Document GKYYz1Q6gGeEG0R8dz0MGabJm

3M Environmental Technology and Services PO Box 33331 St. Paul, MN 55133-3331 6 12 778 6442 Sponsor: 3M Toxicology Services Building 220-23-2 3M Center St. Paul, MN 55144- BACK TO MAIN FINAL REPORT - ANALYTICAL STUDY Study Title: Covance Laboratories ContamhationTesting Performing Laboratory: 3M Environmental Technology and Safety Services 3M ENVIRONMENTAL, LABORATORY Field Analytical Technologies 935 Bush Avenue St. Paul, MN 55106 ET & SS Study NO:FS-980618-1 Initiation Date: June 29, 1998 3M Laboratory Request No: U1927 I 1 3M ENVIRONMENTAL LABORATORY ~ BACK TO MAIN ET & SS STUDY NO: FS-980618-1 CONTENTS 1.0 SUMMARY....................................................................................................................................... 4 2.0 INTRODUCTION............................................................................................................................ 5 2.1 STUDYTITLE................................................................................................. . ................ 5 2.2 PURPOSE......................................................................................................................................... 5 2.3 REGULATORYCOMPLIANCE................................................................................................... 5 2.4 QUALITYASSURANCE................................................................................................................ 5 2.5 SUMMARYOFTESTRESULTS.................................................................................................. 5 Table 2.0-1: Summary of Room Test Results .................................................................................... 6 3.0 MATERIALS.................................................................................................................................... 7 3.1 TEST. CONTROL.AND REFERENCESUBSTANCES............................................................. 7 3.2 SOURCEOF MATERIALS............................................................................................................ 7 4.0 EXPERIMENTAL.OVERVIEW.................................................................................................. 8 4.1 TESTPROGRAM............................................................................................................................ 8 Table 4.0-1: Summary of Adsorbent Tube and Filter Sampling-June 29. 1998............................. 9 Table 4.0-2: Summary of Adsorbent Tube and Filter Sampling-June 30. 1998............................. 9 Table 4.0-3: Summary of Tissue Wipe Sampling- June 29. 1998................................................. 10 Table 4.0-4: Summary of Tissue Wipe Sampling-June 30, 1998................................................. 11 4.2 RESULTS........................................................................................................................................ 11 Table 4.0-5: Summaryof FTIR Results -June 29. 1998................................................................. 12 4.3 PROCESSDESCRIPTION........................................................................................................... 13 Figure 4.0- 1: Room 349 Schematic and Sampling Locations -June 29. 1998................................ 13 Figure 4.0-2: Room 349 Schematic and Sampling Locations -June 30. 1998................................ 13 Figure 4.0-3: Room 3004 Schematic and Sampling Locations - June 29. 1998.............................. 14 Figure 4.0-4: Room 3004 Schematic and SamplingLocations- June 30. 1998.............................. 14 Figure 4.0-5: Room 3045 Schematic and Sampling Locations - June 29. 1998.............................. 15 Figure 4.0-6: Room 3045 Schematic and Sampling Locations -June 30. 1998.............................. 15 5.0 EXPERIMENTAL.METHODS.................................................................................................. 16 Table 5.0- 1: Summary of Sampling Procedures.............................................................................. 16 5.1 FAST GC-ION MOBILITY SPECTROMETRY....................................................................... -17 Figure 5.0-1:Fast GC-Ion Mobility SpectrometryMonitor............................................................. 17 5.2 FOURIER TRANSFORM INFRARED SPECTROSCOPY.EPA METHOD320................18 Figure 5.0-2: Extractive FTIR Schematic ........................................................................................ 19 5.3 MSUEMTMHOADCTAON1I4ST...E...R...S...G...A...S....C...H...R....O...M.....A...T...O...G....R...A....P..H....Y...W.....S..S...S...P..E...C...T...R...O...M....E...T...R...Y.... ....E...P..A. 20 Revision 0 2 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 CONTENTS 5.4 SSOPERCBTERNOTMTUEBTERSY,.F...I.L...T...E...R....S..,..W.....I.P...E...S...,..A...N...D....W.....A...T...E...R....S...A...M.....P..L...E...S...E...L...E...C....T...R...O...S...P...R...AY MAS2S0 6.0 DATA ANALYSIS.......................................................................................................................... 21 7.0 CONCLUSION................................................................................................- :............... 22 8.0 MAINTENANCEOF RAW DATA AND RECORDS................................................................ 23 9.0 APPENDICES ................................................................................................................................ 24 9.1 Protocoland Amendments........................................................................................................... A 9.2 Signed Reports fiom Individual Scientists.................................................................................. B 9.3 Key Personnel Involved in the Study .......................................................................................... C 9.4 Materialsand Equipment............................................................................................................ .D 9.5 Field Data .................................................................................................................................... E 9.6 Field Data Printouts..................................................................................................................... F 9.7 AutoQuant CLS Method.............................................................................................................. G 9.8 Chains of Custody ....................................................................................................................... H Revision 0 3 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 1.0 SUMMARY SUMMARY STUDY IDENTIFICATION Covance Laboratories Contamination Testing 3M ET&SS Study Number: Test Substance: FS-980618-1 - NA Sponsor: 3M Toxicology Services Building 220-2E-2 3M Center St. Paul, MN 55144 Sponsor's Representative: Andrew Seacat 3M Toxicology Services Building 220-2E-2 3M Center St. Paul, MN 55144 Study Director: James T. Wolter 3M Field Analytical Technologies Group 935 Bush Avenue Building 2-3E-09 St. Paul, MN 55106 Test Site: Covance Laboratories 3301 Kingsman Blvd. Madison, WI 53704 Contract Laboratory: Pace Analytical Services, Inc. 1700 Elm Street, Suite 200 Minneapolis, MN 55414 Proposed Study Timetable Experimental Start Date: June 29,1998 Experimental Completion Date: June 30,1998 Draft Report Date: September 9, 1998 Revision 0 4 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDYNO: FS-980618-1 2.0 INTRODUCTION INTRODUCTION 2.1 Study Title Covance Laboratories Contamination Testing - 2.2 Purpose Covance Laboratories has been contractedby 3M to conduct toxicological studies of nmethyl FOSE alcohol, n-ethyl FOSE alcohol, and potassium perfluorooctanesulfonate on rats. Recent results have indicated trace amounts of n-ethyl FOSE metabolites are present in the liver and blood of the control rats used in these studies. It has been speculated that the control rats are being exposed to one or more of these test compounds through the air, either as a particulate or gas. The objective of this study was to investigate potential contamination sources within the study housing area of these studies. 2.3 Regulatory Compliance The testing was not performed for compliance purposes. Testing was requested by John Butenhoff of 3M Toxicology Services for use as internal 3M confidential information only. 2.4 Quality Assurance The protocol and study conduct were reviewed by the quality assurance unit in accordance with 3M Environmental Technology and Safety Services (ET & SS) standard operating procedures and policies. 2.5 Summary of Test Results In air samples taken from Room 3045, EtFOSE-OH was detected by high performance liquid chromatography (HPLC)/electrospray mass spectrometry (ESMS) at levels below the practical quantitation limit (approximately 0.17 p p b k ) but above the method detection limit (approximately 0.02 ppb/L). PFOS was not detected at levels above the blanks in any room. Analysis of wipes from the backs of rats in Room 3045 contained a measurable amount of EtFOSE-OH; wipes from rats in other rooms did not. Due to variations in sampling technique, wipe samples were not quantifiable. Wipes from animal backs were not analyzed for PFOS. Revision 0 5 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 i INTRODUCTION I The Fourier transform infrared (FTIR) test results for the target analytes were below ri 'I the detection limit of the instrumentation(approximately 100 ppb). Fluorochemical compounds were not detected. Ammonia was the only detectable compound within the FTIR spectra other than carbon dioxide and water. The ammonia results are presented in the following table along with the American Cderence of '\ Governmental Industrial Hygienists (ACGIH) Threshold Limit Value (TLV) time- weighted average (TWA) concentration for an 8-hour workday. ! I Table 2.0-1: Summary of Room Test Results Source Constituent Room 349 Ammonia .',J Room 3004 Ammonia .! Room 3045 Ammonia Sampling Method FTIR FTlR FTIR Average Concentration -ACGIH TLV: TWA 8 Hr Work Day 1.60 ppm 25 PPm 7.1 7 ppm 8.26 ppm 25 PPm 25 PPm Revision 0 6 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 I 3.0 MATERIALS i MATERIALS 3.1 Test, Control, and Reference Substances The test and control materials are not applicable to this study. The reference materials were ethylene, nitrogen, alcohol for FTIR monitoring. n-methyl FOSE alcohol an-d n-ethyl FOSE 3.2 Source of Materials The reference materials were as follows: n-methyl FOSE alcohol - Lot 648 n-ethyl FOSE alcohol - TN-A-1884 61691-16 1 Certified gases provided by Oxygen Services Co., Inc.: ', I , .. nominal 20 ppmv ethylene in nitrogen zero grade nitrogen Revision 0 7 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 4.0 EXPERIMENTAL - OVERVIEW EXPERIMENTAL - OVERVIEW 4.1 Test Program Extractive and local open path (LOPIR) FTIR spectroscopy as well as fast gas chromatography (GC)-ion mobility spectrometry (IMS) were used to verify or refute the presence of fluorinated compounds at ppbv levels itl the dietary study housing air at Covance Laboratories. Additionally, silica gel tubes, charcoal tubes and glass fiber filters were used to screen for the presence of the test compounds in the study housing air. It was anticipated that any test compounds present as airborne particulates or adsorbed onto airborne particulates were trapped by both the filters and sorbent tubes. Samples were taken from each room of the rat drinking water for electrospray mass spectrometry (ESMS) analysis. Wipes of the rat cages were taken for extraction and analysis. 6-liter SUMMA passivated canister samples were obtained from each room for analysis by cryofocus GCMS. Three separate studies are currently being conducted for 3M Toxicology at Covance Laboratories, one for each test compound. The control and dosed rats for a given study are housed in the same room, while there are separate rat housing rooms for each study. All three rooms were investigated with the stated techniques on both Monday, June 29 and Tuesday, June 30. Monday was a change-out day for the rat cages where there was expected to be a significant amount of activity in the housing rooms. Tuesday was expected to be non-eventful in the housing areas. The followingtables present a summary of sorbenttubes, filters, and tissue wipes collected during the test program. Samples were identified by room number, type of sample (SG = Silica Gel Tube, C = Charcoal Tube, GF = Glass Fiber Filter), location within the room, and a possible 2 on the end indicating the second time the room had been sampled. Schematics of each room and sampling locations are presented in Figures 4.0-1 through 4.0-6. Revision 0 8 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 EXPERIMENTAL - OVERVIEW Sample ldentlflC8tlOfl 3045C-1AbB 3045GF-A 304556-A 3045C-2AaB 3045GF-B 3045SG-B 3045C-3AbB 3045GF-C 3045SG-C 349C-1AbB 349GF-A 349SG-A 349C2A&B 349GF-B 349SG-B 349C-3AbB 349GF-C 349SG-C Summary of Adsorbent Table 4.0-1: Tube and Filter Sampling - June 29,1998 Sample Start Tlme (hn) 10:40 10:40 8:48 10:40 10:40 8:48 10:40 1040 8:48 Smlplr Stop Tlme (hn) 12:48 12:48 11:48 12:48 12:48 11:48 12:48 12:48 11:48 Sample Duntlon (mln) 128 128 180 128 128 180 128 128 180 Sample Pump ID. 273 3M 45347 ( I ) 134469 E1158 E277 (5) 45351 E2069 E2071 (3) BFE101186 Pump Flow -RItr ( L m ) 0.62 2.03 0.57 0.88 2.05 0.53 1.12 2.60 0.59 Total Volume of Alr Sampled (L) 78.4 260 103 113 262 95.4 143 333 106 14:09 16:12 123 Ell58 0.83 102 14:OQ 1632 123 E274 2.06 253 1409 18:12 123 (I)134489 0.51 62.7 14:09 1612 123 E2069 1.12 138 14:09 16:12 123 E277 2.04 251 14:09 16:12 123 (3) BFElOll86 0.51 62.7 14:OQ 16:12 123 E273 0.60 73.8 1409 16:12 123 3M 45347 2.02 248 14:09 16:12 123 (5) 45351 0.51 62.7 Summary of Adsorbent Table 4.0-2: Tube and Filter Sampling - June 30,1998 Sample