0 0 400- 123 MSD1 312 7E IC = 31 1.7:312.7 (0 1 26 00 \P F 05 A 0 5 8.U ) A P l-E S , Neg, SIM 4 4 S a m p l e N am e : MeOH B l a n k FOSA Hydrolysis pH 11 MeOH Blank 56 . ---- 5 '6 1000- 500^ 4 , , ' ' ' i M 5 D T 4 9 S rE IC = 4 9 7 .5 :4 9 8 .5 ^0 12B00\PFO SA058.D) A P l-E S , Neg, SIM 1/ \ \ --------------- - 45 -------- _ . ------- 6 550500 450 S \ _s- _ ^ / A \ y ^w '-- ' , \ ' 2' ' ' '3 M S D 1 5 T Z T E IC = 5 1 1.7:512.7 (0 1 2600\PFO SA058T5] A Pl-E S , N eg SIM 4 400- 350- 300- . . . , ' M S D T36grE IC =36a.7:3697T(01Z500\P FO S AD 58T3T -5 0 0 i' API-ES, Neg, SIM "1 4' \! \ / .' 5 ._ / _J / -, \ . . 5 ' 6 ... -400 ~ -- ---------- i i ' '3 MSD1 T08, E1C=107,7 :1 0 8.7T012600\P FO SA 05o.D ) API-ESTN eg, SIM 4 1' 340 320 300 280 V ' ' ' 1 ....................... ' ^ ' i .................... \ raSDT6T67EIC=6T577!5T6:71[0TZ6OO\PF0SAO58:D) APFESTNegTSIM 320 -j k300 y/ y\ a --a y \ / V ' - ' - a _ ..a 280 i '' ] ___________________________________ _ ' ^ 1 2 13 1 MSD1'630;E1C=62S.7:530.7 (012600\PFOSA058.D)--API-ES7Neg7SIM /- 4 0 0 -] 350 , 12 34 MSDr526,t1C=525;7T526.7(012600\PFOSA058;Dr_ APr-ES7Neg7SIM 5 0 0 -j 400 ; 300 i 12 MSD1 427, ElC =426,7:427.7 (012600\PFOSA058.D ) 3 API-ES, N eg.'S IM 600 500 400 4 '~ Data4 9/28/00 9:58:36 AM AES/ALS J _______ 6 Page 2 of 6 Page 117 of 126 a 3w m oii _k u U9 k > T1 oin rO>2HT- ow P> p rprj hn- rnrtr ?d fMl> C3 O=tt= wor^c oH> M on 3 in >HO> M CT *nns ocn > o - PFBSA 8 6 - PFOS 3M Environmental Laboratory Report No. EL1132 Page 118 of 126 p f Gs a PFBSMA on pj -i 00*rj S t-J ffi M I f'J? Si p> 3 CD VO VO TX3 o NJ BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 11 o f 55 D a ta F i l e C :\H P C H E M \l\D A T A \012600\P F O S A 067.D S am p le Nam e: 0 8 1 3 9 9 -B L K -ll.0 "M SD 1 499, EIC =49876:499I7~(0`1 26 00 \P F O S A 06 7 :D ) "A P F E S , Ng, S IM i J600 i 4: 500 -400 r i ! 300 - 234 * M S D f 2 98 , E IC=29777:298T7 f0 1 2 6 0 0 \P F O S A 0 5 7 .D V '"A P I:E S , Ng, S IM ~ F O S A H y d ro ly s is M a trix B la n k p H 11 5 6 .... min. 500 : 400 i 300 *t 1 2 3 MSD1 312, EiC=311.7:312T.7 (012600\PF Q S A 067.D ) A PI-E S , Neg, SiM -i1 0 0 0 -i! 500 ii \ '' i ' ' '3 ' ' `MSD"1-4987EiC="49775:'498:51(012600\PFOSA067X)j APPESrNegTSIM 4 f\ J\ 4 600 | 5 0 0 -j 4 0 0 ____ ________ _____________ ____ , ___ -- 1 2 3` MSD1 512, lC = 5 l 1.7:512.7 (O 12600\PFQ SA0673J) A P l-tS , Neg, SIM - ----------- ' - j-- 5 6 m in ' 5 6 min -- . 