Document 3Jjx8vpz53qp3XD0zro8bREQO

ST-460 ToxDocs 13-430 TOXICOLOGY ASSESSMENT AND COMPLIANCE ASSURANCE GROUP 3M COMPANY 13-430: ACUTE INHALATION TOXICITY STUDY OF MTDID 37312 IN MALE RATS FINAL REPORT ToxDocs Study Number 13-430 Test Material Lot Number(s) Strategic Tox Lab Study Number MTDID 37312 Lot 30107 (per GID 103988) ST-460 Other Identification Number(s) FC-10 19F/1H-NMR Analytical Report LIMS ## M13-1896 (see Appendix LIMS Number 1: Certificate of Analysis) Study Director Jill Hart, AAS, LATg Senior Laboratory Technologist Study Monitor Sue Chang, Ph.D. Senior Toxicology Specialist Testing Facility In-Life Start Date 3M Strategic Toxicology Laboratory 3M Center, Bldg 270, room SB324 Saint Paul, MN 55144 December 9, 2013 In-Life Termination Date December 30, 2013 1 of 12 ST-460 `ToxDocs 13-430 TOXICOLOGY ASSESSMENT AND COMPLIANCE ASSURANCE GROUP 3M COMPANY 13-430: ACUTE INHALATION TOXICITY STUDY OF MTDID 37312 IN MALE RATS Compliance Statement and Signature Page `This study was conducted to regulatory guidelines. for research and development purposes and does not conform This final report has been reviewed and approved by: CeHoe Jil AAS, LATg SSteundioyrDLiarbeocrtoartory Technologist [2JAN. 2015" Date 7 2= = `Sue Chang, Ph.D. SSetnuidoyrMToonxiitcoorlogy Specialist (9 Jan, 2015 Date 20f12 ST-460 ToxDocs 13-430 1 Study Summary This study was to evaluate the serum uptake and metabolism of MTDID 37312 (white solid, 99.9%pure, N-ethyl-heptadecafluoro-N-(2-hydroxyethyl)-1-octanesulfonamide, N-EtFOSE) upon inhalation exposure in male Sprague Dawley rats. Using a flow-through setup, male rats (N=4) were exposed, whole body, to approximately 7 ppb (v/v) of N-EtFOSE for 6 hours. Observations were made continuously throughout the exposure. All animals appeared normal during the entire study period and all animals survived until the scheduled necropsy. There were no significant findings or gross lesions observed during the necropsy. Serum samples collected before and after exposure were analyzed for N-EtFOSE concentrations as well as the concentrations of its metabolite, perfluorooctane sulfonate (PFOS), by LCMS/MS. While three of the four animals had quantifiable N-EtFOSE in the serum immediately after the exposure, only one animal had quantifiable serum PFOS at the same time. Eighteen hours after exposure, while only one animal still had quantifiable serum N-EtFOSE, all of them had PFOS present in the serum. The level of serum PFOS continued to increase up to Days 8 - 14 after exposure before it declined on Day 21. Within the limit of the study design, data obtained here suggested N-EtFOSE can be absorbed into blood and metabolized via inhalation exposure. Percent of inhaled N-EtFOSE dose converted to PFOS-equivalent dose ranged from 12.21 7.22% to 21.59 9.52% in male Sprague Dawley rats. 2 Study Objective This study was to evaluate the serum uptake and metabolism of MTDID 37312 (white solid, 99.9%pure, N-ethyl-heptadecafluoro-N-(2-hydroxyethyl)-1-octanesulfonamide, N-EtFOSE) upon inhalation exposure in male Sprague Dawley rats. 3 Test Material Information 3.1 Test Substance Test Material ID Lot Other Identification Purity Physical State of Test Material Chemical Name Chemical Structure MTDID 37312 Lot 30107 (per GID 103988) N-EtFOSE, N-EtFOSE Alcohol, FC-10 99.9% Vapor N-ethyl-heptadecafluoro-N-(2-hydroxyethyl)-1octanesulfonamide CF3(CF2)x-SO2-N(CH2CH3)-CH2CH2-OH 3 of 12 ST-460 ToxDocs 13-430 Molecular Weight Density Vapor Pressure 571 g/mol N/A ~17 ppb @ 23C (estimated) 3.2 Dose Preparation Dose Preparation Physical State of administered material Route of Administration Due to low vapor pressure at room temperature, the test material was coated onto micro beads and the beads were packaged in a sealed stainless steel generator cartridge by the 3M Environmental Lab. The test atmosphere was generated at room temperature when air flow was introduced through the generator cartridge containing N-EtFOSE at a constant flow rate (2 L/min) and into the 40 L chamber. Vapor Inhalation (whole body exposure) 4.1 Test System Information Species Strain Source Age at Initiation of Treatment Weight at Initiation of Treatment Number and Sex Identification IACUC Animal Usage Application Number Rat Sprague-Dawley Harlan 6-8 weeks 253-275 g 4 males Unique tail mark in indelible ink 2013-0001 4.2 Animal Husbandry Housing Diet/Water Housing Environment Test Chamber Environment All rats were group housed in solid bottom cages throughout the study with the exception of the exposure period. Harlan Teklad Rat/Mouse 2018 Diet (Harlan Teklad, Madison, WI) and tap water were available ad libitum throughout the study except during the exposures. Temperature Range 72 3F Humidity Range 30 - 70% Minimum of 10 exchanges of room air per hour 12 hour light/dark cycle Temperature Range 69 - 72F Humidity Range 37 - 93% 4 of 12 ST-460 ToxDocs 13-430 5.1 Study Design Animals were exposed, whole body, to N-EtFOSE at approximately 7 ppb (v/v) for 6 hours. Control animals were not utilized in this study. The study design is presented in the following table: Dose Grou p 1 N-EtFOSE Concentration (ppb) 7 ppb (v/v) (see Section 9.5 as well as Appendix 2) Exposure Time N (males) Interim tail vein bleeding (for sera) Euthanasia 6 hours Pre-exposure; also immediately, 18 h, 21 days 4 24, h, 48 h, 72 h, post Day 8, and Day 14 exposure post exposure 6 Parameters Evaluated 6.1 Clinical Observations Each animal was observed throughout the study for clinical signs of toxicity and mortality. 6.2 Body Weight Body weights were recorded for all animals prior to exposure and on Days 1-4, 7-11, 14, 17-18, and 21 post-exposure. 6.4 Serum Collection Prior to exposure and throughout study period, interim blood samples (approximately 200 uL) were collected via tail vein to labelled collection tubes without anticoagulant at designated time as outlined in Study Design. On Day 21 post-dose, all animals were euthanized via CO2 asphyxiation and for each animal, blood was collected ( 6 mL) via the abdominal aorta and transferred to labeled collection tubes without anticoagulant. The blood samples were allowed to clot for 15 to 30 minutes at room temperature and then centrifuged at 2000 x g for 15 minutes. The resulting supernatant (serum) was transferred to labelled polypropylene microcentrifuge tubes. Serum samples were stored frozen at -70oC pending LC-MS/MS analyses. 6.5 Gross Necropsy, Organ Weights and Tissue Collection Gross necropsies were performed on all animals on Day 21 post-exposure. The livers were harvested from each animal, weighed, and stored frozen at -80 degrees C. There were no other tissues collected. 5 of 12 ST-460 ToxDocs 13-430 6.6 Analytical LC-MS/MS was used to determine the test chamber air samples by using Occupational Safety and Health Administration (OSHA) versatile sampler (OVS) tubes to trap air immediately before the inlet of the exposure chamber and also immediately at the outlet of the chamber followed. The tube absorbent materials were then extracted and analyzed for N-EtFOSE by LC-MS/MS (work performed by 3M Environmental Laboratory). Separately, LC-MS/MS was performed by 3M Medical Department Bioanalytical Lab to determine concentrations of N-EtFOSE and PFOS in the serum samples collected from animals. 7 Statistical Analysis Microsoft Excel software was used to calculate mean and standard deviation. 8 Raw Data The raw data for clinical observations and body weights are recorded in 3M Notebook # 163984, pages 107 - 111. 9 Results 9.1 Clinical Observations Clinical observations were normal throughout the study. All animals survived until the scheduled necropsy. 9.2 Body Weights/Liver Weights Body weights and liver weights are shown below. Animal # 3R674 3R675 3R676 3R677 Tail Mark Blue I Blue II Blue III Blue IV Body Weight (g) Day 0 (pre- Day 1 Day 2 Day 3 Day 4 Day 7 Day 8 Day 9 Day 10 Day 11 Day 14 Day 17 Day 18 Day 21 exposure) 267 271 270 272 278 290 294 296 300 304 318 323 321 334 275 274 275 279 282 296 302 304 310 311 328 338 338 350 253 253 252 259 259 279 284 291 294 297 314 323 329 335 274 277 273 281 282 298 303 310 314 310 335 343 347 354 Liver Weight (g) Day 21 13.20 13.80 14.76 14.51 9.4 Gross Necropsy Gross necropsies were performed on all animals on Day 21 post exposure. There were no abnormal findings nor gross lesions noted. 6 of 12 ST-460 ToxDocs 13-430 9.5 Analytical Results The test atmosphere concentrations of N-EtFOSE done with OVS sampling indicated that NEtFOSE concentrations inside the inhalation chamber varied between 9.43 0.33 ppb v/v (mean concentration at inlet) and 5.31 1.34 ppb v/v (mean concentration at outlet) (see Appendix 2: 3M Environmental Laboratory Final Analytical Report E13-0880). The difference in concentrations between inlet and outlet could be attributed, in part, by the adhesion property of N-EtFOSE onto the furs of the rats as well as inhalation chamber surfaces. Therefore, for the study results reported herein, the approximated overall mean of 7 ppb (7.37 2.35 ppb, rounded to 7 ppb) obtained at both inlet and outlet was used to represent test chamber concentration for N-EtFOSE. Data for serum concentrations of N-EtFOSE and PFOS are shown in the table below: Animal # 3R674 3R675 3R676 3R677 Serum N-EtFOSE concentrations before and after 6-hour exposure to N-EtFOSE, ng/mL Before After Pre- Immediately 18 hrs 24 hrs 48 hrs 72 hrs Day 8 Day 14 Day 21 exposure < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ 3.1 2.2 < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ 1.3 < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ 1.3 < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ < LLOQ Animal # 3R674 3R675 3R676 3R677 Serum PFOS concentrations before and after 6-hour exposure to N-EtFOSE, ng/mL Before Pre- exposure < LLOQ < LLOQ < LLOQ < LLOQ Immediately < LLOQ 3.3 < LLOQ < LLOQ 18 hrs 6.2 14.3 5.5 5.0 24 hrs 6.7 13.6 5.0 7.1 After 48 hrs 72 hrs 7.1 7.7 16.0 17.7 7.0 7.9 5.9 7.5 Day 8 11.6 19.4 10.2 9.4 Day 14 11.2 22.3 10.9 10.6 Day 21 7.4 18.9 4.9 5.7 LLOQ = lower limit of quantitation (0.5 ng/mL for N-EtFOSE and PFOS) 9.6 Theoretical N-EtFOSE Dose Inhaled Theoretical resting ventilation volume for Sprague Dawley Rats = 0.102 L/min Based on experimental determination from a group of 16 Sprague Dawley rats with a mean body weight of 364 grams and mean ventilation volume of 28 mL/min/100g BW; Strohl et al., J Appl Physiol (1985). 1997 Jan;82(1):317323. Mean chamber [N-EtFOSE] = 7 ppb v/v = 0.16 ug/L [7 x 10-9 x (571 g/mol)] / (24.45 L/mol) = 0.00000016 g/L = 0.16 ug/L 7 of 12 ST-460 ToxDocs 13-430 Theoretical amount of N-EtFOSE inhaled in 6 hours (360 minutes) = 5.88 ug 0.102 L/min x 360 min x 0.16 ug/L = 5.88 ug 9.7 Theoretical PFOS-equivalent Dose derived from Serum PFOS Concentration Animal # Serum PFOS concentration after N-EtFOSE inhalation exposure, ng/mL PFOS-equivalent dose, ug/kg Assuming each time point is Cmax Dose = Cmax x Vd; Vd = 300 mL/kg Immediately 18 hrs 24 hrs 48 hrs 72 hrs Day 8 Day 14 Day 21 Immediately 18 hrs 24 hrs 48 hrs 72 hrs Day 8 Day 14 Day 21 3R674 < LLOQ 6.2 6.7 7.1 7.7 11.6 11.2 7.4 1.9 2.0 2.1 2.3 3.5 3.4 2.2 3R675 3.3 14.3 13.6 16.0 17.7 19.4 22.3 18.9 1.0 4.3 4.1 4.8 5.3 5.8 6.7 5.7 3R676 < LLOQ 5.5 5.0 7.0 7.9 10.2 10.9 4.9 1.7 1.5 2.1 2.4 3.1 3.3 1.5 3R677 < LLOQ 5.0 7.1 5.9 7.5 9.4 10.6 5.7 1.5 2.1 1.8 2.2 2.8 3.2 1.7 9.8 Percent Dose Converted from Inhaled N-EtFOSE Dose to Serum PFOS Dose Animal # 3R674 3R675 3R676 3R677 Mean SD BW during exposure (g) 267 275 253 274 267.3 10.14 Theoretical inhaled N-EtFOSE Dose (umol/kg) 0.0386 0.0374 0.0407 0.0376 0.0386 0.0015 PFOS-equivalent dose relative to inhaled N-EtFOSE dose, % Immediately 18 hrs 24 hrs 48 hrs 72 hrs Day 8 Day 14 Day 21 -- 9.66 10.42 11.01 11.95 18.07 17.44 11.53 0.00 22.99 21.86 25.72 28.45 31.19 35.85 30.38 -- 8.15 7.42 10.27 11.65 15.07 16.10 7.18 -- 8.04 11.32 9.43 11.91 15.09 16.95 9.03 0.00 12.21 12.75 14.11 15.99 19.85 21.59 14.53 7.22 6.30 7.77 8.31 7.68 9.52 10.72 10 Conclusions While three of the four animals had quantifiable N-EtFOSE in the serum immediately after the exposure, only one animal had quantifiable serum PFOS at the same time. Eighteen hours after exposure, while only one animal still had quantifiable serum N-EtFOSE, all of them had PFOS present in the serum. The level of serum PFOS continued to increase up to Days 8 - 14 after exposure before it declined on Day 21. Within the limit of the study design, data obtained here suggested N-EtFOSE can be absorbed into blood and metabolized via inhalation exposure. Percent of inhaled N-EtFOSE dose converted to PFOS-equivalent dose ranged from 12.21 7.22% to 21.59 9.52% in male Sprague Dawley rats. 8 of 12 ST-460 ToxDocs 13-430 Appendix 1: Certificate of Analysis 9 of 12 ST-460 ToxDocs 13-430 3M MATERIALS RESOURCE DIVISION ANALYTICAL LABORATORY LIMS Request No. M13-1896 To: Sue Chang - (733-9073) -Toxicology Assessment and Compliance Assurance - 220-6W-08 Dave Ehresman - (733-5070) - Toxicology Assessment and Compliance Assurance 236-1B-22 Kent Lindstrom - (733-9882) - 3M Environmental Lab- 260-5N-17 From: Tom Kestner - (733-5633) - 3M MRD Analytical Laboratory - 236-2B-11 Subject: 1H/19F-NMR Characterization of TCR-1085: Purified N-Et FOSE Alcohol for Tox Study Date: November 24, 2013 ____________________________________________________________________________________ SAMPLE DESCRIPTION: TCR-1085 is purified N-Et FOSE alcohol. The nominal product is C8F17-SO2N(CH2CH3)CH2CH2OH (white powder). NMR Spectra #'s Summary of NMR Spectra Acquired for TCR-1085 Experiments Descriptions H131896.401 F131896.401 400 MHz 1H-NMR spectrum for a portion of the sample dissolved in acetone-d6 and spiked with small amounts of CFCl3 and p-HFX internal standard. 376.3 MHz 19F-NMR spectrum for a portion of the sample dissolved in acetone-d6 and spiked with small amounts of CFCl3 and p-HFX internal standard. OBJECTIVE: The sample of TCR-1085 was subjected to 1H-NMR and 19F-NMR spectral analyses to determine the purity of the nominal product and to characterize as many impurity components as possible. Joel Miller also performed an LCMS analysis to assist in the characterization of impurity components and his results were reported previously. In addition, you requested that I prepare and issue a certificate of analysis as a separate document in support of an upcoming 3M toxicology study. EXPERIMENTAL: A 62 mg portion of the TCR-1085 sample was totally dissolved in ~ 0.7 mL of deuterated acetone (acetoned6) and then the solution was spiked with small amounts of CFCl3 and 1,4-bis(trifluoromethyl)benzene (pHFX) for NMR analyses. A 400 MHz 1H-NMR spectrum and a 376.3 MHz 19F-NMR spectrum were acquired using an Agilent VNMRS 400 FT-NMR spectrometer that was operating with a 5mm inverse- detection gradient probe at an analysis temperature of 22-23 C. RESULTS: The combined 19F-NMR and 1H-NMR spectral data indicate the sample of TCR-1085 consists of ~ 99.9 relative wt.