ldentlflcatlon 3045C-IA26B2 3045GF-A2 3045SG-A2 3045C-2A2682 3045GF-82 3045SG-B2 Sample Start T h e (hn) 8:27 8:27 8:27 8:27 8:27 8127 Sample Stop Tlme (hn) 10s 1034 1034 1034 1034 1034 Sample Duntlon (mln) 127 127 127 127 127 127 - Sample Pump ID. E1158 3M 45347 (1) 134469 E273 E277 (5) 45351 Pump Flow (Lpm) 0.83 2.01 0.60 0.60 2.05 0.53 Total Volume of Air Sampled (L) 105 255 76.2 76.2 260 67.3 3004C-1AbB 632 1057 145 E2069 1.11 161 3004GF-A 832 1057 145 E274 2.06 298 3004SG-A 832 1057 145 (3) BFEI01186 0.63 91.4 3004C-2A6B 1l:M 1252 108 E2069 1.11 120 3004GF-B 11:04 1252 108 E274 2.07 224 3004SG-B 11:M 1252 108 (3) BFEI01186 0.56 60.5 349C-IA2192 1053 12:45 112 E1158 0.81 90.7 349GF-A2 1053 12:45 112 3M 45347 2.02 226 349SGd2 10% 12:45 112 (1) 134469 0.60 67.2 349C-2A2bB2 1053 12:45 112 E273 0.59 68.1 349GF-92 10:53 12:45 112 E277 2.04 228 349%-BP 1053 12:45 112 (5) 45351' 0.60 67.2 'Note: Initial flow used for total volume sampled. Revision 0 9 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY No: FS-980618-1 EXPERIMENTAL - OVERVIEW Summary of Table Tissue Wipe 4.0-3: Sampling - June 29,1998 Sample Description Tissue Blank in Room 3045 Tissue Blank in Room 3045 Door Handle in Room 3045 Front Center Floor in Room 3045 Middle Center Floor in Room 3045 Back Center Floor in Room 3045 Bottom of Cage Side of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Side of Cage Back of Rat Bottom of Cage Back of Rat Tissue Blank in Room 3004 Template Blank in Room 3004 Wipe Blank in Room 3004 Door Handle in Room 3004 Front Center Floor in Room 3004 Middle Center Floor in Room 3004 Back Center Floor in Room 3004 Bottom of Cage Side of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Side of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Back of Rat Sample Identification Wipe # l Wipe #2 Wipe #3 Wipe #4 Wipe #5 Wipe #6 Wipe #7 Wipe #8 Wipe #9 Wipe #10 Wipe #11 Wipe #12 Wipe #13 Wipe #14 Wipe # I5 Wipe #16 Wipe #17 Wipe #18 Wipe #19 Wipe #20 Wipe #21 Wipe #22 Wipe #23 Wipe #24 Wipe #25 Wipe #26 Wipe #27 Wipe #28 Wipe #29 Wipe #30 Wipe #31 Wipe #32 Wipe #33 Wipe #34 Wipe #35 Wipe #36 Wipe #37 Wipe #38 Wipe #39 Wipe #40 Wipe #41 - Room Number 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3045 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 3004 Sample Time (hm) u10 . 1l:ll 11:46 11:41 11343 11344 11315 11:16 11:17 11:21 11% 11:25 11:26 11:29 11:30 11:33 11334 11335 11:37 11338 14:25 1426 14:53 14:52 14:49 1430 1451 14:30 14:31 14:32 1435 14:s 14:38 14:39 14:41 14:42 1443 14:44 14:45 14:46 14:47 Cage Identification C90716 C90716 C90716 c90739 C90739 c90744 c90744 C90946 C90946 C90951 C90951 C90951 C90956 -C90956 - C92518 C92518 C92518 C92523 C92523 C92528 C92528 C92757 C92757 C92757 C92762 C92762 C92767 C92767 Revision 0 10 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 EXPERIMENTAL- OVERVIEW Summary of Table Tissue Wipe 4.0-4: Sampling - June 30,1998 Sample Description Wipe Blank in Room 349 Wipe Blank in Room 349 Template Blank in Room 349 Front Center Floor in Room 349 Middle Center Floor in Room 349 Back Center Floor in Room 349 Door Handle in Room 349 Bottom of Cage Side of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Side of Cage Back of Rat Bottom of Cage Back of Rat Bottom of Cage Back of Rat Sample Identification Wipe #42 Wipe #43 Wipe #44 Wipe #45 Wipe #46 Wipe #47 Wipe #48 Wipe #49 Wipe #50 Wipe #51 Wipe #52 Wipe #53 Wipe #54 Wipe #55 Wipe #56 Wipe #57 Wipe #58 Wipe #59 Wipe #60 Wipe #61 Wipe #62 Room Number 349 349 349 349 349 349 349 349 349 349 349 349 349 349 349 349 349 349 349 349 349 Sample Time (hm) 1BOO . 15:Ol 15:02 15:20 15:21 15:22 15:23 1594 15:06 15:07 15:07 15:08 15:lO 15:ll 15:12 15:14 15:15 15:16 15:17 15:18 1519 Cage Identification c94491 c94491 c94491 C94496 C94496 C94492 C94492 C94526 C94526 C94526 C94521 C94521 c94522 C94522 4.2 Results The results of FTIR analysis are presented in Table 4.0-5 on page 12. The results of the fast GC-ion mobility spectrometry, sorbent tubes, filters, tissue wipes, canisters, and water analyses are presented in the Signed Reports from Individual Scientists Section of the Appendix. ! ! I 'I Revision 0 11 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 EXPERIMENTAL - OVERVIEW Summary of - Table 4.04: FTlR Results June 29,1998 Ammonia Method (Results in ppmv) Room 3045 cO007.abs c0008.abs c0009. abs cOOlO.abs cO011.abs c0012.abs c0013.abs c0014.abs c0015.abs c0016.abs c0017.abs cOOl8.abs cO01 9.abs cO020.abs cO02l.abs cO022.abs cO023.abs cO024.abs cO025.abs Average, ppmv = 6/29/98 9:02 6/29/98 9:04 6/29/98 9:06 6/29/98 9:07 6/29/98 9:09 6/29/98 9:11 6/29/98 9: 13 6/29/98 9: 14 6/29/98 9:20 6/29/98 9:21 6/29/98 9:23 6/29/98 9:25 6/29/98 9:27 6/29/98 9:28 6/29/98 9:30 6/29/98 9:32 6/29/98 9% 6/29/98 9% 6/29/98 9:37 NH, 7.138 7.881 7.46 7.477 7.642 7.624 7.787 7.772 7.928 8.131 8.605 8.632 8.673 8.348 8.705 9.354 9.129 9.371 - 9.338 8.26 - Error+0.08 0.09 0.08 0.08 0.08 0.08 0.09 0.09 0.09 0.09 0.09 0.09 0.09 0.09 0.1 0.11 0.1 - 0.11 0.11 0.09 Room 349 c0026.abs c0027.abs cO028. a bs c0029.abs c0030.abs dM3l.abs c0032.abs cO033.abs c0034.abs Average, ppmv = 6/29/98 9:47 6/29/98 9:49 6/29/98 9:50 6/29/98 9:52 612~119a:SI w2919a 9 : s 6/29/98 9157 6/29/98 959 6/29/98 1O:Ol NH, 1.794 1.772 I.656 1.698 1.591 1.54 1.425 1.463 - 1.464 I.60 Error+- 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02 - 0.02 0.02 Room 3004 c0035.abs c0036.abs ~0037a.bs C0038. abs c0039.abs cO040.abs cO04l.abs Average, ppmv = 6/29/98 IO: 11 6/29/98 10:12 6/29/98 10:14 6/29/98 1036 6/29/98 10:18 6/29/98 1039 6/29/98 10:21 NH, 7.218 7.168 6.845 7.119 7.182 - 7.296 7.393 7.17 - Error+0.08 0.08 0.08 0.08 0.08 0.08 - 0.08 0.08 Revision 0 12 3M ENVTRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 I EXPERIMENTAL - OVERVIEW I I 4.3 Process Description I Three separate studies are currently being conducted for 3M Toxicology Services at Covance Laboratories, one for each test compound: of n-methyl FOSE alcohol, n- 1, ethyl FOSE alcohol, and potassium perfluorooctanesulfonate: The control and dosed rats for a given study are housed in the same room, while there are separate rat housing rooms for each study. 1 - BackRoom Door a = C94526 (Upper Right Comer) b = (294521 (2nd From Top Right) c = C94522 (3rd From Top Right) d = C94491 (Upper Left Comer) e = C94496 (2nd From Top Left) f = C94492 (3rd From Top Left) A = Approx. 3 ft. High B = Approx. 5 ft. High (Cage Top) C = Approx. 5 ft. High (Cage Top) u Center Room I Front Room Door A Figure 4.0-1: Room 349 Schematic and Sampling Locations- June 29,1998 Door A = Approx. 3 ft. High B = Approx. 5 A. High (Cage Top) I I 0 Sink Door A I Figure 4.0-2: Room 349 Schematic and - Sampling Locations June 30,1998 Revision 0 13 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 EXPERIMENTAL - OVERVIEW Sink Back Room jE 7 - J l u r' nc CenterRoom I Front Room Door a = C92518 (3rd From Right) b = C92523 (2nd From Right) c = C92528 (Far Right) d = C92757 (2nd From Left) e = C92762 (3rd From Left) f = C92767 (4th From Left) Figure4.03: - Room 3004 Schematic and Sampling Locations June 29,1998 ~~ Figure4.04: Room3004 Schematic and Sampling - Locations June 30,1998 Revision 0 14 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 EXPERIMENTAL - OVERVIEW 1 - I I a b c a = C90956 (3rd From Left) b = C90951 (2nd From Left) c = C90946 (5th From Left) d = C90716 (2nd From Left) e = C90739 (2nd From Right) f = C90744 (Far Right) A = Approx. 3 ft. High I B = Approx. 5 ft. High (Cage Top) C = Approx. 5 ft. High (Cage Top) I A ~~ Figure 4.0-5: Room 3045 Schematic and Sampling Locations - June 29,1998 I Door A Figure 4.0-6: Room 3045 Schematic and Sampling Locations - June 30,1998 Revision 0 15 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDYNo: FS-980618-1 5.0 - EXPERIMENTAL METHODS EXPERIMENTAL - METHODS The following table summarizes the U.S. EPA methods and their respective sources. Table 5.0-1: - Summary of Sampling Procedures Title 40 CFR Part 63 (Julv 1, 1996) Method 320 "Measurementof Vapor Phase Organic and Inorganic Emissions by Extractive Fourier Transform Infrared (FTIR) Spectroscopy" Methods for Determination of Toxic Oraanic COmDOUndS in Air (June 1988) MethodTO14 "Determinationof Volatile Organic Compounds (VOCs) in Ambient Air Using Summa Passivated Canister Sampling and Gas ChromatographicAnalysis" Due to the screening nature of this study, specific methods were not followed. Instead, the testing used the guidance provided by US EPA Methods 320 and T014. The data quality objectives for this testing were quantitative screening. Major aspects of the sampling, recovery and analytical procedures are summarized on the following pages. Revision 0 16 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY No: FS-980618-1 EXPERIMENTAL - METHODS 5.1 Fast GC-Ion Mobility Spectrometry A hand-portable, GCAMS Environmental Vapor Monitor I1 was used for direct monitoring of atmospheric vapors. The GCAMS instrument is based on the combination of Graseby Ionics, IMS technology for ultra sensitive-detectionof gas phase analytes with high speed automated vapor sampling - transfer line gas chromatography sampling and separation capabilities developed by FemtoScan. The instrument was operated in the postive ion (G) mode in which the instrument creates and detects positive ions created fiom the ionization of the GC column effluent. fiSide View R TODView / sampling inlet Rear View OnlOff +G/H mode selector connector WkU Revision 0 Figure 5.0-1 : Fast GC-Ion Mobility spectrometry Monitor 17 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 - EXPERIMENTAL METHODS 5.2 Fourier Transform Infrared Spectroscopy- EPA Method 320 FTIR testing was performed using US EPA Method 320 guidelines. Room air was sampled through five feet of unheated, W' PFA Teflon sample transfer line and a nickel coated stainless 10-m infrared multi-pass gas cell witka gas sampling pump for the extractive system. A 90-m path was used for the LOPIR instrument that was utilized by maneuvering the system to a selected area within the room and collecting data for a certain period of time. All components were constructed of nickel-coated metal, stainless steel or Teflon to reduce the number of reactive sites within the sampling system. The sampling configuration allows the operator to deliver spike gas, sample gas or spiked sample gas. The data quality objectives for this project were identified as "Quantitative Screening." FTIR Instrument. The FTIR equipment employed for this field test was Midac Model I2000 extractive FTIR system and the LOPIR instrument. Both systems were configured with ZnSe beam splitters and a 1-mm mercury cadmium telluride (MCT) detector. All gas cell windows were ZnSe. The inside walls and mirror housing of the multi-pass gas cell were nickel coated stainless steel construction. The spectrometers have an ultimate resolution of 0.5 cm" unapodized. The software used to acquire and manipulate all data was Midac AutoQuant 3.01. The CLS methods used for analyte quantitation are included in the AutoQuant CLS Method Section of the Appendix. A portable computer was used for data acquisition. FTIR Instrument Settings. Apodized (triangle) data was collected from 4500 to 650 cm-' with 64 co-added scans at 0.5 cm-' resolution (gain 1). Gas cell pressure was continuously monitored for the extractive system using a Pressure Digital Manometer (PDM) attached directly to the FTIR sample cell. Reference Spectra. The Hanst spectrum for ammonia was used for sample quantitation. Spectra developed by 3M Company were used for ethylene. Background SDectra. Background spectra were generated on the test instrument using compressed cylinders of high purity dry nitrogen. Any test system change included the generation of additional background spectra. AutoOuant Method Pathlength Determination. The certified concentration of ethylene was inserted for the instrument pathlength in the method. The method then returned the instrument pathlength rather than the ethylene concentration. The instrument pathlength was found by averaging all pathlength determinations for the given instrument during the testing. A 90-m pathlength, based on instrument calibration performed within the laboratory prior to the test, was used for the analysis of ammonia. Revision 0 18 3M ENVIRONMENTALLABORATORY BACK TO MAIN ET & SS STUDY No: FS-980618-1 EXPERIMENTAL- METHODS Fourier Transform Infrared Spectroscopy (Continued) Data Storage. All data were collected and stored as interferogram, single-beam, and . absorbance spectra on Zip disks during the testing. All data were also stored on CD ROMs located in the 3M ET & SS Archives. Each spectrunarecorded during the field tests was assigned a unique file name with the extensions .int, .sb, and .abs for interferogram, single-beam, and absorbance data, respectively. Hard copies of data sheets containing these names, instrumental conditions, gas cell temperature, gas cell nominal pathlength, gas cell pressure, and other notes were collected. Figure 5.0-2: Extractive FTlR Schematic Revision 0 19 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 EXPERIMENTAL - METHODS 5.3 SUMMA Canisters Gas ChromatographylMass Spectrometry - EPA Method TO14 EPA Method TO14 was used to measure concentrations of various compounds in Rooms 349,3004 and 3045. Air was drawn from the sourceinto a pre-evacuated SUMMA@passivated canister. To analyze the contents of the SUMMA@canisters, the water vapor in the gas sample was reduced by a N ~ i o n @dryer, and the compounds were concentrated by collection into a cryogenically cooled trap. The cryogen was removed and the temperature of the trap raised. The compounds originally collected in the trap were revolatilized, separated on a gas chromatograph (GC) c o l m , then identified and quantified by a detector. The SUMMA@canisters were analyzed by Pace Analytical Services located in St. Paul, Minnesota. 