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HomeMy WebLinkAboutNC0003298_Monitoring Report_20111228NPDES DOCUWENT SCANNINS COVER SHEET NPDES Permit: NC0003298 Riegelwood Paper Mill Document : Permit Issuance Wasteload Allocation Authorization to Construct (AtC) Permit Modification Speculative Limits Monitoring Report Instream Assessment (67B) Environmental Assessment (EA) Permit History Document Date: December 28, 2011 IrJblas document le; prLated cork reuse paper - %aore aszy content on the re'erse Bide INTERNATIONALS PAPER RIEGELWOOD MILL JOHN L. RIEGEL ROAD RIEGELWOOD, NC 28456 December 28, 2011 Certified Mail: 7005 1820 0007 8389 4367 Mr. Jay Sauber Chief, Environmental Sciences Section NC DENR Division of Water Quality 1621 Mail Service Center Raleigh, NC 27699-1621 SUBJECT: Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, NC — 2011 Report NPDES Permit No. NC0003298 Dear Mr. Sauber: Please find enclosed the 2011 annual report for fish tissue dioxin monitoring conducted on the Cape Fear River in the vicinity of International Paper's Riegelwood Mill. If you have questions or need additional information, please call me at 910/362-4753. Sincerely, Kimberly W. Fa(l, P.E. Senior Environmental Engineer Enclosure cc: James H. Gregson, Surface Water Protection Supervisor NCa DENR — Wilmington Regional Office 127 Cardinal Drive Extension Wilmington, NC 28405 Jeff Poupart, Point Source Branch Supervisor NC DENR Division of Water Quality 512 North Salisbury Street Raleigh, NC 27603 -1.4viv@ig JAN - 3 N1 DEI, FTE QUALITY POINT 5�WfTCH kwf S:\Groups\Environmental\Wastewater\Fish Tissue1201 I\Annual Fish "I issue dioxin Report 2011 12281 I.docx DIOXIN MONITORING STUDY OF FISH TISSUE FROM THE CAPE FEAR RIVER IN THE VICINITY OF THE INTERNATIONAL PAPER COMPANY MILL AT RIEGELWOOD, NORTH CAROLINA 2011 REPORT Prepared for International Paper Company Riegelwood Mill John L. Riegel Road Riegelwood, North Carolina 28456 Prepared by CZR Incorporated 4709 College Acres Drive, Suite 2 Wilmington, North Carolina 28403 December 2011 DIOXIN MONITORING STUDY OF FISH TISSUE FROM THE CAPE FEAR RIVER IN THE VICINITY OF THE INTERNATIONAL PAPER COMPANY MILL AT RIEGELWOOD, NORTH CAROLINA TABLE OF CONTENTS Page TABLE OF CONTENTS LIST OF TABLES iii LIST OF FIGURES iii LIST OF APPENDICES iii 1.0 INTRODUCTION 1 2.0 METHODS 2 2.1 Sampling Stations 2 2.2 Species Selection 8 2.3 Sample Collection Methodology 8 2.4 Sample Preparation and Shipment 11 2.5 Chemical Analysis 12 3.0 RESULTS AND DISCUSSION 13 3.1 Fish Collection 13 3.2 Tissue Analyses 13 REFERENCES 21 ii LIST OF TABLES Table Page 2-1 Summary of physicochemical measurements taken in conjunction with fish collections on the Cape Fear River during 2011 7 2-2 Fish collection dates, techniques, effort, and fish caught in the Cape Fear oft, River study areas during 2011 9 3-1 Summary of 2011 fish composites submitted from three Cape Fear River stations in the vicinity of the International Paper Company Mill at Riegelwood, North Carolina 14 oft; 3-2 Fish composite data for three Cape Fear River stations in the vicinity of the International Paper Company Mill at Riegelwood, North Carolina, collected during 2011 17 3-3 Summary of analytical results from fish tissue composites collected in the ram, Cape Fear River near the International Paper Company Mill at Riegelwood, North Carolina, during 2011 18 3-4 Comparison of dioxin (2,3,7,8-TCDD) concentrations among gamefish and bottom feeder composites from the Cape Fear River from 1992 to 2011 20 Ant LIST OF FIGURES Figure Page, 2-1 Sampling Stations — Sites of Fish Collection on the Cape Fear River near Riegelwood, NC 3 2-2 Sampling Station 1 -- Site of Fish Collection on the Cape Fear River near Riegelwood, NC 4 2-3 Sampling Station 2 -- Site of Fish Collection on the Cape Fear River near Riegelwood, NC 5 2-4 Sampling Station 3 -- Site of Fish Collection on the Cape Fear River near Riegelwood, NC 6 LIST OF APPENDICES APPENDIX A: DIOXIN MONITORING STRATEGY APPENDIX B: NORTH CAROLINA SCIENTIFIC COLLECTION PERMITS APPENDIX C: LETTER OF TRANSMITTAL/CHAIN OF CUSTODY APPENDIX D: LABORATORY DATA REPORTS /02, iii eseAt Oto1 1.0 INTRODUCTION International Paper Company's (International Paper) NPDES permit (No. NC0003298) for the Riegelwood mill requires the collection and analysis of fish tissue for the presence of dioxins and furans. The mill is located along the Cape Fear River near Riegelwood, Columbus County, North Carolina. The dioxin monitoring program is administered by the North Carolina Division of Water Quality (DWQ), formerly the Division '" ) of Environmental Management. International Paper contracted CZR Incorporated (CZR) to ei`` collect fish samples during 2011. To maintain report consistency, the format and style of this report are similar to CZR Incorporated's past monitoring reports (1993 through 2010 "AN Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the Federal Paper Board's Mill at Riegelwood, North Carolina) which were