% of the nominal product, CnF2n+1-SO2-N(CH2CH3)-CH2CH2OH, in at least six isomeric forms, where n is mainly 8. Trace amounts of two impurities were also assigned. The qualitative and quantitative compositional results that were derived from a single trial 19F/1H-NMR cross integration spectral analysis are summarized in TABLE-1. The relative weight percent concentrations shown in TABLE-1 should be very close to their respective absolute wt.% values. Trace amounts of unassigned components are also detected in the NMR spectra but additional work would be needed in an effort to assign or quantify the other impurities. Small amounts of longer or shorter chain fluorochemical homolog impurities could have easily gone undetected because the 19F-NMR technique is not particularly well suited for characterizing small amounts 10 of 12 ST-460 ToxDocs 13-430 of homologs unless the chains are very short (i.e., C1-C3). Characterization of fluorochemical homolog impurities was performed by Joel Miller using LCMS. If you have any questions about these NMR results, or if any further work is needed, please let me know. . Tom Kestner c: Joel Miller Scott Schmick TABLE-1 Sample: TCR-1085, Purified N-Et FOSE alcohol Compositional Results by 19F/1H-NMR Cross Integration Spectral Analysis Structural Assignments 1 19F/1H-NMR Relative Wt.% Concentrations Sum of at least 6 desired product isomers: CnF2n+1-SO2-N(CH2CH3)-CH2CH2-OH where n assumed to be 8 for calculation purposes Purity = 99.9% CF3(CF2)x-SO2-N(CH2CH3)-CH2CH2-OH (Normal chain, where x assumed to 7 for calculation purposes) CF3(CF2)x-CF(CF3)-(CF2)y-SO2-N(CH2CH3)-CH2CH2-OH (Internal monomethyl branch, where x+y assumed to be 5, and x 0, y 0, for calculation purposes) (CF3)2CF-(CF2)x-SO2-N(CH2CH3)-CH2CH2-OH (Isopropyl branch, where x assumed to be 5 for calculation purposes) CxF2x+1-CF(CF3)-SO2-N(CH2CH3)-CH2CH2-OH (Alpha branch, where x assumed to be 6 for calculation purposes) (CF3)3C-(CF2)x-SO2-N(CH2CH3)-CH2CH2-OH (t-butyl branch, where x assumed to be 4 for calculation purposes) CF3-(CF2)x-C(CF3)2-(CF2)y-SO2-N(CH2CH3)-CH2CH2-OH (Internal gem-dimethyl branch, where x+y assumed to be 4, and x 0, for calculation purposes) Probable carboxamide CmF2m+1-CO-NH-CH2CH3 where m assumed to be 7 for calculation purposes Probable N-Me FOSE alcohol CnF2n+1-SO2-N(CH3)-CH2CH2-OH where n assumed to be 8 for calculation purposes 70.55% 16.93% 10.36% 1.67% 0.24% 0.12% 0.12% 0.018% 1. Trace amounts of unassigned impurity components are also detected in the NMR spectra. 11 of 12 ST-460 ToxDocs 13-430 Appendix 2: 3M Environmental Laboratory Final Analytical Report E13-0880 12 of 12 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 Final Analytical Report Analysis of Gas-Phase EtFOSE-OH in Air Samples Collected from an Exposure Chamber with OVS-Tubes During an Inhalation Toxicology Study with Rats Laboratory Request Number: E13-0888 Method or Regulatory Requirement: Non-GLP Testing Laboratory 3M Environmental Health and Safety Operations (EHS Opns) 3M Environmental Laboratory Analytical Lead Cleston Lange, Ph.D. 3M Environmental Health and Safety Operations 3M Environmental Laboratory 3M Center, Bldg 260-5N-17 St. Paul, MN 55144 Phone: 651-733-9860 clange@mmm.com Project Requester Sue Chang 3M Toxicology 3M Center, Bldg 220-6W-08 St. Paul, MN 55144 Phone: 651-737-9073 s.chang@mmm.com Page 1 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 1 Introduction / Summary The objective of this study was to measure the level of gas-phase 2-[N- (ethyl)perfluorooctanesulfonamido]-ethyl alcohol (a.k.a. EtFOSE-OH) in air that was delivered to a polyacrylate exposure chamber during a 6 hour inhalation exposure study with rats conducted by 3M-Strategic Toxicology in collaboration with the 3M EHS Opns Environmental Laboratory. Air flowing from a generator cartridge that contained glass beads coated with solid EtFOSE-OH delivered gas-phase EtFOSE-OH to the exposure chamber at a nominal flow rate of 2 L/min. Air samples were collected immediately before the inlet of the exposure chamber and also immediately at the outlet of the chamber. Samples were collected at the inlet and outlet via a split flow gas line to an OVS sampler tube with a nominal sampling flow rate of 0.1 L/min and with an ~60 minute collection time for each OVS (nominal 6 Liters total collected per OVS tube). Six inlet samples and six outlet samples were collected sequentially during the 6 hour exposure period. Herein are provided the analytical measurement result for those OVS samples provided from the EtFOSE-OH inhalation exposure study conducted in December 2013, as well as all of the associated QC samples prepared and analyzed with those samples. For analysis of EtFOSE-OH, each OVS tube was disassembled into three fractions following the procedures described in method ETS-8-105.0. Each fraction was extracted with 10 mL acetone containing d9-EtFOSE-OH as an internal standard (IS). The extracts were then quantitatively analyzed by LC/MS/MS against solvent calibration standards. A lower limit of quantitation (LLOQ) of 0.100 ng/mL was achieved during the analyses. The total mass quantity of EtFOSEOH trapped on each OVS was determined based on the summed quantity of EtFOSE-OH extracted and measured for each of the three OVS tube fractions. For preparation of the quality control (QC) samples included with each analytical batch, fresh OVS tubes were fortified onto the inlet filter with 10, 100, 1000 or 10000 ng of EtFOSE-OH, without air passed through them. Once spiked, each was disassembled, extracted and analyzed the same as samples in the batch; prior method development work (study E13-0722) showed no loss of EtFOSE-OH from QCs with up to 60 Liters of air passed through them. The QC results demonstrated an overall excellent recovery and data accuracy of 99.2 + 5.9% for all QC levels. In general, the amount of EtFOSE-OH captured at the inlet to the exposure chamber was on the order of 1500 ng, and at the outlet was on the order of 1000 ng. Recovery (+ standard deviation) for the 1000 ng QCs (n = 6) was therefore the best indicator of the data accuracy for the study and showed an accuracy of 101% + 3.4%. Blanks prepared with samples were essentially devoid of any significant levels of EtFOSE-OH and were less than the lower limit of quantitation (LLOQ). As listed in Table 1 and plotted in Figure 1, the determined air concentrations of EtFOSE-OH at the inlet were significantly higher than at the outlet. Throughout the course of the exposure, it was apparent that equilibrium (i.e. inlet/outlet ratio of 1) was not established. The inlet/outlet air concentration ratio at the onset of the study for the 0-1 hr sampling and 1-2 hr sampling were 2.7 and 2.4, respectively. However, an inlet/outlet ratio of approximately 1.50 was achieved after the first 2 hours and was relatively stable after that, as shown in Figure 2. The gas-phase concentration at the chamber inlet for the 2-3 hour sampling was 222 ng/L (9.5 ppbV) and the outlet was 148 ng/L (6.3 ppbV), and for the 5-6 hour sampling the inlet/outlet ratio was 1.46 with an inlet concentration of 225 ng/L (9.6 ppbV) and outlet concentration of 155 ng/L (6.6 ppbV). Additionally, as part of the LC/MS/MS analysis, sufficient chromatographic resolution of linear and branched isomers was achieved to allow estimation of the percent linear isomer and percent as total-branched isomers. While the EtFOSE-OH used to construct the EtFOSE-OH generator cartridge was 70% linear isomer EtFOSE-OH (30% branched isomers) EtFOSE-OH, the EtFOSEOH collected from gas-phase samples at room temperature in the inlet and outlet of the test Page 2 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 chamber showed enrichment for branched isomers. This observation was consistent with isomer enrichment observed during the previous test chamber equilibration study E13-0722. During this study, at the initiation of delivery of gas phase EtFOSE-OH from the generator tube to the exposure chamber, the EtFOSE-OH isomer composition was ~38% linear isomer at the inlet. However, a significant change in the isomer composition at the inlet occurred over the course of the 6 hour exposure period which was not observed at the outlet, and increased to 62% linear isomer by the end of the exposure. In contrast, the isomer composition appeared relatively stable at the outlet during the entire 6 hour exposure period and composed of ~32% linear isomer at the beginning to and ~34% linear isomer at the end of the exposure period (see Figure 2). These results indicate that deposition of branched EtFOSE-OH on the chamber walls likely occurred during the earlier conducted pre-study chamber equilibration study E13-0722, and during this study sublimation of branched EtFOSE-OH off of the walls, and possibly preferential deposition of linear isomer onto the surface from the incoming gas, contributed to a continuous level of enrichment of branched isomers in exhaust air measured at the outlet. Based on these analytical results, exposure levels of gas-phase EtFOSE-OH concentrations were between ~6 and 9 ppbV during the exposure based on inlet and outlet concentration. Furthermore, it was shown that the gas-phase EtFOSE-OH was enriched with branched isomers. The inhalation-dose of highly-branched EtFOSE-OH could have a profound impact on the absorption, distribution, metabolism and excretion (ADME) properties of the EtFOSE-OH, and should be considered when comparing these inhalation-dose results to previous toxicological studies. Table 1. Summarized Results for EtFOSE-OH Concentration and Linear Isomer Composition EtFOSE-OH Sample ID Sample Description Actual Air Volume Captured on OVS (L) Total Recovere d from OVS (ng) Air Concentration (ng/L) Air Concentratio n (ppbV) Linear Isomer (Percent of Total) E13-0880-003 Test #1 Inlet, 0.1 L/min 6.77 1397 206 8.79 38.4% E13-0880-004 Test #1 Outlet, 0.1 L/min 6.86 524 76.4 3.25 31.5% E13-0880-005 Test #2 Inlet, 0.1 L/min 6.77 1520 225 9.56 45.9% E13-0880-006 Test #2 Outlet, 0.1 L/min 6.86 652 95.1 4.05 28.2% E13-0880-007 Test #3 Inlet, 0.1 L/min 6.77 1501 222 9.45 52.4% E13-0880-008 Test #3 Outlet, 0.1 L/min 6.86 1013 148 6.29 32.3% E13-0880-009 Test #4 Inlet, 0.1 L/min 6.77 1544 228 9.71 55.8% E13-0880-010 Test #4 Outlet, 0.1 L/min 6.86 958 140 5.95 32.2% E13-0880-011 Test #5 Inlet, 0.1 L/min 6.77 1505 222 9.47 59.7% E13-0880-012 Test #5 Outlet, 0.1 L/min 6.86 919 134 5.71 32.3% E13-0880-013 Test #6 Inlet, 0.1 L/min 5.64 1271 225 9.59 61.5% E13-0880-014 Test #6 Outlet, 0.1 L/min 5.71 885 155 6.59 33.6% The analytical measurement uncertainty for these study results was estimated at + 12% based on QC results. [a] Value was estimated based on peak area response of the linear isomer chromatographic peak versus total peak area of linear + branched isomer peaks (see Figure 3 for LC/MS/MS Chromatogram of EtFOSE-OH). Page 3 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 Air Concentartion (ppbV) Inlet & Outlet Gas-Phase EtFOSE-OH Concentration (Study E13-0880) 10.00 9.00 8.00 7.00 6.00 5.00 4.00 3.00 2.00 0 50 100 150 200 250 300 350 400 Exposure Time (min) Figure 1. Measured concentration in exposure chamber inlet air and outlet air samples collected and analyzed during a rat inhalation exposure study as study E13-0880. (Inlet , outlet ) Inlet/Outlet Gas-Phase EtFOSE-OH Concentration Ratio (Study E13-0880) 3.00 Inlet/Outlet Ratio 2.50 2.00 1.50 1.00 0 50 100 150 200 250 300 350 400 Exposure time (min) Figure 2. plot of inlet/outlet ratio for the determined gas-phase EtFOSE-OH concentration in exposure chamber inlet-air and outlet-air samples collected on OVS tubes during a rat inhalation exposure study. Page 4 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 2 Analytical and Preparatory 2.1 Reference Substance Table 2. Reference Substances Substance TCR No. Source Use Chemical Name Chemical Formula Formula Wt. Isomer Composition Purity Expiration EtFOSE-OH (linear + branched) TCR-1085 3M, Purified by HPLC at Pace Analytical Services Generator Cartridge Loading and QC fortifications 2[(N-methyl)perfluorooctanesulfonamido]ethyl alcohol EtFOSE-OH (linear) TCR09-0061-1/10 Wellington Calibration Standard Preparations 2[(N-methyl)perfluorooctanesulfonamido]ethyl alcohol d9-EtFOSE-OH TCR09-0053-2/4 TCR09-0053-3/4 Wellington Quantitation Internal Standard Deuterated 2[(N-methyl)perfluorooctanesulfonamido]ethyl alcohol C12H10F17NO3S C12H10F17NO3S C12HD9F17NO3S 571 Mixed Linear (70%) & Branched (30%) Isomers 99.9% 7/31/2016 571 580 Pure Linear Isomer Pure Linear Isomer 50 g/mL Solution in MeOH 2/23/2014 50 g/mL Solution in MeOH 2/18/2014 2.2 Analytical Sample and Sample Batch Preparation Disassembly and extraction of the OVS tubes was performed following method ETS-8-105.0. Each OVS sampling tube was dismantled into three sets of components, as follows: component 1 was the 1st bed of XAD-4 resin and 1st PUF plug; component 2 was the XAD-4 resin from the 2nd bed and the 2nd polyurethane foam (PUF) plug; and component 3 was the glass fiber filter, HDPE retaining ring and glass tube housing. Each of the three components was separately extracted with 10 mL of acetone containing d9-EtFOSE-OH which served as IS. This resulted in three 10 mL analytical sample extracts per OVS tube (net 10-fold dilution of each solid state component set). The LC/MS/MS analysis of the extracts was conducted using the parameters described in Tables 3, 4 and 5. Two analytical batches were analyzed to collect the data for reporting and were batches m131210a and m131211a. Calibration standards were prepared for each analytical batch ranging from nominal 0.100 ng/mL to 500 ng/mL and were prepared by fortifying pure linear EtFOSE-OH at known levels into acetone containing d9-EtFOSE-OH, same acetone mix as used to extract samples. Quantitation was by internal standard method. Calibration curve regression was performed with 1/x weighting and coefficient of determination (R2) for the calibration curve regressions were > 0.995. Reinjection of calibration standards during the analysis was performed as continuing calibration verification (CCVs) during each run and all results for CCVs were within 100 + 10% for all Page 5 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 analytical runs reported. Additional new purchased OVS tubes of the same type were used for the exposure chamber experiments (ORBOTM65P OVS Fluoride Tube with Glass Fiber Filter, Supelco Item 20029-U) and were used to prepare quality control (QC) samples for each analytical batch. The QC samples were fortified with reference substance TCR-1085 (70% linear, 30% branched isomers) and was the same reference substance used to make the generator cartridge. The QCs were fortified at four levels, each level in triplicate, and each level prepared by spiking 10.0 ng, 100 ng, 1000 ng or 11400 ng of EtFOSE-OH (mixed linear/branched isomer material) onto the filter in the OVS inlet side. QCs did not have air passed through them; however, previous method development work as part of study E13-0722 showed that EtFOSE-OH is retained on OVS tubes with up to 60 liters of air passed through them, a volume of air that was ~10-fold more than the volume of air collected on OVS tubes during this study. The component-3 extract is where EtFOSE-OH is typically trapped and retained, and for the 11400 ng QC the component-3 extract was diluted 1000-fold (as s dilution QC). However, samples did not require dilution, hence, the dilution QC was determined to be unnecessary. Results of QCs were used to verify the performance of the analytical method. The QC results are summarized in the results section in Table 8, and individual QC OVS component results are shown in Table 9. Laboratory media blanks were control OVS tubes without fortification and without air passed through them/ Results of media blanks are provided in the results section as Table 6. The Air Pre-Test and Post-Test air blanks were collected by passing non-dosed tank-air through them. The air used was the same tank air as passed through the generator column and test chamber during the exposure. Results for air blanks are presented in the results section as Table 7. 