5.4 Sorbent Tubes, Filters, Wipes, and Water Samples Electrospray Mass Spectrometry Samples were collected using peristaltic pumps that were calibrated prior to sampling using a piston driven BIOSm dry-cal meter. Sampling media used for the collection of fluorochemicalscontained silica gel in tubes, charcoal in tubes, or glass fiber from filters. Wipe samples were collected using methanol as a soaking agent and a lOOcm*paper template. Water samples were collected in 1-gallon polyethylene bottles from an individual rack selected in each of the rooms analyzed. Sorbent tubes and filter samples were stationed at two to three locations within the room being sampled, once the sample pump flow had been calibrated. One silica gel tube, two charcoal tubes (front and back), and a glass fiber filter were stationed at each location. Pump flow rates were approximately 0.5 to 2.1 lpm for each monitoring location. Additional tissue wipe sampling of rats, rat cages, floor areas, and door handles also was completed for each of the sampling rooms. Sampling was performed by soaking a tissue with methanol, wiping the sample area of 100 cm2inside a template (or the back of the animal selected), and placing the tissue inside a 40-ml I-Chemm sample vial. All samples taken at the facility were placed on ice during the transportation from the facility to the laboratory. The samples were analyzed by Pace Analytical Services and 3M Industrial Hygiene located in St. Paul, Minnesota. Revision 0 20 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 6.0 DATA ANALYSIS I DATA ANALYSIS Midac AutoQuant 3.01 software was used for collection and analysis of FTIR I sample spectra generated during the testing. The spectral library standard for 1 ammonia (H85NH3) was selected fiom the Hanst Library for data analysis. The - AutoQuant classic least squares method is presented in the AutoQuant CLS Method -1 Section of the Appendix. 1 I Revision 0 21 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET &E SS STUDY NO: FS-980618-1 7.0 CONCLUSION CONCLUSION EtFOSE-OH detected in air samples indicates that contamination in control animals may be due to respiration of gas phase or airborne particles of EtFOSE-OH. Filter samples collected by wiping the backs of test animals were also determined to contain EtFOSE-OH. Test material transferred from animal to animal during -handlingepisodes by the animal technicians may be another route of contamination exposure. It should be noted that the studies taking place at Covance Laboratories are for toxicology purposes. Although the ammonia concentrations determined for each of the rooms are less than the ACGIH TLV TWA for humans, the extrapolation for the effect of these concentrations on rats should be considered. Revision 0 22 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDYNO: FS-980618-1 8.0 MAINTENANCE OF RAW DATA AND RECORDS MAINTENANCE OF RAW DATA AND RECORDS All original data, or copies thereof, were available at 3M ET&SS to facilitate review and auditing the study during its progress and before acceptance of the final report. When the final report is completed, control material reserve samples, all original paper data, including those items listed below will be retained in the archives of 3M ET&SS for a period of ten years following signing of the final report. The following raw data and records will be maintained in the study folder in the archives: Approved protocol and amendments Study correspondence Shipping records Raw data (field and laboratory) Approved final report (original signed copy) Electronic copies of data Supporting records to be retained separately from the study folder in the archives will include, but not necessarily be limited to the following: Training records Calibration records Instrument maintenance logs Standard operating procedures, equipment procedures, and methods Appropriate samples Approved By: 6%T&%- ( James T. Wolter, Ph.D. &udy Director LJ Revision 0 ?/2 3/? c Completion Date 23 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 I 9.0 APPENDICES APPENDICES 9.1 h.otoco1 and Amendments........................................................................................................... A 9.2 Signed Reports from Individual Scientists.................................................................................. B 9.3 Key Personnel Involved in the Study .......................................................................................... C . 9.4 Materials and Equipment............................................................................................................ .D 9.5 9.6 FFiieelldd DDaattaa P...r.i.n..t..o.u..t..s..........................................................................................................................................................-................................................................................. E F 9.7 AutoQuant CLS Method............................................................................................................. .G 9.8 Chains of Custody ....................................................................................................................... H I I I Revision 0 24 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET &L SS STUDY NO: FS-980618-1 i 9.1 Protocol and Amendments A ' -1 I .. i i I .. Revision 0 BACK TO MAIN Sponsor: :' i ' -1 3M Toxicology Services i L , Bldg 220-2E-2 St. Paul, MN 55144 - PROTOCOL Study Title: Covance Laboratories Contamination Testing Performing Laboratory: 3M Environmental Technology and Safety Services 3M ENVIRONMENTAL LABORATORY 3M Field Analytical Technologies Group 935 Bush Avenue St. Paul, MN 55106 ET & SS Study NO:FS-980618-1 Initiation Date: June 29, 1998 Author: James T. Wolter 3M Laboratory Request No: U1927 q I I Approved By: & @ yDirector Date Andrew Seacat Date Sponsor's Representative 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 CONTENTS I1 1.0 SUMMARY....................................................................................................................................... 1 2.0 INTRODUCTION............................................................................................................................ 2 3.0 TEST, CONTROL, AND REFERENCEMATERIALS........................-....................................... 3 4.0 EXPERIMENTAL.OVERVIEW.................................................................................................. 4 5.0 EXPERIMENTAL.METHODS.................................................................................................... 5 6.0 DATA ANALYSIS............................................................................................................................ 6 7.0 REPORT........................................................................................................................................... 7 8.0 MAINTENANCEOFRAW DATA AND RECORDS.................................................................. 8 9.0 GENERALPROJECTOUTLINE.................................................................................................. 9 Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 1.0 SUMMARY SUMMARY 1 STUDY IDENTIFICATION - Covance Laboratories Contamination Testing 3M ET&SS Study Number: FS-980618-1 Test Material: NA Sponsor: 3M Toxicology Services St. Paul, MN Sponsors Representative: Andrew Seacat 3M Toxicology Services Bldg 220-2E-2 St. Paul, MN 55144 Study Director: James T. Wolter 3M Field Analytical Technologies Group 935 Bush Avenue Building 2-3E-09 St. Paul, MN 55106 Test Site: Covance Laboratories 3301 Kingsman Blvd. Madison, WI 53704 Proposed Study Timetable Experimental Start Date: June 29,1998 Experimental Completion Date: June 30, 1998 Final Report Date: July 10,1998 Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO:FS-9806184 2.0 INTRODUCTION INTRODUCTION 2 2.1 Study Title Covance Laboratories Contamination Testing 2.2 Purpose Covance Laboratories has been contracted by 3M to conduct toxicological studies of nmethyl FOSE alcohol, n-ethyl FOSE alcohol, and potassium perfluorooctanesulfonateon rats. Recent results have indicated trace amounts of n-ethyl FOSE metabolites are present in the liver and blood of the control rats used in these studies. It has been speculated that the control rats are being exposed to one or more of these test compounds through the air, either as a particulate or gas. The objective of this study is to investigate potential contamination sources within the rat housing area of these studies. 2.3 Regulatory Compliance This testing is not being performed for regulatory compliance. 2.4 Quality Assurance The protocol, study conduct, and the final report will be audited by the quality assurance unit in accordance with 3M Environmental Technology and Safety Services (ET & S S ) standard operating procedures and policies. Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 3.0 TEST, CONTROL, AND REFERENCE MATERIALS TEST. CONTROL. AND REFERENCE MATERIALS 3 Test and control materials are not applicable to this study. - r The reference materials are as follows: n-methyl FOSE Alcohol - Lot 648 n-ethyl FOSE Alcohol - TN-A-1884 61691-16 nominal 20 ppmv ethylene in nitrogen zero grade nitrogen i '\ J I i :i Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 4.0 EXPERIMENTAL - OVERVIEW EXPERIMENTAL - OVERVIEW 4 4.1 Test Program Local open path Fourier transform infrared spectroscopy (LOPIR) and Fast GC-Ion Mobility Spectrometry will be used to verify or refUte the presence of fluorinated compounds at ppbv levels in the dietary study housing air at Covance Laboratories. Additionally, charcoal and glass fiber adsorption tubes will be used to screen for the presence of the test compounds in the study housing air.It is anticipatedthat any test compounds present as airborne particulates or adsorbed onto airborne particulates will be trapped by both the glass fibers and charcoal. Samples will be taken of the rat drinking water for LC/MS/MS analysis. Wipes of the rat cages will be taken for extraction and analysis. 6 liter SUMMA passivated canister samples will be taken for analysis by cryofocus GC/MS. Samples will be taken fiom housing room air and the air intakes and exhausts for the rooms. Three separate studies are currently being conducted for 3M Toxicology at Covance Laboratories, one for each test compound. The control and dosed rats for a given study are housed in the same room, while there are separate rat housing rooms for each study. All three rooms will be investigated with the stated techniques on both Monday, June 29 and Tuesday, June 30. Monday is a change-out day for the rat cages where there is expected to be a significant amount of activity in the housing rooms. Tuesday is expected to be noneventful in the housing areas. Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY No: FS-980618-1 5.0 - EXPERIMENTAL METHODS EXPERIMENTAL - METHODS 5 Localized Open Path Fourier Transform Infrared Spectroscopy (LOPIR) will follow guidance given in US EPA Method 320. Details of the quantitation method used will be provided in the final report. - Adsorption methods are currently being developed and validated for the target compounds. Coconut Charcoal and Glass Fibers will be used as adsorbants. Details of the methods will be provided in the final report. 6 Liter SUMMA Passivated Canister samples will be taken and analyzed by cryofocussed GCMS. Details of the method will be given in the final report. Details of the Ion-Mobility Spectrometer method will be provided in the final report. 5.1 Process Description A schematic of Covance Laboratories specifically identifying and documenting the rat housing rooms, ventilation, and location of control and dosed rat cages will be provided in the final report. Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDYNo:FS-980618-1 ' ` 6.0 DATA ANALYSIS DATAANALYSIS 6 1' The data analysis will be performed in accordance with the methods stated in this ' protocol. - ! ' !, 1c .I Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 7.0 REPORT REPORT 7 The final report will include the following information if applicable: A summary of the test. - A brief process description, indicating equipment operation during testing; as well as any other information which may influence the final report. A simple schematic diagram or photo of the laboratory, showing the sampling locations. 0 The sampling and analytical procedures, detailing all aspects of sampling and analysis. Diagrams or photos of test equipment and methods will be included. 0 Complete raw field data, lab analyses and the test results (showing all calculations). Calibration data regarding all sampling and measuring equipment utilized during testing. Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 8.0 MAINTENANCE OF RAW DATA AND RECORDS MAINTENANCE OF RAW DATA AND RECORDS 8 All original data, or copies thereof, will be available at 3M ET&SS to facilitate review and auditing the study during its progress and before acceptance of the final report. When the final report is completed, control material reserve samples, all original paper data, including those items listed below will be retained in the ar7hives of 3M ET&SS for a period of ten years following signing of the final report. The following raw data and records will be maintained in the study folder in the archives: Approved protocol and amendments Study correspondence Shipping records Raw data (field and laboratory) Approved fmal report (original signed copy) Electronic copies of data Supporting records to be retained separately fkom the study folder in the archives will include, but not necessarily be limited to the following: Training records Calibration records Instrument maintenance logs Standard operating procedures, equipment procedures, and methods Appropriate samples Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDYNO: FS-980618-1 9.0 GENERAL PROJECT OUTLINE GENERAL PROJECT OUTLINE 9 Field Analytical Technologies / General Project Outline To: From: - Dale Bacon - ET & S Environmental Lab 2-3E-09 Ron Cressman ET & S Environmental Lab 2-3E-09 Jess Eldridge - ET & 5 Field Analytical Technologies 2-3E-09 Timothy Gutzkow - Pace Kurt Oldenburg- ET & 5 Field Analytical Technologies 2-3E-09 - Bill Reagen ET & 5 Field Analytical Technologies 2-3E-09 Jeff Stock - ET & 5 Field Analytical Technologies 2-3E-09 Tom Wagner - Quest Analytical - Anh-Dao Vo ET & 5 Field Analytical Technologies 2-3E-09 Jim Wolter - ET&S Field Analytical Technologies 2-3E-09 Date: June 18,1998 Subject: Covance ContaminationTesting Project Number - FS-980618-1 Lab Request No.