modeled and derived from the September 1992 report (EA Report No. 12347.01) titled "Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of Federal Paper's Riegelwood, North Carolina Mill" prepared by EA Engineering, Science, and Technology, Inc. Monitoring protocols were established in September 1990 to comply with the Special rat, Order by Consent (SOC) EMC WQ No. 84-30 AD II effective 12 July 1990. The protocols comply with both the NPDES permit and the SOC. The following sections discuss sampling stations, sample collection techniques, sample preparation, and analytical results. else roit PAR 1 Alb1 2.0 METHODS o oft, ors,2.1 Sampling Stations ems Fish collections occurred in the sampling areas established from previous studies (EA Engineering, Science, and Technology, Inc., 1992). Sampling stations were originally selected as required by the current NPDES permit and SOC. North Carolina's current DWQ fish tissue dioxin monitoring strategy for the Riegelwood mill is provided in Appendix A. One station was located upstream of the mill's discharge and the remaining stations were located downstream of the mill (Figure 2-1). Station 1 is approximately 11 miles upstream of Lock & Dam No. 1 in the vicinity of Elwell's Ferry (SR 1730). This station is a control site located approximately 20 miles upstream of the mill ouffall and separated from the mill by a physical barrier, Lock & Dam ,", No. 1 (Figure 2-2). Station 2 is approximately 2 miles downstream of the mill discharge near Green Bank Landing (Figure 2-3). Station 3 is approximately 13 miles downstream of (A) the mill discharge near the confluence of the Cape Fear River and the Black River (Figure 2-4). Generally, fish habitat was sparse and varied among the three sampling stations. The available fish habitat consisted of inundated tree roots, aquatic macrophytes, (081 taken in conjunction with fish collections at each sampling station are found in Table 2-1. 611.111 Obo overhanging riparian vegetation, snags, and fallen timber. Physicochemical measurements LEGEND SAMPLING STATION + SITE OF PAPER MILL SOURCE: NORTH CAROUNA DEPARTMENT OF TRANSPORTATION, USGS TOPOGRAPHIC MAP MOSAICS, NC STATEPLANE, NAD83 FEET, 1:24000—SCALE, USGSTopoTile018,SID 0 20,000 40,000 SCALE IN FEET SAMPLING STATIONS SITES OF FISH COLLECTION ON THE CAPE FEAR RIVER NEAR RIEGELWOOD, NC SCALE: AS SHOWN DATE: 12/09/08 APPROVED BY: DRAWN BY: TLJ FILE: 1340-KEY ZR INCORPORATED DMNONYENEAL CONSILTUDS 4709 COLLEGE ACRES DRIVE SUITE 2 WILMINGTON, NORTH CAROUNA 28403 TEL 910/392-9253 FAX 910/392-9139 CP#1340.16 FIGURE 2-1 3 / ...„.„,„, -.42t,? ! 1 1 kt, `. .�Q�i� o f • .___,.... cr._ _. /, ,� lc -,,, )1: c,_ - .,,,,i1To ,:.\---\ _� `"mac- �-� — *--.. , \1'J _ ��s C—k ��.'_ 4. sue. • ► ��7'`'S (i __ NN --..,..._ c.____ ...... A Vil II �(1{ \jams _, - 73'' 1 '`‘, :......„ _.. /^ Nt h ,. >' r• i____ -- .� \`- 1 S "_� . . Q. �\\}J, . 1 .Y� ..��•2:@DO ;��/y: I :•�t�;� J 7T *4.''' BY • Ilk , ., . LEGEND SAMPLING STATION 1 SAMPLING STATION f... SITES OF FISH COLLECTION ON THE CAPE FEAR RIVER NEAR RIEGELWOOD, NC 0 2,000 4,000 SCALE: AS SHOWN APPROVED BY: DRAWN BY: TLJ DATE: 12/09/08 FILE: 1340—SP1 ,' : 4709 COLLEGE ACRES DRIVE CP# 1340.16 SOURCE: SCALE IN FEET NORTH CAROLINA DEPARTMENT OF TRANSPORTATION, USGS TOPOGRAPHIC MAP MOSAICS, NC STATEPLANE, NAD83 FEET, 1:24000-SCALE, USGSTopoTile018.SID SUITE 2 a � WILMINCTON, NORTH CAROLINA 29403 :' INCORPORATED TEL 910/392-9253 DMRONVENru CONSULT/MS FAX 910/392-9139 FIGURE 2-2 ))))))))))))))))))))))))))))))))))))))))))� LEGEND SAMPLING STATION SOURCE: NORTH CAROLINA DEPARTMENT OF TRANSPORTATION, USGS TOPOGRAPHIC MAP MOSAICS, NC STATEPLANE, NAD83 FEET, 1:24000—SCALE, USGSTopoTile018.SID 0 2,000 4,000 SCALE IN FEET SAMPLING STATION 2 SITES OF FISH COLLECTION ON THE CAPE FEAR RIVER NEAR RIEGELWOOD, NC SCALE: AS SHOWN DATE: 12/09/08 ZR INCORPORATED DMRONN[NTAL CON0ULT ATS APPROVED BY: 4709 COLLEGE ACRES DRIVE SUITE 2 WILMINGTON, NORTH CAROLINA 28403 TEL 910/392-9253 FAX 910/392-9139 DRAWN BY: TLJ FILE: 1340-SP1 CP# 1340.16 FIGURE 2-3 ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) ) 0) k . --- li.- , 4. .. i . _ a, ..... • 4 .... . ....... ...., ...' • _ . .. ..14. 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ON, Landjovi r - -/; 4. -AL a. • -a - • 6.5.„ - .4._ 4, • . - 4-1 Aa. - ic • - - 4. 1-4 ' 4.- ... 