2.3 LC/MS/MS Analysis Table 3. Instrument Information (Study E13-0880) Instrument Name ETS-MaryAnn (batches m131210a & m131211a) Analytical Method ID ETS-8-105.0 for Extraction Liquid Chromatograph Agilent 1200 Analytical column Betasil C18 (100 x 2.1 mm; 5 m); 30C Injection Volume 1.0 L Mass Spectrometer API 5000 Triple Quadrapole Ion Source Turbo Spray Polarity Negative Software Analyst 1.6.1 Page 6 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 Table 4. Liquid Chromatography Conditions (Study E13-0880) Step Total Time Number [min] Flow Rate [mL/min] 0 0.00 0.500 1 0.50 0.500 2 2.50 0.500 3 3.10 0.500 4 3.11 0.500 5 4.50 0.500 Percent A [2mM Aqueous Ammonium Acetate] 20.0 20.0 99.0 99.0 20.0 20.0 Percent B [2 mM Ammonium Acetate in Methanol] 80.0 80.0 1.0 1.0 80.0 80.0 Table 5. Mass Transitions (Study E13-0880) Analyte Mass Transitions (MRMs) Monitored EtFOSE-OH C9Analog [a] C7 Analog[a] 630>59 680>59 580>59 d9-EtFOSE-OH (IS) 639>59 [a] Mass transitions for C9 and C7 Analogs of EtFOSE-OH were included, but not used for quantitation during this study. 2.4 Calculations The results as part per billion by volume (ppbV) is a gas phase concentration value (nL/L), and was determined as described below: First the volume of EtFOSE-OH in the air sample is calculated by the ideal gas law, as follows: PV= nRT or, [V = nRT/P] where, V=VEtFOSE-OH (L) and is the volume occupied by EtFOSE-OH in the air sample from the OVS n = mole EtFOSE-OH captured on OVS using 571 g/mole conversion value R is the ideal gas constant at 0.08206 [(atm*mol) /(L*K)] P is assumed 1 atm T is assumed 23 C (296.15 K). Then, ppbV (nL per Liter of Air) was calculated where VAir = volume of air sample through the OVS in liters, and =VEtFOSE-OH is the volume of EtFOSE-H in that air sample entered in nL ppbV = VEtFOSE-OH (nL) / VAir (L) All other calculations were performed per 3M EHSO Environmental Laboratory standard operating procedures (SOPs). Page 7 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 3 Results 3.1 Media Blanks OVS Tube media blanks results were below the LLOQ. The results are summarized in Table 6. An LLOQ of 0.100 ng/mL translates to an LLOQ of 1.00 ng per OVS component, hence, 3 ng per OVS tube for the three components. Table 6. Summarized Results for OVS Tube Media Blanks EtFOSE-OH Sample ID Sample Description E13-0880-001 E13-0880-016 OVS Media Blank 1 OVS Media Blank 2 Nominal Air Volume Captured (L) 0 0 Total Recovered from OVS (ng) < 3.00 < 3.00 Air Concentration (ng/L) NA NA Air Concentration (ppbV) NA NA 3.2 Air Blanks Laboratory blanks were devoid of EtFOSE-OH and all results were below the lower limit of quantitation of 0.100 ng/mL (i.e. <1.00 ng per component, < 3.00 ng per OVS). Results of laboratory blanks are summarized in Table 7. Table 7. Summarized Results for Air Blanks Sample ID E13-0880-001 E13-0880-016 Sample Description Air Pre-Test Blank, nominal flow 1 L/min Air Post-Test Blank , nominal flow 1 L/min Nominal Air Volume Captured (L) 6 7 EtFOSE-OH Total Recovered from OVS (ng) < 3.00 < 3.00 Air Concentration (ng/L) < 0.500 < 0.429 Air Concentration (ppbV) < 0.0213 < 0.0182 Page 8 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 3.3 QC Results Four levels of quality control (QC) samples were prepared, each level in triplicate, by spiking OVS tubes with 10.0 ng, 100 ng, 1000 ng and 11400 ng of EtFOSE-OH, and then extracting the same as samples. For the 11400 ng QC, the component-3 10 mL acetone extract was diluted 10fold prior to analysis to achieve a result within the range of the calibration (total dilution of 100fold for that OVS solid state component). As summarized in Table 8, the QC results showed excellent data accuracy and precision with an overall average and standard deviation of 99.2% + 5.9% (RSD 6.0%). EtFOSE-OH was efficiently recovered off of the OVS tubes at all levels with all QC recoveries within 100 +17%. The majority of EtFOSE-OH was recovered from component 3 (glass fiber filter, HDPE retaining ring and glass tube housing) with some captured from component 2 (the 1st bed of XAD-4 resinbeads and 1st PUF plug). Component 3 (2nd bed and 2nd polyurethane foam (PUF) plug) typically did not contain much EtFOSE-OH. The estimated analytical measurement uncertainty for this study was calculated from statistical analysis of the QC results, per 3M EHSO Environmental Laboratory SOP ETS-12-12.2. Table 8. QC Summary Results (Study E13-0880) Analytical Batch ID m131210 m131211a Average Recovery Std. Dev. RSD n Overall Average Overall Standard Deviation Overall RSD N Estimated Analytical Measurement Uncertainty (95% CI) EtFOSE-OH Recovery from OVS QCs 10.0 ng QC 100 ng QC 1000 ng QC 11400 ng QC 83.3% 96.5% 96.4% 103% 101% 94.4% 104% 104% 95.7% 92.3% 98.9% 107% 95.2% 97.4% 98.9% 87.3% 103% 103% 105% 104% 101% 99.3% 105% 107% 95.3% 96.1% 101% 104% 6.2% 6.5% 6 6.2% 6.5% 6 3.4% 3.3% 6 2.8% 2.7% 6 99.2% 5.9% 6.0% 24 + 12% Page 9 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 3.4 Individual Sample Results Table 9. Individual QC Results (Study E13-0880) QC ID Analytical Fortification OVS Tube Run ID Level (ng) Component KDM10- 1 Dec2013-017 m131210a 10.0 2 3 KDM10- 1 Dec2013-018 m131210a 10.0 2 3 KDM10- 1 Dec2013-019 m131210a 10.0 2 3 KDM10- 1 Dec2013-020 m131210a 100 2 3 KDM10- 1 Dec2013-021 m131210a 100 2 3 KDM10- 1 Dec2013-022 m131210a 100 2 3 KDM10- 1 Dec2013-023 m131210a 1000 2 3 KDM10- 1 Dec2013-024 m131210a 1000 2 3 KDM10- 1 Dec2013-025 m131210a 1000 2 3 KDM10- 1 Dec2013-026 m131210a 11400 2 3 KDM10- 1 Dec2013-027 m131210a 11400 2 3 KDM10- 1 Dec2013-028 m131210a 11400 2 3 KDM10- 1 Dec2013-029 m131211a 10.0 2 3 Determined Amount (ng) <1.00 <1.00 8.33 <1.00 <1.00 10.1 <1.00 <1.00 9.57 6.91 <1.00 89.6 4.26 <1.00 90.1 5.53 <1.00 86.8 110 <1.00 854 161 <1.00 879 94.9 <1.00 894 1580 2.28 10200 965 4.11 10900 1690 1.15 10500 <1.00 <1.00 9.52 Total EtFOSE-OH (ng) [a] QC Recovery [a] Average Recovery 8.33 83.3% 93.3% 10.1 101% (RSD 9.7%) 9.57 95.7% 96.5 96.5% 94.4% 94.4 94.4% (RSD 2.2%) 92.3 92.3% 964 96.4% 99.8% 1040 104% (RSD 3.9%) 989 98.9% 11800 11900 12200 9.52 103% 104% 107% 95.2% 105% (RSD 1.8%) 97.2% (RSD Page 10 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 Table 9. Individual QC Results (Study E13-0880) QC ID KDM10Dec2013-030 KDM10Dec2013-031 KDM10Dec2013-032 KDM10Dec2013-033 KDM10Dec2013-034 KDM10Dec2013-035 KDM10Dec2013-036 KDM10Dec2013-037 Analytical Run ID m131211a m131211a m131211a m131211a m131211a m131211a m131211a m131211a Fortification Level (ng) 10.0 10.0 100 100 100 1000 1000 1000 OVS Tube Component 1 2 3 1 2 3 1 2 3 1 2 3 1 2 3 1 2 3 1 2 3 1 2 3 Determined Amount (ng) <1.00 <1.00 9.74 <1.00 <1.00 9.89 5.29 <1.00 82.0 5.92 <1.00 96.7 8.59 <1.00 94.9 59.5 <1.00 991 60.4 <1.00 976 69.3 <1.00 937 Total EtFOSE-OH (ng) [a] 9.74 QC Recovery [a] 97.4% Average Recovery 1.9%) 9.89 98.9% 87.3 87.3% 97.8% 103 103% (RSD 9.3%) 103 103% 1050 105% 103% 1040 104% (RSD 2.2%) 1010 101% 1 1120 KDM10- m131211a Dec2013-038 11400 2 <1.00 11320 3 10200 KDM10- 1 1130 Dec2013-038 m131211a 11400 2 <1.00 11930 3 10800 KDM10- 1 1160 Dec2013-039 m131211a 11400 2 <1.00 12160 3 11000 All values are rounded to 3 significant figures, but precise data was used in data calculations. 99.3% 105% 107% 104% (RSD 3.7%) [a] Values of Zero (0) were used for results below the LLOQ (<LLOQ) when calculating total EtFOSE-OH and QC recoveries. Page 11 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 Table 3. Individual Air Sample Results (Study E13-0880) Sample ID Component Extracted EtFOSE-OH Component Amount Measured (ng) EtFOSE-OH Amount from OVS tube (ng) and [Percent Linear Isomer] 1 Inlet Test #1 2 3 1 Outlet Test #1 2 3 1 Inlet Test #2 2 3 1 Outlet Test #2 2 3 1 Inlet Test #3 2 3 1 Outlet Test #3 2 3 1 Inlet Test #4 2 3 1 Outlet Test #4 2 3 1 Inlet Test #5 2 3 1 Outlet Test #5 2 3 1 Inlet Test #6 2 3 1 Outlet Test #6 2 3 2.07 14.7 1380 18.7 2.94 502 3.11 16.9 1500 18.8 19.9 613 169 22.3 1310 55.8 27.9 929 9.69 24.2 1510 122 21.2 815 413 32.1 1060 149 10.3 760 <1.00 10.5 1260 89.6 17.9 777 1397 [38.4%] 524 [31.5%] 1520 [45.9%] 652 [28.2%] 1501 [52.4%] 1013 [32.3%] 1544 [55.8%] 958 [32.2%] 1505 [59.7%] 919 [32.3%] 1271 [61.5%] 885 [33.6%] Air Volume Captured (L) 6.77 6.86 6.77 6.86 6.77 6.86 6.77 6.86 6.77 6.86 5.64 5.71 EtFOSEOH Air Concentra tion ( b) 8.79 Inlet/Out let Ratio 2.70 3.25 9.56 2.36 4.05 9.45 1.50 6.29 9.71 1.63 5.95 9.47 1.66 5.71 9.59 1.46 6.59 Page 12 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 4 Conclusion A lower limit of quantitation (LLOQ) of 0.100 ng/mL was achieved during the analyses. The total mass quantity of EtFOSE-OH trapped on each OVS was determined based on the summed quantity of EtFOSE-OH measured for each of the three OVS fractions. Quality control (QC) samples were prepared with each analytical batch by fortifying fresh OVS tubes with EtFOSE-OH at nominal 10, 100, 1000 and 10000 ng, each level prepared in triplicate, and then disassembling, extracting and analyzing them the same as samples. QC result demonstrated an overall excellent data accuracy of 99.2 + 5.9% for all QC levels. In general, the amount of EtFOSE-OH captured at the inlet was on the order of 1500 ng per OVS, and at the outlet was on the order of 1000 ng per OVS. Recovery results for the 1000 ng QCs (n = 6) was therefore the best indicator of the data accuracy for the study and showed an accuracy of 101% + 3.4%. Blanks prepared with samples essentially did not contain any significant levels of EtFOSE-OH and were less than the lower limit of quantitation (LLOQ). Analysis results for the individual OVS components for samples and QCs showed that typically 90-100% of the EtFOSE-OH was captured in component 3 (glass fiber filter, HDPE retaining ring and glass tube housing), ~0-10% in component 1 (1st XAD bed and PUF, middle stage) and less than 1% was captured on component 2 (2nd XAD bed and 2nd PUF), the final stage of the OVS, indicating no breakthrough. Based on these analytical results, exposure levels of gas-phase EtFOSE-OH concentrations were between ~6 and 9 ppbV during the exposure based on the measured inlet and outlet concentration. Furthermore, as shown in Figure 3, it was demonstrated that the gas-phase EtFOSE-OH in the exposure chamber was enriched with branched isomers. Page 13 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 A B C Figure 3. The LC/MS/MS chromatograms of EtFOSE-OH (left) and corresponding linear d9-EtFOSE-OH internal standard peak (right). Samples from top to bottom were the component-3 extracts of the following samples and analyzed in the same analytical run m131210a: A) 200 ng/mL calibration standard prepared with linear EtFOSE-OH obtained commercially from Wellington Laboratories; B) 1000 ng QC fortified with substance TCR-1085 (70% linear, 30% branched isomers) and was same substance as used to make the generator cartridge for dosing; and C) the isomer profile of component 3 extract of sample E13-0880-006 (1-2 hour sampling point, chamber outlet) showing the enrichment of branched isomers in gas-phase EtFOSE-OH (~28% linear isomer and ~72% branched isomers). Page 14 of 15 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Measurement of EtFOSE-OH in Air Samples During Rat Inhalation Toxicology Study in December 2013 5 Data/Sample Retention Samples generated during this study E13-0880 will be retained indefinitely, or until requested by the study Requestor to dispose of them, and will only be disposed of with laboratory management approval. 