5 ...- . 6 min t Cl CD O oo oo oo oo 400 300 - ' ........1 " 1 1 1 MSD1 369, E IC =368.7:369.7 (012600\PFOSA067:D ) i 1 r" 1 4 API-ESTNegTSIM ~ '` 5 '6 min. r '\ 1\ / ------------- ......................... i 1 ' " ............................. r .............................. 1 ............................ MSD1 108, EIC "=T0777:f08:7l012600\PFO SA067:DT" A P F E S 7N eg rS IM 5 ' '6 min 350 300250 - A J . 'i . 2 _ 3 400 300 1' i' '3 ' MSD1 630rEIC=62977T630r710T2600\PFOSA067.'D) A PFE S , Neg, SIM _/ 4 . . . . - ____ 5 '' 4 '' 5 .. .... -- 6 min 6 min 400 300- 1 2' 3 MSU1 526, E lC = 52 5.7 :52 6.7 (0 1 2 6 0 0 \P F O S A 0 6 7 .D )A P I-E S , Neg, SIM 600 -, 500 4 400 J 123 MSD1 '4 27 , EIC=426.7r427:7'{0126G 0\PFO SAG 67^D) A P l-E S , Neg, SIM 4000 to 8, 2000- 123 Data4 9/28/00 9:59:57 AM AES/ALS 4 4 4 -- 5 6 m in 5 6 min 5 6 m in Page 2 of 6 Page 119 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 12 of 55 Data File C:\HPCHEM\1\DATA\012600\PFOSA068.D S am p le N am e: 0 8 1 3 9 9 - L C S - ll.0 'M S D 1 499,~EIC=498.6r499.7 (0 1 26 00 \P F O S A 06 8 :D r API-ES, Ng, S IM - 60000 40000 20000 0 o u. >0.. /, "MSDr298rEIC=297:7:298;7'(0i260Q\PFOSA066:Dr"APr-ES7Reg7SlM~ < w 50000 CD Li. ; q- o-I-, ..... f 12 34 " MSD1 312rE!C=3TL7T312 7 (0 12600\P FO S A 06frD )^A P I-E S rN eg, S 1M "~ FOSA Hydrolysis pH 11 Lab Control -j1 0 0 0 0 0 J 50000 0 i- T _M SO 1~4987E IC =497.5!4984r((yi2600\P FO SA 068X i] 100000- API:E S ,N e g 7 S IM " 50000 04 _ M S D T 5127EIC =5T 1T:5T27~{O T2600\P FO S A 06irD } APEES7Neg7SIW " i 100000 ; 50ooo] ! 04 = _ t ' 2 " 1 1 1 3 r~ ~ M S D T 3 6 9 7 E IC = 3 6 8 :7 i3 6 9 :7 "(0 1 2 6 0 0 \P F O S A 0 6 ffD ] A P I: E S 7 N e g 7 S IM ------------ j 1000 ! 800 j 600- i 400- TXX ~M SD 1T08rE IC =107r7n08777012600\P FO S A 068.D J API-ES7Neg7 S!M ~ fc\ A.O', /!t\ 44Ml. /V X M SD X 6167610*61 577T6T677_(OT2600\PFOSA068:D)-- APFESTNigTSIM" 1 ' 2' 3 " M S D T"6307E IC =629:7:63071(0'T2600\PFO S A 068D ) API-E S 7N eg7SIM ` 4 400 /3 0 0 ~W S D r5 2 6 7 E IC = 5 2 5 7 :5 2 6 X 1 0 12600\PFOS A 0 6 8 ;D r"API-ES7 Neg7SJM_ 1 : 100000 50000 o 12 3 M S D T 4 2 77 E I0 42 6 7:4 27 7 r(0 12 6 00 \P F O S A 06 8.D r4A P [-E S ;M e g 7S iM 4 10000 07 Data4 9/28/00 10:00:08 AM AES/ALS o ' u. , Q_ ' Page 2 of 4 Page 120 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h R un # 17 o f 55 D a ta F i l e C :\H P C H E M \1\D A T A \012600\P F O S A 073.D S a m p le ame : 80399P F