7 LEGEND SAMPLING STATION SOURCE: NORTH CAROLINA DEPARTMENT OF TRANSPORTATION, USGS TOPOGRAPHIC MAP MOSAICS, NC STATEPLANE, NAD83 FEET, 1:24000-SCALE, USGSTopoTile018.SID 0 2,000 4,000 SCALE IN FEET SAMPLING STATION 3 SITES OF FISH COLLECTION ON THE CAPE FEAR RIVER NEAR RIEGELWOOD, NC SCALE: AS SHOWN DATE: 12/09/08 APPROVED BY: DRAWN BY: TLJ FILE: 1340-SP1 ZR INCORPORATED DATRONUENTAL CONSULTANTS 4709 COLLEGE ACRES DRIVE SUITE 2 WILMINGTON, NORTH CAROLINA 28403 TEL 910/392-9253 FAX 910/392-9139 CP#1340.1 6 FIGURE 2-4 Table 2-1. Summary of physicochemical measurements taken in conjunction with fish collections on the Cape Fear River during 2011.a Station Date Time Temperature Conductivity (C) (pS) pH Salinity D.O Secchi (ppt) (mg/l) (in) 1 22 Aug 1915 30.6 218.9 7.3 0.1 8.05 38.75 1 23 Aug 1100 29.0 212.4 6.9 0.1 5.58 37.50 1 13 Sept 0940 27.2 191.9 6.4 0.1 5.73 --b 2 23 Aug 1615 29.8 224.6 6.9 0.1 5.37 42.50 2 24 Aug 0925 29.3 291.8 7.1 0.1 4.75 40.50 2 25 Aug 0925 29.1 297.4 7.1 0.1 4.21 43.50 2 13 Sept 1100 28.0 386.4 6.5 0.2 4.63 ----b 2 14 Sept 0800 27.6 380.0 7.1 0.2 5.52 29.50 3 23 Aug 1500 29.8 364.0 7.1 0.2 4.60 30.50 3 24 Aug 1200 29.4 338.0 7.0 0.2 4.30 32.00 3 25 Aug 1145 28.8 311.2 6.9 0.1 4.04 34.50 3 13 Sept 1455 27.5 250.7 6.6 0.1 4.04 ----b 3 14 Sept 1135 27.5 268.0 6.9 0.1 3.30 24.25 aMeasurements made 0.5 m below surface. bData not available 7 2.2 Species Selection The goal of the fish collection effort was to obtain four composite samples at each sampling location with each sample consisting of ten individuals of the same species and of similar length and weight. Larger (adult) specimens were given preference. Composites at each station were composed of gamefish and bottom feeding species fillets. Target species listed in the state's dioxin strategy include: • one composite sample for largemouth bass with sunfish (bluegill, redbreast, etc.) as fallback species; one composite sample for bluegill with other sunfish (redbreast, redear, etc.) as fallback species; one composite sample for catfish (order of preference being flathead, channel, blue, and others) or carp; one composite sample for catfish (order of preference being flathead, channel, blue, or others with fallback species as edible finfish). 2.3 Sample Collection Methodology Various active and passive methods of fish collection were used to obtain target species. Fish were collected under scientific fish collecting Permit Number SECP-707778 (North Carolina Division of Marine Fisheries) and License Number 11-SFC00004 (North Carolina Wildlife Resources Commission) (Appendix B). A telephone crank generator was used in an attempt to shock catfish while slowly moving along the river by boat. Stunned fish caught in the electrical field float to the surface where they can be dip -netted from the boat. Gill nets (flounder nets; 5.50-inch mesh x 20 mesh x 100 yards and 5.75-inch mesh x 15 mesh x 100 yards), trot lines, and hook and line fishing were also used to collect fish. Descriptions of effort and gear types used are given in Table 2-2. 8 Table 2-2. Fish collection dates, techniques, effort, and fish caught in the Cape Fear River study areas during 2011. Station Sampling dates Gear type Level of effort Fish caught 1 1 1 2 22 Aug 11 23 Aug 11 13 Sept 11 23 Aug 11 2 24Aug 11 2 25 Aug 11 Hook & Line Hook & Line Gillnets Trot Lines Crank Shocker Gillnets Trot Lines Crank Shocker Hook & Line Crank Shocker Hook & Line Gillnets Trot Lines Hook & Line Gillnets Trot Lines Crank Shocker 2 12 Sept 11 Hook & Line Crank Shocker 2 lines, 0.75 hours 2 lines, 0.75 hours 8 nets, 1 night 2 lines, 50 hooks 0.25 hours 4 nets, 1 night 2 lines, 50 hooks 0.25 hours 6 bluegill (5 bluegill released) 11 bluegill (2 released) 14 blue catfish (1 blue catfish released), 1 channel catfish, 1 longnose gar (released) 1 blue catfish 0 fish 3 blue catfish, 1 flathead catfish 1 blue catfish 0 fish 2 lines, 0.50 hours 4 bluegill 0.25 hours 2 lines, 0.75 hours 4 nets, 1 night 1 line, 26 hooks 0 fish 4 bluegill 4 blue catfish, 3 flathead catfish, 1 common carp 1 blue catfish (released), 1 channel catfish (released), 1 longnose gar (released) 2 lines, 0.50 hours 1 bluegill 4 nets, 1 night 6 blue catfish (1 blue catfish released), 5 common carp, 1 southem flounder (released) 1 line, 25 hooks 0 fish 0.50 hours 0 fish 2 lines, 0.50 hours 4 bluegill 0.25 hours 0 fish 9 eaq !�1 Station Sampling dates Gear type Level of effort Fish caught �'► 2 13 Sept 11 Gillnets 4 nets, 1 night 2 blue catfish, 2 common carp, 1 longnose gar (released) Trot Lines 2 lines, 50 hooks 3 blue catfish, 1 flathead catfish Crank Shocker 0.25 hours 0 fish 2 14 Sept 11 Gillnets 1 net, 1 night 3 blue catfish Trot Lines 1 line, 24 hooks 0 fish 3 23 Aug 11 Hook & Line 2 lines, 0.50 hours 2 bluegill (1 bluegill released) Crank Shocker 0.25 hours 0 fish 3 24 Aug 11 Hook & Line 2 lines, 1.00 hours 14 bluebill on) Gillnets 4 nets, 1 night 3 blue catfish, 1 flathead catfish, 5 gizzard shad (released), 2 longnose gar (released) emeN Trot Lines 2 lines, 50 hooks 0 fish 3 25 Aug 11 Gillnets 4 nets, 1 night 1 blue catfish, 2 gizzard shad (released) Trot Lines 2 lines, 50 hooks 2 blue catfish Crank Shocker 0.25 hours 0 fish (4112 3 13 Sept 11 Hook & Line 2 lines, 0.25 hours 5 bluegill ,4EKN Crank Shocker 0.25 hours 0 fish 3 14 Sept 11 Gillnets 7 nets, 1 night 4 blue catfish, (1 blue catfish released) 2 flathead catfish, 1 gizzard shad (released) Trotlines 2 lines, 49 hooks 2 blue catfish Crank Shocker 0.25 hours 0 fish effaN ribs 10 2.4 Sample Preparation and Shipment Collected fish were descaled or skinned, filleted, and preserved by CZR. SGS Environmental