6 Attachments E13-0880 Final Analytical Report, Appendix-A: "Field Summary: Ethyl-FOSE Rat Exposure Chamber Test"; Lab Request Number E13-0880 (3M EHS Opns. Environmental Laboratory-Field Services Group Report) 7 Signatures The following 3M Environmental Laboratory personnel have reviewed and approved this report: Cleston C. Lange, Ph.D., Analytical Lead (MKMXEPP] WMKRIH F] 'PIWXSR ' 0ERKI (2 G!97 WX!12 P!7X 4EYP SY!1 )RZMVSRQIRXEP 0EFSVEXSV] EYXLIRXMGEXIH F] 06% IQEMP!GPERKI$QQQGSQ S!1 GR!'PIWXSR ' 0ERKI 6IEWSR - EQ ETTVSZMRK XLMW HSGYQIRX (EXI Date William K. Reagen, Ph.D., Technical Director (MKMXEPP] WMKRIH F] ;MPPMEQ / 6IEKIR (2 G!97 WX!12 P!7X 4EYP SY!0EFSVEXSV] (MVIGXSV SY!1 )RZMVSRQIRXEP 0EFSVEXSV] EYXLIRXMGEXIH F] 06% IQEMP![OVIEKIR$QQQGSQ S!1 GR!;MPPMEQ / 6IEKIR 6IEWSR - EQ ETTVSZMRK XLMW HSGYQIRX (EXI Date The results and report were audited by Quality Associates, Inc. (QAI) QAI Representative (MKMXEPP] WMKRIH F] 8ER]E / 6YHI (2 G!97 WX!12 P!7X 4EYP SY!1 )RZMVSRQIRXEP 0EFSVEXSV] EYXLIRXMGEXIH F] 06% IQEMP!XVYHI$QQQGSQ S!1 GR!8ER]E / 6YHI 6IEWSR - LEZI VIZMI[IH XLMW HSGYQIRX (EXI Date Page 15 of 15 E13-0880 Final Analytical Report, Appendix-A Field Summary 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Ethyl-FOSE Rat Exposure Chamber Test Laboratory Request Number: E13-0880 Client's Department: 108022 Method or Regulatory Requirement: On-Site Modified EPA Method 320 Testing Laboratory 3M Environmental, Health and Safety Operations 3M Environmental Laboratory 3M Environmental Laboratory Brian Mader, Ph.D. 3M EHS Opns Environmental Laboratory 3M Center Building, 260-5N-17 St. Paul, MN 55144 Phone: (651) 733-9866 Fax: (651) 778-6176 3M Toxicology Sue Chang, Ph.D. 3M Center, Building 220-6W-08 St. Paul, MN 55144 Phone: (651) 733-9073 Page 1 of 13 E13-0880 Final Analytical Report, Appendix-A 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 3M Environmental Laboratory - On-site FTIR/OVS Tubes Report Author: Jess Eldridge Field Team: Jess Eldridge, Sue Chang, Jill Hart, Trina John Field Report Project Number: E13-0880 Date of Report: January 10, 2014 1 Introduction / Summary The purpose of this testing was to support 3M Strategic Toxicology by performing a study on rats exposed to ethyl-FOSE generated from a generator cartridge. This test was a followup to the preliminary work performed under lab request E13-0722. Testing consisted of FTIR and OVS tube LC/MS based measurements of the target compound at the inlet and outlet of the test chamber. If other compounds were present, they would be reported by FTIR if feasible. On-site Fourier Transform Infrared (FTIR) spectroscopy testing and OSHA Versatile Sampler (OVS) tube sampling (Supelco) were conducted in Room SB 322/324 located in Bulding 270 for the 3M Toxicology and 3M Materials Resources Division groups. A "Breathing Air" quality compressed gas cylinder # P411310802/019928 was used to flow air through the ethyl-FOSE generator tube at a rate of 2.1 lpm into and through the 40 liter exposure chamber. Gas exiting the chamber was flowed through the FTIR cell and exhausted in the adjacent vent hood. The continuous air flow measurement was made using a calibrated rotometer supplied by the 3M Toxicology lab; SN 337973-1. The chamber inlet and outlet locations were configured each with a valved sampling port from which an OVS sample could be drawn via SKC AirChek 52 pump. The pumps were set to sample at approximately 100 cc/min for each test per location. Pump # 150 was used at the inlet location and Pump # 222 was used at the outlet location for the entire testing event. A beginning and end flow rate was measured for each OVS sample via a Dry-Cal flow meter; 3M Instrument # 158675. A "dummy" OVS tube was used to measure the flows rather than the actual sampling tubes assuming the flow rates would be consistent between all tubes. Since the exposure chamber was under slight pressure, a flow rate at the inlet and outlet sampling locations were performed once while plumbed into the system. A correction factor was then determined to apply to all other flow rates measured throughout this event based upon measurements made during the preliminary test under lab request E13-0722. A detailed spreadsheet of exact flow rates, correction factors, and test times is presented in Section 7. The FTIR results are shown in Section 8. Hand written notes taken during the event including the lot numbers and expiration dates per OVS sample are shown in Section 9. The Chain of Custody Forms are shown in Section 10. The General Project Outline (GPO) is shown in Section 11. Page 2 of 13 E13-0880 Final Analytical Report, Appendix-A 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 December 9th, 2013 Summary: Testing began on December 9th 2013 and included continuous FTIR testing and six one hour OVS tube samples collected at the inlet and outlet of the exposure chamber for the entire day. A breathing air cylinder OVS tube sample was collected from 8:18 to 8:24 at a flow rate of 1 lpm. This test was performed as a blank to confirm the absence of ethyl-FOSE in the cylinder. The OVS tube tests were numbered 1-6. Test 1 was from 9:12 to 10:12, Test 2 was from 10:15 to 11:15, Test 3 was from 11:18 to 12:18, and Test 4 was from 12:21 to 13:21, Test 5 was from 13:24 to 14:24, and Test 6 was from 14:27 to 15:17 (50 minutes). A blank OVS tube was submitted along with the other samples; designated time 8:22. The exposure test was complete and the system shut down at 15:19. The system was opened and the rats were removed by Jill Hart, Trina John, and Sue Chang for the continuance of the biological phase of the exposure test. The breathing air cylinder was connected directly to the FTIR at 15:30 flowing at 1 lpm until 15:37. This test was performed to confirm the presence of carbon monoxide, carbon dioxide, and methane as was observed in the preliminary testing. The same cylinder was used for the rat exposure test as used for the preliminary testing. At 15:43 the generator tube exhaust was plumbed directly to the FTIR to test whether the ethy-FOSE could be directly measured. The flow rate was 2 lpm into the FTIR. Spectral collection continued until 15:51 at which time the sampling was discontinued. The FTIR data showed the presence of methanol, methane, carbon monoxide, carbon dioxide, and ammonia. The methanol was coming from within the chamber apparently from past cleaning activities. There was a thin white plastic sheet material on the bottom of the chamber that we suspected acted like a sponge slowly emitting the methanol. The ammonia was presumed to be from rat urine. The concentration continued to increased throughout the test. After all the samples were collected the flow of air through the generator tube and exposure chamber was stopped and everything valved closed and plugged/capped. The test was ended at 14:09 12/9/13. Page 3 of 13 E13-0880 Final Analytical Report, Appendix-A 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 2 Methods - Analytical and Preparatory The exposure chamber testing was performed by plumbing an air supply line from the breathing air cylinder to the rotometer then to the ethyl-FOSE generator tube. From the generator tube a T was installed with a valve to provide a sampling port for the OVS tubes. From that point the tube continued to the inlet of the exposure chamber located on one end. Exiting the chamber from the other end is another T with a valve to provide a sampling port for the outlet OVS location. After the T the line continues to the FTIR cart. The line was attached to one of the sampling inlet ports on the control panel. From the panel the line continues to the FTIR sample cell inlet where sample gas traverses the length of the cell out the exhaust line where the gases were vented into the adjacent hood. FTIR measurements were initially collected continuously then after several minutes the frequency was changed to 5 minute intervals. The overall sampling system was leak checked each day prior to testing. Cylinder air was flowed at 2 lpm into the entire system while the final exhaust was plugged. The pressure on the system was monitored by the pressure sensor in the FTIR. When the system was pressurized between 1-2 psia above ambient, the cylinder valve was closed. The system was checked for pressure change over at least a 5 minute time frame. Acceptance criteria is <4% change. All leak checks ranged between 0 and -0.51%. A schematic of the sampling system is shown in Figure 1 below. Figure 1 - Sample System Schematic Page 4 of 13 E13-0880 Final Analytical Report, Appendix-A 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 The method used for the FTIR analyses was a modified procedure of ETS-8-31.2 "Measurement of Vapor Phase Compounds by Extractive Fourier Transform Infrared (FTIR) Spectroscopy", which is based upon NIOSH 3800 and EPA Method 320. For these tests the exposure chamber air was extracted through a Midac I-series FTIR system. The FTIR system was equipped with a nominal 20.0 meter optical pathlength gas cell operated at ambient temperatures. The FTIR continuously collected data throughout the tests and created average sample spectra approximately every 60 seconds. FTIR results were generated using Midac AutoQuantTM software and are reported in ppmv (parts per million by volume). The software utilizes a classical least squares (CLS) algorithm to compare a sample spectrum to a set of reference spectra. The least-squares algorithm computes what fraction of each reference spectrum must be added to reproduce the sample spectrum. The equivalent proportion of reference spectra is equal to the concentration in the sample. CLS assumes a linear relationship between absorbance and concentration. Concentrations of analytes in representative FTIR sample spectrum were verified using manual subtraction of a reference spectrum from the sample spectrum utilizing Galactic software. The relative fraction of the reference spectrum, or subtraction factor, was then used to calculate the concentration of the sample in ppmv using the following equation: ppmv = (subtraction factor) (reference spectrum concentration at cell temp (ppmv*m)) pathlength for sample analysis (m) 3 FTIR Analysis Spectral features from representative sample spectra were evaluated and carbon monoxide, carbon dioxide, methane, methanol, and water were detected. Ethyl-FOSE was not detected in any chamber exhausts during this study. There were several other unknown spectral features observed at the startup of the testing. These features dropped below detection several minutes after startup. It is suspected these features were related to the white plastic material at the bottom of the exposure chamber. Methanol was also attributed to residual effects within the chamber due most likely to past cleaning activities. All quality control requirements including daily pathlength determinations and sampling system leak checks met the requirements of EPA Method 320 and ETS-8-31.2. Page 5 of 13 E13-0880 Final Analytical Report, Appendix-A 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 4 FTIR Test Results - Data Plots Figure 1 - All Test Compounds Plotted 10.0 ethylFOSE Methanol Ammonia Methane CO ppm ppm 0.0 0 50 100 150 200 250 300 350 400 450 Minutes Figure 2 - All Test Compounds Excluding Ammonia 2.80 2.60 2.40 2.20 2.00 1.80 1.60 1.40 1.20 1.00 0.80 0.60 0.40 0.20 0.00 0 50 100 150 200 250 300 350 400 450 Minutes ethylFOSE Methanol Methane CO Page 6 of 13 E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A 7 Flow Rates, Correction Factors, Test Times 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Page 8 of 13 E13-0880 Final Analytical Report, Appendix-A E13-0722 B270 Tox Chamber Ethyl-FOSE Conditioning Sweep gas pressure setting = 10 psi Sweep gas flow rate = 2 lpm; calibrated rotometer Flow rate checked on inlet connected to pressurized system @ 8:55 11/14/13 = 115 cc/min; not connected @ 8:36 = 104.5 cc/min Flow rate checked on outlet connected to pressurized system @ 10:15 11/20/13 = 116 cc/min; not connected @ 10:09 = 108 cc/min Inlet = pump #IH0000150 Outlet = pump #IH0000222 Dry-Cal # 3M Instrument # 158675, #E0000003898 Lab Request E13-0722 - Preliminary Chamber Test By: JSE 11/26/13 Diff, cc/min Diff, cc/min Avg, cc/min EtFOSE-OH P-Chem Structure C8F17SO2N(CH2CH3)CH2CH2OH MW 571 10.5 T 23 8 P (atm) 1 9.25 Date Start Time Stop Time Elpased (hr) Gas 11/14/2013 10:25 11:25 1.00 Air 11/14/2013 10:25 11:25 1.00 Air 11/14/2013 12:20 13:20 1.00 Air 11/14/2013 12:20 13:20 1.00 Air 11/14/2013 14:20 15:20 1.00 Air 11/14/2013 14:20 15:20 1.00 Air 11/14/2013 15:22 16:22 1.00 Air 11/14/2013 15:22 16:22 1.00 Air 11/15/2013 8:42 9:42 1.00 Air 11/15/2013 8:42 9:42 1.00 Air 11/15/2013 10:42 11:42 1.00 Air 11/15/2013 10:42 11:42 1.00 Air 11/15/2013 12:42 13:42 1.00 Air 11/15/2013 12:42 13:42 1.00 Air 11/15/2013 13:44 14:44 1.00 Air Ethyl FOSE Air Conc. Ethyl Air Conc. Ethyl Test Location Initial flow, cc/min Final flow, cc/min Avg flow, cc/min Cor. Factor, cc/min Adj flow, cc/min Run Time, min Volume, L (ng/OVS tube) FOSE (ng/L) FOSE (ppbV) 1 Inlet 104.5 104 104.25 9.25 113.5 60 6.810 1710 251 11 1 Outlet 103 107 105 9.25 114.25 60 6.855 6.1 0.89 0.04 2 Inlet 104 103 103.5 9.25 112.75 60 6.765 3120 461 20 2 Outlet 107 108 107.5 9.25 116.75 60 7.005 30.6 4.4 0.19 3 Inlet 103 103 103 9.25 112.25 60 6.735 3510 521 22 3 Outlet 108 109 108.5 9.25 117.75 60 7.065 72.7 10 0.44 4 Inlet 103 103 103 9.25 112.25 60 6.735 4040 600 25 4 Outlet 108 109 108.5 9.25 117.75 60 7.065 124.0 18 0.75 5 Inlet 104 104 104 9.25 113.25 60 6.795 3990 587 25 5 Outlet 105 105 105 9.25 114.25 60 6.855 124.0 18 0.8 6 Inlet 104 104 104 9.25 113.25 60 6.795 4640 683 29 6 Outlet 105 105 105 9.25 114.25 60 6.855 145.0 21 0.9 7 Inlet 104 103 103.5 9.25 112.75 60 6.765 5080 751 32 7 Outlet 105 105 105 9.25 114.25 60 6.855 219.0 32 1.4 8 Inlet 104 103 103.5 9.25 112.75 60 6.765 5480 810 34 11/15/2013 11/20/2013 11/20/2013 11/21/2013 11/21/2013 11/22/2013 11/22/2013 11/25/2013 11/25/2013 12/4/2013 12/4/2013 13:44 9:06 9:06 9:05 9:05 8:51 8:51 9:54 9:54 9:18 9:18 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 12/9/2013 9:12 9:12 10:15 10:15 11:18 11:18 12:21 12:21 13:24 13:24 14:27 14:27 14:44 10:06 10:06 10:05 10:05 9:51 9:51 10:55 10:55 10:18 10:18 10:12 10:12 11:15 11:15 12:18 12:18 13:21 13:21 14:24 14:24 15:17 15:17 1.00 Air 8 1.00 Nitrogen 9 1.00 Nitrogen 9 1.00 Nitrogen 10 1.00 Nitrogen 10 1.00 Nitrogen 11 1.00 Nitrogen 11 1.02 Nitrogen 12 1.02 Nitrogen 12 1.00 Nitrogen 13 1.00 Nitrogen 13 1.00 Air 1 1.00 Air 1 1.00 Air 2 1.00 Air 2 1.00 Air 3 1.00 Air 3 1.00 Air 4 1.00 Air 4 1.00 Air 5 1.00 Air 5 0.83 Air 6 0.83 Air 6 Outlet 105 105 Inlet 104 104 Outlet 108 108 Inlet 105 104 Outlet 109 108 Inlet 104 104 Outlet 106 106 Inlet 104 103 Outlet 108 108 Inlet 104 104 Outlet 105 104 Inlet Outlet Inlet Outlet Inlet Outlet Inlet Outlet Inlet Outlet Inlet Outlet Lab Request E13-0880 - Exposure Test w Rats 104 103 104 106 104 103 104 106 104 103 104 106 104 103 104 106 104 103 104 106 104 103 104 106 105 104 108 104.5 108.5 104 106 103.5 108 104 104.5 103.5 105 103.5 105 103.5 105 103.5 105 103.5 105 103.5 105 9.25 114.25 60 6.855 302.0 44 1.9 9.25 113.25 60 6.795 4590 675 29 9.25 117.25 60 7.035 865.0 123 5.2 9.25 113.75 60 6.825 3660 536 23 9.25 117.75 60 7.065 1170.0 166 7.0 9.25 113.25 60 6.795 4140 609 26 9.25 115.25 60 6.915 1140.0 165 7.0 9.25 112.75 61 6.878 2950 429 18 9.25 117.25 61 7.152 1450.0 203 8.6 9.25 113.25 60 6.795 1770 260 11 9.25 113.75 60 6.825 748.0 110 4.7 9.25 112.75 60 