- U1927 Test Date@) June 2930,1998 Monitoring Requested by: Name: John Butenhoff Toxicology Services Bldg 220-2E-2 Telephone No. (612) 733-1962 FAX NO.(612) 733-1733 Monitoring Coordinated by: Jim Wolter 3M / ET= Building 2-3E-09 935 Bush Ave. PO Box 33331 St. Paul, MN 55133-3331 Telephone No. (612) 778-7644 Cellular No. (612) 270-0387 Pager No. 1-888415-0942 FAX No. (612) 778-4226 Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 GENERAL PROJECT OUTLINE 10 Plant Location / Contact - Plant Name: Covance Laboratories Address: 3301 Kingsman Blvd. Madison, WI 53704 Plant Contact: Peter Tomford 608-241-7207. Project Objective Covance Laboratories has been contracted by 3M to conduct toxicological studies of n-ethyl FOSE alcohol, methyl FOSE alcohol, and potassium perfluorooctanesulfonate on rats. Recent results have indicated trace amounts of n-ethyl FOSE metabolites are present in the liver and blood of the control rats used in these studies. It has been speculated that the control rats are being exposed to one or more of these test compounds through the air, either as a particulate or gas. The objective of this study is to measure the concentrations of the target analytes at the lowest limits of detection possible at the time of testing. LOPIR will be used to verify or refute the presence of fluorochemicals in the air at ppbv or greater concentrations. Method development and validation for sampling and subsequent extraction/ desorption using adsorption techniques are currently underway. Project Schedule Equipment Preparation - Friday, June 26 Travel - Sunday, June 28 Equipment Set-up - Monday, June 29 Monitoring/Testing -June 29-30 Return Travel - Tuesday, June 30 Processes Requiring Testing Indoor Air and Cages at Covance Test Parameters n-ethyl FOSE alcohol, methyl FOSE alcohol, perfluorooctanesulfonylfluoride, perfluorooctanesulfonic acid or salts of perfluoroctanesulfonic acid Test Conditions Ambient Gas Stream Characteristics Indoor Air Test Methods LOPIR, Adsorption/GC, Canister GC/MS, LCMS Estimated Project Cost $5,000 Revision 0 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 GENERAL PROJECT OUTLINE 11 Reporting Requirements Type of report@)required; 3 copies of Comprehensive Final Report for John Butenhoff 1copy of Comprehensive Final Report for LIRm Archives 1copy of Comprehensive Final Report for Field Archives 1copy of Comprehensive Final Report for QAU Archives Supplemental Information The following personnel will need plant entrance and non-escort privileges: - -Jim Wolter 3M - -KurtOldenburg 3M - -Andrew Seacat 3M -Timothy Johnson - 3M -Timothy Gutzkow - PACE Laboratories (3M contract No. E-4878-S) - -Tom Wagner Quest Analytical Invoicing must be sent to monitoring coordinator including; - Invoice Date - Project Description - Test Dates - 3M Project No. - 3M Lab Request No. - Cost Itemization Revision 0 BACK TO MAIN GLP Study Protocol Amendment Study Number: U1927 Study Title: Covance Laboratories Contamination Testing Study Director: James T. Wolter Amendment Date: September 9, 1998 - Amendment Number: 1 The study protocol in the experimental overview section stated that samples would be taken from the air intakes and exhausts for the rooms. These samples were not obtained during the study conduct. The study protocol does not refer to silica gel as an adsorbent media. Silica gel, charcoal, and glass fiber were used as adsorbents during the study conduct. The study protocol states that the finalreport will include a schematic of Covance Laboratories specifically identifying the rat housing rooms, ventilation, and location of control and dosed rat cages. Location of ventilation, control rat cages, and dosed rat cages were not documented. These changes would not be expected to have an effect on the outcome of the study. Approved by: I 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 , q 9.2 Signed Reports from Individual Scientists B I , Revision 0 BACK TO MAIN I Analytical Results and Summary 3M Lab Request U1927 - Covance Contamination Testing I i I / Contract Laboratory: Pace - I Prepared by: William J. Arseneau 1 BACK TO MAIN ANALYTICAL SUMMARY Lab Request No.: U1927 Contract Lab: Pace-I Department: 0211 Project No.: FS980618-1 3M -Requester:J. T . Wolter Project Lead: J. T . Wolter Project Description: Covance Contamination Testing Sample Matrix:Whole air samples collectedin S U M M A canisters. Sample Available Date: 08/01/98 Summary Prepared by: William Arseneau, Pace1 Date: 9/3/98 Introduction Three whole air samples were submitted for gas chromatographytmass spectrometry analysis. The samples were received in 3 liter (L)SUMMA canisters. The sampleswere analyzed at ambient temperature by a method closely resembling the US Environmental Protection Agency (USEPA) Compendium Method TO-14.Method TO-14 requires a specificlist of target compounds. The analytes of interest for this project are ethylfosealcohol (etFOSE-OH),methylfosealcohol (meFOSE-OH)and perfluorooctanesulfonylfluoride (POSF). An attempt to detect etFOSE-OH and meFOSE-OHwas unsuccessfulat concentrationsup to 5 ppmv. A ppbv detection limit is not attainableusing this method. Analytical Results All quantitativedata associated with this report are to be considered estimates. The typical five-point calibration curve associated with method TO-14 was not analyzed. A threepoint calibration curve at 25, 50, and 100parts per billion by volume (ppbv) was analyzed for POSF to show that the instrument was capable of detecting the target analytes at these concentrations. Based on the response of the 25 ppbv calibration standard the quantitation limit is estimatedat 10ppbv. POSF was not detected in the samples at or above 10ppbv, but several other compounds were detected. These compoundswere reported as tentativelyidentified compounds (TICS)in the Report of LaboratoryAnalysis found in Appendix A. The TICSwere quantified against the average response factor !?om the total ion chromatogramsof the POSF in the calibration curve (See Appendix A). 2 BACK TO MAIN Analytical Summary Modified PA Compendium Method TO14 Summary A MicroscalePurge-and-Traptechnique was used to a n a l y z a e standardand the sampleassociatedwith lab request R2584. An aliquot of the whole air sample contained in a SUMMA canister was trapped under integrated mass flow control on a glass bead trap held at -150C. The condensed sample on the glass bead trap was then quantitatively transferred to a Tenax trap held at -10C. The Tenax was then desorbed onto an open-tubularcryofusing trap held at -180C. The cryofusing trap was then heated to transfer the VOC's to the head of the analyticalcolumn where the samplecomponentswere separated and finally detected by a mass spectrometer in the scan mode. A detailed listing of the analytical parameters can be found under Procedure Method TO-14 is a method designed for the analysis of volatile organic compounds in ambient air where - SUMMA canistersare used for sampling. The working range for Method TO-14 is 0.10 to 200 parts per billion by volume (ppbv). An aliquotof air, typically50 500 cc,is removed from the canister under electronicmass flow control and cryogenicallyfocused on a glass bead trap. The condensedsampleis then desorbed onto to the analytical column for separation of the sample components. The detector specified in Method TO-14 is a mass spectrometer. This method yields a very precise and accurate technique for the analysis of ambient level air samples collected in SUMMA canisters. Sample Preparation The sampleswere pressurized with zero grade nitrogen to a final pressure of 15.0psig (29.7psia) in order to introducethe samplesinto the Entech air concentrator. The dilution factor was accounted for in the sampleresult calculationsand the practical quantitation limitswere adjusted accordingly. Procedure GC/MS/Gas Loop Parameters (Instrument ID ccAlphie"') A Hewlett-Packard 5890 GC coupled to a Hewlett-Packard 5989 MS and an Entech 7000 air sample preconcentratorand 7016 canister autosampler were used. The GCMS gas loop injection system configurationis listed below: GC column: R1x-624 6Om, 0.32mm i.d., 1,s micron film thickness, ~ ~ 7 7 3 9 8 . GC oven temperatureprogram: Initial temp.: Ramp 1: Ramp 2 Injection port temp.: Interface temp.: Purge A: split flow: Column head press. Solvent delay: -20C for 1.0 min. 15"C/min. to 60C, hold 0 min. 10C/min.to 150Chold 0.67 min. 260C 200C Initial value OFF 20 mumin. 5 psi hold 6 min. ramp to 15psi at 1psi/min. None 3 BACK TO MAIN 7000 PreconcentratorROl6Canister Manifold During Concentration Module No.1, Glass Bead Cryotrap Module No.2, Sorbent Packed Cryoaap ModuleNo.3, Focusing Trap Temuerature f'Q -150 -10 -180 Desorb/Transfer/Iniect Preheat f'C) Module No. 1, Glass Bead Cryoaap 20 ModuleNo.2, SorbentPacked Cryotrap 50 ModuleNo.3, FocusingTrap N/A Final TemD. ("C) 20 180 loa - Time (min.) 2 3.5 2 Media Concenaate!d/Transferred Volume (cc) Sample 200 Sweep/Dry Purge 50 * Transfer to Packed Column 40 Line Conditioning Sample Flush Before Trapping Carrier Flush Before Trapping Total Cycle Time Flow Rate ~scc/min.) 150 100 10 5 Sec. 2 sec. 38 min. System Bakeout ModuleNo.1, Glass Bead Trap ModuleNo.2, SorbentPacked Trap Ternmature P Q 130 190 Time &fin.) 5 5 Regulated Zone ,. , 8-Port Valve 8 1 GC Transfer Line I Manifold Transfer Line 16-PositionSelect Valve Sample Container Transferline: 100 Temuerature PC) 100 100 100 100 Ambient Mass spectrometerparameters: Ionization mode: Scan range: Scans per second Source temp.: Quadrupole temp.: +E1 29 to 550 a m u 1.3 250C 125C Instrument Calibration Procedure A three-point calibration curye was established for POSF by analyzing different volumes of a custom prepared standard. Tbe percent relative standard deviation (%RSD) for the target compound was 2.9%. The calibration is considered acceptableif the %RSD is less than or equal to 30%. 4 BACK TO MAIN 1 Qualitative Analysis Samplemass spectraare compared to the mass spectrum of a standard of the suspectedcompound. Two criteriamust be satisfied to verify the target compound identifications: (1)elution of the sample componentat the same GC retention time as the standard component, and (2) correspondenceof the sample componentand standard componentmass spectra. Standard and samplemass spectra are compared using reference spectra obtained on the GCMS system being used. The mass spectra used for comparison are fiom the same standard as that used for retention time comparison. Mass spectral requirements are as follows: All ions present in the standard mass spectra at a rzative intensitygreater than 10%(most abundant ion in the spectrum equals 100%) must be present in the sample spectrum. '! The relative intensities of ions specified above must agree within +/- 20% between the standard , and sample spectra. Ionsgreatex than 10%in the sample spectrumbut not present in the standard spectrummust be considered and accounted for by the analyst making the comparison. The verification process should favor a false positive. Non-target componentspresent in the sample were tentativelyidentified based on a spectral library search. The spectrum of a tentatively identified compound (TIC) was compared to a NBS and WILEY reference spectral library. Based on the ions present and the relative abundance of each ion, the software determined the best spectral match. A retention time index was also taken into consideration in the search algorithm. The TICSlisted in this report were not closely reviewedby the analyst and are listed in the report based solely on a computer search of the sample spectra. Quantitative Analysis An internal standard quantitation technique was used to calculate the analyte concentration. For calibrated compounds, a relative response factor was calculated as follows for each level of calibration: Equation 1 i" ResponseFactor ( ~ f =) - (CJ (Ax) '_J where, A, = Reconstructed ion chromatogram area for the compound; C, = Concentration of the compound (ppbv). The average relative response factor was then determined based on the calibration points. This average relativeresponse factor was then used to calculatethe concentrationof an analytein the sampleas follows: 1 ' I i 5 BACK TO MAIN Equation 2 j where, - A, = Sample extractedion chromatogram area for the quantitationion of compound x, C, = Concentration of the associatedinternalstandard (ppmv), 0, = Dilution factor, Ai = Extrackd'ion chromatogram area for the internal standard quantitation - ion, R = Average relative response Wor for compound x. Equation 2 was also used for tentatively identified compounds. Quality Control Procedure Prior to standard or sampleanalysis, a system performancecheck sample (50ng Cbromofluorobenzene) was analyzed to verify the mass spectralperformance. This performance samplewas compliant. In addition to the calibration curve, a method blank and closing calibration check standard were analyzed. The closing calibration check standard met acceptancecriteria (*25% difference). 6 BACK TO MAIN Closing These analytical summary and associated analytical results have been reviewed and are approved for releaseby the followinganalysts. A n y questionsor comments may be directed to either Bill or Dennis. William J.&&;. Pace-I Analytical Chemist Dennis R Seeger, Pace1 Fhalytical Advanced Chemist (612) 7784093 :... . I 1 Ji.'