O S A -023 M SD1 499. ErC=498.Sr4997T0T2600\PFO SA073T3) A P I-E S , Neg, SIM 10000 - F O S A H y d ro ly s is p H 11 D a y 0 - S am ple T rip 012 ~MSD1 298, E rC ~297.7:298.7 (012600\PF O S A 073.D ) 3 A P l-E b, Neg, SIM 4 50000 < (0 co /Il 0 V 123 M S D 1 3 1 2 T E IC = 3 1 T 7 :3 1 2 7 `( 0 1 2 6 0 0 \P F O S A 0 7 3 .D r A P F E S T N e g , S IM ' 100000 - 4 50000 01 2 ' 4 ''' MSD1 498, E IC =497.5.498.5 (012600VPFUSAU73.U) A PI-ES, Neg, SIM 4 ' i ,S ' /- 5 5 5 6 6 -- ^6 m in min 100000 0 i i ' ' 'i ' ' ' ' M 5 U i 51Z, E IC = 5 1 1*7:512.7 (1 Z60\P FO S AD73;D ) A P F E S 7 N e g 7 S IM 4` o\ /u -\ 1000 -| f\ 5 min 500 J /V 1 - __________ -- ---------- -- ----------------------------------- _ ------------ ---------- ! v 1i 3 "MSD1 369, E l0=368.71369.7 ( l2600\P FO SA 073.D ) API-ES, Neg, SIM 1000 750 500- _ / v _____________________________________ _____/ v -- 1 2 ' ' 'i ' ' ' ' M S D n 0 87E IC =107;7:108.7 (012600'R FO S O T73X >r~AP !-E S rrN eg7S IM 4 4 400 L3 0 0 - A __ __________________________________________________________ .. ., 2 '3 ' ' MSD1 616, EIC =615.7:616.7 (0 l2 60 0 \P F S A 07 3 .D ) API-fcb, Neg, b lM 500 - 4 400 A_ _ 300 . . ., 2 ~MSD1 630, E IC =6Z9.7:530.7 (012600\PFOSA073.D ) 3 A P I-E S , Neg, SIM 4' - 5 6' 5 . .^. . 5 min T 6 min. 400 - /A . 300- 4I . 1 ' ' ' 3 ' ' 'M S D 1 5 26 , E IC = 5 2 5 :7 :5 2 6 :7 "(0 1 2 6 0 0 \P F O S A 0 7 3 `.D ] A P I-E S , N g. S IM - 5 - 6 min 350 300 ------ - - ' "- ,, ________ ...__.. 123 MSD1 4 i, b lu =420.7:427.7 (U12bUU\PFUbAQ73,U) A PI-E S , Neg. SIM 11 1 oo o 1 10000 j 5 ,/f V 12 3 Data4 9/28/00 10:00:55 AM AES/ALS 4' 4 '' 65 min 5 6 m in Page 2 of 4 Page 121 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 18 o f 55 D a ta F i l e C :\H P C H E M \1\D A T A \012600\P F O S A 074.D MSD1 499,~E!C=498.6:49977'(012600\PFO SA074:D)-- A P F E S rN e g .S IM i 40000 -j 120000 ` 1 ~ M S D T 29 8 7^T C = 29 7 T yZ 98 7 7 r (0'IZ 50 0 \P F U S A Q 74 X )] 50000 oi= A P F E S 7N eg ,""S IM _ w< Q-t/,CuQ.'.\ M S D T 3 T 2 . EIC =31 F 7 :3 `12rT(C T125C iO \P FO SA 074:D p'AP i-E S , N e g / SIM " 100000 50000 - '0 - 1 1 1 i ' 1 1 ' 2 1 ' ' 1 5 1 1 ' 1 r - M S D T 4 9 B , E IC = 4 97 :5 T 4 9 8 T 5 l0 1 2 6 0 0 iP F a S A 0 7 4 :D ) " A P P E S T N e g T S IM ------------ S am p le Name: 80399PFO SA -024 FOSA Hydrolysis pH 11 D ay 0 - Sample Spike ;W\ 2\ 500 400 300 r'" 1 ' T' '2T' * '3 T TV M S D r6 3 0 7 E IC ^ 6 2 9 -.7 :6 3 0 