6.765 1397 207 8.8 9.25 114.25 60 6.855 524.0 76 3.2 9.25 112.75 60 6.765 1520 225 9.6 9.25 114.25 60 6.855 652.0 95 4.0 9.25 112.75 60 6.765 1501 222 9.4 9.25 114.25 60 6.855 1013.0 148 6.3 9.25 112.75 60 6.765 1544 228 9.7 9.25 114.25 60 6.855 958.0 140 5.9 9.25 112.75 60 6.765 1505 222 9.5 9.25 114.25 60 6.855 919.0 134 5.7 9.25 112.75 50 5.6375 1271 225 9.6 9.25 114.25 50 5.7125 885.0 155 6.6 Inlet Outlet Comment Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Pre-test Date/ Time 11/14/13 11:25 11/14/13 13:20 11/14/13 15:20 11/14/13 16:22 11/15/13 9:42 11/15/13 11:42 11/15/13 13:42 11/15/13 14:44 11/20/13 10:06 11/21/13 10:05 11/22/13 9:51 11/25/13 10:55 12/4/13 10:18 Ethyl-FOSE Gas-phase Concentration Generator Chamber Chamber Outlet Outlet Generator Outlet ppbV ppbV Outlet ng/L ng/L 11 0.04 251 0.89 20 0.19 461 4.4 22 0.44 521 10 25 0.75 600 18 25 0.77 587 18 29 0.90 683 21 32 1.36 751 32 34 1.87 810 44 29 5.23 675 123 23 7.04 536 166 26 7.01 609 165 18 8.62 429 203 11 4.66 260 110 Comment Exposure Test Exposure Test Exposure Test Exposure Test Exposure Test Exposure Test Date/ Time 12/9/2013 10:12 12/9/2013 11:15 12/9/2013 12:18 12/9/2013 13:21 12/9/2013 14:24 12/9/2013 15:27 Ethyl-FOSE Gas-phase Concentration Generator Chamber Chamber Outlet Outlet Generator Outlet ppbV ppbV Outlet ng/L ng/L 8.8 3.2 207 76 9.6 4.0 225 95 9.4 6.3 222 148 9.7 5.9 228 140 9.5 5.7 222 134 9.6 6.6 225 155 E13-0880 Final Analytical Report, Appendix-A Start Date Time 11/14/2013 10:25 11/15/2013 8:30 11/19/2013 15:40 11/26/2013 14:44 12/9/2013 9:12 Stop Date Time 11/14/2013 16:24 11/15/2013 14:52 11/26/2013 13:00 12/4/2013 10:44 12/9/2013 9:19 Elpased (hr) 5.98 12.35 177.68 365.68 365.80 Elapsed (min) 359 741 10661 21941 21948 Flow-rate (LPM) 2 2 2 2 2 Volume (L) 718 1482 21322 43882 43896 12/9/2013 9:19 12/9/2013 15:19 371.80 22308 2.1 46847 E13-0722 Prelim Chamber Test E13-0722 Prelim Chamber Test E13-0722 Prelim Chamber Test E13-0722 Prelim Chamber Test E13-0880 Exposure test w Rats shut system down @15:19 12/9/13 sampling done @ 15:17 E13-0880 Final Analytical Report, Appendix-A 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 8 FTIR Data, Method Map, Pathlength, Spectra, Leak Checks, QA/QC Page 9 of 13 E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A Method Name: B270 ethyl-FOSE Method Path: C:\E13-0880 B270 Ethyl-FOSE Rat Exp. Test\Method\B270 ethyl-FOSE\B270 ethyl-FOSE.aq4 Method Type: AutoQuant 4.0 Non-Linear Analysis Mode MethodParameters Wavenumber range: 650.00 - 4500.00 cm-1 Default Pathlength = 24.1800 M Gain = 0 Apodization = Triangle Phase Correction = Mertz Resolution = 0.5 cm-1 Baseline Correction: Single Linear Exclusion Criterion: 2500 Compound: Ethylene Description: Molecular Weight: Alarms: Primary Spectrum: Ethylene Disabled J2KETY.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: 0 206.6000 ppm-m 0.1000 M 0.9699 atm 20.00 C 850.00 - 1100.00 cm-1 Compound: ethylFOSE Description: Molecular Weight: Alarms: Primary Spectrum: ethylFOSE Disabled Ethyl FOSE 17PPB.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: Region #2: Region #3: 0 0.1700 ppm-m 10.0000 M 1.0000 atm 25.00 C 1000.00 - 1056.00 cm-1 1057.00 - 1131.00 cm-1 807.00 - 834.00 cm-1 Compound: Methanol Description: Molecular Weight: Alarms: Spectrum: Methanol Disabled MeOh_25T.spc Reference Concentration: Reference Pathlength: Reference Pressure: 0 1.0000 ppm-m 1.0000 M 1.0000 atm E13-0880 Final Analytical Report, Appendix-A Spectrum: Primary Spectrum: Compound: Temp Description: Molecular Weight: Alarms: Compound: Press Description: Molecular Weight: Alarms: Compound: Ammonia Description: Molecular Weight: Alarms: Spectrum: Primary Spectrum: Spectrum: Reference Temperature: Region #1: meoh_z5a.spc Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: MEOHZ9A.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: 25.00 C 1028.00 - 1038.00 cm-1 224.6000 ppm-m 1.0000 M 1.0000 atm 25.00 C 1028.00 - 1038.00 cm-1 22.5000 ppm-m 1.0000 M 1.0000 atm 25.00 C 1028.00 - 1038.00 cm-1 temperature 0 Disabled pressure 0 Disabled Ammonia Disabled NH3_25T.spc Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: nh3_12.spc Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: nh3_9.spc Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: 0 1.0000 ppm-m 1.0000 M 1.0000 atm 25.00 C 800.00 - 1165.00 cm-1 52.6000 ppm-m 1.0000 M 1.0000 atm 25.00 C 800.00 - 1165.00 cm-1 99.0000 ppm-m 1.0000 M 1.0000 atm 25.00 C E13-0880 Final Analytical Report, Appendix-A Compound: Methane Description: Molecular Weight: Alarms: Primary Spectrum: Spectrum: Spectrum: Compound: CO Description: Molecular Weight: Alarms: Spectrum: Spectrum: Primary Spectrum: Region #1: 800.00 - 1165.00 cm-1 Methane Disabled AIHZME.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: CH4_25A.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: CH4_25T.spc Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: 0 100.0000 ppm-m 1.0000 M 1.0000 atm 25.00 C 2900.00 - 3035.00 cm-1 273.0000 ppm-m 1.0000 M 1.0000 atm 25.00 C 2900.00 - 3035.00 cm-1 1.0000 ppm-m 1.0000 M 1.0000 atm 25.00 C 2900.00 - 3035.00 cm-1 CO Disabled 7CO.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: 67CO.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: 113CO.SPC Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: 0 6.6000 ppm-m 1.0000 M 1.0000 atm 25.00 C 2100.00 - 2181.00 cm-1 66.6900 ppm-m 1.0000 M 1.0000 atm 25.00 C 2100.00 - 2181.00 cm-1 112.7000 ppm-m 1.0000 M 1.0000 atm 25.00 C E13-0880 Final Analytical Report, Appendix-A Compound: Moisture Description: Molecular Weight: Alarms: Primary Spectrum: Region #1: 2124.00 - 2160.00 cm-1 Moisture Disabled U0000030.spc Reference Concentration: Reference Pathlength: Reference Pressure: Reference Temperature: Region #1: Region #2: Region #3: 0 1.0000 ppm-m 24.5700 M 0.9406 atm 22.10 C 2900.00 - 3150.00 cm-1 2200.00 - 2000.00 cm-1 1345.00 - 1200.00 cm-1 E13-0880 Final Analytical Report, Appendix-A Ethylene Cylinder Number SG9104949BAL Concentration , ppmV 20.3 Date 12/9/2013 8:08 12/9/2013 8:09 12/9/2013 8:09 12/9/2013 8:10 12/9/2013 8:11 12/9/2013 8:11 12/9/2013 8:12 12/9/2013 16:00 12/9/2013 16:01 12/9/2013 16:02 12/9/2013 16:03 12/9/2013 16:03 12/9/2013 16:04 12/9/2013 16:04 12/9/2013 16:05 12/9/2013 16:06 12/9/2013 16:06 Method B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE Filename U0000006 U0000007 U0000008 U0000009 U0000010 U0000011 U0000012 Sample Line N/A N/A N/A N/A N/A N/A N/A Average Ethylene (ppm) 21.8714 24.0072 24.2399 24.2151 24.1698 24.1984 24.2151 24.21 SEC (ppm) 0.0891 0.1004 0.1012 0.0995 0.0996 0.0996 0.1009 U0000139 U0000140 U0000141 U0000142 U0000143 U0000144 U0000145 U0000146 U0000147 U0000148 N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A Average 24.1959 24.0793 24.0897 24.1542 24.1643 24.1092 24.1952 24.1802 24.0867 24.132 24.15 0.1039 0.1048 0.1046 0.1028 0.1024 0.1036 0.1034 0.1036 0.1029 0.1036 Overall Average 24.18 E13-0880 Final Analytical Report, Appendix-A Date 12/9/2013 7:59 12/9/2013 7:59 12/9/2013 8:00 12/9/2013 8:05 12/9/2013 8:05 12/9/2013 8:08 12/9/2013 8:09 12/9/2013 8:09 12/9/2013 8:10 12/9/2013 8:11 12/9/2013 8:11 12/9/2013 8:12 12/9/2013 8:49 12/9/2013 8:49 12/9/2013 8:50 12/9/2013 8:51 12/9/2013 8:51 12/9/2013 8:52 12/9/2013 9:03 12/9/2013 9:04 12/9/2013 9:04 12/9/2013 9:05 12/9/2013 9:05 12/9/2013 9:06 12/9/2013 9:07 12/9/2013 9:07 12/9/2013 9:08 12/9/2013 9:15 12/9/2013 9:15 12/9/2013 9:16 12/9/2013 9:16 12/9/2013 9:17 12/9/2013 9:18 12/9/2013 9:18 12/9/2013 9:19 12/9/2013 9:19 12/9/2013 9:20 12/9/2013 9:21 12/9/2013 9:21 12/9/2013 9:22 12/9/2013 9:23 12/9/2013 9:28 12/9/2013 9:33 12/9/2013 9:38 12/9/2013 9:43 12/9/2013 9:48 12/9/2013 9:53 12/9/2013 9:58 12/9/2013 10:03 12/9/2013 10:08 12/9/2013 10:13 12/9/2013 10:18 12/9/2013 10:23 12/9/2013 10:28 12/9/2013 10:33 12/9/2013 10:38 12/9/2013 10:43 12/9/2013 10:48 12/9/2013 10:53 12/9/2013 10:58 12/9/2013 11:03 12/9/2013 11:08 12/9/2013 11:13 12/9/2013 11:18 12/9/2013 11:23 12/9/2013 11:29 12/9/2013 11:34 12/9/2013 11:39 12/9/2013 11:44 12/9/2013 11:49 12/9/2013 11:54 12/9/2013 11:59 12/9/2013 12:04 12/9/2013 12:09 12/9/2013 12:14 12/9/2013 12:19 12/9/2013 12:24 12/9/2013 12:29 12/9/2013 12:34 Method B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE B270 ethyl-FOSE Filename U0000001 U0000002 U0000003 U0000004 U0000005 U0000006 U0000007 U0000008 U0000009 U0000010 U0000011 U0000012 U0000013 U0000014 U0000015 U0000016 U0000017 U0000018 U0000019 U0000020 U0000021 U0000022 U0000023 U0000024 U0000025 U0000026 U0000027 U0000028 U0000029 U0000030 U0000031 U0000032 U0000033 U0000034 U0000035 U0000036 U0000037 U0000038 U0000039 U0000040 U0000041 U0000042 U0000043 U0000044 U0000045 U0000046 U0000047 U0000048 U0000049 U0000050 U0000051 U0000052 U0000053 U0000054 U0000055 U0000056 U0000057 U0000058 U0000059 U0000060 U0000061 U0000062 U0000063 U0000064 U0000065 U0000066 U0000067 U0000068 U0000069 U0000070 U0000071 U0000072 U0000073 U0000074 U0000075 U0000076 U0000077 U0000078 U0000079 Sample Line N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A Ammonia (ppm) 0 0.0164 0 0.0062 0.008 0.0015 0 0.0041 0.0048 0 0 0.0145 0.0078 0 0.0006 0.0122 0 0.002 0 0.0002 0.0144 0.0062 0 0.0062 0.0072 0.0023 0.0143 0.027 0.0053 0.0111 0.0044 0.0019 0.0044 0.0022 0 0 0.0008 0 0.008 0 0.0005 0 0 0 0 0 0 0 0 0 0 0 0 0.2226 0.6911 0.7556 0.8087 0.6755 0.7345 1.3016 0.9866 1.2612 1.6276 1.4892 1.6732 1.791 1.7606 1.9827 2.2443 2.4505 2.4921 2.588 2.8893 3.2634 3.6378 3.3373 3.6776 4.3525 4.5781 SEC (ppm) 0.0082 0.0089 0.0088 0.0066 0.0066 0.0241 0.0271 0.0272 0.0268 0.0269 0.0268 0.0272 0.0064 0.0065 0.0068 0.0066 0.0066 0.0062 0.0064 0.0066 0.0068 0.0066 0.0066 0.0071 0.0064 0.0068 0.0064 0.0338 0.0337 0.0331 0.033 0.0324 0.0321 0.0322 0.0315 0.0315 0.0309 0.0308 0.0303 0.0308 0.0305 0.0321 0.0349 0.0354 0.0346 0.0373 0.0371 0.0371 0.037 0.0379 0.0379 0.038 0.0373 0.0373 0.0367 0.0369 0.0372 0.0363 0.0362 0.0376 0.0368 0.0374 0.0376 0.0379 0.0384 0.0385 0.0379 0.038 0.0383 0.0393 0.0392 0.0397 0.0405 0.041 0.0424 0.0414 0.0425 0.0446 0.0448 CO (ppm) 0 0 0 0.0031 0.0022 0 0 0 0 0 0 0 0.0137 0.023 0 0.0278 0 0 0.048 0.0447 0.0508 0.045 0.0442 0.0456 0.0321 0.0389 0.0339 0.7795 0.8342 0.8761 0.8752 0.9413 0.9307 0.9675 0.9999 1.0403 1.0697 1.1389 1.1284 1.1515 1.2115 1.4198 1.5841 1.7063 1.7969 1.8919 1.9656 1.9919 2.0431 2.0542 2.0789 2.1154 2.1468 2.1485 2.1507 2.1435 2.1505 2.1554 2.1571 2.1804 2.1723 2.156 2.2097 2.1819 2.2114 2.1814 2.2071 2.2111 2.1894 2.221 2.1992 2.2063 2.2057 2.2117 2.2359 2.2181 2.216 2.2067 2.2357 SEC (ppm) 0.0112 0.0115 0.0125 0.0123 0.0121 0.0115 0.0119 0.012 0.0122 0.0114 0.0122 0.0128 0.0118 0.0104 0.0117 0.0124 0.0118 0.0112 0.0129 0.0131 0.0122 0.0119 0.0129 0.0111 0.0118 0.0125 0.0117 0.0977 0.0971 0.0967 0.095 0.0955 0.0935 0.0937 0.0944 0.0934 0.0908 0.0925 0.0916 0.0915 0.0912 0.0958 0.1013 0.1033 0.1018 0.1085 0.1066 0.1082 0.1086 0.1089 0.1111 0.1085 0.1072 0.1055 0.1058 0.104 0.1036 0.1037 0.1037 0.1041 0.1042 0.1041 0.1029 0.1049 0.105 0.1058 0.1052 0.1034 0.1035 0.1024 0.1053 0.1037 0.1059 0.1049 0.1064 0.1048 0.1072 0.1067 0.1045 Ethylene (ppm) 0.0787 0.0815 0.083 0 0 18.353 20.1471 20.3409 20.3145 20.2869 20.3085 20.3176 0 0.0013 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0475 0.0003 0.0301 0 0 0.0247 0.0078 0.0185 0.0079 0.0342 0.0112 0 0.0076 0 0.0469 0.0364 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 SEC (ppm) 0.0229 0.0254 0.025 0.0165 0.016 0.0761 0.0858 0.0864 0.0849 0.0851 0.0851 0.0862 0.0159 0.0161 0.0159 0.0171 0.0166 0.0152 0.026 0.0256 0.0266 0.0259 0.0257 0.0261 0.0239 0.0244 0.024 0.1412 0.072 0.0707 0.0703 0.1308 0.1271 0.0685 0.0675 0.0665 0.0659 0.0667 0.0644 0.1107 0.0654 0.0948 0.0735 0.0733 0.0806 0.0807 0.0809 0.0793 0.0787 0.0808 0.0801 0.0797 0.0775 0.0795 0.0952 0.0979 0.1001 0.0923 0.095 0.0751 0.0736 0.0743 0.074 0.0756 0.0773 0.0761 0.0753 0.0756 0.0764 0.0774 0.079 0.0792 0.0795 0.0809 0.0826 0.0807 0.0826 0.0862 0.0867 Methane (ppm) 0.0143 0.0228 0 0 0 0.0095 0.0171 0 0.0117 0 0 0.0095 0.0185 0 0 0 0.0156 0 0 0.009 0 0.0295 0.0122 0.0538 0.0467 0 0.0143 0.8684 0.8627 0.9291 0.9425 0.9871 1.0282 1.0327 1.0528 1.111 1.1329 1.2 1.174 1.1717 1.2406 1.4314 1.5467 1.6494 1.6749 1.739 1.7575 1.8083 1.871 1.8327 1.8277 1.8689 1.8606 1.8462 1.8956 1.897 1.9129 1.8878 1.9178 1.8802 1.8842 1.9146 1.9023 1.9248 1.9178 1.8936 1.8499 1.9199 1.9275 1.9278 1.9092 1.9242 1.9277 1.8733 1.89 1.8878 1.9162 1.8812 1.9158 SEC (ppm) 0.0154 0.0152 0.015 0.0162 0.0163 0.0523 0.0414 0.0381 0.0387 0.0367 0.0345 0.0355 0.0162 0.0152 0.0173 0.0169 0.0164 0.0161 0.0522 0.053 0.0543 0.0539 0.0513 0.0528 0.0522 0.0528 0.0519 0.1331 0.1304 0.1299 0.1277 0.1282 0.126 0.1281 0.1273 0.1272 0.1243 0.1253 0.125 0.1245 0.1252 0.1263 0.1338 0.1335 0.1332 0.1388 0.1392 0.1419 0.1413 0.1419 0.1414 0.1416 0.1409 0.1417 0.1427 0.1414 0.1414 0.1388 0.1424 0.1426 0.1426 0.1414 0.1378 0.1401 0.1394 0.1401 0.141 0.1405 0.1394 0.1408 0.1404 0.1394 0.1403 0.1433 0.1429 0.1409 0.1423 0.1429 0.1438 Methanol (ppm) 0 0 0 0 0 0.0506 0.0634 0.0797 0.0393 0.0902 0.0581 0.0393 0.0293 0 0 0 0.0163 0 0.4717 0.4695 0.5042 0.4358 0.488 0.4476 0.4646 0.411 0.4749 2.8434 2.8142 2.7659 2.6898 2.6331 2.5186 2.5297 2.5196 2.3565 2.3762 2.2142 2.1761 2.1661 2.1124 1.7107 1.3751 1.1296 1.0162 0.9006 0.8441 0.7047 0.705 0.6799 0.6447 0.6422 0.5503 0.5349 0.4677 0.5289 0.4557 0.4677 0.3788 0.3753 0.4213 0.4216 0.3472 0.2957 0.2953 0.2741 0.2831 0.261 0.2585 0.2382 0.2277 0.2226 0.1856 0.2076 0.183 0.1221 0.1049 0.0891 0.0005 SEC (ppm) 0.0189 0.0182 0.0275 0.0266 0.0225 0.0703 0.0762 0.0827 0.0838 0.0808 0.0817 0.0799 0.0287 0.0255 0.0283 0.0246 0.0251 0.0268 0.0281 0.0325 0.031 0.0331 0.027 0.0437 0.0292 0.0371 0.0286 0.0983 0.0899 0.0978 0.0954 0.1013 0.0955 0.0942 0.0982 0.0973 0.0895 0.0868 0.0886 0.0994 0.0749 0.0827 0.0848 0.0883 0.0747 0.0839 0.0863 0.0803 0.0817 0.0806 0.0875 0.0895 0.0739 0.0794 0.0825 0.0826 0.0846 0.0744 0.0757 0.0751 0.0691 0.0759 0.0866 0.0788 0.0786 0.0878 0.0802 0.0778 0.0889 0.0861 0.0976 0.0901 0.1006 0.1038 0.1174 0.0935 0.0999 0.1068 0.1701 Moisture (ppm) 0 0 0 0 0.0001 0.0069 0.0025 0.0018 0.0014 0.0012 0.0012 0.0011 0 0.0001 0 0 0 0 0.0153 0.0152 0.015 0.0148 0.0147 0.0145 0.0144 0.0143 0.0143 0.2939 0.2907 0.2882 0.2854 0.2843 0.2824 0.2794 0.2782 0.2764 0.2726 0.2722 0.2702 0.2715 0.2714 0.2776 0.2942 0.2975 0.2958 0.3116 0.3119 0.3137 0.317 0.3141 0.3172 0.3175 0.3151 0.3168 0.315 0.3147 0.3163 0.3157 0.3176 0.317 0.3174 0.3129 0.3132 0.3156 0.3142 0.3154 0.3134 0.3139 0.3108 0.3088 0.3113 0.3117 0.3142 0.3142 