. 7 1 Appendix A Report of Laboratory Analysis BACK TO MAIN I 8 BACK TO MAIN 3M Environmental Laboratory Report of Laboratory Analysis Pace-I 3M Lab Request No.: Department: Project No.: Date Received: Project Description: 3M Sample No.: Sample Desc.: Canister No.: Date Collected: Analytical Method: Date Analyzed: Method Analvtq POSF U1927 021 1 Fs98061a-1 8/3/98 Covance Contamination Testing U1927-123 Room 3045 E1900 6/29/981053 GUMS 9/4/98 Molecular Weieht 502 Requester Name: Project Led: Phone No.: J.T. Wolter J.T.Wolter (612)778-6176 Report Date: September 10,1998 Initial Pressure (psia): 14.7 Final Pressure (psia): 29.7 Pressure Dilution Factor: 2.0 Analytical Dilm`on Factor: 1 -Quantitation Liplit DDbv 10 Analyte Estimated Concentration pDbv udscm ND ND Tentativelv IdentiTed Compounds (TIC) Methane, chlorodifluoroPropane, 2-methylButane Acetaldehyde Methanol Butane, 2-methylPentane Ethanol 2-Propanone 1-(3'-Cyclopentenyl)-pentanone Hexane Methane, dichloro2-Propenal Butanal Cyclopropane Benzene, methyl1,2-Benzisothiazolc Molecular Weight 86 58 58 44 32 72 72 46 58 152 86 45 56 72 42 92 135 - Quality Fit Factor % 83 a3 74 9.0 2.0 90 a3 72 9.0 9.0 86 5.0 5.0 12 4.0 90 91 Estimated TIC Concentration DDbv udscm Q 22 79 N,J 14 34 N J 7.3 18 NJ 6.0 11 N J 28 37 NJ 9.1 27 N,J 3.0 9.0 N,J 14 27 NJ 6.0 14 N J 2.4 15 N J 2.9 10 N J 11 21 N,J 2.6 6.1 NJ 3.9 12 N J 2.1 3.7 N,J 6.2 24 N,J 24 130 N J Definitions: J Estimated concentration, quantitated amount is either below the detection limit or an estimate for a TIC. N Presumptive identification based on spectral library search. ND Not Detected at or above the quantitation limit, ppbv Parts per Billion by Volume u&cm Micrograms per Standard Cubic Meter psia Pounds per Squm Inch Absolute 9 BACK TO MAIN 3M Environmental Laboratory Rennrt ofImhnraton A d v & 3M Lab Request No.: U1k7 ~ ~~ Requester Name: J.T. Wok& Department: 0211 Project Lead: J.T. Wolter Project No.: FS980618-1 Phone No.: (612) 778-6176 Date Received: 8/3/98 Project Description: Covance Contamination Testing Report Date: September 10,1998 3M Smnple No.: U1927-124 Inirial Pressure (psia): 14.7 Sample Desc.: Room 349 Final Pressure (psia): 29.7 Canister No.: E349 Pressure Dilution Factor: 2.0 Date Collected: 6f29/98 1529 Analytical Dilution Factor: 1 Analytical Method: GUMS Date Analyzed: Method Analvtes POSF 9/4/98 Molecular Weight 502 -Quantitation Limit EJ2h 10 Analyte Estimated Concentration & udscm ND ND Pace-I I I, Tentativelv Identified Comwonds mC) j Acetaldehyde I . .I< Methanol Ethanol ,- 1, 2-Ropauone 2-Propanol. %methyl- Hexane Oxirane, (ethoxymethy1)- R O P ~ 2I.I2-~d,hethyl- 2-Butanone 1-Pentene,2,4,4-trimethyl- 2-Hexanone. 5-methyl- Benzothiazole Molecular Weight 44 32 46 58 74 86 102 86 72 112 114 135 Quality Fit Factor !& 83 1.0 72 80 78 90 4.0 46 59 78 72 87 Estimated TIC Concentration EEk 30 udscm Q 55 N,J 3200 4300 N,J 11 21 N,J 43 100 N J 11 34 N J 9.1 33 N J 1.4 5.9 N,J 44 160 N,J 6.8 20 N,J 9.8 46 NJ 20 95 N,J 15 84 N,J Definitions: J J Estimated concentration,quantitated amount is either below the detection limit or an'estimatefor a "IC. N Presumptiveidentificationbased on spectrallibrary search. ND Not Detected at or above the quantitation limit. ppbv Parts per Billion by Volume uglscm Micrograms per StandardCubicMeter psia Pounds per SquareInch Absolute 10 BACK TO MAIN 3M Environmental Laboratory Report of Labomtory A d @ h Pace-I 3M Lab Request No.: U1927 Requester Name: J.T.Wolter Departmew: 0211 Project h a d : J.T.Wolter Project No.: Fs980618-1 Phone No.: (612) 778-6176 Date Received: Project Description: Covance Contamination Testing Report Date: September 10,1998 3M Sample No.: U1927-125 Initial Pressure (psia): 14.7 Sample Desc.: Room 3004 Final Pressure (psia): 29.7 Canister No.: E1893 i. . Date Collected: 6/30/98 1224 Analytical Method: GCJlW Pressure Dilurwn Factor: 2.0 Analytical Dilution Factor: 1 Date Analyzed: Method Analvtes POSF 9/4/98 Molecular Weight 502 -Quantitation Limit DDbv 10 Analyte Estimated Concentration & udscq ND ND Tentativelv Identiried Cornmunds (TIC) Acetaldehyde '! Methanol Butane, 2-methyl- I Ethanol 2-prOPanone 1-propanol Butanal 2-Butanone Isooctane l-BUtanol Benzene, 1-ethyl-2-methyl- Benzene, 1-ethyl4methyl- Benzene, 1-ethyl-3-methyl- Disulfide, dimethyl Benzene, methyl- Benzene, 1,2,3-trimethyl- Benzothiazole Molecular Weirht 44 32 72 46 58 60 72 72 114 74 120 120 120 94 92 120 86 - Quality Fit Factor % 83 2.0 4.0 86 64 9.0 22 9.0 78 9.0 74 91 59 91 64 94 2.0 Estimated TIC Concentration & udscm 19 35 87 120 7.8 23 28 54 7.6 18 8.5 21 6.7 20 4.3 13 5.2 25 4.7 14 22 110 17 85 5.0 25 4.2 16 2.8 11 28 140 10 36 .. Definitions: J Estimated concentration,quantitated amount is either below the detection limit or an estimate for a TIC. N Presumptive identificationbased on spectral library search. ND Not Detected at or above the quantitation limit ppbv Partsper Billion by Volume ug/scm Micrograms per Standard Cubic Meter psia Pounds per Square Inch Absoluk 11 BACK TO MAIN 3M Environmental Laboratory Rsport of L a b o d t y A ~ Y s ~ Pace-I 3M Lab Request No.: Department: Project No.: U1927 0211 FS9806181 RequesterN m : Project Lead: Phone No.: J.T. Wolter J.T. Wolter (612) 778-6176 I Date Received: 8/3/98 Project Description: Covann ContaminationTesting Repon Date: September 10,1998 3M Sample No.: Method Blank t 1) Samplc Desc.: Method Blank Canister No.: NA \' Date CoUected: NA I '1 Analytical Method: GC/MS I Date AnaiyZed: 9/4/98 'i yethod Analvts ti POSF Initial Pressure (psia): 29.7 Final Pressure (psia): 29.7 Pressure Dilution Factor: 1.0 Analytical Dilution Factor: 1 Molecular Weight 502 - Quantitation Limit Dobv 5 Analyte Estimated Concentration E&! udscm ND ND i ............ ................... ........"........u.........................".......... "Y......*................."...".."..........e........................... e.. TentativelyIdentified Comwunds (TIC) i 1 None Detected _.I Molecular Weieht NA - QualitJrFit Factor % NA Estimated TIC Concentration eDbv udscm Q m m ,' j I Definitions: J Estimated concentration.quantitated amount is either below the detection limit or an estimate for a TIC. N Presumptive identification based on spcchd library search. ND Not Detected at or above the quantitation limit ppbv Parts per Billion by Volume ug/scm Micrograms per Standard Cubic Meter psia Pounds per Square Inch Absolute 12 BACK TO MAIN 3M Environmental Laboratory - Fluorine Analytical Chemistry Team Lisa Dick / Kris Hansen Fluorine Analytical Chemistry Team Building 2-3E-09 612-778-7540 / 612-778-6018 ladick@mmm.com/ kjhansen@mmm.com Summary report: Analysis of Air Samples and Animal Wipe Samples Collected at Covance Laboratory Summary: Possible fluorochemical contamination of the animal housing facilities at Covance Laboratory became an issue when detectable levels of fluorochemicals were identified in control test animals. Analysis of liver and sera samples from the control animals indicated the presence of perfluoroocantesulfonate (PFOS) and other metabolites of 2(N-ethylperfluorooctane su1fonamido)-ethyl alchol (ethyl-FOSE-OH). Air and airborne particle samples were collected at Covance by Jim Wolter and Kurt Oldenburg of the 3M Environmental Lab Field Group. [Details of the sampling procedure can be found in a report by Jim Wolter and Kurt Oldenburg.] Filters wiped across the backs of study animals were collected and analyzed. Wipe samples from cages, , doorhandles, and floors were collected but not analyzed. In air samples taken from Room 3045, EtFOSE-OH was detected by high pressure liquid chromatography - electrospray mass spectrometry (HPLCESMS) at levels below the practical quantitation limit (approximately 0.17 ppb/L) but above the method detection limit (approximately 0.02 ppb/L). PFOS was not detected at levels above the blanks in any room. This is not unexpected because PFOS is a non-volatile salt. Analysis of wipes from the backs of rats by gas chromatography - mass spectrometry (GC/MS) in Room 3045 contained a measurable amount of EtFOSE-OH; wipes from rats in other rooms did not. Due to variations in sampling technique, wipe samples were not quantifiable. Due to sample limitations, wipes from animal backs were not analyzed for PFOS. EtFOSE-OH Levels in Covance Lab Environment Covance Sample Location Number of samples EtFOSE-OH detection Room 3045 Air Samples 4 out of 8 0.02 ppb/L < detect < 0.17 ppb/L (GF and charcoal) Room 3004,349 Air Samples 16 Non-detect (GF and charcoal) Room 3045 Rat Backs 6 Detect (8 ppb/wipe average) Room 3004,349 Rat Backs 12 Non-de tect I ,I .i Experimental summary: Sample preparation: Methanol or ether extraction offilters and wipe samples ' . 1i Glass fiber filter and charcoal adsorbates were split and then prepared by extraction with I either ether or methanol. All of the charcoal inside the sterile tubes was extracted with methanol. Final sample volumes were 1 mL. Rat back wipes were prepared by extraction with ether to a final volume of 1 mL. 09/21/98 BACK TO MAIN GC: Analysis of EtFOSE-OH in extracts In gas chromatography, an aliquot of sample is injected and vaporized onto a ,. I chromatographic column. Individual components of the sample adsorb to the stationary phase of i the column. As the temperature is raised, components are eluted from the column based on physical and chemical characteristics. An inert gaseous mobile phase carries the components 1 " through the column. Carrier gas flow rate, column temperature and gas pressure are adjusted to optimize chromatographicseparation. MS: Analysis of EtFOSE-OH in extracts - One method for producing ions for mass spectra is by bombardment with energetic electrons. In addition to the formation of a molecular ion, a series of reactions leads to the , formation of other fragment ions that may be larger or smaller than the molecular ion and are 'i useful for compound identification and quantitation. HPLC: Analysis of PFOS and EtFOSE-OH in extracts In HPLC, an aliquot of extract is injected and passed through a liquid phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the , column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of I time. For example, in a standard solution PFOS may elute at 10.5 minutes. Retention times I between a standard PFOS solution and the analyte extracted from filter fibers in this analysis were matched to within 1% on the HPLC system. / ESMS: Analysis of PFOS and EtFOSE-OH in extracts Following HPLC separation, ESMS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray, one of the softest ionization techniques available, is generally operated at relatively mild temperatures. Molecules are ionized, fragmented, and detected. Initially, the mass to charge range m/z = 100 to 1210 is monitored following direct flow injection of the samples. Ions characteristic of known fluorochemicals were observed. These results are used to select ions that can be monitored selectively for quantitative results. Analysis of organic fluorine standard compound indicates that the primary ion characteristic of EtFOSE-OH is m/z = 630 amu, corresponding to the mass of the compound complexed to acetate anion from the running buffer: CgF17S02N(C2HS)(CH2CH20H)/CH3C00-. The primary ion for PFOS is m/z = 499 amu, corresponding to the mass of the anion C8FI7SO3-. Single ion monitoring was used to determine the concentrations of these ions in the samples. Quality control summary: Methanol blanks were analyzed periodically to ensure complete isolation of the sample. Charcoal and glass fiber filter blanks collected on site were also analyzed and found to be blank. Quantitation of HPLC-ESMS data for fluorochemicals in air samples is based on the linear regression of 5 point standard curves from 10 ppb to 1000 ppb or matrix spike recovery comparisons. Quantitation of wipe samples is difficult due to variations in sampling technique but qualitative data is reliable. Quantitation of GC-MS peaks is based on the recovery of known spike amounts in the same sample matrix and on the linear regression of 5 point standard curves. 09/21/98 BACK TO MAIN Instrumental specifics: GC/Mass Spectrometers Hewlett-Packard ATD 400 Gas Chromatograph and Mass Spectrometer Column: J& W DB-624 30m Temperature ramp: 50C to 250C @ 20"C/min ' _ i I 250C hold 5 min - Carrier gas: Spike volume: Helium 25 ClL Oven temperature: 180C Trap low temp.: -30C Desorb time: 10 min. Trap fast: Yes Trap high temp.: 250C Line temperature: 225C Pressure: 18.4 psi Valve temperature: 225C 1 Trap hold: Desorb flow: 5 min. 25 mLlmin I Ions monitored: 540,448 amu Source temperature: 250C Quad temperature: 125C EM volts: 2598 V Interface temperature: 250C HPLC system Hewlett-Packard Series 1100Liquid Chromatograph Column: Keystone Betasil C18 column, 2 X 100 mm, 5 pm particle size I. , ,d Flow rate: 300 pVmin ,'... Solvent A: 2.0 m M ammonium acetate ;I Solvent B: Methanol :i Solvent Gradient: 40% to 90% B in 8.5 minutes Hold at 90% B for 3 minutes Return to 40% B in 1 minute Hold at 40% B for 1 minute Injection volume: 10 pL Run time: 13.5 minutes Electrospray Mass Spectrometer Micromass Platform 11atmospheric pressure ionization (API)mass spectrometer Mass Lynx 2.1 software Cone voltage: - 60V Mode: electrospray negative Source temperature: 90C Analyzer pressure: 9.2 x lo-' mBar Ions: 630,526,499 Electrode: cross-flow 09121I98 BACK TO MAIN Conclusions: EtFOSE-OH detected in air samples indicates that contamination in control animals may be due to respiration of gas phase or airborne particles of EtFOSE-OH. Filter samples collected by wiping the backs of test animals were also determined to contain EtFOSE-OH. Test material transferred from animal to animal during handling episodes by the animal technicians may be . ..,I another route of contamination exposure. - Personnel involved with project: Extractions: GCMS: LCIMS: Ogi Krupljanin Kent Lindstrom Lisa Dick, Kris Hansen, Joy Jenkins 1/2/98,1/9/98,8/10/98 8/12/98 1/2/98,1/13/98 Raw data archival: ESMS: Chromatograms included with report. Electronic copy stored on CD within Environmental Lab - Fluorine Analytical Chemistry Team area (Harold Johnson). GCMS: Chromatograms included with report. Electronic copy stored on tape cartridge within Environmental Lab - 2"dFloor (Steve Sanders). 