J l0 1 2 6 0 0 \P F O S A 0 7 4 T D )-- A P I-E S rN e g T S lM ---------- - 400 V ' 300 12 3 " MSD1 5267E IC S 525;7:526X (012600\P F O S A 074:D r~ A P r-E S 7N igrS IW 4 ~~ 100000 4 50000 -j o4= 12 3 _ M S D f "4 2 7 7 E 10=42677:427771(0 T2600\P F O S A 0 7 4 X ))~ A P F E S 7 N e g 7 S lM 15000 A 10000 -I co Si 5000 4 0-1= / H* * 4 Data4 9/28/00 10:01:03 AM AES/ALS A. mfi o Page 2 of 4 Page 122 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 46 o f 55 D a ta F i l e C :\H P C H E M \l\D A T A \012600\P F O S A 102.D ~ M S D T 4 9 9 ,` E tC =498.6:499:T (0T 2600\P F O S A 102.D y APr-ES, N eg, S IM ' ! 10000-j ! oi _ M S C rr2 9 8 rH iC = 2 9 7 :7 :2 9 8 7 7 _(& i2 6 0 0 \P F O S A T 0 2 :D ] A P F E S rN e g T S IM - : 50000 4 3 la. , i o4 . T 2 '' 3' ' ' 4 M S D r 3 1 2 7 E IC = 3 T F 7 :3 1 2 .7 (0 1 2 6 0 0 \P F O S A 1 0 2 .D y ~ A P F E S 7 N e g 7 S IM ------------ 100000 50000 - . . t ' ' 5~" ' ' ' s- ' ' ' ' r S1SDT4987ErC=497T5395:5`((7126001PFOSA102:D) APFESTNegTSIM- S am ple Nam e: 80399PFO SA -167 FOSA Hydrolysis pH 11 / \ Day 42 - Sample Trip I------------------- M SDrffT6;EIC=615;7T616T"(012600\PFO SA102.D )" 7A,PFES7Neg7SIM" 500 400 300`1 2 3 - M SDT5307EIC=629.7:63Ci7'[012600\PFOSA102:D) AP7ES7Neg7SIM 4 400 i 300 12 3 - MSDT5267EIC=525T:52677~(01'2600\PFOSAT02".D ) A Pl-E S7N eg7S IM 4 400 350 300 1 " MSD1" 4277ErC="426` 7:427:71fO 2600\P FO S A T0Z'D ) 10000\ 0-U APPESA NegTSIM" <n a lz \ Data4 9/28/00 10:05:07 AM AES/ALS Page 2 of 4 Page 123 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 Batch Run # 47 of 55 Data File C:\HPCHEM\l\DATA\012600\PFOSA103.D ^M S D T 4 99 7 E rcs49 8 :6 r4 S g:r(ai2 6 00 \P F O S A T 03 :D r~ A P [:E S rN e g T S IM ~ 1 40000 20000 o- oVi LL ;'CL / Cl ' M S D r2 9 8 7 E IC = 2 9 7 7 7 T 2 9 8 ` 7" (0 1 2 6 0 0 \P F O S A "'i0 3 :D )"A P rE S 7 N e g 7 S lM -- ' 1 i 50000 A M< At 0- _ _1 2 3 4 _ raSD T3TZrHrC =3TT7T32:7`(02 600\P FOS AT 03TD) 'AP F E S7NgTS IM------------ 100000 I 50000 i ' 04 "" Ti ' ' ' T5 ' 1TT5 T T ' TT " M S D TM 8 7 E IC ^ 4 9 7 :5 :4 g a :5 '( 0 T 2 6 0 0 \P F O S A f0 3 D r 'A P i- E S 7 N g 7 S IM ------------ 200000 - 100000 0 i ~T 'H S D T5T2rE IC =5T1777512.r(012600\P FO S A 103:D )" T A P reS 7N egrS !M _ S am ple Nam e: 80399PFO SA -168 FOSA Hydrolysis pH 11 Day 42 - Sample Spike < l* \ 10000 0 Data4 9/28/00 10:05:15 AM AES/ALS Page 2 of 4 Page 124 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL1132 