Services (5500 Business Dr., Wilmington, North Carolina 28405) was responsible for final sample preparation (i.e., homogenization) and chemical analysis. To prevent cross -contamination between stations and composites, all equipment used to handle fish (excluding nets) was solvent rinsed with pesticide -grade acetone and hexane or was wrapped with aluminum foil (e.g., measuring boards and scale pans) which was changed between composites. Fish from different stations were held in separate coolers and disposable latex gloves were worn and frequently changed when handling fish during each phase of sample preparation. As fish were collected, they were placed on wet ice until processing. Fish were filleted with knives on cutting boards wrapped with aluminum foil (dull side up). Cutting board wraps were changed and fillet knives were solvent rinsed between composites. Fillet samples consisted of flesh from both sides of each specimen, including the skin (for gamefish) but not the scales. Catfish and carp specimens were skinned. Samples were wrapped in aluminum foil (dull side toward the fish) to shield it from light and were labeled with sample location, species, and date of collection. All labeled samples making up a single composite were placed in individual plastic "zip -lock" bags, then all composite sample bags were sealed inside a larger bag for each station. Samples were frozen to await delivery to the laboratory for analysis. Where available, a portion of each composite was retained from laboratory analysis and remains frozen with International Paper Company or CZR Incorporated. On 6 October 2011, the frozen samples were hand -delivered to SGS Environmental Services in Wilmington, North Carolina, in coolers packed with ice. A copy of the letter of transmittal/chain of custody that accompanied samples is included in Appendix C. 11 e /lb1 rotbk 2.5 Chemical Analysis SGS Environmental Services performed the chemical extraction and analyses in Asis accordance with EPA Method 8290 for 2,3,7,8-TCDD and 2,3,7,8-TCDF. The presence of tetrachlorinated dibenzo-p-dioxins and dibenzofurans was detected using high -resolution chromatography/high-resolution mass spectrometry. All summary results were reported as 2,3,7,8-TCDD; 2,3,7,8-TCDF; and estimated Total Toxic Equivalent Values (TEVs). Total extractable lipid content was also determined `®` for each composite sample. A composite sample of blue catfish from Station 1 was designated for duplicate laboratory analysis. A quantity sufficient for re -extraction of each composite sample (where available) was retained and will be held frozen for a period of 30 days at the lab following the analysis. Duplicate samples will be held at CZR for three months following the completion of this report. root 3.0 RESULTS AND DISCUSSION 3.1 Fish Collection robs A summary description of the 2011 fish composites is found in Table 3-1. Gamefish ram, and bottom feeder target species were collected from each of the three stations. Gamefish or water -column feeding species submitted for analysis included bluegill (Lepomis offg macrochirus) from Stations 1, 2, and 3. Bottom feeder species submitted for analysis included blue catfish (lctalurus furcatus) from Stations 1, 2, and 3; common carp (Cyprinus `®' carpio) from Station 2; and flathead catfish (Pylodictis olivaris) from Stations 1, 2, and 3. Sample composites with calculated average total fish lengths and weights are found in rat, Table 3-2. ram+ 3.2 Tissue Analyses Dioxin (2,3,7,8-TCDD) concentrations (all reported in parts per trillion — ppt) in all composite samples represent values between the method detection limit and the lower method calibration limit or were not detected and therefore represent estimates (Table 3-3). The highest concentration of dioxin was 0.439 ppt found in flathead catfish composite oft, number 6 (composite of 4 individuals) at Station 2. The next highest concentration was 0.399 ppt found in common carp composite number 8 (composite of 8 individuals), also located at Station 2. The only reported dioxin concentration from Station 1 was 0.295 ppt. Reported dioxin concentrations from Station 2 ranged from 0.339 ppt to 0.439 ppt, and there were no detected dioxin concentrations at Station 3. ,, Furan (2,3,7,8-TCDF) concentrations (all reported in parts per trillion — ppt) in all composite samples represent values between the method detection limit and the lower method calibration limit or were not detected and therefore represent estimates (Table 3-3). The highest concentration of furan was 0.434 ppt found in common carp at Station 2. The only reported furan concentration from Station 1 was estimated at 0.277 ppt. Reported �► furan concentrations ranged from an estimated 0.112 ppt to 0.434 ppt at Station 2, and from an estimated 0.140 ppt to an estimated 0.149 ppt at Station 3. 