0912 119 8 To: S. KNS Analyst: Glenn Johnson 'i Request AT: A142581 I Project #: 841741A6L4 Date: 811 7/96 , #I .. Analysis done by capillary GClECB N-MeFOSE N-MeFOSE BACK TO MAIN FI-E t-.FOS.E- - - - 106 ,t 10 I 0.041 1 c: 0.008 d I c 0.607 I 0.007 Fast GC-Ion Mobility Parameters Scan Timing Duration: 60 s Frequency: 3.003 Hz Scan Data Range ./( , SSttaorpt:: 509.3.6313 ss Peak Width: 2 s Resolution Factor: 30 AVS Control Timers GC Cycle Timing Duration: 59 s Delay: 1s AVS Sampling Duration: 2.00 s Delay: 1 s Lh4S Separation Scan Timing Duration: 0.01 s Trigger: 0.0002 s Frequency: 5e4 Hz Averages: 8 Scan Axis Range Start:2e-5 s stop: 0.01 s Peak Width: 0.0002 s Resolution Factor: 30 BACK TO MAIN BACK TO MAIN n-Methyl FOSE-OH Qrn) 40, e I I tl 30, 20- 0.002 0.004 0.006 Time (Seconds) 0.008 0.01 n-Ethyl FOSE-OH BACK TO MAIN 5040, 30, 20, IO, 0.002 0.004 0.006 Time (Seconds) 0.008 0.01 BACK TO MAIN Ethyl FOSE Room Cage 6 50- 40, n v) 0 30, 20- I .! IO, 0.002 0.004 0.006 Time (Seconds) 0.008 0.01 BACK TO MAIN Methyl FOSE Room 50- d, v) 40, S 30- 20- IO- 0.002 0.004 0.006 Time (Seconds) 0.008 0.01 PFOS Room BACK TO MAIN 50. 40. n tn 0 30, 20- IO- 0.002 0.004 0.006 Time (Seconds) 0.008 0.01 BACK TO MAIN Environmental Lab Air 50, 40- 30- 20IO- 0.002 0.004 0.006 Time (Seconds) 0.008 0.01 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 1 ' 9.3 Key Personnel Involved in the Study C Revision 0 3M Environmental Laboratorv .:i I Key Personnel Involved In the Study Project Coordination: John Butenhoff '--! Andrew Seacat ! , . ( James Wolter Sampling: Tim Gutzgow Shawn Kruse Kurt Oldenburg James Wolter EPA Method TO14 Analysis: i Bill Arseneau 1 Sorbent Tubes, Filters, Wipes, and Water Analysis: Lisa Dick Kris Hansen Shawn Kruse '1 Documentation and Reporting: 1 1 Elizabeth Daugherty Tim Gutzgow ' If-7, James Wolter ?* J Archives: i"p1 Rich Youngblom Quality Assurance Unit: I Tom Wagner BACK TO MAIN 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY No: FS-980618-1 I I 9.4 Materials and Equipment '. j 1 ! ; I\ D. !I i 'I Revision 0 a ET&S I I Environmental Laboratory 1l I Field Analytlcrl Tochnologlas Group FTlR Equipment Checklist Page BACK TO MAIN / / of I Expendable Kit FTlR Support Kit 1 Gas Conditioning Kir I Mass Flow Kit Power Kit' i Pump Kit' 1 Regulator Kit I RotometerKti Swagelok Kit 1' I m o m p u t e r Kit' I I ) OMimTipFIDKit I 0MicroTip PID Kit I lpl=cKllKit I 0ClimbingKit' / 0 50' Rope I Clip 0 0 (0 0 0 I UTranswrtKit O / 0Tents ~ 0 I c ] Tams I 1 0MET Station' 1 0Communication Radios' Gas Standards H G a s S t ' d 9 1 ?U+JI O- @Gas St'd #2 f* -ax / I I I e - Summa Canister IL - - s u m m a Canister 6L 'ommentslAdditional: 42 i o l orm Completed by: d ' ~~ m 1 Date Completed: L / c . & / ? ~ Trailer - Mobile Lab I L7 Truck - Mobile Lab I I Present on Site: I ! 3M ENVIRONMENTAL LABORATORY i 9.5 Field Data BACK TO MAIN ET & SS STUDY NO: FS-980618-1 Bi 1;iI c' iI Revision 0 I I '- I I ET&SS I Extractive FTlR AutoQuant ! Environmental Laboratory I Fleld Analytical Technologlor Group Sample Collection Data Sheet I BACK TO MAIN Page Iof I I I I I I Comments: i.! i i File Name (24 hrs I I I ~~ - Description I I i I ! ~ ~ 1 710,~1 .StatK: I Diluant i I ( p ) (in H20) ' (factor) I rL . Comments. I 3M ETBSS 935 Bush Avenue Mail to: Buildlng 2.3E-09 PO Box 33331 St. Paul. Minnesota 55133-3331 REV070997 BACK TO MAIN 1 I ET&SS i Extractive FTlR AutoQuant I Environmental Laboratory Sample Collection Oata Sheet ' Field Annlytlcrl Technologies Group , Prolect Name: b&f& I Process Name: Page c o ~ ~ e c t ~ e sCco:t/* an): I 0 : Backup. hmD I Method Desc: U, ML 3 e Interval: \ Method Subdirectory: Created: Interferogram Time I eaOm File Name i (24 hrs) 1 ,Wmc ! p:S9 Air ~ c & D , 4 I (rW i # Samples: Collect Subdirectory: I #Scans: Method File Name: Single Beam Descrtptlon c k d -~hiIl* rq h 7% 6 4 1 Pathlength: 16* 4 Residual -Absorbance Flow (Ipm) Statlc I Diluant (in H20) 1 (factor) yY , -52 -- -5.6 I i .II Comments: 1 I 1 3M ETBSS 335 Bush Avenue Mail to: Building 2-3E-09 PO Box 33331 St. Paul. Minnesota 55133-3331 REV070997 ace Anutrcal Field & Air Services BACK TO MAIN 0 Project Ddi/LE -1 F j Sampling Location ' A, Date 6 - 7 Test NO. Pump Type: BConstant Rate Stroke Counter Identification Number 273 Sample Type: U S o u r c e m m b i e n t Personal tt -: Operators <G& /S.Q ' Barometric Pressure Inches Hg 0 Sample Medium: Filter @Carbon Tube 0lmpinger [7Other A ! Source Gas Temperature 1 Estimated Moisture Content I .5 T Sample Medium I.D. No. % v/v Backup Medium I.D. No. Concurrent Airflow : Yes NO Sampling Method &*kcrl v& Stroke Counting Sample a,i Blank Preparation Sample Train Description t Analytical :Additional Parameters Comments - 30y<c - / A I e& , I A5 13' 9c ace Analvtical Field & Air Services I BACK TO MAIN STAQ p.** 3045- Project LG Pump Type: P C o n s t a n t Rate Stroke Counter 7 Samplin Location 1 Date 2 Y -zq--4s Identification Number -7h 4q.3 7 Test NO., A Sample Type: USource H m b i e n t Personal f-; Operators TW / S R K hlA Barometric Pressure Inches Hg , Source Gas Temperature 5O C , 1 Estimated Moisture Content /G % v/v Concurrent Airflow: 0Yes mo Sample Medium: NFilter 0 lmpinger Sample Medium I.D. No. G Backup Medium I.D. No. Sampling Method Carbon Tube Other d S S Flsia c . 3 - I we? Sampling Rate Settin =t 2.t ' 3 iI Blank Preparation 8. J Sample Train Description 1; t .i 1: Analytical Parameters Adeitional Comments 304g&f- A - AS '31 pc A n a l v t r d ace F. ie-ld & Air Services I I Field Data Sheet BACK TO MAIN Operators Source Gas Temperature ! fstimated Moisture Content L Concurrent Airflow: c]Yes Inches Hg OF O/O vlv 0 No Pump Type: @Constant Rate 0 Stroke Counter ldentification Number 13W4 Sample Type: OSource Sample Medium: 0Filter Ambient c]Personal c] Sample Medium 1.0. No. Backup Medium I.D. No. \lank Preparation \- i I'Sample Train Description S;[iC, u T& - 395SG- A nalytical Parameters 1kdditional Comments ("r) .: *Isrr169 2. 0,57 pm \ AS 131 ace Analvtical Field & Air Services S?F--PLE- C O L L E C T / E n J UFFjel d Data Sheet BACK TO MAIN B ' Project Sampling Location Date d-c-zq' 48 Test No. I Operators 7 = 4 5 P K r rr' Barometric Pressure r m L , Source Gas Temperature A 2- 1 - Inches Hg Y II Estimated Moisture Content h).h % VIV Concurrent Airflow : Yes YmO Pump Type: Faconstant Rate Stroke Counter Identification Number / I 23 Sample Type: OSource m m b i e n t 0 Personal Sample M e d p w w a r b o n Tube 0lmpinger 0Other Sample Medium I.D. No. Backup Medium I.D. No. t Sampling Method n%kc7-1vE? Sampling Time Sample Sampling Rate Start stop Duration Rotameter Callbrated Sertinc LPM 18:Yo /2-'@ - (28,+,,, c ,(7% Initial Count - Stroke Counting Sample Final Total Stroke volume Count Strokes Volume - - / 1 )2 . d L- t.I Blank Preparation 1 Sample Train Description J .: Analytical Parameters !< I L. .9dditional C o m m e n t s 3045c;- Z A k & - I AS '31 A eA n w a l Field & Air Services I' n BACK TO MAIN -\ I i Project c oV # W c F -: Sampling Location Pump Type: W n s t a n t Rate Stroke Counter Identification Number - a97 Date 6 - = 9 - T g Test No. ,AS, ample Type: U S o u r c e M m b i e n t 0 Personal ' f h Operators T e k , Barometric Pressure Source Gas Temperature /up Inches Hg * - 5 c SY Sample Medium: a l t e r c]Carbon Tube 0lmpinger Other Sample Medium 1.0. No. G P5 +CS-&L~ \ Estimated Moisture Content , M A Concurrent Airflow: C] Yes % v/v w3\Jo Backup Medium I.D. No. Sampling Method G L L - C7-r v & t 1I ',Blank Preparation 1; Sample Train Description . 1.. 1 Analytical Parameters Additional Comments i 30%- G 4- B - 1N \ VY -- - ceu \ gF7 AS 13! P- ace Analvtrcal Field & Air Services 9 5%&E 6cCe-.?--tc)J I Field Data Sheet BACSKTTAOQMAIN I I i\ I Co&@ Project ./ - [-Sampling Location % -WA=+++ Date 4/29&? Operators w L ~ Test No. bY.6 (R) Barometric P r e s s u t Inches Hg , Source Gas Temperature OF Estimated Moisture Content % vlv kiConcurrent Airflow: 0Yes No Pump Type: EConstant Rate Identification Number 5351 Stroke Counter Sample Type: Sample Medium: Source Ambient 0 Personal 0 0 Filter Carbon Tube -d 0 lmpinger p o t h e r Sample Medium I.D. No. Backup Medium 1.0. No. Sampling Method [{ RNou.n 1' 1 2 Sampling Time Start stop 8;43 Sample Duration i9rtt;n Sampling Rate Rotameter Calibrated Setlinq LPM 0853 Initial Count Stroke Counting Final Count Total Stroke Strokes Volume Sample Volume 1 3lank Preparation I :Sample Train Description 1 3nalytical Parameters 3 O q 55&?-8 - AS 13t ace Analytical . Field & Air Services f BACK TO MAIN Project Sampling c C O \ / . 4 * v c E Location Pump Type: Identification =onstant Number Rate Stroke Counter do 64 Date 6 2y -9 Test No. Sample Type: OSource WArnbient Personal 0 (-< Operators Te / s e K Sample Medium: Filter &rbon Tube ` Barometric Pressure td* Inches Hg lrnpinger Source Gas Temperature I 5 C .:PSample Medium I.D. No. I { Estimated Moisture Content w pr Ol0 v/v Backup Medium I.D. No. Concurrent Airflow: 0 Yes 0 - - Sampling Method h-* Other ve Run Sampling Time Sample Sampling Rate ' z,s, No. Start stop Duration Rotameter Calibrated Settino LPM lo-40 /2:% / 1.12 2 3 I"1 4 E 6 Initial Count - Stroke Counting Final Total Stroke Count Strokes Volume Sample volume / - - jYZ3bL .I 1 Blank Preparation i, Sample Train Description Ik j: I Analytical Parameters - . Z O q S C 3A & - AS 131 C ace Analvttcal Field & Air Servicks BACK TO MAIN 1 Project 0V,WCf Pump Type: w o n s t a n t Rate Stroke Counter C Sampling Location - ' ['Date -23 7 w T/* I-' * c OBapreormateotrrsic Pressure Test /reg Source Gas Temperature ,a. ! * Estimated Moisture Content Concurrent Airflow: No, .& , InchesHg r.9"cQF- % v/v Yes Em0 IdentificationNumber ??a d - ? { Sample Type: USource Ambient Personal Sample Medium: m l t e r 0 Carbon Tube 0 lmpinger 0 Other Sample Medium I.D. No. &GGL Backup Medium I.D. No. Sampling Method 6 ~A47r-r 1 U E Blank Preparation i -_ I:Sample Train Description I 4nalytical Parameters Additional Comments n 3 0 95 &/=-e- a03 1 1. AS 131 S i L t P C G GuEcmUk' iiel d Data Sheet BACK TO MAIN $Operators T66/312IL I 3arometric Pressure Source Gas Temperature iI Estimated Moisture Content Concurrent Airflow: 0 Yes I'( Pump Type: @Constant Rate Stroke Counter Identification Number &E loll% Inches Hg Sample Type: USource gArnbient c]Personal 64 sil'i& Sample Medium: 0 Filter Carbon Tube 0 lmpinger WOther OF Sample Medium I.D. No. Yo vlv Backup Medium I.D. No. No Sampling Method *~~ Sampling Rate Rotameter I Calibrated Settin Initial Count Stroke Counting- Final Total Stroke Count Strokes Volurns Sample Volume 10642 9 ii )lank Preparation & Sample Train Description 5;I'lq L u halytical Parameters 3OYESG- c - I * &I 'nddit ional Comments WEto186 = Q4 b m t t 1 A S 131 Field & Air Services BACK TO MAIN 1 I cp%N Project ce A Sampling Location Date 6 I 7-!7-5 Test No. Ir- Operators 7&/ s # K 1 Barometric Pressure )y\* Inches Hg Pump Type: Constant Rate Stroke Counter Identification Number E /..gp Sample Type: USource Ambient Personal Sample Medium: [7 Filter p a r b o n Tube [7 lrnpinger 0Other ~ Source Gas Temperature 2 1 -SocJ7 Sample Medium I.D. No. 1c. Estimated Moisture Content 0 Concurrent Airflow : Yes f- I o/o v/v BNo Backup Medium I.D. No. Sampling Method ZQhtTIvE Sampling Rate -Rotameter CaE;ted Settina Initial count /*.I33 Stroke Counting I Sample Final Count volume Total Stroke Strokes Volume i Blank Preparation E. Sample Train Description r'l I Analytical Parameters 1 Additional Comments A 3Y9C-/Ai:B - A d AS 131 ace Analvtical Field & Air Services 5mt- Fde)li 6LLEC-r, 0.J Data Sheet BACK TO MAIN ! I Project . I 2 Sampling Location 1 - 0 Date A 2 5 -98 0 [-> Operators Test No. Pump Type: Constant Rate Stroke Counter Identification Number a74 Sample Type: C]Source =Ambient Personal Sample Medium: @Filter Carbon Tube , Barometric Pressure AJft- Inches Hg Source Gas Temperature 2 I a rc 0 lrnpinger GS Sample Medium 1.0. No. Other 5 58- 1 Estimated Moisture Content 1 fi A O h v/v Backup Medium I.D. No. Concurrent Airflow: Yes B N o Sampling Method Sampling Rate I Stroke Counting I Sample 1 Blank Preparation ! L-. Sample Train Description E: Analytical Parameters i Additional Commen?s f l 347 CG- AS l j ! A ace Analytical Field & Air Services 5U-f- IFi ic=no.* e I d Data Sheet BACK TO MAIN \ Project COVWCE Sampling Location Pump Type: gConstant Rate Stroke Counter Identification Number 3, ) 3 Y Y $ 7 b a t e A -27-9 Test No. Sample Type: OSource @Ambient c]Personal r-- Operators *T&-+&/SK& / a Barometric Pressure dA -e G.C~ Source Gas Temperature I Inches Hg Sample Medium: c] Filter 0 lrnpinger +FSample Medium I.D. No. 0 Carbon Tube @Other cp I Estimated Moisture Content fl74 Concurrent Airflow: 0 Yes NO &-* % v/v Backup Medium I.D. No. Sampling Method T) Run 12 Sampling Time stop Sample Duration Sampling Rate Rotameter Calibrated -Setting LPM 0.41 Initial -Count Stroke Counting I' 3lank Preparation fiSample Train Description -r I 4nalytical Parameters 3q75G-A - nalvtrca I Field & Air Services - BACK TO MAIN I ' Project r: B Ea069 Sampling Location Date f/>--24-4* Test No. T&G /SA f" 0 E ~ ~Pressure&~. ~ I Inc~hes Hg Pump Type: B C o n s t a n t Rate identification Number c]Stroke Counter Sample Type: U S o u r c e E A r n b i e n t c]Personal Sample Medium: Filter Carbon Tube t ~ c lrnpinger Other ' Source Gas Temperature a i - 5 " ~4. Sample Medium I.D. No. I Estimated Moisture Content -& % v/v Ba? ckup Medium l I.D. N- o. Concurrent Airflow: c]Yes P N o Sampling Method Ta-fCTIY* y Run f; No. I Sampling Time Start Stop Sample Duration Sampling Rate Settinq Initial Count Stroke Counting Final Count Total Stroke Strokes Volume Sample 1 Blank Preparation Sample Train Description 349c-Ga fl tl Analytical Parameters I- Additional Comments CChr)b-L T d S AS 131 (? Field & Air Services 1 i 1 Field Data Sheet BACK TO MAIN 'I Project n (,OV74+ Cf- Pump Type: m o n s t a n t Rate Stroke Counter 1 - f-1 Sampling Location Date c 7-9 98 . Operators +7& Identification Number Fa77 1-54 . I 0 Test No. Sample Type: U S o u r c e F m b i e n t Personal Sample Medium: m i l t e r Carbon Tube Barometric Pressure pfi Inches Hg c]lmpinger c]Other Source Gas Temperature &2 !. 