0.3161 0.3146 0.3156 0.3153 0.3154 SEC (ppm) 0 0 0 0 0 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0 0 0 0 0 0 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.0011 0.001 0.001 0.0011 0.001 0.001 0.0011 0.0011 0.0011 0.0011 0.0011 0.001 0.001 0.001 0.0011 0.0011 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.0009 0.001 0.0009 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 Press (atm) 0.9689 0.9698 0.9677 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9694 0.9698 0.9698 0.9702 0.9698 1.0195 1.0195 1.0195 1.0195 1.0171 1.0195 1.0199 1.0195 1.0199 0.9698 0.9698 0.9685 0.9706 0.9706 0.9702 0.971 0.9706 0.9706 0.9706 0.9677 0.971 0.971 0.971 0.971 0.9706 0.9706 0.9706 0.971 0.9706 0.971 0.971 0.9706 0.971 0.9706 0.9706 0.971 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.971 0.971 0.971 0.971 0.971 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 SEC (atm) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Temp (C) 21.5453 21.5453 21.7026 21.5453 21.5453 21.5453 21.6239 21.5453 21.5453 21.5453 21.4667 21.5453 21.4667 21.4667 21.4667 21.5453 21.4667 21.5453 21.5453 21.4667 21.6239 21.7026 21.4667 21.7026 21.4667 21.7026 21.6239 21.7026 21.4667 21.4667 21.4667 21.6239 21.6239 21.7026 21.7026 21.5453 21.7026 21.5453 21.7026 21.6239 21.7026 21.6239 21.7812 21.6239 21.7812 21.5453 21.7026 21.7026 21.7026 21.6239 21.7026 21.6239 21.7026 21.7026 21.7026 21.7026 21.8598 21.7026 21.7026 21.9385 21.7026 21.7026 21.8598 21.8598 21.7026 21.9385 21.7026 21.8598 21.9385 21.8598 21.8598 21.7812 21.8598 21.7812 21.9385 21.8598 21.9385 21.8598 21.9385 SEC (C) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 ethylFOSE (ppm) 0 0 0 0 0.0002 0 0 0 0 0.0001 0 0 0 0 0 0 0 0 0.0017 0.0015 0.0016 0.0015 0.0016 0.0016 0.0016 0.0018 0.0017 0 0 0.0001 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 SEC (ppm) 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 E13-0880 Final Analytical Report, Appendix-A 12/9/2013 12:39 B270 ethyl-FOSE U0000080 N/A 12/9/2013 12:44 B270 ethyl-FOSE U0000081 N/A 12/9/2013 12:49 B270 ethyl-FOSE U0000082 N/A 12/9/2013 12:54 B270 ethyl-FOSE U0000083 N/A 12/9/2013 12:59 B270 ethyl-FOSE U0000084 N/A 12/9/2013 13:04 B270 ethyl-FOSE U0000085 N/A 12/9/2013 13:09 B270 ethyl-FOSE U0000086 N/A 12/9/2013 13:14 B270 ethyl-FOSE U0000087 N/A 12/9/2013 13:19 B270 ethyl-FOSE U0000088 N/A 12/9/2013 13:24 B270 ethyl-FOSE U0000089 N/A 12/9/2013 13:29 B270 ethyl-FOSE U0000090 N/A 12/9/2013 13:34 B270 ethyl-FOSE U0000091 N/A 12/9/2013 13:39 B270 ethyl-FOSE U0000092 N/A 12/9/2013 13:44 B270 ethyl-FOSE U0000093 N/A 12/9/2013 13:49 B270 ethyl-FOSE U0000094 N/A 12/9/2013 13:54 B270 ethyl-FOSE U0000095 N/A 12/9/2013 13:59 B270 ethyl-FOSE U0000096 N/A 12/9/2013 14:04 B270 ethyl-FOSE U0000097 N/A 12/9/2013 14:09 B270 ethyl-FOSE U0000098 N/A 12/9/2013 14:14 B270 ethyl-FOSE U0000099 N/A 12/9/2013 14:19 B270 ethyl-FOSE U0000100 N/A 12/9/2013 14:24 B270 ethyl-FOSE U0000101 N/A 12/9/2013 14:29 B270 ethyl-FOSE U0000102 N/A 12/9/2013 14:34 B270 ethyl-FOSE U0000103 N/A 12/9/2013 14:39 B270 ethyl-FOSE U0000104 N/A 12/9/2013 14:44 B270 ethyl-FOSE U0000105 N/A 12/9/2013 14:49 B270 ethyl-FOSE U0000106 N/A 12/9/2013 14:54 B270 ethyl-FOSE U0000107 N/A 12/9/2013 14:59 B270 ethyl-FOSE U0000108 N/A 12/9/2013 15:04 B270 ethyl-FOSE U0000109 N/A 12/9/2013 15:09 B270 ethyl-FOSE U0000110 N/A 12/9/2013 15:14 B270 ethyl-FOSE U0000111 N/A 12/9/2013 15:19 B270 ethyl-FOSE U0000112 N/A 12/9/2013 15:35 B270 ethyl-FOSE U0000113 N/A 12/9/2013 15:36 B270 ethyl-FOSE U0000114 N/A 12/9/2013 15:36 B270 ethyl-FOSE U0000115 N/A 12/9/2013 15:37 B270 ethyl-FOSE U0000116 N/A 12/9/2013 15:37 B270 ethyl-FOSE U0000117 N/A 12/9/2013 15:38 B270 ethyl-FOSE U0000118 N/A 12/9/2013 15:39 B270 ethyl-FOSE U0000119 N/A 12/9/2013 15:44 B270 ethyl-FOSE U0000120 N/A 12/9/2013 15:45 B270 ethyl-FOSE U0000121 N/A 12/9/2013 15:45 B270 ethyl-FOSE U0000122 N/A 12/9/2013 15:46 B270 ethyl-FOSE U0000123 N/A 12/9/2013 15:46 B270 ethyl-FOSE U0000124 N/A 12/9/2013 15:47 B270 ethyl-FOSE U0000125 N/A 12/9/2013 15:48 B270 ethyl-FOSE U0000126 N/A 12/9/2013 15:48 B270 ethyl-FOSE U0000127 N/A 12/9/2013 15:49 B270 ethyl-FOSE U0000128 N/A 12/9/2013 15:49 B270 ethyl-FOSE U0000129 N/A 12/9/2013 15:50 B270 ethyl-FOSE U0000130 N/A 12/9/2013 15:51 B270 ethyl-FOSE U0000131 N/A 12/9/2013 15:51 B270 ethyl-FOSE U0000132 N/A 12/9/2013 15:55 B270 ethyl-FOSE U0000133 N/A 12/9/2013 15:55 B270 ethyl-FOSE U0000134 N/A 12/9/2013 15:56 B270 ethyl-FOSE U0000135 N/A 12/9/2013 15:56 B270 ethyl-FOSE U0000136 N/A 12/9/2013 15:57 B270 ethyl-FOSE U0000137 N/A 12/9/2013 15:58 B270 ethyl-FOSE U0000138 N/A 12/9/2013 16:00 B270 ethyl-FOSE U0000139 N/A 12/9/2013 16:01 B270 ethyl-FOSE U0000140 N/A 12/9/2013 16:02 B270 ethyl-FOSE U0000141 N/A 12/9/2013 16:03 B270 ethyl-FOSE U0000142 N/A 12/9/2013 16:03 B270 ethyl-FOSE U0000143 N/A 12/9/2013 16:04 B270 ethyl-FOSE U0000144 N/A 12/9/2013 16:04 B270 ethyl-FOSE U0000145 N/A 12/9/2013 16:05 B270 ethyl-FOSE U0000146 N/A 12/9/2013 16:06 B270 ethyl-FOSE U0000147 N/A 12/9/2013 16:06 B270 ethyl-FOSE U0000148 N/A 4.7143 4.3564 4.3951 4.4325 4.704 4.8292 4.8793 5.0059 4.4362 4.5703 4.8279 4.273 4.1152 4.0323 4.1195 4.184 4.1938 4.6446 4.9885 5.1158 5.3908 5.4873 6.0468 6.7935 7.0278 7.5309 8.0732 8.3954 8.5224 9.2226 9.5705 10.1112 10.5619 0 0.0007 0 0.0092 0.0033 0.0008 0.0152 7.7074 5.7211 3.4022 0.7415 0.2044 0.1227 0.1005 0.099 0.0757 0.0839 0.069 0.0715 0.0635 0.0734 0.061 0.0426 0.0431 0.0433 0.0362 0.1204 0.0852 0.0633 0.051 0.0686 0.0535 0.0465 0.0511 0.0555 0.0567 0.0451 0.0444 0.0441 0.0447 0.0445 0.0453 0.0459 0.0461 0.0445 0.0455 0.047 0.0449 0.0448 0.0442 0.0442 0.0447 0.0443 0.0454 0.0462 0.0464 0.0474 0.0478 0.0494 0.0522 0.0532 0.0545 0.056 0.0569 0.0572 0.0603 0.0617 0.0639 0.0654 0.0067 0.0064 0.007 0.0067 0.0065 0.0066 0.0065 0.0481 0.0363 0.0247 0.0086 0.007 0.0065 0.0068 0.0069 0.0069 0.0065 0.0068 0.0068 0.0069 0.0064 0.0066 0.0067 0.0068 0.0068 0.0068 0.0278 0.0281 0.0281 0.0276 0.0276 0.0279 0.0278 0.0279 0.0277 0.0279 2.2215 2.2544 2.2371 2.2133 2.2236 2.2161 2.2358 2.2086 2.2406 2.2315 2.2414 2.2436 2.249 2.2645 2.2496 2.2656 2.2277 2.2188 2.2294 2.2494 2.2397 2.2373 2.2423 2.2364 2.2683 2.2512 2.2209 2.2307 2.2297 2.2718 2.2446 2.2396 2.2299 0.0052 0.0299 0.0139 0.0106 0.0115 0.0217 0.0077 2.0068 1.9319 1.8213 1.7723 1.7792 1.7548 1.7768 1.7745 1.7631 1.7674 1.768 1.7646 1.7872 0.1995 0.0459 0.0156 0.0059 0.0059 0 0 0 0 0 0 0 0 0 0 0 0.106 0.106 0.1041 0.1058 0.1041 0.1034 0.1047 0.106 0.1064 0.1072 0.1098 0.11 0.1079 0.1069 0.1088 0.1074 0.1064 0.1056 0.1056 0.1061 0.1056 0.1052 0.1064 0.1064 0.1063 0.1037 0.1053 0.1056 0.1043 0.1053 0.1056 0.1055 0.1048 0.0118 0.0109 0.0119 0.0124 0.0115 0.0125 0.0115 0.0735 0.051 0.0325 0.0262 0.0259 0.0266 0.0265 0.0266 0.0264 0.0263 0.0271 0.0275 0.0263 0.0115 0.0122 0.0117 0.0117 0.0121 0.0114 0.0108 0.0124 0.0113 0.0117 0.0124 0.0118 0.012 0.0122 0.0123 0.0121 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0017 0.0126 0 0.0182 0.0378 0.0198 0 0 0 0 0 0 0 0 0 20.3142 20.1975 20.2208 20.2746 20.2774 20.2353 20.3048 20.2923 20.213 20.2487 0.0871 0.0856 0.0852 0.0846 0.0859 0.0859 0.0872 0.0874 0.0855 0.0884 0.0902 0.0879 0.0876 0.0862 0.086 0.0862 0.0855 0.0871 0.0882 0.0889 0.0893 0.0905 0.092 0.0972 0.0996 0.1012 0.1038 0.1055 0.1062 0.1115 0.115 0.1187 0.8278 0.0165 0.0165 0.017 0.0171 0.0163 0.0166 0.0162 0.0861 0.0648 0.0447 0.0631 0.0235 0.0191 0.0181 0.0181 0.0178 0.0173 0.0174 0.0181 0.0169 0.0168 0.0176 0.0172 0.0175 0.0168 0.0172 0.0888 0.0893 0.0894 0.0878 0.0875 0.0885 0.0884 0.0883 0.0879 0.0884 1.9128 1.9093 1.9217 1.912 1.8999 1.9198 1.8984 1.9145 1.9072 1.9282 1.9211 1.9268 1.9104 1.8679 1.8936 1.87 1.8574 1.9247 1.8988 1.8917 1.9278 1.9094 1.9452 1.9174 1.9146 1.9729 1.9332 1.9488 1.9613 1.9707 1.9694 1.9289 1.9123 0 0 0 0.0054 0.0003 0 0 1.9121 1.8797 1.7688 1.8058 1.8549 1.8702 1.8807 1.9062 1.852 1.8821 1.8733 1.8509 1.9265 0.1794 0.0452 0.0287 0.0002 0.021 0.005 0.0021 0 0 0.0426 0.0409 0.0169 0.0263 0.0067 0.0185 0.0159 0.1426 0.1429 0.1425 0.1428 0.1428 0.1413 0.143 0.145 0.141 0.1432 0.1434 0.1444 0.143 0.1428 0.144 0.1435 0.1414 0.1413 0.1434 0.1433 0.1436 0.1447 0.1429 0.1435 0.1438 0.1411 0.1423 0.1438 0.1439 0.1435 0.1423 0.1444 0.1434 0.0184 0.019 0.0177 0.018 0.0192 0.0181 0.0192 0.1177 0.0988 0.0824 0.0625 0.0437 0.0398 0.0393 0.0377 0.0365 0.0362 0.0368 0.038 0.0363 0.0198 0.0177 0.0179 0.0173 0.0186 0.0177 0.0423 0.0388 0.038 0.0375 0.0363 0.0371 0.0373 0.0378 0.0376 0.0371 0.1106 0.073 0.0738 0.0877 0.0654 0.0481 0.0462 0.0527 0.0425 0.0732 0.0359 0.104 0.0905 0.0795 0.0919 0.1399 0.0966 0.0425 0.0273 0.0117 0.0146 0.0572 0 0 0 0 0 0 0 0 0 0 0 0 0.0136 0 0.0296 0 0.042 0.017 0 0 0 0 0 0 0 0 0 0 0 0 0 0.038 0 0 0.0135 0.0296 0.0222 0.0449 0.0499 0.0893 0.0698 0.0603 0.0647 0.0998 0.0122 0.0842 0.0643 0.1181 0.1163 0.116 0.1014 0.1171 0.1189 0.1214 0.1275 0.1069 0.1183 0.1208 0.1118 0.1074 0.1112 0.107 0.1143 0.1128 0.1121 0.1171 0.1835 0.1987 0.1263 0.1334 0.1407 0.1432 0.1536 0.155 0.1629 0.1685 0.1743 0.1887 0.1902 0.2068 0.0285 0.0328 0.0216 0.0268 0.041 0.0262 0.028 0.1537 0.1053 0.0733 0.0365 0.0279 0.0256 0.0254 0.0262 0.0265 0.0272 0.0304 0.0283 0.0301 0.024 0.0238 0.0259 0.0318 0.0288 0.0258 0.0855 0.0788 0.0833 0.0782 0.0842 0.082 0.0803 0.09 0.0819 0.0817 0.3144 0.3149 0.316 0.3147 0.314 0.3162 0.3158 0.3153 0.3159 0.3161 0.3168 0.3164 0.316 0.315 0.316 0.3143 0.3134 0.3161 0.3134 0.316 0.3163 0.3167 0.3176 0.3179 0.3185 0.3158 0.3163 0.3154 0.3146 0.3183 0.3164 0.3152 0.3168 0.0006 0.0008 0.0007 0.0007 0.0007 0.0007 0.0006 0.2445 0.1514 0.0686 0.0138 0.0019 0.0007 0.0005 0.0004 0.0003 0.0003 0.0003 0.0004 0.0003 0.0006 0.0005 0.0005 0.0005 0.0005 0.0004 0.0023 0.0015 0.0014 0.0014 0.0013 0.0012 0.0012 0.0011 0.0011 0.0011 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.0009 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0 0 0 0 0 0 0 0.0008 0.0009 0.0006 0.0002 0.0001 0.0001 0.0001 0.0001 0.0001 0.0002 0.0002 0.0002 0.0002 0.0001 0 0 0 0 0 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.971 0.9685 0.971 0.9706 0.971 0.971 0.9706 0.9706 0.971 0.971 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.9706 0.971 0.9685 0.9706 0.9706 0.9698 0.9706 0.971 0.971 0.9706 0.9706 0.9714 0.9689 0.9706 0.9718 0.9706 0.9677 0.9722 0.971 0.971 0.971 0.971 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.9685 0.971 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.971 0.9706 0.9706 0.971 0.9698 0 21.8598 0 0 21.9385 0 0 21.9385 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.9385 0 0 21.8598 0 0 21.8598 0 0 21.9385 0 0 21.8598 0 0 21.9385 0 0 21.9385 0 0 21.7026 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.7026 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.9385 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.9385 0 0 22.0957 0 0 22.0171 0 0 22.0171 0 0 22.0957 0 0 22.0957 0 0 21.9385 0 0 22.0171 0 0 22.0957 0 0 21.8598 0 0 22.0171 0 0 21.9385 0 0 22.0171 0 0 21.9385 0 0 22.0171 0 0 22.0171 0 0 22.0171 0 0 22.0171 0 0 21.8598 0 0 21.8598 0 0 21.9385 0 0 21.7812 0 0 21.8598 0 0 21.8598 0 0 21.7026 0 0 21.7812 0 0 21.8598 0 0 21.8598 0 0 21.9385 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.8598 0 0 21.9385 0 0 21.8598 0 0 21.2308 0 0 21.7026 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0002 0.0001 0 0.0001 0 0 0 0.0001 0.0003 0.0003 0.0003 0.0002 0 0.0001 0 0.0003 0 0.0001 0.0002 0.0001 0.0002 0.0001 0.0001 0 0 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0006 0.0006 0.0006 0.0006 0.0006 0.0006 0.0006 0.0006 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0004 0.0003 0.0002 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 E13-0880 Final Analytical Report, Appendix-A Time 7:59:05 7:59:40 8:00:16 8:05:03 8:05:39 8:08:44 8:09:20 8:09:56 8:10:32 8:11:08 8:11:44 8:12:20 8:49:23 8:49:59 8:50:35 8:51:11 8:51:47 8:52:23 9:03:27 9:04:03 9:04:39 9:05:15 9:05:51 9:06:27 9:07:03 9:07:39 9:08:15 9:15:02 9:15:38 9:16:14 9:16:50 9:17:26 9:18:02 9:18:38 9:19:14 9:19:50 9:20:26 9:21:02 9:21:38 9:22:14 9:23:34 9:28:35 9:33:36 9:38:37 9:43:38 9:48:39 9:53:40 9:58:41 10:03:42 10:08:43 10:13:44 10:18:45 10:23:46 10:28:47 10:33:48 10:38:49 10:43:50 10:48:51 10:53:53 10:58:54 11:03:55 11:08:56 11:13:57 11:18:58 11:23:59 11:29:00 11:34:01 11:39:02 11:44:03 11:49:04 11:54:05 11:59:06 12:04:07 12:09:08 12:14:09 12:19:11 12:24:12 12:29:13 12:34:14 12:39:15 12:44:16 12:49:17 12:54:18 12:59:19 13:04:20 13:09:21 13:14:22 13:19:23 13:24:24 13:29:26 13:34:27 13:39:28 Filename U0000001 U0000002 U0000003 U0000004 U0000005 U0000006 U0000007 U0000008 U0000009 U0000010 U0000011 U0000012 U0000013 U0000014 U0000015 U0000016 U0000017 U0000018 U0000019 U0000020 U0000021 U0000022 U0000023 U0000024 U0000025 U0000026 U0000027 U0000028 U0000029 U0000030 U0000031 U0000032 U0000033 U0000034 U0000035 U0000036 U0000037 U0000038 U0000039 U0000040 U0000041 U0000042 U0000043 U0000044 U0000045 U0000046 U0000047 U0000048 U0000049 U0000050 U0000051 U0000052 U0000053 U0000054 U0000055 U0000056 U0000057 U0000058 U0000059 U0000060 U0000061 U0000062 U0000063 U0000064 U0000065 U0000066 U0000067 U0000068 U0000069 U0000070 U0000071 U0000072 U0000073 U0000074 U0000075 U0000076 U0000077 U0000078 U0000079 U0000080 U0000081 U0000082 U0000083 U0000084 U0000085 U0000086 U0000087 U0000088 U0000089 U0000090 U0000091 U0000092 Ammonia (ppm) 0 0.0164 0 0.0062 0.008 0.0015 0 0.0041 0.0048 0 0 0.0145 0.0078 0 0.0006 0.0122 0 0.002 0 0.0002 0.0144 0.0062 0 0.0062 0.0072 0.0023 0.0143 0.027 0.0053 0.0111 0.0044 0.0019 0.0044 0.0022 0 0 0.0008 0 0.008 0 0.0005 0 0 0 0 0 0 0 0 0 0 0 0 0.2226 0.6911 0.7556 0.8087 0.6755 0.7345 1.3016 0.9866 1.2612 1.6276 1.4892 1.6732 1.791 1.7606 1.9827 2.2443 2.4505 2.4921 2.588 2.8893 3.2634 3.6378 3.3373 3.6776 4.3525 4.5781 4.7143 4.3564 4.3951 4.4325 4.704 4.8292 4.8793 5.0059 4.4362 4.5703 4.8279 4.273 4.1152 SEC (ppm) 0.0082 0.0089 0.0088 0.0066 0.0066 0.0241 0.0271 0.0272 0.0268 0.0269 0.0268 0.0272 0.0064 0.0065 0.0068 0.0066 0.0066 0.0062 0.0064 0.0066 0.0068 0.0066 0.0066 0.0071 0.0064 0.0068 0.0064 0.0338 0.0337 0.0331 0.033 0.0324 0.0321 0.0322 0.0315 0.0315 0.0309 0.0308 0.0303 0.0308 0.0305 0.0321 0.0349 0.0354 0.0346 0.0373 0.0371 0.0371 0.037 0.0379 0.0379 0.038 0.0373 0.0373 0.0367 0.0369 0.0372 0.0363 0.0362 0.0376 0.0368 0.0374 0.0376 0.0379 0.0384 0.0385 0.0379 0.038 0.0383 0.0393 0.0392 0.0397 0.0405 0.041 0.0424 0.0414 0.0425 0.0446 0.0448 0.0451 0.0444 0.0441 0.0447 0.0445 0.0453 0.0459 0.0461 0.0445 0.0455 0.047 0.0449 0.0448 FM U, % #DIV/0! 108.5% #DIV/0! 212.9% 165.0% 3213.3% #DIV/0! 