13 Table 3-1. Summary of 2011 fish composites submitted from three Cape Fear River stations in the vicinity of the International Paper Company Mill at Riegelwood, North Carolina. Station Composite Species Length Weight (g) Fillet A (g) Ka 1 Channel catfish 475 1,050 58 0.98 1 1 Bluegill 160 80 15 1.95 1 1 Bluegill 160 65 10 1.59 1 1 Bluegill 129 40 5 1.86 1 1 Bluegill 158 60 10 1.52 1 1 Bluegill 139 40 5 1.49 1 1 Bluegill 135 40 10 1.63 1 1 Bluegill 130 40 5 1.82 1 1 Bluegill 172 110 15 2.16 1 1 Bluegill 149 65 10 1.96 1 1 Bluegill 145 60 10 1.97 1 2 Flathead catfish 555 1,575 160 0.92 1 3 Blue catfish 563 1,690 240 0.95 1 3 Blue catfish 600 2,300 332 1.06 1 3 Blue catfish 571 2,300 335 1.24 1 3 Blue catfish 499 1,325 325 1.07 1 3 Blue catfish 600 2,350 361 1.09 1 3 Blue catfish 510 1,400 210 1.06 1 3 Blue catfish 521 1,350 171 0.95 1 3 Blue catfish 593 1,950 270 0.94 1 4 Blue catfish 640 3,025 455 1.15 1 4 Blue catfish 670 2,950 401 0.98 1 4 Blue catfish 696 2,825 332 0.84 1 4 Blue catfish 709 3,325 411 0.93 1 4 Blue catfish 631 2,610 399 1.04 1 4 Blue catfish 611 2,900 404 1.27 1 4 Blue catfish 600 2,500 416 1.16 1 4 Blue catfish 542 2,800 328 1.76 1 4 Blue catfish 600 2,375 361 1.10 1 4 Blue catfish 666 3,200 352 1.08 2 Bluegill 142 40 5 1.40 2 Bluegill 131 40 5 1.78 2 Blue catfish 733 4,900 576 1.24 2 Blue catfish 230 258 40 2.12 2 Blue catfish 405 525 78 0.79 2 Blue catfish 525 1,150 160 0.79 2 Blue catfish 805 8,850 840 1.70 2 5 Bluegill 150 65 10 1.93 14 Table 3-1. (continued) Station Composite Species Length (mm) Weight (g) Fillet A (g) Ka 2 5 Bluegill 161 75 10 1.80 2 5 Bluegill 146 50 10 1.61 2 5 Bluegill 133 45 10 1.91 2 5 Bluegill 148 64 10 1.97 2 5 Bluegill 145 58 10 1.90 2 5 Bluegill 134 46 5 1.91 2 5 Bluegill 146 60 10 1.93 2 5 Bluegill 160 70 10 1.71 2 5 Bluegill 146 60 5 1.93 2 5 Bluegill 160 65 10 1.59 2 6 Flathead catfish 630 2,500 306 1.00 2 6 Flathead catfish 645 3,200 357 1.19 2 6 Flathead catfish 725 4,050 521 1.06 2 6 Flathead catfish 795 5,108 548 1.02 2 7 Blue catfish 574 1,750 256 0.93 2 7 Blue catfish 637 2,800 413 1.08 2 7 Blue catfish 649 2,650 337 0.97 2 7 Blue catfish 650 2,600 401 0.95 2 7 Blue catfish 640 2,200 356 0.84 2 7 Blue catfish 589 2,100 332 1.03 2 7 Blue catfish 613 2,400 398 1.04 2 7 Blue catfish 577 1,900 306 0.99 2 7 Blue catfish 640 3,850 444 1.47 2 7 Blue catfish 695 3,750 504 1.12 2 7 Blue catfish 642 3,075 390 1.16 2 7 Blue catfish 680 3,400 445 1.08 2 8 Common carp 621 3,450 338 1.44 2 8 Common carp 610 3,500 425 1.54 2 8 Common carp 605 2,925 378 1.32 2 8 Common carp 613 3,150 374 1.37 2 8 Common carp 642 3,450 392 1.30 2 8 Common carp 645 3,700 465 1.38 2 8 Common carp 621 3,300 474 1.38 2 8 Common carp 558 2,350 322 1.35 3 Blue catfish 855 6,800 836 1.09 3 9 Bluegill 151 66 10 1.92 3 9 Bluegill 146 55 5 1.77 3 9 Bluegill 154 64 10 1.75 3 9 Bluegill 158 69 10 1.75 3 9 Bluegill 155 68 5 1.83 3 9 Bluegill 155 68 10 1.83 3 9 Bluegill 132 45 5 1.96 3 9 Bluegill 138 45 5 1.71 3 9 Bluegill 138 40 10 1.52 15 Table 3-1. (concluded) Station Composite Species Length (mm) Weight (g) Fillet A (g) Ka 3 9 Bluegill 142 50 10 1.75 3 10 Bluegill 158 70 10 1.77 3 10 Bluegill 177 85 10 1.53 3 10 Bluegill 180 114 15 1.95 3 10 Bluegill 176 125 20 2.29 3 10 Bluegill 171 104 15 2.08 3 10 Bluegill 159 80 10 1.99 3 10 Bluegill 155 72 5 1.93 3 10 Bluegill 178 104 15 1.84 3 10 Bluegill 160 80 10 1.95 3 10 Bluegill 181 100 15 1.69 3 11 Flathead catfish 557 1,950 228 1.13 3 11 Flathead catfish 623 2,550 219 1.05 3 11 Flathead catfish 570 1,840 208 0.99 3 12 Blue catfish 595 2,250 300 1.07 3 12 Blue catfish 701 3,600 516 1.05 3 12 Blue catfish 748 3,600 488 0.86 3 12 Blue catfish 536 1,600 242 1.04 3 12 Blue catfish 520 1,150 174 0.82 3 12 Blue catfish 592 2,110 324 1.02 3 12 Blue catfish 725 4,300 540 1.13 3 12 Blue catfish 670 3,200 424 1.06 3 12 Blue catfish 664 3,100 329 1.06 3 12 Blue catfish 632 2,560 434 1.01 aFulton..type condition factor - (weight(g)/length(mm)3)*100000 16 Table 3-2. Fish composite data for three Cape Fear River stations in the vicinity of the International Paper Company Mill at Riegelwood, North Carolina, collected during 2011. Station Composite Typea Species number Number in composite Average length (mm) Average weight (g) Average fillet weight (g) 1 1 G Bluegill 10 147.7 60.0 9.5 1 2 B Flathead catfish 1 555.0 1,575.0 160.0b 1 3 B Blue catfish 8 557.1 1,833.1 280.5 1 4 B Blue catfish 10 636.5 2,851.0 385.9 2 5 G Bluegill 11 148.1 59.8 9.1 2 6 B Flathead catfish 4 698.8 3,714.5 433.0 2 7 B Blue catfish 12 632.2 2,706.3 381.8 2 8 B Common carp 8 614.4 3,228.1 396.0 3 9 G Bluegill 10 146.9 57.0 8.0 3 10 B Bluegill 10 169.5 93.4 12.5 3 11 B Flathead catfish 3 583.3 2,113.3 218.3 3 12 B Blue catfish 10 638.3 2,747.0 377.1 aG = Gamefish/water-column feeder; B = Bottom feeder. bSingle fish composite. 