5 ' c d Sample Medium I.D. No. GIfi55 f i d k I ,A- i Estimated Moisture Content i 0 Concurrent Airflow: Yes % v/v Em0 Backup Medium I.D. No. Sampling Method Run Sampling Time Sample No. Start stop Duration - 1 14:OS 2 16: / a 123,,, Sampling Rate Rotameter Calibrated Settina LPM / 2o4 3 4 -e- 6 Initial -Count Stroke Counting Sample Final Total Stroke volume Count Strokes Volume e - - as3.321 ,Blank Preparation t 1 .Sample Train Description 34q61.F-B Analytical Parameters cLl3s I ' I Additional Comments r: BACK TO MAIN &LECnciJ I F i e l d Data Sheet I i Project ~o .Sampling Location ['Date 6 29 -Ys v , w ~ ~ Pump Type: $1Constant Rate 0 Stroke Counter f3 IdentificationNumber BFE !&7d-BL .I, Test No. Sample Type: OSource BArnbient c]Personal tc Sample Medium: 0Filter 0 Carbon Tube :[ Pressr'2A Inches Hg 0lmpinger wothe&E+ 1 Source Gas Temperature Estimated Moisture Content Concurrent Airflow: c .' ai.s o cPT Yo v/v Sample Medium I.D. No. Backup Medium I.D. No. L I C r4 &?L " I Sample Duration I23/h,H Sampling Rate Rotameter Settinq Calibrated LPM - 6s-l Initial Count - Stroke Counting Final Total Count Strokes c - Sample Stroke volume Volume - J273L I 3.lank Preparation t.iSample Train Description i lnalytical Parameters \ Additional Comments r- 3 q 9 sc)-A - 0 . s Lfm A S 131 ace Analytical , Field & Air Services BACK TO MAIN ng iratn Field Data Sheet 1 I 1 Project ccV . W C - F a 7 3 Pump Type: Constant Rate Identification Number Stroke Counter / i Barometric Pressure ~ Source Gas Temperature 1I Estimated Moisture Content Concurrent Airflow: Inches Hg G L i , 5"c--oFi' f l .A Yo VIV Yes BNO f l Sample Type: USource S r n b i e n t c]Personal Sample Medium: Filter Carbon Tube 0lrnpinger Other Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method k4 x mcr,c/& I 1 21 3 [_* Blank Preparation 1 : Sample Train Description f Analytical Parameters 1 Additional Comments n 13x7-344 B - A S 13: f ace Analvtrcal Field & Air Services , BACK TO MAIN \ I IC;\ Project C V Ad = E Sampling Locat Pump Type: @Constant Rate aStroke Counter Identification Number 45347 .Date 6 . 2 rI OBapreormateotrrsic Pressure Source Gas Temperature . . I 0. Sample Type: C]Source @Ambient Personal a Sample Medium: @Filter Carbon Tube 0 d k Inches Hg lmpinger c]Other a c+ I a 5 - e --4F, Sample Medium I.D. No. FS E@- I Estimated Moisture Content Concurrent Airflow: 0 Yes % v/v BNo Backup Medium I.D. No. Sampling Method 774ACT,lAE 1 :Blank Preparation e. 1 Sample Train Description 1- I; Id I A naIyticaI Paramete rs 1. Additional Comments /I 349 &-e - - / a n-al Field & Air Services 5G- CrLECTlo.d Field Data Sheet BACK TO MAIN I I Project c -Samplin Location 8 Date -7 9 Operators i- A, n ! Barometric Pressure 5,) Source Gas Temperature Test No- . , Inches Hg I ST Pump Type: Constant Rate ldentification Number Stroke Counter S3 Sample Type: a S o u r c 7 G a m y i e n t g b e r s o n a l Sample Medium: 0 Filter Carbon Tube lmpinger m o t h e r G s F . Sample Medium 1.D. No. CA- Gr-L I Estimated Moisture Concurrent Airflow: Content A % v/v 0Yes Po Backup Medium I.D. No. Sampling Method k-Cr, vz? I 3lank Preparation Lz Sample Train Description L, 4nalytical Parameters 3 4 4 SG--IC. Additiona1 Comments 5 ' 1 c * Get- 'z 0 - T / L p , p-LOLL.' AS 131 ace Andvtical Field & Air Sorvichs BACK TO MAIN [ Barometric Pressure &k 1 Source Gas Temperature 21.8 'c Estimated Moisture Content 5% 5 I Concurrent Airflow: 0 Yes Inches *Hg % v/v EN0 Pump Type: @Constant Rate [jStroke Counter Identification Number E 1/58 Sample Type: Sample Medium: Source @rnbient 0 Personal 0Filter @Carbon Tube a lmpinger Other Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method k c nv s Sampling Rate I Stroke Counting d w d Blank Preparation L 1.". Sample Train Description q&q 3 0 Y 5 C - j A 2 t Is2 i Analytical Parameters 1 Additional Comments ! I' r I r/n AS 131 BACK TO MAIN fi :Barometric Pressure N* Source Gas Temperature 21.8 ; Estimated Moisture Content 5Y.5 Concurrent Airflow: Li IJ Yes I I I Inches Hg bF, % v/v WNO Pump Type: %Constant Rate Stroke Counter a Identification Number 443 47 S m p k Type: OSource Ambient Personal Sample Medium: Filter Carbon Tube 0 lmpinger 0 Other Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method & VF Sampling Rate Rotameter Calibrated Setting LPM Initial Count Stroke Counting Final Count Total Stroke Strokes Volume 1 Sample Volume 1 3lank Preparation Sample Train Description 6149 f,!% f-; \j-p, 3WG+= A 2 . Analytical Parameters 1 Additional Comments (2)'47347 5 2,O( Ppm I A S 131 ace Analma1 Field & Air Services BACK TO MAIN I I hl I Project an@ c sampling Location Pw) 3 4 9 bv JW a-. [.Date 6~ 4 Operators % 8 Test i o . K /le0 0 aika $ bI arometric Preseure /dA Inches Hg -< Source Gas Temperature z \ * 8 % Pump Type: @Constant Rate Stroke Counter Identification Number 13 969 Sample Type: OSource Ambient Personal Sample Medium: Filter Carbon Tube lmpinger Bother Sample Medium I.D. No. i Estimated Moisture Content Concurrent Airflow: 5-9.4 Yes % v/v Ita No Backup Medium I.D.No. Sampling Method [>lank Preparation f iL Sample Train Description 5,\:4 T& V Analytical Parameters 3oq3-%-- fi2 - - A S 131 ace An-al Field & Air Services 5 r n L E . GLLm-w. G D a t a Sheet BACK TO MAIN Project L J ~ ~ Q .'Sampting Location r& 'Date b!v!qg [-'Operators 1s 1 Barometric Pressure Nb+ Inches Hg Source Gas Temperature ?I-!? 'c- % I Estimated Moisture Conten,t% , % v/v Concurrent Airflow: Yes ELNO Pump Type: &%onstant Rate 0 Stroke Counter Identification Number E233 Sample Type: OSource BAmbient Personal Sample Medium: c]Filter UCarbon Tube 0 lmpinger Other Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method W c r vre Initial -Count Stroke Counting Final -Count Total Strokes z Stroke - Volume Sample Volume b 3lank Preparation a". Sample Train Description &&/bp -304q-p- Z A Z + Z k Z - ~ II Jnalytical Parameters I ' Additional Comments i.: (w5 ) *E273 = 0,60 Poln I e An&tical ~ Field & Air Services BACK TO MAIN Projec, buanQ '-:Sampling Location wq M I 'Date 6/30/4x I- 1 loperators Lo 15p IC Barometric Pressure f l P 1 s , Source Gas Temperature 21-8C- Estimated Moisture Content $9- E '7 Concurrent Airflow: Yes bi Inches Hg 9e % vlv @No Sample 'F-stop b-3Y Duration 27 IUIA ! Pump Type Cons ant Rate 0 Stroke Counter ldentification Number E 277 Sample Type: USource &Ambient c]Personal Sample Medium: &Filter c]Carbon Tube c]lmpinger c]Other Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method &,mPcflVE r , ,Blank Preparation i Sample Train Description Llss,+;b&\hq - \ L l \J lnalytical Parameters 30ygc4- ZL f AS 131 -Field & Air Services Midget Sampling Train Field Data Sheet BACK TO MAIN Project h 241e aampling Location ,d [;ate S K K I ~ pperators TU '. 3arometric Pressure 3745 00 Hdi )a /&L; [b) Test N o . - L . RI* Inches Hg , Source Gas Temperature Z \ S i % l Zstimated Moisture Content 59.6 Concurrent Airflow: ayes NOOO/ viv Pump Type: UConstant Rate Stroke Counter Identification Number 4 5-35] Sample Type: USource @Ambient Personal a Sample Medium: Filter lrnpinger Carbon Tube Other J&!%i$d! Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method s.t . 4 -. C 7f I V E I 3lank Preparation I,. 1.: 5;I Sample Train Description i~ I T& - 30455G-Dz 1 Additional Comments ( * S ) *4535I = 0.53 brn I 1 h. Field & Air Services A j i e l d Data Sheet BACK TO MAIN I Barometric Pressure Inches Hg , Source Gas Temperature ZI.6 ' t- % 1 Estimated Moisture Content 68-1 O/O v/v Concurrent Airflow: Yes I8No Pump Type: E C o n s t a n t Rate Identification Number E Z W Stroke Counter Sample Type: USource @Ambient Sample Medium: 0Filter @Carbon 0lrnpinger 0Other Sample Medium I.D. No. Personal Tube Backup Medium 1.0. No. Sampling Method 3lank Preparation I - 4nalytical Parameters >' AdditionaI Comments Ern69 3 1.1h( m Field & Air Services BACSKTTAOQMAIN Project L7 ll&.\Co Pump Type: H C o n s t a n t Rate c]Stroke Counter 'Sampling Location 'Date b h d q 8 1 .-bo..l04 h;Xdo.jt hlI5 Test No. Identification Number E27Y Sample Type: OSource Ambient 0 Personal ,*Operators 760MK/E~ /, Barometric Pressure AJA Inches Hg Sample Medium: $IFilter Carbon Tube lmpinger flOther Source Gas Temperature z'*6 1 ,L Estimated Moisture Content D Concurrent Airflow: Yes a,f -I % % v/v No Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method MhC Y I V F l Slank Preparation h. _.I Sample Train Description E 61455 +\ c lnalytical Parameters 1 AdditionaI Comments f i,: 3@ s/ &-74 I AS 131 Field & Air Services 1 6 g & p L E lf.LflO/J Field Data Sheet BACSKTTAOQMAIN r'roject cn\kmcp ?ampling Location h q y;qh &? &I+ I b a t e ~ I Z P148 Test No. iWIw operators 7~b F' i larometric Pressure (J-A Inches Hg x Source Gas Temperature 21-6 ? ' ,L. istimated Moisture Content % v/v BF Pump Type: trl/Constant Rate Stroke Counter Identification Nu rnber E ol 11w Sample Type: USource @Ambient 0 Personal Sample Medium: 0 Filter 0 Carbon Tube lmpinger @Other si bd Sample Medium I.D. No. Backup Medium I.D. No. Concurrent Airflow: 0 Yes @No Sampling Method I I 5 i lank Preparation 51;~& 1.- Sample Train Description f' rL k J 6 3 0 ~SyG- A S 131 ace Analytical Field & Air Services Tr=lhFieId Data Sheet BACK TO MAIN I 1 ' Project bmLyz14 Jsampling Location &ionstant Rate Stroke Counter 3u4 & h k ? & 43(r d ~ ~Numbe~r E i m ~ ~ ~ [:Date ~ 3 / 4 ~ Test No. 2 Sample Type: USource &Ambient Personal .A Operators T&/S(?K ['Barometric Pressure Inches Hg Sample Medium: @Filter 0 lmpinger Carbon Tube Other [ Source Gas Temperature @ Estimated Moisture Content Concurrent Airflow: 0Yes PT Sample Medium I.D. No. aYOv/v No Backup Medium I.D.No. Sampling Method -, -*AA-tr/V Sampling Rate Rotameter Calibrated Settinq LPM I Stroke Counting Initial Count I 1 I I 1 I I I I I I I I I I I I I I I Sample Volume 3lank Preparation LE - Sample Train Description &qs31kt 4nalytical Parameters I1 [Additional Comments (SKCI) %277 3 4 9 g - B2 I AS 111 nalmal Field & Air Services r I i r^LLECT-IOd Field Data Sheet BACK TO MAIN I I ' Project doan@ 3q9 an ~ (0) ~ r 4 h ~ Pump Type: WConstant Rate 0 Stroke Counter Id~entifica~tionNu~mber r 459-S1 ,ud Source Gas Temperature Test No. -. 2 1 a Inches Hg Sample Type: 0Source Ambient c]Personal Sample Medium: 0 Filter Carbon Tube 0 lrnpinger m o t h e r s'ce YSample Medium I.D. No. i Zstimated Moisture Content +K I: Concurrent Airflow: 0 Yes o/o v/v EN0 Backup Medium I.D. No. Sampling Method r I 1 * I I ' I I [-I Sampling Rate -Rotameter Set tinq Calibrated LPM O,j31 Initial -Count Stroke Counting Final Count Total Stroke Strokes Volume - - - I Sample Volume 1,>!lank Preparation Sample Train Description Analytical Parameters i! I ',,dditional Comments s\l;a 4 I& - 34*?S.e-Bs.L 1 ace Analytical Field & Air Services BACK TO MAIN i Field Data Sheet I I e,,,,, I [ Project %;ping Location 30 4'5- r' & Z ? - 4 8 Test No. I Operators T< 4 flj t Barometric Pressure AT Inches Hg I Source Gas Temperature a a F 1 Estimated Moisture Content .G* % VIV Concurrent Airflow: 0Yes E m 0 e- Pump Type: c]Constant Rate Identification Number 0 Stroke Counter E /4e Sample Type: Source-bient 0Personal Sample Medium: 0Filter Carbon Tube 0lmpinger m o t h e r h a Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method 6 e P - S Sampling Rate I Stroke Counting I SamDie 1 1 Blank Preparation t I,Sample Train Description Analytical Parameters Additional Comments - - - - AS :3: BACK TO MAIN Train Field Data Sheet I Project n( o V . l y 3 C E [i Sampling Location K.0- 7y7 Pump Type: Constant Rate ldentification Number Stroke Counter Date ~ - 2 ~ - T~est kNo. f <-* 1 ' OBapreormateotrrsic Pressure 1 Inches Hg Sample Type: OSource BArnbient Personal Sample Medium: 0Filter 0lmpinger LL- Carbon Tube Other < , Source Gas Temperature 2 I * 1 Estimated Moisture Content b Concurrent Airflow : 0 Yes cYo viv EN0 Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method ~~ ~ ~~ Sampling Rate Rotameter Calibrated Settina LPM ~~ Initial count Stroke Counting Final Count Total Stroke Strokes Volume Sample [,Blank Preparation I-': Sample Train Description I Analytical Parameters Additional Comments - - - - L A S 131 ace AnalvtrcL Field & Air Services r It ' LE c C<-T'Ur/ Data Sheet BACK TO MAIN 1 i Project Sampling Location &Qh 3aoLj Pump Type: 0Constant Rate 0Stroke Counter Identification Number PrH3 i Date d-3' -9 g Test No. I Sample Type: U S o u r c e B A m b i e n t c]Personal ; Operators T&G< Sample Medium: Filter c]Carbon Tube I- fi( l Barometric Pressure p- Inches Hg c]lmpinger a O t h e & - 6C , Source Gas Temperature 7 Estimated Moisture Content fl*?&F <Sample Medium I.D. No. v/v Backup Medium I.D. No. fwz%Q Concurrent Airflow : 0Yes @No Sampling Method Sampling Rate Settin Initial count Stroke Counting I Final I Total I Stro~k- e Count Strokes Volumc Sample Volume 1 Blank Preparation kLW Sample Train Description f" l.i IAnalytical Parameters .4dditional Comments -c- 7 - - . AS '3: ace Analykal ( Field & Air Services BACK TO MAIN r i n - Field Data Sheet j I Y Pump Type: Constant Rate Stroke Counter Identification Number l r ) -Ra, Too Sample Type: @uce 0Ambient Personal i-, Operators -%? Barometric Pressure Source Gas Temperature Sample Medium: Filter 0Carbon Tube 0 mk Inches Hg lmpinger N o t h e r &17CL- .a Ld'C 4 Sample Medium I.D. No. i Estimated Moisture Content % v/v Backup Medium I.D. No. Concurrent Airflow: U Y e s B N o Sampling Method A D W AAc)L K+ I I I Run Sampling Time SamDIe Sampling Rate No. Start stop J Duration Rotameter Set tina Calibrated LPM Stroke Counting 1 2 3 -4- -5- 6 1 Blank Preparation L.2 Sample Train Description i Analytical Parameters Additional Comments fi - - - L AS ' Y ! ace Andvtical Field & Air Services LCEt-rwy' rlg wain Field Data Sheet BACK TO MAIN Project rd&dCS [ , Sampling Location co * 3 c v - r I Date ~ ~ 3 0 - Tcest~No.