1326.8% 1116.7% #DIV/0! #DIV/0! 375.2% 164.1% #DIV/0! 2266.7% 108.2% #DIV/0! 620.0% #DIV/0! 6600.0% 94.4% 212.9% #DIV/0! 229.0% 177.8% 591.3% 89.5% 250.4% 1271.7% 596.4% 1500.0% 3410.5% 1459.1% 2927.3% #DIV/0! #DIV/0! 7725.0% #DIV/0! 757.5% #DIV/0! 12200.0% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 33.5% 10.6% 9.8% 9.2% 10.7% 9.9% 5.8% 7.5% 5.9% 4.6% 5.1% 4.6% 4.3% 4.3% 3.8% 3.4% 3.2% 3.1% 3.1% 2.8% 2.5% 2.3% 2.5% 2.3% 2.0% 2.0% 1.9% 2.0% 2.0% 2.0% 1.9% 1.9% 1.9% 1.8% 2.0% 2.0% 1.9% 2.1% 2.2% CO (ppm) 0 0 0 0.0031 0.0022 0 0 0 0 0 0 0 0.0137 0.023 0 0.0278 0 0 0.048 0.0447 0.0508 0.045 0.0442 0.0456 0.0321 0.0389 0.0339 0.7795 0.8342 0.8761 0.8752 0.9413 0.9307 0.9675 0.9999 1.0403 1.0697 1.1389 1.1284 1.1515 1.2115 1.4198 1.5841 1.7063 1.7969 1.8919 1.9656 1.9919 2.0431 2.0542 2.0789 2.1154 2.1468 2.1485 2.1507 2.1435 2.1505 2.1554 2.1571 2.1804 2.1723 2.156 2.2097 2.1819 2.2114 2.1814 2.2071 2.2111 2.1894 2.221 2.1992 2.2063 2.2057 2.2117 2.2359 2.2181 2.216 2.2067 2.2357 2.2215 2.2544 2.2371 2.2133 2.2236 2.2161 2.2358 2.2086 2.2406 2.2315 2.2414 2.2436 2.249 SEC (ppm) 0.0112 0.0115 0.0125 0.0123 0.0121 0.0115 0.0119 0.012 0.0122 0.0114 0.0122 0.0128 0.0118 0.0104 0.0117 0.0124 0.0118 0.0112 0.0129 0.0131 0.0122 0.0119 0.0129 0.0111 0.0118 0.0125 0.0117 0.0977 0.0971 0.0967 0.095 0.0955 0.0935 0.0937 0.0944 0.0934 0.0908 0.0925 0.0916 0.0915 0.0912 0.0958 0.1013 0.1033 0.1018 0.1085 0.1066 0.1082 0.1086 0.1089 0.1111 0.1085 0.1072 0.1055 0.1058 0.104 0.1036 0.1037 0.1037 0.1041 0.1042 0.1041 0.1029 0.1049 0.105 0.1058 0.1052 0.1034 0.1035 0.1024 0.1053 0.1037 0.1059 0.1049 0.1064 0.1048 0.1072 0.1067 0.1045 0.106 0.106 0.1041 0.1058 0.1041 0.1034 0.1047 0.106 0.1064 0.1072 0.1098 0.11 0.1079 FM U, % #DIV/0! #DIV/0! #DIV/0! 793.5% 1100.0% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 172.3% 90.4% #DIV/0! 89.2% #DIV/0! #DIV/0! 53.8% 58.6% 48.0% 52.9% 58.4% 48.7% 73.5% 64.3% 69.0% 25.1% 23.3% 22.1% 21.7% 20.3% 20.1% 19.4% 18.9% 18.0% 17.0% 16.2% 16.2% 15.9% 15.1% 13.5% 12.8% 12.1% 11.3% 11.5% 10.8% 10.9% 10.6% 10.6% 10.7% 10.3% 10.0% 9.8% 9.8% 9.7% 9.6% 9.6% 9.6% 9.5% 9.6% 9.7% 9.3% 9.6% 9.5% 9.7% 9.5% 9.4% 9.5% 9.2% 9.6% 9.4% 9.6% 9.5% 9.5% 9.4% 9.7% 9.7% 9.3% 9.5% 9.4% 9.3% 9.6% 9.4% 9.3% 9.4% 9.6% 9.5% 9.6% 9.8% 9.8% 9.6% Ethylene (ppm) 0.0787 0.0815 0.083 0 0 18.353 20.1471 20.3409 20.3145 20.2869 20.3085 20.3176 0 0.0013 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0475 0.0003 0.0301 0 0 0.0247 0.0078 0.0185 0.0079 0.0342 0.0112 0 0.0076 0 0.0469 0.0364 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 SEC (ppm) 0.0229 0.0254 0.025 0.0165 0.016 0.0761 0.0858 0.0864 0.0849 0.0851 0.0851 0.0862 0.0159 0.0161 0.0159 0.0171 0.0166 0.0152 0.026 0.0256 0.0266 0.0259 0.0257 0.0261 0.0239 0.0244 0.024 0.1412 0.072 0.0707 0.0703 0.1308 0.1271 0.0685 0.0675 0.0665 0.0659 0.0667 0.0644 0.1107 0.0654 0.0948 0.0735 0.0733 0.0806 0.0807 0.0809 0.0793 0.0787 0.0808 0.0801 0.0797 0.0775 0.0795 0.0952 0.0979 0.1001 0.0923 0.095 0.0751 0.0736 0.0743 0.074 0.0756 0.0773 0.0761 0.0753 0.0756 0.0764 0.0774 0.079 0.0792 0.0795 0.0809 0.0826 0.0807 0.0826 0.0862 0.0867 0.0871 0.0856 0.0852 0.0846 0.0859 0.0859 0.0872 0.0874 0.0855 0.0884 0.0902 0.0879 0.0876 FM U, % 58.2% 62.3% 60.2% #DIV/0! #DIV/0! 0.8% 0.9% 0.8% 0.8% 0.8% 0.8% 0.8% #DIV/0! 2476.9% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 303.2% 47133.3% 467.1% #DIV/0! #DIV/0! 554.7% 1730.8% 718.9% 1668.4% 390.1% 1150.0% #DIV/0! 1721.1% #DIV/0! 313.4% 402.7% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! M ethane (ppm) 0.0143 0.0228 0 0 0 0.0095 0.0171 0 0.0117 0 0 0.0095 0.0185 0 0 0 0.0156 0 0 0.009 0 0.0295 0.0122 0.0538 0.0467 0 0.0143 0.8684 0.8627 0.9291 0.9425 0.9871 1.0282 1.0327 1.0528 1.111 1.1329 1.2 1.174 1.1717 1.2406 1.4314 1.5467 1.6494 1.6749 1.739 1.7575 1.8083 1.871 1.8327 1.8277 1.8689 1.8606 1.8462 1.8956 1.897 1.9129 1.8878 1.9178 1.8802 1.8842 1.9146 1.9023 1.9248 1.9178 1.8936 1.8499 1.9199 1.9275 1.9278 1.9092 1.9242 1.9277 1.8733 1.89 1.8878 1.9162 1.8812 1.9158 1.9128 1.9093 1.9217 1.912 1.8999 1.9198 1.8984 1.9145 1.9072 1.9282 1.9211 1.9268 1.9104 SEC (ppm) 0.0154 0.0152 0.015 0.0162 0.0163 0.0523 0.0414 0.0381 0.0387 0.0367 0.0345 0.0355 0.0162 0.0152 0.0173 0.0169 0.0164 0.0161 0.0522 0.053 0.0543 0.0539 0.0513 0.0528 0.0522 0.0528 0.0519 0.1331 0.1304 0.1299 0.1277 0.1282 0.126 0.1281 0.1273 0.1272 0.1243 0.1253 0.125 0.1245 0.1252 0.1263 0.1338 0.1335 0.1332 0.1388 0.1392 0.1419 0.1413 0.1419 0.1414 0.1416 0.1409 0.1417 0.1427 0.1414 0.1414 0.1388 0.1424 0.1426 0.1426 0.1414 0.1378 0.1401 0.1394 0.1401 0.141 0.1405 0.1394 0.1408 0.1404 0.1394 0.1403 0.1433 0.1429 0.1409 0.1423 0.1429 0.1438 0.1426 0.1429 0.1425 0.1428 0.1428 0.1413 0.143 0.145 0.141 0.1432 0.1434 0.1444 0.143 FM U, % 215.4% 133.3% #DIV/0! #DIV/0! #DIV/0! 1101.1% 484.2% #DIV/0! 661.5% #DIV/0! #DIV/0! 747.4% 175.1% #DIV/0! #DIV/0! #DIV/0! 210.3% #DIV/0! #DIV/0! 1177.8% #DIV/0! 365.4% 841.0% 196.3% 223.6% #DIV/0! 725.9% 30.7% 30.2% 28.0% 27.1% 26.0% 24.5% 24.8% 24.2% 22.9% 21.9% 20.9% 21.3% 21.3% 20.2% 17.6% 17.3% 16.2% 15.9% 16.0% 15.8% 15.7% 15.1% 15.5% 15.5% 15.2% 15.1% 15.4% 15.1% 14.9% 14.8% 14.7% 14.9% 15.2% 15.1% 14.8% 14.5% 14.6% 14.5% 14.8% 15.2% 14.6% 14.5% 14.6% 14.7% 14.5% 14.6% 15.3% 15.1% 14.9% 14.9% 15.2% 15.0% 14.9% 15.0% 14.8% 14.9% 15.0% 14.7% 15.1% 15.1% 14.8% 14.9% 14.9% 15.0% 15.0% M ethanol (ppm) 0 0 0 0 0 0.0506 0.0634 0.0797 0.0393 0.0902 0.0581 0.0393 0.0293 0 0 0 0.0163 0 0.4717 0.4695 0.5042 0.4358 0.488 0.4476 0.4646 0.411 0.4749 2.8434 2.8142 2.7659 2.6898 2.6331 2.5186 2.5297 2.5196 2.3565 2.3762 2.2142 2.1761 2.1661 2.1124 1.7107 1.3751 1.1296 1.0162 0.9006 0.8441 0.7047 0.705 0.6799 0.6447 0.6422 0.5503 0.5349 0.4677 0.5289 0.4557 0.4677 0.3788 0.3753 0.4213 0.4216 0.3472 0.2957 0.2953 0.2741 0.2831 0.261 0.2585 0.2382 0.2277 0.2226 0.1856 0.2076 0.183 0.1221 0.1049 0.0891 0.0005 0.1106 0.073 0.0738 0.0877 0.0654 0.0481 0.0462 0.0527 0.0425 0.0732 0.0359 0.104 0.0905 SEC (ppm) 0.0189 0.0182 0.0275 0.0266 0.0225 0.0703 0.0762 0.0827 0.0838 0.0808 0.0817 0.0799 0.0287 0.0255 0.0283 0.0246 0.0251 0.0268 0.0281 0.0325 0.031 0.0331 0.027 0.0437 0.0292 0.0371 0.0286 0.0983 0.0899 0.0978 0.0954 0.1013 0.0955 0.0942 0.0982 0.0973 0.0895 0.0868 0.0886 0.0994 0.0749 0.0827 0.0848 0.0883 0.0747 0.0839 0.0863 0.0803 0.0817 0.0806 0.0875 0.0895 0.0739 0.0794 0.0825 0.0826 0.0846 0.0744 0.0757 0.0751 0.0691 0.0759 0.0866 0.0788 0.0786 0.0878 0.0802 0.0778 0.0889 0.0861 0.0976 0.0901 0.1006 0.1038 0.1174 0.0935 0.0999 0.1068 0.1701 0.1181 0.1163 0.116 0.1014 0.1171 0.1189 0.1214 0.1275 0.1069 0.1183 0.1208 0.1118 0.1074 FM U, % #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 277.9% 240.4% 207.5% 426.5% 179.2% 281.2% 406.6% 195.9% #DIV/0! #DIV/0! #DIV/0! 308.0% #DIV/0! 11.9% 13.8% 12.3% 15.2% 11.1% 19.5% 12.6% 18.1% 12.0% 6.9% 6.4% 7.1% 7.1% 7.7% 7.6% 7.4% 7.8% 8.3% 7.5% 7.8% 8.1% 9.2% 7.1% 9.7% 12.3% 15.6% 14.7% 18.6% 20.4% 22.8% 23.2% 23.7% 27.1% 27.9% 26.9% 29.7% 35.3% 31.2% 37.1% 31.8% 40.0% 40.0% 32.8% 36.0% 49.9% 53.3% 53.2% 64.1% 56.7% 59.6% 68.8% 72.3% 85.7% 81.0% 108.4% 100.0% 128.3% 153.2% 190.5% 239.7% 68040.0% 213.6% 318.6% 314.4% 231.2% 358.1% 494.4% 525.5% 483.9% 503.1% 323.2% 673.0% 215.0% 237.3% ethylFOSE (ppm) 0 0 0 0 0.0002 0 0 0 0 0.0001 0 0 0 0 0 0 0 0 0.0017 0.0015 0.0016 0.0015 0.0016 0.0016 0.0016 0.0018 0.0017 0 0 0.0001 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 SEC (ppm) 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0004 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 FM U, % M oisture (ppm) 0 0 0 0 0.0001 0.0069 0.0025 0.0018 0.0014 0.0012 0.0012 0.0011 0 0.0001 0 0 0 0 0.0153 0.0152 0.015 0.0148 0.0147 0.0145 0.0144 0.0143 0.0143 0.2939 0.2907 0.2882 0.2854 0.2843 0.2824 0.2794 0.2782 0.2764 0.2726 0.2722 0.2702 0.2715 0.2714 0.2776 0.2942 0.2975 0.2958 0.3116 0.3119 0.3137 0.317 0.3141 0.3172 0.3175 0.3151 0.3168 0.315 0.3147 0.3163 0.3157 0.3176 0.317 0.3174 0.3129 0.3132 0.3156 0.3142 0.3154 0.3134 0.3139 0.3108 0.3088 0.3113 0.3117 0.3142 0.3142 0.3161 0.3146 0.3156 0.3153 0.3154 0.3144 0.3149 0.316 0.3147 0.314 0.3162 0.3158 0.3153 0.3159 0.3161 0.3168 0.3164 0.316 SEC (ppm) 0 0 0 0 0 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0 0 0 0 0 0 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.0011 0.001 0.001 0.0011 0.001 0.001 0.0011 0.0011 0.0011 0.0011 0.0011 0.001 0.001 0.001 0.0011 0.0011 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.0009 0.001 0.0009 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 Press (atm) 0.9689 0.9698 0.9677 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9698 0.9694 0.9698 0.9698 0.9702 0.9698 1.0195 1.0195 1.0195 1.0195 1.0171 1.0195 1.0199 1.0195 1.0199 0.9698 0.9698 0.9685 0.9706 0.9706 0.9702 0.971 0.9706 0.9706 0.9706 0.9677 0.971 0.971 0.971 0.971 0.9706 0.9706 0.9706 0.971 0.9706 0.971 0.971 0.9706 0.971 0.9706 0.9706 0.971 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.971 0.971 0.971 0.971 0.971 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.971 0.9685 Temp (C) 21.5453 21.5453 21.7026 21.5453 21.5453 21.5453 21.6239 21.5453 21.5453 21.5453 21.4667 21.5453 21.4667 21.4667 21.4667 21.5453 21.4667 21.5453 21.5453 21.4667 21.6239 21.7026 21.4667 21.7026 21.4667 21.7026 21.6239 21.7026 21.4667 21.4667 21.4667 21.6239 21.6239 21.7026 21.7026 21.5453 21.7026 21.5453 21.7026 21.6239 21.7026 21.6239 21.7812 21.6239 21.7812 21.5453 21.7026 21.7026 21.7026 21.6239 21.7026 21.6239 21.7026 21.7026 21.7026 21.7026 21.8598 21.7026 21.7026 21.9385 21.7026 21.7026 21.8598 21.8598 21.7026 21.9385 21.7026 21.8598 21.9385 21.8598 21.8598 21.7812 21.8598 21.7812 21.9385 21.8598 21.9385 21.8598 21.9385 21.8598 21.9385 21.9385 21.8598 21.8598 21.8598 21.8598 21.8598 21.8598 21.9385 21.8598 21.8598 21.9385 E13-0880 Final Analytical Report, Appendix-A 13:44:29 13:49:30 13:54:31 13:59:32 14:04:36 14:09:37 14:14:38 14:19:39 14:24:40 14:29:41 14:34:42 14:39:43 14:44:44 14:49:45 14:54:46 14:59:47 15:04:48 15:09:49 15:14:50 15:19:51 15:35:16 15:36:11 15:36:47 15:37:22 15:37:58 15:38:34 15:39:10 15:44:24 15:45:00 15:45:36 15:46:12 15:46:48 15:47:24 15:48:00 15:48:36 15:49:12 15:49:48 15:50:24 15:51:00 15:51:36 15:55:00 15:55:36 15:56:12 15:56:48 15:57:24 15:58:00 16:00:50 16:01:59 16:02:35 16:03:11 16:03:47 16:04:23 16:04:59 16:05:35 16:06:11 16:06:47 U0000093 U0000094 U0000095 U0000096 U0000097 U0000098 U0000099 U0000100 U0000101 U0000102 U0000103 U0000104 U0000105 U0000106 U0000107 U0000108 U0000109 U0000110 U0000111 U0000112 U0000113 U0000114 U0000115 U0000116 U0000117 U0000118 U0000119 U0000120 U0000121 U0000122 U0000123 U0000124 U0000125 U0000126 U0000127 U0000128 U0000129 U0000130 U0000131 U0000132 U0000133 U0000134 U0000135 U0000136 U0000137 U0000138 U0000139 U0000140 U0000141 U0000142 U0000143 U0000144 U0000145 U0000146 U0000147 U0000148 4.0323 4.1195 4.184 4.1938 4.6446 4.9885 5.1158 5.3908 5.4873 6.0468 6.7935 7.0278 7.5309 8.0732 8.3954 8.5224 9.2226 9.5705 10.1112 10.5619 0 0.0007 0 0.0092 0.0033 0.0008 0.0152 7.7074 5.7211 3.4022 0.7415 0.2044 0.1227 0.1005 0.099 0.0757 0.0839 0.069 0.0715 0.0635 0.0734 0.061 0.0426 0.0431 0.0433 0.0362 0.1204 0.0852 0.0633 0.051 0.0686 0.0535 0.0465 0.0511 0.0555 0.0567 0.0442 0.0442 0.0447 0.0443 0.0454 0.0462 0.0464 0.0474 0.0478 0.0494 0.0522 0.0532 0.0545 0.056 0.0569 0.0572 0.0603 0.0617 0.0639 0.0654 0.0067 0.0064 0.007 0.0067 0.0065 0.0066 0.0065 0.0481 0.0363 0.0247 0.0086 0.007 0.0065 0.0068 0.0069 0.0069 0.0065 0.0068 0.0068 0.0069 0.0064 0.0066 0.0067 0.0068 0.0068 0.0068 0.0278 0.0281 0.0281 0.0276 0.0276 0.0279 0.0278 0.0279 0.0277 0.0279 2.2% 2.1% 2.1% 2.1% 2.0% 1.9% 1.8% 1.8% 1.7% 1.6% 1.5% 1.5% 1.4% 1.4% 1.4% 1.3% 1.3% 1.3% 1.3% 1.2% #DIV/0! 1828.6% #DIV/0! 145.7% 393.9% 1650.0% 85.5% 1.2% 1.3% 1.5% 2.3% 6.8% 10.6% 13.5% 13.9% 18.2% 15.5% 19.7% 19.0% 21.7% 17.4% 21.6% 31.5% 31.6% 31.4% 37.6% 46.2% 66.0% 88.8% 108.2% 80.5% 104.3% 119.6% 109.2% 99.8% 98.4% 2.2645 2.2496 2.2656 2.2277 2.2188 2.2294 2.2494 2.2397 2.2373 2.2423 2.2364 2.2683 2.2512 2.2209 2.2307 2.2297 2.2718 2.2446 2.2396 2.2299 0.0052 0.0299 0.0139 0.0106 0.0115 0.0217 0.0077 2.0068 1.9319 1.8213 1.7723 1.7792 1.7548 1.7768 1.7745 1.7631 1.7674 1.768 1.7646 1.7872 0.1995 0.0459 0.0156 0.0059 0.0059 0 0 0 0 0 0 0 0 0 0 0 0.1069 0.1088 0.1074 0.1064 0.1056 0.1056 0.1061 0.1056 0.1052 0.1064 0.1064 0.1063 0.1037 0.1053 0.1056 0.1043 0.1053 0.1056 0.1055 0.1048 0.0118 0.0109 0.0119 0.0124 0.0115 0.0125 0.0115 0.0735 0.051 0.0325 0.0262 0.0259 0.0266 0.0265 0.0266 0.0264 0.0263 0.0271 0.0275 0.0263 0.0115 0.0122 0.0117 0.0117 0.0121 0.0114 0.0108 0.0124 0.0113 0.0117 0.0124 0.0118 0.012 0.0122 0.0123 0.0121 9.4% 9.7% 9.5% 9.6% 9.5% 9.5% 9.4% 9.4% 9.4% 9.5% 9.5% 9.4% 9.2% 9.5% 9.5% 9.4% 9.3% 9.4% 9.4% 9.4% 453.8% 72.9% 171.2% 234.0% 200.0% 115.2% 298.7% 7.3% 5.3% 3.6% 3.0% 2.9% 3.0% 3.0% 3.0% 3.0% 3.0% 3.1% 3.1% 2.9% 11.5% 53.2% 150.0% 396.6% 410.2% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0017 0.0126 0 0.0182 0.0378 0.0198 0 0 0 0 0 0 0 0 0 20.3142 20.1975 20.2208 20.2746 20.2774 20.2353 20.3048 20.2923 20.213 20.2487 0.0862 0.086 0.0862 0.0855 0.0871 0.0882 0.0889 0.0893 0.0905 0.092 0.0972 0.0996 0.1012 0.1038 0.1055 0.1062 0.1115 0.115 0.1187 0.8278 0.0165 0.0165 0.017 0.0171 0.0163 0.0166 0.0162 0.0861 0.0648 0.0447 0.0631 0.0235 0.0191 0.0181 0.0181 0.0178 0.0173 0.0174 0.0181 0.0169 0.0168 0.0176 0.0172 0.0175 0.0168 0.0172 0.0888 0.0893 0.0894 0.0878 0.0875 0.0885 0.0884 0.0883 0.0879 0.0884 #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 2764.7% 303.2% #DIV/0! 198.9% 94.2% 174.7% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 0.9% 0.9% 0.9% 0.9% 0.9% 0.9% 0.9% 0.9% 0.9% 0.9% 1.8679 1.8936 1.87 1.8574 1.9247 1.8988 1.8917 1.9278 1.9094 1.9452 1.9174 1.9146 1.9729 1.9332 1.9488 1.9613 1.9707 1.9694 1.9289 1.9123 0 0 0 0.0054 0.0003 0 0 1.9121 1.8797 1.7688 1.8058 1.8549 1.8702 1.8807 1.9062 1.852 1.8821 1.8733 1.8509 1.9265 0.1794 0.0452 0.0287 0.0002 0.021 0.005 0.0021 0 0 0.0426 0.0409 0.0169 0.0263 0.0067 0.0185 0.0159 0.1428 0.144 0.1435 0.1414 0.1413 0.1434 0.1433 0.1436 0.1447 0.1429 0.1435 0.1438 0.1411 0.1423 0.1438 0.1439 0.1435 0.1423 0.1444 0.1434 0.0184 0.019 0.0177 0.018 0.0192 0.0181 0.0192 0.1177 0.0988 0.0824 0.0625 0.0437 0.0398 0.0393 0.0377 0.0365 0.0362 0.0368 0.038 0.0363 0.0198 0.0177 0.0179 0.0173 0.0186 0.0177 0.0423 0.0388 0.038 0.0375 0.0363 0.0371 0.0373 0.0378 0.0376 0.0371 15.3% 15.2% 15.3% 15.2% 14.7% 15.1% 15.2% 14.9% 15.2% 14.7% 15.0% 15.0% 14.3% 14.7% 14.8% 14.7% 14.6% 14.5% 15.0% 15.0% #DIV/0! #DIV/0! #DIV/0! 