17 Table 3-3. Summary of analytical results from fish tissue composites collected in the Cape Fear River near the International Paper Company Mill at Riegelwood, North Carolina, during 2011. Detailed case narratives of the laboratory results are found in Appendix D. Station 1 1 1 1 1 2 2 2 2 3 3 3 3 Notes: a b c d e 9 Species Composite (#) Bluegill (1) Flathead catfish (2) Blue catfish (3) Blue catfish (4) Blue catfish (13)f Bluegill (5) Flathead catfish (6) Blue catfish (7) Common carp (8) Bluegill (9) Bluegill (10) Flathead catfish (11) Blue catfish (12) 2,3,7,8-TCDD (ppt) Concentration N D(0.123)° ND(0.117)c'd 0.295e'g ND(0.181)c ND(0.205)c N D(0.184)° 0.439e ND(0.200)c 0.399e ND(0.107)c ND(0.208)c ND(0.156)° ND(0.256)c Percent recover? 71.0 89.0 87.0 69.0 95.0 96.0 101.0 72.0 96.0 92.0 98.0 97.0 83.0 2,3,7,8-TCDF (ppt) Percent Percent Concentration recover? TEVb lipid ND(0.050)c 72.0 0.128 0.26 ND(0.048fd 90.0 0.122 0.17 0.277e'g 88.0 0.323 2.44 ND(0.219)c 69.0 0.203 3.69 0.234e 99.0 0.228 1.38 ND(0.053)c 97.0 0.189 0.54 0.112e'g 104.0 0.450 0.73 ND(0.085)c 72.0 0.209 3.13 0.434e 97.0 0.442 1.71 0.140e'9 96.0 0.121 0.52 0.149" 100.0 0.223 0.49 0.147e 100.0 0.171 0.32 ND(0.083)c 84.0 0.264 1.18 ± 5% statistical variability. Estimated Maximum possible Toxic Equivalent Value [TCDD conc. + (0.1*TCDF conc.)] using detection limits and/or estimated concentration. Not detected. Estimated Detection Limit for sample is reported in parenthesis. Single specimen sample. Amount detected is between the Method Detection Limit and the Lower Calibration Limit. Duplicate sample of composite #4. Estimated Maximum possible Concentration. 18 Percent lipid contents ranged from 0.17 (flathead catfish at Station 1) to 3.69 (blue catfish from Station 1). Reported TEV estimates represent the maximum possible values from each sample. Analytical results for fish tissue composites collected and submitted during 2011 are summarized in Table 3-3. Laboratory data reports (149 pages) provided by SGS Environmental Services are included in Appendix D. The US Environmental Protection Agency recommends a screening value of 0.7 ppt for dioxins; however, the State of North Carolina currently uses a dioxin concentration of 4.0 ppt in issuing an advisory (NCDENR 2006). Dioxin concentrations below this amount are considered safe and acceptable by the North Carolina Division of Water Quality. None of the samples submitted for analysis in 2011 contained dioxin concentrations above the state advisory level. Conclusive concentrations of dioxin were not detected from any samples and the highest concentration of 0.439 ppt in flathead catfish from Station 2 was between the method detection limit and the lower method calibration limit. Average dioxin concentrations from game and bottom feeding fish in the vicinity of the Riegelwood Mill have remained well below the state advisory standard during the course of annual sampling periods over the last twenty years (Table 3-4). 19 ''°'iN Table 3-4. Comparison of dioxin (2,3,7,8-TCDD) concentrations among gamefish and bottom feeder composites from the Cape Fear River from 1992 to 2011. 'iit‘ 2,3,7,8-TCDD average concentration (ppt) Year Fillet composite type Station 1 Station 2 Station 3 Amq 1992 Gamefish 0.09 0.38 0.35 Bottom feeder 0.15 2.09 1.15 rifq 1993 Gamefish 0.09a 0.17b 0.33 oltN Bottom feeder 0.16 0.59 0.38 1994 Gamefish 0.08 0.32 0.22 Bottom feeder ND 0.20 0.42 filli 1995 Gamefish ND ND ND roq Bottom feeder ND 0.21b ND 1996 Gamefish ND ND ND At\ Bottom feeder ND 0.37b 0.12 oak, 1997 Gamefish ND 0.20a ND Bottom feeder 0.17b 0.25a 0.06b 'im' 1998 Gamefish ND ND ND esiiN Bottom feeder ND ND 0.31 1999 Gamefish ND 0.08b ND `'it' Bottom feeder 0.05b 0.17b 0.31 b " 2000 Gamefish ND 0.18b 0.09b Bottom feeder ND° ND ND 2001 Gamefish ND 0.11b 0.11b oq Bottom feeder ND° 0.19b 0.08b 2002 Gamefish ND ND ND Bottom feeder 0.26b 0.29b ND 2003 Gamefish ND ND ND Bottom feeder ND 0.05b 0.63 2004 Gamefish ND ND 0.26 (At\ Bottom feeder 0.25b 0.14 0.10 2005 Gamefish 0.23 0.12 0.20 Bottom feeder 0.34a 0.43 0.26a oft, 2006 Gamefish 0.07b ND ND oq Bottom feeder 0.22a 0.24a 0.36a 2007 Gamefish ND ND ND '"'' Bottom feeder 0.33a 0.15a 0.07b " 2008 Gamefish ND ND ND Bottom feeder 0.42a 0.11 0.33a 2009 Gamefish 0.42 0.32 0.56b rfi Bottom feeder 0.70 1.13 0.49 2010 Gamefish ND ND 0.14b Bottom feeder 0.30b 0.29b 0.12b eats 2011 Gamefish ND ND ND /alb+ Bottom feeder 0.10b 0.42 ND *1992 data were obtained from EA Report No. 12347.01 (EA Engineering, Science, and Technology, Inc., 1992). ND = Not detected; detection limits were not used in calculating average concentrations of 2,3,7,8-TCDD. a Values represent average of dioxin concentrations and estimated concentrations. b Values represent average of estimated concentrations. __,a14\° Estimated concentration found in replicate. ARN A°` 20 REFERENCES EA Engineering, Science, and Technology, Inc. 1992. Dioxin Monitoring Study of Fish Tissue from the Vicinity of Federal Paper Board Company's Riegelwood Mill. Prepared for Federal Paper Board Company, Inc., EA Engineering, Science, and Technology, Inc., Smyrna, Georgia. Report No. 12347.01. Taylor, K., and K. M. Rudo. 1990. Risk Assessment of Dioxin Contaminated Fish. Division of Epidemiology, NC Department of Environment, Health, and Natural Resources. Raleigh, North Carolina. CZR Incorporated. 