~ -- Operators < Barometric P r e s s z L Inches Hg Source Gas Temperature &I.S"' I 1 Estimated Moisture Content 5 9. 5- o/o vlv Concurrent Airflow: F' 0Yes mo Pump Type: 0Constant Rate Identification Number A c]Stroke Counter cn h 30y T Sample Type: @Source 0Ambient Personal Sample Medium: Filter Carbon Tube c]lmpinger m o t h e r, - Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method e LJ- ~eP?-A&&.B*L- 0 e=&r Sampling Rate Stroke Counting I Settina I' I I I Blank Preparation Sample Train Description f i ' Analytical Parameters Additional Comments - c - i i. AS 131 e Advtical Field & Air Servichs Midget Sampling Train Field Data Sheet BACK TO MAIN SBAQ Project C o v ,+ ' t E- Sampling Location & 3YY Da.t+e - Operators <&Te-st No. Barometric Pressure Source Gas Temperature Inches Hg -z/.c: mF'- Estimated Moisture Content ,A!!&-- Concurrent Airflow: 0 Yes % v/v Pump Type: 0 Constant Rate 0 Stroke Counter Identification Number /J--&- 3y9 Sample Type: F $ s o m e Ambient 0 Personal Sample Medium: Filter Carbon Tube 0lmpinger B o t h e r- , Sample Medium I.D. No. Backup Medium 1. Sampling Method I Sampling Rate . - Rotameter Calibrated Setting LPM Initial Count Stroke Counting Final Count Total Stroke Strokes Volume volume BIank Preparation Sample Train Description Analytical Parameters Additional Comments - - 4 1 i AS 131 ace Analvtical Field & Air Services s P *L c -iing QnLLEC7Wd I rain Field Data Sheet BACK TO MAIN SUAQ Project c-53 Sampling Location d- +LJe e a '- Date 25-$s Test No. 1 Operators Ti&+ 4,z' Barometric Pressure z0 Source Gas Temperature Inches Hg A' "F Estimated Moisture Content hxk % VIV Concurrent Airflow: 0 Yes El No e.6 Pump Type: Constant Rate Stroke Counter Identification Number clr, COp4kF-dT s Sample Type: OSource WAmbient 0 B*6w Personal Sample Medium: =Filter H C a r b o n Tube c]lmpinger p t h e &Lr!-s Sample Medium I.D. No. q-iitn' Backup Medium I.D. No. Sampling Method e cK B'Wk Pa*.** wri a,. XEtOLJ I Analytical Parameters \ - / i AS 131 ace An&ticaI Field & Air Services SfifLC Cc L L k n t ? d T r h Field Data Sheet BACK TO MAIN Project cE Sampling Location Y* d C e &* Date 6''Q--qg Test No. I Operators Barometric Pressure Source Gas Temperature -/'* '70 Inches Hg "F Estimated Moisture Content &'.+ % v/v Concurrent Airflow: 0 Yes Em0 Pump Type: Constant Rate 0 Stroke Counter Identification Number -&I-. < rorr~. Sample Type: OSource m m b i e n t 0 e&&;' Personal Sample Medium: Filter @Carbon Tube fi GL glmpinger mother WPI Sample Medium I.D. No. 7 0t c)tK~c Backup Medium I.D. No. Sampling Method 8 C - k eRF9* TlU SaotJ I I Sampling Rate I Stroke Counting Sample Volume e Sample Train Description - - Li - t Analytical Parameters AS 131 . ace Andvtical 4- 344 1 &-27-7g BACK TO MAIN Pace Analytical Services, Inc. 1700 Elm Street - Suite 200 Minneapolis. MN 55414 Tel: 612-617-6400 F a : 612-617-6444 ace An-al . I i; ! 6 - 2 9 - ?g BACK TO MAIN - Pace Analytical Services, Inc. 1700 Elm Street Suite 200 Minneapolis, MN 55414 Tel: 612-617-6400 Fax: 612-617-6444 il e Analvm. al 6-z7 - 9 8 BACK TO MAIN Pace Analvtical Services. Inc. 1700 Elm Street - Suite' 200 Minneapolis, MN 55414 Tel: 612-617-6400 Fax: 612-617-6444 l- i I 1 ! J ' 327' -Z Si -1.. c r-----7 . , . I ace A n a l w a l (,-3O-?g BACK TO MAIN Pace Analytical Services, Inc. 1700 Elm Street - Suite 200 Minneapolis, MN 55414 Tel: 612-617-6400 F a : 612-617-6444 i e Advtrcal Field & Air Services BACSKTATOQMAIN l 1 , Project dvm@ 1- Samplin Location 1 'Date 673@/48 Test No. l-.,Operators T66 /SflC I 1, Barometric Pressure ZSA Inches Hg c*c Source Gas Temperature 2 1a 1 Estimated Moisture Content Concurrent Airflow: 0 Yes F % v/v BNo Pump Type: gConstant Rate Identification Number E 206q Stroke Counter Sample Type: OSource BAmbient 0 Personal Sample Medium: Filter BCarbon Tube lrnpinger 0 Other Sample Medium I.D. NO. Backup Medium I.D.No. Sampling Method g x n Q / F&f/ VE 1 3lank Preparation 1:Sample Train Description &b$ 'I q-nalytical Parameters Additional Comments IL ;J E a69 - Tubt I 7- 3@iC--2A&yi6q. e Analytical Field & Air Services BACK TO MAIN Project bU41ncE Pump Type: @Constant Rate c]Stroke Counter I (-Sampling Location h s f i k m n w +(turn Date 6 k JI48 Test No. rwOperators 1 6 6/J PIC- Identification Number E 2-H Sample Type: OSource @ Ambient 0 Personal Sample Medium: $I Filter c]Carbon Tube 1, Barometric Pressure Inches Hg lmpinger 0Other 1 Source Gas Temperature 4 L U s 5C -T Sample Medium I.D. No. 1 Estimated Moisture Content hl f% " Concurrent Airflow: nyes Yo vlv @NO Backup Medium I.D. No. Sampling Method n Q A c7-Jv s Sampling Time Start I Stop Sample Duration Sampling Rate Rotameter Calibrated Seltina LPM - 2\07 I Initial Count Stroke Counting Final Count Total Stroke Strokes Volume Sample t 1 3lank Preparation L, $h Sample Train Description 61455 [ - ,: $ltW I qnalytical Parameters I '-Additional Comments (SW) *E2-71f 300 w- G AS 131 ce Advtrml Field & Air Services BACK TO MAIN i' Data Sheet I \i Project IbWW cn W n%f r w oklccr(\ Pump Type: &Constant Rate Stroke Counter Identification Number BfE la 1186 hate ~~ 0 Test No. Sample Type: OSource Ambient Personal t.w 766 Sample Medium: 0 Filter Carbon Tube 9 ~Pressurre - ~ A ~ t Inch~es, Hgc 0 lrnpinger H o t h e r 'h~ 1, Source Gas Temperature 2 h f;c@ cL, 2F Estimated Moisture Content Concurrent Airflow: 0Yes % v/v %No Sample Medium I.D. No. Backup Medium I.D.No. Sampling Method G7-j V Blank Preparation i-. I:Sample Train Description & J& v - ( 5 ) , A I ' 4 nalyt i c a I Param elers \+ I ~ Additional Comments I' BFE lo\186 54 B - Field & Air Services I fl Field Data Sheet BACaKJTAOkMl AIN 1 Project hhlw 1-*SamplingLocation 'Date 6 f 3/q% bflyq h u - ~ (A) Test No. 02 \ Inches Hg ' Source Gas Temperature / S / . S G q=- Estimated Moisture Content I Concurrent Airflow: de* Yes Yo viv KJBo II; 11% Pump Type: MConstant Rate Identification Number E 0 Stroke Counter Sample Type: 0 Source @Ambient [rl Personal Sample Medium: Filter @Carbon Tube 0 lmpinger 0 Other Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method M h C 7 ) vi5 ] 3lank Preparation L Sample Train Description t L ,. Analytical Parameters L!Tube - 34~c+t2 I.\ Additional Comments E It58 + 162 AS 131 r 1aiVI i c ~ Field & Air Servichs /Field Data Sheet BAC25K1 ATOUMAIN b 1 &l1)&\@ Project - Sampling Location PoOa 3q9 \)cu;T A) IPlY /9x Test No. =L ,,Operators TfhIfPIC [ Barometric Pressure Source Gas Temperature A InchesHg /-ai.S'L I IJ l Estimated Moisture Content i Concurrent Airflow: @A- Yes Yo VIV EN0 Pump Type: HConstant Rate Identification Number 9j3Y7 Stroke Counter Sample Type: USource %Ambient Personal Sample Medium: @Filter Carbon Tube 0 lmpinger 0 Other Sample Medium I.D. No. Backup Medium I.D. No. Sampling Method &&vk c.n Y F -5- 2 ,OZ Stroke Counting I SamDle i 3lank Preparation I4nalytical Parameters I `ndditional Comments A S 131 .s.iw'e CoLLEerIod 1 Field Data Sheet BAC3K1TAOUMAIN i - lank Preparation L. 'Sample Train Description 1- ( : ,Analytical Parameters s\ 1;s 2 TJX 3q79--A2 A S 131 a . Field & Air Servicgs v i e r i e l d Data Sheet BACKSTTOAMQAIN Project ~ D + M Q Pump Type: $/Constant Rate 0 Stroke Counter i Sarnplin Location kfl 374 h $ h rakli3) IdentificationNumber bbl% .A, a t, Date Test No. Sample Type: C]Source Ambient Personal /sp Tb6 Sample Medium: 0 Filter $J Carbon Tube 1I, ~ ~ rP r ~e s s~u r :~h l At ~Inchecs Hg 0 lmpinger Other daj Source Gas Temperature ' Estimated Moisture Content a 5 % 4Sample Medium I.D. No. Yov/v Backup Medium I.D.No. Concurrent Airflow: r] Y e s $(No Sampling Method iCTQr74ACTf P Blank Preparation L. Sample Train Description cat"br 3L/pc72fl3 + d P a i: f 3AnaIyticaI Parameters hdditional Comments CJKC5-J k . 7 3 AS 131 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO:FS-980618-1 9.6 Field Data Printouts F I',. Bt ! tE,:: 1. Revision 0 '-.--.I --..1.2 1 .8 .6 .4 .2. 0 1200 11b0 Absorbance / Wavenumber (cm-1) File # 1 = COO21 Rm. 3045 racks 4+5,static,-90M,amb,IH inst. BACK TO MAIN 1 5 4 M-l 1do0 9b0 800 Stacked X-Zoom CURSOR 6/29/98 9:31 AM Res=None -._. I--. .4 .3 -2 .l 0 -.1-.2 Absorbance / Wavenumber (cm-1) File # 1 = COO34 Rm. 349,,static,-SOM,amb,IH inst. BACK TO MAIN k 3000 ... - - 25 IO 2000 --------- ------------1500 1alii---- Stacked X-Zoom CURSOR 6/29/98 1O:Ol AM Res=None - - --f 1 ___'--.rc -7- .8 .6 .4 .2 0 -.2 4000 ._ . - _-.- - -. . --7-- - - - - 3d00 Absorbance / Wavenumber (cm-I) File # 1 = COO38 Rm. 3004 by grp G,static,-SOM,amb,IH inst. 3000 BACK TO MAIN 25b0 2d00 1500 1000 Stacked X-Zoom CURSOR 6/29/98 0:16 AM Res=None 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO:FS-980618-1 1 I 1 9.7 AutoQuant CLS Method G Revision 0 lethod Map generated 07-08-1998 3:25:07 PM Method Name: Ammonia I Yethod Path: C:\AUTOQ3\METHODS\AMMONIA\AMMONIA.ME : lethod Type: AutoQuant 3.0 ! Linear Analy- sis mode 'emperature & Pressure Adjustments: OFF I 1 [ass Emission Computations: OFF Parameters : Wavenumber range: Fingerprint zoom: 650.00 - 4500.00 650.00 - 1400.00 t re', Path Lenqth = 90 Interfere Criterion = 2500 L Gain number = .5 i t Apodization = Phase Correct = Resolution = Triangle Mertz .5 Baseline Correction: Quadratic 'iompound 0 : NH3 Alarms: Disabled Output: Disabled Spectrum: H85NH3.SPC Primary: Yes Reference concentration = 85.00 Region #1: 879.08 - 1044.79 i BACK TO MAIN 3M ENVIRONMENTAL LABORATORY BACK TO MAIN ET & SS STUDY NO: FS-980618-1 I I 9.8 Chains of Custody H C1 n f,: 1: \' Revision 0 Form 35176. PWO c Address C2 1 3M Project Tnlr CP- t T v m 3M Facllity Contact BACK TO MAIN I =Tu C o d r - , d A b # %s,- F S - ?Bb6 Jg - I 3MPmjdNumber 3M Department Number @r.o.nal Accwn@vyr*gSamples Last Page Orignator See Reverse Side For Instructions Form 35176 - PWO 1 -#Y Address Clty. Slate. Zlp Code I - - 1 !io&, 0 3M ProjectTHle O V MCs; 3M Facility Contact 3M Telephone Number BACK TO MAIN I '3 J rA7hrdL4T I ad F5 - 6 IQ- 1 3M Pro* Number W'O 3M DepartmentNumber Lab Requeslrremplale Number Item # /--/ a Time /I.'f1 4 Date Shipped Via 7b/9f-- By/Affiliation Time fL' Date 7/1h f . - ~~ See Reverse Side For Instructions ,mitt ui CUstody 3M EnvironmentalLaboratory Fom 35176 - P D #i- 10785 BACK TO MAIN rs-rcJ 3M Project Lead TnJ Item # 1 13 Relinquished By/Affil@ Time . I /.' f4 Date YA/W Shipped Via c)wnnal . A c c c r n o a n y q Samples Lasl Page .Oriqnrlor ~- See Reverse Side For Instructions --.--- f - - - r - - - u.liairfui Cuslody necoru - 3M EnvironmentalLaboratory Form 35176. PWO r"co0.q F--- , _ - _ A t- d -- - BACK TO MAIN Item # 1 - 13 Relinquished 6ylAffiliat.n Time 11: / q Date -711/ 9 f Shipped Via p c e i v r d By/Affiliafion Time / I za Date $/9f t I I I I I Orqinal . AccampanyingSamples Lasl Page. Orignator I I 1 See Reverse Side For Instructions -Form 351 76 - FWO Address 8 L / MCS2 CW. State. Zip Code 3M Project THle 3M / r Y FacllltyContacl w 4 3M Telephone Number BACK TO MAIN I 3M PrOjecl Number 7e.r I ~ n n p l ~ f$-980618- 1 3M DeparlmentNumber Lab RequesVlemplate Number U I927 item # L./@ Relinquished By/Affiiiatiop Time Date W I I /,`47 h178 f7 Shipped Via m v e $ By/Affiliation & Time /l,`z*r 1 Date 7A/?f-- d a i h uu C e 5 ~ d ~y c o- r ~ 3M EnvironmentalLaboratory Address =e r4-p 5 L, *d -- \ - -1 11506 3- Be%-AC.ewKesiTc.O MAIN I-d 3M Projecl Lead ST.d (? v&R/ce 3M Pro1 THle 0 3M Facllity Conlacl cnhlw$A-T,LJ /J -7. L * 3M Proled Number - 9Pcs(5/a- F S / 3M DeparlmenlNumber vsiaiflUY Cktddy necorcj 3M Environmental Laboratory Form 35176. PWO Address IC V Stale ZlpCode 11507 BACK TO pa tie quest at MAIN G 3 3M Project Lead F 3M Faclltty Contact I,3M Telephone Number 3M Pmlea Number 3M Departmenl Number ,I & 1937 Lab RequesVTemplateNumber item # Relinquished ByIAffiliation Time I . I/ /4F 3/ 3 I I Date 7-1-98 7/fhf- Shipped Via t meivp.d.By/Affiliation Time I / . 'za Date -.- --. O-qmaI . Accomoanymg SarnDler Lasl Page. Orignnlor See Reverse Side For instructions Form 3St76-,PwO Address City. State. Zip Code Ah / s o n L J r . 1 2 3 1. 4 5 6 7 -- 8 9 10 11 3M Facility Contacl 31 Telephone Number BACK TO MAIN I 3M Prujed Number !=</ 7Pd/,,p c 3M Deparlment Number II Lab RequesVTemplateNumber Number Containers of each Preservatives # E Samples Split See Attachment EE E 70 3* I'! s2! I 24 O-g-al. Accompanyhg Samples Last Page. Orignaloi See Reverse Side For Instructions CW. Slate. Zip Code . --- Sampler Slpnature 4-2 Item ' # 7 Samwe { ' DescriW o n 3M Telephone Number J- contrector f?eC_, Date 7- {-4s? Date Time Matrix Nu, I ber Cc of ea Preservz BACK TO MAIN Lab RequesVTemplaleNumber n [ AY7S3 Samples Split See Attachment 12 13 I Item # I RelinquishedBylAffillation-d Time I I r?ngwl . AcComovywq Samples L a d Page .Orignalor I I I See Reverse Side For Instructions n a i T CC3d)..Jcor, 3M Environmental Laboratory F o 35~176. PWO 3MF y /mnCOV- Address CF C i . State. Zip Code cf. / c_. .-&A - 3M FacllityContacl 3M Telephone Number SnJ- - BACleKquesTO MAIN --` t cJ-7-bJ 3M Pmjecl Number - /=-3-57go4 7&- ' r k i A n y r & I 3M DepartmentNumber Lab RequesVTemplale Number I I I I I 1 1 1 1 1 1 I I Lost Page. Orignslw See Reverse Side For Instructions 3M EnvironmentalLaboratory City. Slate. Zip Code BACK TO MAIN - *'.I .. 3M Requealer s 11537 T W '3M Prolea Lead I I3M Telephone Number II Lab RequesVTemplateNumber I 10 11 12 13 - Item # Relinquished By/Aff iliation 1- 6 Time //:/v I Date 3-1-9s Shipped Via c ) . ~ * a l LcrornDanvtng Samn1.S Lnsl Page. Orignator Time I/ Date -?/I/Sf See Reverse Side For Instructions