666.7% 12800.0% #DIV/0! #DIV/0! 12.3% 10.5% 9.3% 6.9% 4.7% 4.3% 4.2% 4.0% 3.9% 3.8% 3.9% 4.1% 3.8% 22.1% 78.3% 124.7% 17300.0% 177.1% 708.0% 4028.6% #DIV/0! #DIV/0! 176.1% 177.5% 439.1% 283.7% 1128.4% 406.5% 466.7% 0.0795 0.0919 0.1399 0.0966 0.0425 0.0273 0.0117 0.0146 0.0572 0 0 0 0 0 0 0 0 0 0 0 0 0.0136 0 0.0296 0 0.042 0.017 0 0 0 0 0 0 0 0 0 0 0 0 0 0.038 0 0 0.0135 0.0296 0.0222 0.0449 0.0499 0.0893 0.0698 0.0603 0.0647 0.0998 0.0122 0.0842 0.0643 0.1112 0.107 0.1143 0.1128 0.1121 0.1171 0.1835 0.1987 0.1263 0.1334 0.1407 0.1432 0.1536 0.155 0.1629 0.1685 0.1743 0.1887 0.1902 0.2068 0.0285 0.0328 0.0216 0.0268 0.041 0.0262 0.028 0.1537 0.1053 0.0733 0.0365 0.0279 0.0256 0.0254 0.0262 0.0265 0.0272 0.0304 0.0283 0.0301 0.024 0.0238 0.0259 0.0318 0.0288 0.0258 0.0855 0.0788 0.0833 0.0782 0.0842 0.082 0.0803 0.09 0.0819 0.0817 279.7% 232.9% 163.4% 233.5% 527.5% 857.9% 3136.8% 2721.9% 441.6% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 482.4% #DIV/0! 181.1% #DIV/0! 124.8% 329.4% #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! 126.3% #DIV/0! #DIV/0! 471.1% 194.6% 232.4% 380.8% 315.8% 186.6% 224.1% 279.3% 253.5% 160.9% 1475.4% 194.5% 254.1% 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.0002 0.0001 0 0.0001 0 0 0 0.0001 0.0003 0.0003 0.0003 0.0002 0 0.0001 0 0.0003 0 0.0001 0.0002 0.0001 0.0002 0.0001 0.0001 0 0 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0005 0.0006 0.0006 0.0006 0.0006 0.0006 0.0006 0.0006 0.0006 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0004 0.0003 0.0002 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.0002 0.315 0.316 0.3143 0.3134 0.3161 0.3134 0.316 0.3163 0.3167 0.3176 0.3179 0.3185 0.3158 0.3163 0.3154 0.3146 0.3183 0.3164 0.3152 0.3168 0.0006 0.0008 0.0007 0.0007 0.0007 0.0007 0.0006 0.2445 0.1514 0.0686 0.0138 0.0019 0.0007 0.0005 0.0004 0.0003 0.0003 0.0003 0.0004 0.0003 0.0006 0.0005 0.0005 0.0005 0.0005 0.0004 0.0023 0.0015 0.0014 0.0014 0.0013 0.0012 0.0012 0.0011 0.0011 0.0011 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.0009 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0 0 0 0 0 0 0 0.0008 0.0009 0.0006 0.0002 0.0001 0.0001 0.0001 0.0001 0.0001 0.0002 0.0002 0.0002 0.0002 0.0001 0 0 0 0 0 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.0001 0.971 0.9706 0.971 0.971 0.9706 0.9706 0.971 0.971 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.9706 0.971 0.9685 0.9706 0.9706 0.9698 0.9706 0.971 0.971 0.9706 0.9706 0.9714 0.9689 0.9706 0.9718 0.9706 0.9677 0.9722 0.971 0.971 0.971 0.971 0.9706 0.971 0.9706 0.9706 0.9706 0.9706 0.9685 0.971 0.9706 0.9706 0.9706 0.9706 0.971 0.9706 0.9706 0.971 0.9706 0.9706 0.971 0.9698 21.8598 21.9385 21.9385 21.7026 21.8598 21.8598 21.8598 21.8598 21.8598 21.8598 21.7026 21.8598 21.8598 21.8598 21.8598 21.9385 21.8598 21.8598 21.8598 21.9385 22.0957 22.0171 22.0171 22.0957 22.0957 21.9385 22.0171 22.0957 21.8598 22.0171 21.9385 22.0171 21.9385 22.0171 22.0171 22.0171 22.0171 21.8598 21.8598 21.9385 21.7812 21.8598 21.8598 21.7026 21.7812 21.8598 21.8598 21.9385 21.8598 21.8598 21.8598 21.8598 21.9385 21.8598 21.2308 21.7026 E13-0880 Final Analytical Report, Appendix-A M anual Validation 2/4/2014 By: JSE Trial 1 2 1 2 3 1 2 3 1 2 3 Compound Ammonia Ammonia CO CO CO Methane Methane Methane Methanol Methanol Methanol Ref Spectrum NH3_12 NH3_12 113CO 113CO 113CO AIHZME AIHZME AIHZME MEOHZ9A MEOHZ9A MEOHZ9A Conc, ppm-m 52.6 52.6 112.7 112.7 112.7 100 100 100 22.5 22.5 22.5 Region 800-980 800-980 2124-2160 2124-2160 2124-2160 2900-3035 2900-3035 2900-3035 960-1085 960-1085 960-1085 Samp Spectrum U80 U80 U80 U80 U30 U80 U80 U30 U40 U40 U47 SF PL, m AQ value, ppmV 2.52 24.18 4.71 2.48 24.18 4.71 0.44 24.18 2.22 0.47 24.18 2.22 0.13 24.18 0.9 0.46 24.18 1.91 0.46 24.18 1.91 0.2 24.18 0.93 2.05 24.18 1.96 2.08 24.18 1.96 0.85 24.18 0.84 Gramsvalue, ppmV 5.48 5.39 2.05 2.19 0.60 1.90 1.90 0.83 1.91 1.94 0.79 % recovery 116.4% 114.5% 92.4% 98.7% 66.7% 99.6% 99.6% 88.9% 97.3% 98.7% 94.2% Ammonia LOQ = 0.30 ppmV based upon the FMU of 30% and a manual review of spectrum 54. CO LOQ = 0.90 ppmV based upon FMU of 17 % on spectrum 30 and manual subtraction: matrix interference Methane LOQ = 0.9 ppmV based upon FMU of 28% on spectrum 30 and manual subtraction Methanol LOQ = 0.5 ppmV based upon FMU of 30% on spectrum 54 and manual subtraction SEC = Sample Error Concentration calculated by AutoQuant software FMU = Fractional Model Uncertainty FMU = (2x SEC)/predicted value The lower the SEC thus FMU the better the predictive model is performing LOQ is based upon manual spectral interpretation and factoring in the FMU values The FMU calculation evaluates the predictive model performance on a real sample matrix per compound Primary model performance factors are FTIR instrument condition, quality of reference spectra, matrix interference, and spectral regions chosen in method E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Figure __ Sample System Schematic Rotometer Generator OVS Sampling OVS Sampling Exposure Chamber Air Cylinder Typical FTIR Exh. to Vent Hood Page 13 of 13 E13-0880 Final Analytical Report, Appendix-A 9 Hand Written Notes 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Page 10 of 13 E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A 10 Chain of Custody Forms 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Page 11 of 13 E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A E13-0880 Final Analytical Report, Appendix-A 11 General Project Outline (GPO) 3M ENVIRONMENTAL LABORATORY PROJECT NO. E13-0880 Page 12 of 13 E13-0880 Final Analytical Report, Appendix-A 3 Field Analytical Services & Technologies / General Project Outline To: cc: From: Date: Subject: Sue Chang - 3M Toxicology Paul Lieder - 3M Toxicology Jill Hart - 3M Toxicology Kris Murphy - Pace Analytical Services Cleston Lange - 3M EHS Operations, Environmental Laboratory 260-5N-17 Jess Eldridge - 3M EHS Operations, Environmental Laboratory 260-5N-17 Brian Mader - 3M EHS Operations, Environmental Laboratory 260-5N-17 Dec 6, 2013 3M B270 ethyl-FOSE Rat Exposure Chamber Test Department No. 108022 Lab Request No. E13-0880 Test Date(s) Dec 9, 2013 Monitoring Requested by: Sue Chang 3M Toxicology 3M Center, Building 220-6W-08 St. Paul, MN 55144 Email: s.chang@mmm.com Phone No: 651-737-9073 Monitoring Coordinated by: Brian Mader, Ph.D. 3M EHS Opns Environmental Laboratory 3M Center, Building 260-5N-17 St. Paul, MN 55144 E-mail:bmader@mmm.com Phone No.: (651) 733-9866 Fax: (651) 778-6176 All verbal and written correspondence will be directed to the Monitoring Coordinator. Revision No. 0 3 Confidential E13-0880 Page 1 of 5 E13-0880 Final Analytical Report, Appendix-A Plant Location / Contact(s) 3M Center Building 270 Room SB322/324 St. Paul, MN 55144 3M Company B270-2A-8 Plant Contact: Jill Hart Phone Number: 651-733-8586 Project Objective The purpose of this testing is to support 3M Strategic Toxicology exposure study and perform FTIR and OVS-based measurements of the concentration of the target compound ethyl-FOSE generated from a generator cartridge and in the exhaust of an exposure chamber during a rat exposure chamber test. The goal of the test is to measure the gas-phase concentration of ethyl-FOSE. The test will be done at the 3M Strategic toxicology lab at SB322/324 located on the third floor of B270. The initial target concentration for the ethyl-FOSE is approximately 5-10 ppbV for a 6 hour rat exposure. The material will be introduced into the chamber via a generator tube containing ~ 65 gm of glass beads coated with ~ 700 mg of ethyl-FOSE and flowing 2 lpm air through the tube. In addition to FTIR, samples will be collected on OVS adsorbant sample tubes for analysis in the 3M Env Lab via HPLC/MS. If other compounds are present as detected by the FTIR, they will be analyzed and reported. Project Schedule December 6th, 2013 December 9th, 2013 December 10th, 2013 December 11-13th, 2013 December 20th, 2013 January 6th, 2014 Equipment Preparation, Set-up Begin Monitoring Replicate tests(if needed), demobilization Analysis of Samples Preliminary Data needed. Final Report Due Process(es) Requiring Testing Exposure chamber air sampled inline on the new "flow through" system. Test Conditions and Locations Condition 1: Quality control - no test chemicals nor animals (1) Breathing Air Background - cylinder a. Prior to and after the toxicity test take a 5 minute OVS tube sample of the cylinder breathing air; flow set at 1 lpm for each sample. The pressure of the cylinder will drive the sampling - no pump will be used. Condition 2: Steady-State Chamber Testing (1) Chamber Test a. Collect samples continuously with the FTIR during the testing with target chemical present. Revision No. 0 3 Confidential E13-0880 Page 2 of 5 E13-0880 Final Analytical Report, Appendix-A b. Two locations will be sampled with OVS tubes ; immediately downstream of the generator tube and immediately downstream of the test chamber(s). c. During the 6 hour run time, six 60 min samples will be collected contiguously at both locations. There will be several minutes between removing one set of samples and re-setting new tubes in place for the next one hour period. d. Sample rates through the OVS tubes will be set to approximately 0.1 lpm; measured and set on each pump. The actual flow rates and samples volume will be documented. Gas Stream Characteristics Experiments will be conducted with ethyl-FOSE as the target compound. Other compounds may be present as well and will be analyzed and identified on-site. Based on the preliminary generator cartridge monitoring performed under lab request E13-0722 the expected concentration will be in the range of 5-10 ppbV. Table 1. ethyl-FOSE Standard Information Test Methods + OVS Analysis by LC/MS ETS-8-105.0 Analysis of the Ethyl FOSE concentration will be conducted at the 3M Environmental Lab using the appropriate 3M Env. Lab SOP. The analysis will include analysis of blanks as well as the use of multipoint calibrations curves and QA/QC procedures that may include LCS and LMS spikes. The target compound is ethyl-FOSE but the presence of other compounds will be reported as will the relative distribution of branched versus liner materials present in the OVS samples. The MS/MS ion masses monitored are for EtFOSE-OH acetate adduct, and is 630 > 59 (acetate adduct) +EPA Method 320 modified for speciated FTIR analysis PQL 2 Quantitative Monitoring Project Quality Level 2 (PQL 2) is appropriate for emission factor estimates and noncompliance test measurements. PQL 2 is appropriate when the project objectives specify the data will not be incorporated in compliance tests of manufacturing emissions, but can be used for use in certain environmental permitting and regulatory activities such as emission factor estimation. Revision No. 0 3 Confidential E13-0880 Page 3 of 5 E13-0880 Final Analytical Report, Appendix-A As per SOP ETS-8-31 the project quality level (PQL) for this project has been identified as PQL 2 with the following project specific goals to be met: + Selection and preparation of the relevant equipment, supplies and spectral libraries. - Midac Fourier Transform Infrared Spectrometer (FTIR), heated sample cell, nonIntrinsically Safe (non-IS) heated sample lines, and rotary vane or diaphragm pumps for sample ports. - EPA, MIDAC and 3M library standards. etc + Use of quantitative FTIR spectral libraries and methods provided by the 3M Environmental Lab with a documented concentration. For each compound the series of reference spectra should span the range of ppmV-m values expected to be observed during the testing. + Pre-test calculations and documentation: - Estimated absorption path-length. - Determination of the detector linearity as per SOP ETS-8-031. - FTIR maintenance as per SOP ETS-9-58 + Testing procedures and documentation: + As per SOP ETS-8-031 including but not limited to: + Direct and system calibration with calibration transfer standard (CTS). + Desired Analytical Uncertainty (AU) value = 50% + Direct and system calibration with calibration transfer standard (CTS). + Potential Interferents: - Water - Carbon Dioxide + Data Analysis: - The concentration determinations using AutoQuant 4.0 CLS analytical program and/or MD Grams. + Reporting: - Comprehensive report (See Reporting Requirements section) Estimated Project Cost All managed outsourced testing expense for this project will be charged to the department number identified on page one of the GPO. Estimated Total Project Cost ~ $3,000 - $5,000 Actual project costs are determined on a time and materials basis in accordance with the existing 3M Environmental Laboratory contract. Reporting Requirements Type of report(s) required: + On-site results will be reported to the Project Requestor as requested during the project + Final Reports - The "Comprehensive Final" report due to the 3M Project Requestor 4 weeks from the test date. Supplemental Information Revision No. 0 3 Confidential E13-0880 Page 4 of 5 E13-0880 Final Analytical Report, Appendix-A + 3M facility personnel must provide: - One dedicated 20-amp, 110-120 VAC electrical power circuit (reachable with extension cords) at the test location. - Designated representatives - Daily work permits as necessary. + 3M facility must identify proper PPE and if necessary the type of full face respirator that is to be worn. + 3M facility must verify non-intrinsically safe equipment is acceptable at the test locations. + 3M facility must ensure that the test conditions are maintained during the test and properly documented. + 3M facility must provide OSHA approved safe access to test locations. + 3M facility must install all test ports that will be needed prior to the test. + Perform all process operations and attempt to maintain consistent operating parameters throughout the testing time frame including pressures, temperature, etc. Contract Lab Requirements: + Contract technicians must follow all applicable safety protocols while on-site at the 3M facility (see plant safety officer for appropriate safety procedures). + Invoicing must be sent to monitoring coordinator including; - Invoice Date - Project Description (Must be similar to the description found on the 3M Lab Request) - Test Date(s) - 3M 6 Digit Department No. - 3M Site Source No. (If a site source has been assigned it will be found on the 3M Lab Request) - 3M Project No. (If a project number has been assigned it will be found on the 3M Lab Request) - 3M Lab Request No. - Cost Itemization Revision No. 0 3 Confidential E13-0880 Page 5 of 5