1993. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of Federal Paper Board's Mill at Riegelwood, North Carolina. CZR Incorporated. 1994. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of Federal Paper Board's Mill at Riegelwood, North Carolina. CZR Incorporated. 1995. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of Federal Paper Board's Mill at Riegelwood, North Carolina. CZR Incorporated. 1996. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 1997. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 1998. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 1999. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2000. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2001. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. 21 CZR Incorporated. 2002. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2003. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2004. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2005. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2006. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2007. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2008. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2009. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. CZR Incorporated. 2010. Dioxin Monitoring Study of Fish Tissue from the Cape Fear River in the Vicinity of the International Paper Company Mill at Riegelwood, North Carolina. NCDENR. 2006. Standard Operating Procedures Fish Tissue Assessments. North Carolina Department of Environmental and Natural Resources, 13 pp. 22 APPENDIX A DIOXIN MONITORING STRATEGY Monitoring Strategy for International Paper Company at Riegelwood, North Carolina Composite Sample Guidance All fish samples will be composited to maximize the number of sampled individuals and the potential of sampling contaminated fish. Composite samples will consist of single species, ideally represented by a maximum of ten individual fish. Composites will be prepared by combining fillet fish tissue from similar sized individual fish, with a preference for larger fish. Individual length and weight (metric) will be recorded for each fish and the average weight and length for composites will be calculated. Whole fish tissue analysis is not required. Fillets will be prepared by leaving skin on and removing scales for most species, with the exception of catfish which will be skinned. Individual fish will be identified to species. A sufficient quantity of each (un-extracted) composite sample will be retained and archived (frozen) for a period of three months following submission of the final report. Sample Collections Total laboratory samples to be analyzed = 13 (12 samples and one duplicate) Sampling Site 1 - Cape Fear River in the vicinity of SR 1730 Bladen County Four composite samples will be analyzed for dioxin at this station: -one composite sample for largemouth bass with sunfish as fallback species, -one composite sample for bluegill with other sunfish as fallback species (redbreast, redear, etc.), - one composite sample for catfish (flatheads, channels, blue, other) or carp, - one composite sample for catfish (flatheads, channels, blue, other) with other edible finfish as fallback species. Sampling Site 2 - Cape Fear River in the vicinity of Bryant Mill Creek Four composite samples will be analyzed for dioxin at this station: -one composite sample for largemouth bass with sunfish as fallback species, - one composite sample for bluegill with other sunfish as fallback species (redbreast, redear, etc.), - one composite sample for catfish (flatheads, channels, blue, other) or carp, -one composite sample for catfish (flatheads, channels, blue, other) with other edible finfish as fallback species. Sampling Site 3 - Cape Fear River in the vicinity of confluence with Black River Four composite samples will be analyzed for dioxin at this station: -one composite sample for largemouth bass with sunfish as fallback species, -one composite sample for bluegill with other sunfish as fallback species (redbreast, redear, etc.), -one composite sample for catfish (flatheads, channels, blue, other) or carp, -one composite sample for catfish (flatheads, channels, blue, other) with other edible finfish as fallback species. Laboratory Analysis and Reporting Procedures Samples will be analyzed for Dioxin and Furans in accordance with analytical protocols set out in Appendix C of USEPA/Paper Industry Cooperative Dioxin Screening Study (EPA 440/1-88-025, March 1988) or other equivalent analytical protocol approved by EPA. Analysis will include the determination of concentrations of 2,3,7,8 TCDD and 2,3,7,8 TCDF. Dioxin analysis will be performed using high resolution Mass Spectrometry as required by EPA Methods 624, 625, 8290, 1613 or other approved methods. Required Analysis of Dioxins and Furans Matrix Compound Quantitative Limits Fish 2,3,7,8 TCDD 1 part per trillion Fish 2,3,7,8 TCDF 1 