B a tc h Run # 49 o f 55 D a ta F i l e C :\H P C H E M \l\D A T A \012600\P F O S A 105.D MSD1^4997ElC=49B.6:4997r(012600\PFOSA1057DJ API-ESTNegTSlRT 500 J 400 J 300 12 MSCT1 298rEIC=2977:2987r(CT12600\PFOSAT05:D] 34 APFES7 NgTSIM---------- 600 400 T _MSD1'312rHIC=J1T.77312.7 (012600\PFOSA1057D) APFESTNegTSlM'" 1000 -j 500 | t i ' ''i ''' ' M S D 1 4 9B 7E IC = 49/ .5:498.5 (U12600\PFQSAT05T>J A P F E S 7 N e g 7 S IK t 4 S a m p l e N a m e : MeOH B l a n k FOSA Hydrolysis pH 11 MeOH Blank ` MS0110S.BIC^107:7ri08:7`(012600\PFOSS105X>r_APreSi;Nefl7SISr 300 275250 T T" T _ MSDr61B7EIC =6T5:7:616.7(ff12600\P FOSA105.D r~APFES7Nea7SIM- 320 ! 300 | 280 1i /'' i ....... A /' 5"" ".............r - MSDT630;EIC=B29T73B3ini0T2600\PFOSAT05D) APFESTNegTSlM 400 350 300 ....T ........................2 ' i 4 - MSDT5267EIC=52577T52677~(0`12600\PFOiSAT05TDJ APFESTTCegTSIM---------- ! 400 350 300 K 12 34 ~MSD1~427, EIC=42677r427.7l0T2600\PFOSA105.Dr AP|:ES.'Neg7SIM---------- ! 600 A 500 -j 400 T Data4 9/28/00 10:05:34 AM AES/ALS A -v\ / \ / V A . "W ___ 6 J --J: ....................m in Page 2 of 6 Page 125 of 126 BACK TO MAIN 3M Environmental Laboratory Report No. EL 1132 Batch Run # 51 of 55 Data File C:\HPCHEM\l\DATA\012600\PFOSA107.D ~MSDr4997E[C=498:67499.7T0T26001PFOSAT07:D} 10000 5000 APl-ES^NegTSIM- w a h\ 0 12 34 _ MSDT2987EIC5297:7:2987''{012600\PFOSA107TI)~APrESri` NegrS!H---------- | 75000.| vj 50000 A 25000 -I 1 0-D T 4 M S D 1 -312rE lC =3ir.7:31Z7`(0'i2600\PFO SA107Dr_APi:ES:Neg7SIM" 100000 50000 0 4 ----------------------------------------------------------------------------------------------------- " : i i 4 ..................M SD 1"498rEIC=497^r49B;5X012600\PFOSAT07X>)-- API-ES7Neg7SlM----------- 20000 A j 10000 I 04 TT ~MSD~r5T2TEIC=51T7:512T"(0T2600\PFOSAT07iD) APFESTNegTSIM- 20000 - 10000 0i 4 111i ' ' ' ' _M S D n6 9 7 E IC = 36 8 :7 :3 6 9 .r(0 12 5 0 0\P F O S A 1 0 7 :D )_~APP ES7NSgrSIM ' 4 S am ple Nam e: 9 9 0 3 9 -1 4 0 -0 2 FOSA Hydrolysis pH 11 Std 2 - 2nd inj m\ /CD\ /it. \ I CL v ft Av 400 350 -i 300 . ^ ' ' 1 j ' ' ' ' 5 ' ' ' 1 J~~ M S D T'5 267 "E iC = 52 5 77 i5 26 7 7'(O 1 2 60 0 \P F O S A T 0 7 iD ) A P F E S 7 N g T S lM ------------ 20000 -i 100004 ol _ '] '' ' ' '3 " T 4~ : MSD"1~4277Erc='4 26777427jr (012600\PF O S A T077D ) A P l: E S 7 N g7 S l M------------- 15000 J . 10000J 50000 74= k 2 Data4 9/28/00 10:05:53 AM AES/ALS A ,---'-' ;mOf t Page 2 of 4 Page 126 of 126