part per trillion Results will be reported in ppt with a minimum quantitative limit of 1 ppt. Where the compound is detected at concentrations less than the minimum quantitative limit, an estimate of the concentration will be given. If a compound is not detected it will be so noted. Reports A monitoring report will be submitted that will include: -sampling locations shown on copies of topographical maps (1:2400); -analytical methods and procedures with name of laboratory; -individual specimen description (species, length, weight, condition); -composite descriptions (species, average length, average weight); -All results will be reported as 2,3,7,8 TCDD and 2,3,7,8 TCDF in parts per trillion (PPt)• Monitoring reports (with results) will be sent in triplicate and directed to: Mr. Steve Tedder Chief, Water Quality Section Division of Environmental Management PO Box 27687 Raleigh, North Carolina 27611 A-2 APPENDIX B NORTH CAROLINA SCIENTIFIC COLLECTION PERMITS Atk Scientific Fish Collecting License AA'',, ® North Carolina Wildlife Resources Commission Division of Inland Fisheries Phone: (919) 707-0220 MSC 1721 Fax: (919) 707-0028 Raleigh, NC 27699-1721 AUTHORITY STATUTES r, 113-272.4 PERMITTEEILICENSEE SAMUEL COOPER CZR, INC. 4709 COLLEGE ACRES DRIVE SUITE 2 WILMINGTON, NC 28403 PERMIT NUMBER 11-SFC00004 EFFECTIVE 02/01/2011 EXPIRES 12/31/2011 , Conditions and Authorizations: . The above permittee is authorized to collect the species/organism fisted below. The permittee is requirements and laws specified by the U.S. Fish and Wildlife Service as they pertain to these species/organisms. or possession of federally or state listed endangered, threatened, or special concern species Is license. SPECIES/ORGANISMS: Amblyopsfdae; Amiidae; Anguillidae; Aphredoderldae; Atherinopsidae; Catostomidae; Centrarchidae; Cottidae; Cyprinidae; Eiassomatidae; Esocidae; Fundulidae; Ictalurldae; Lepisosteidae; Moronidae; Petrcmyzontidae; Poeciliidae; Salmonidae; Umbridae BODIES OF WATER: Print Date: 03/25/2011 required to comply not authorized under Clupeidae; Percidae; with all The take this MICH CAPE FEAR - Bladen County CAPE FEAR- Brunswick County CAPE FEAR - Columbus County CAPE FEAR- Pender County ROANOKE -Bertie County ROANOKE - Marlin County ROANOKE -Washington County TAR-PAMLICO - Beaufort County COUNTIES: Beaufort Bertie Bladen Brunswick ChowanColumbus SAMPLING METHOD: Electrofishing, Boat; Net, Dip; Net, Fyke; Net, Gill; Seines; ASSISTANTS: SHERRY BANNER JULIA BERGER KATHARINE BRALY AEL HUBBARD JIM HUDGENS BEN KEARNS LORRIE PULLEY MAVERICK RABER JASON HALL SPECIAL CONDITIONS: 1 I g -EU W _Ii MAR 2 5 2011 CZR Incorpore:ed Wiir-incl:n, NC Martin Pender Washington Trawls; Other NICOLE CARPENTER ALEXANDER CRAIG LALIBERTE ADRIAN MOON DAN MOORE RANDALL PATRICK AMICO This permit/license is non -transferable and expires at midnight on the above specified expiration date. ISSUED BY: deA.14: AK ete/e, TITLE: Chief ea q f''41 eats ItN est Ogit embN tit) tbN esbN taas ENDANGERED NORTHN.C.G.S. 2. AUTHORITY - STATUTES 113-331 THRU 113-337 REGULATIONS 15A N.C.A.C. 10I.0001 THRU .0005 SPECIES PERMIT] RESOURCES North Carolina Wildlife Resources Commission CIAVAASSO Division of Wildlife Management MSC 1722 Tele: (919) 707-0050 Raleigh, NC 27699-1722 FAX: (919) 707-0067 1. PERMITTEE 3 al�l� • Samuel Cooper r-Ct1 r f CZR, Inc. 4709 College Acres Drive Wilmington, NC 28403 • TELE: (910) 392-9253 FAX: (910) 392-9139 3. PERMIT NUMBER NCE-2011Es22 4. RENEWABLE fl YES 5. MAY COPY / / ❑ YES NO 6. EFFECTIVE 03/07/2011 7. EXPIRES 12/31/2011 8. NAME AND TITLE OF PRINCIPAL OFFICER Will is :a business) • N/A 7. TYPE OF PERMIT • Survey, Incidental Take 10. SPECIES AUTHORIZED: • State -Listed Endangered, Threatened, & Special Concern Fish Species EXCLUDING Federally -listed Endangered, Threatened, and Special Concern Fish Species 11. LOCATION WHERE AUTHORIZED ACTIVITY MAY BE CONDUCTED: • Statewide 12. CONDITIONS AND AUTHORIZATIONS: A. Authorized for incidental take of state -listed fish species while conducting fish collection activities as a designated agent of the NC Wildlife Resources Commission. A Fish Collection License is required from the NCWRC, Div. of Inland Fisheries. B. Possession and transportation of dead specimens is permitted only as authorized by this permit. 1. Unless specifically authorized by this permit, collected voucher specimens must be deposited in the North Carolina Museum of Natural Sciences, Raleigh, North Carolina or the Smithsonian Institution, Washington, D.C. C. All activities must be supervised ON -SITE by the permittee. 1. All individuals conducting activities under this permit must carry a copy of this permit in their possession and a letter of authorization signed by the permittee. The permittee will be responsible for all actions of individuals working under his supervision. 2. Authorized subpermittees: Jim Hudgens, Julia Berger, Sherry Banner, Lorrie Laliberte, Katharine Braly, Randall Pulley, Michael Hubbard, Nicole Carpenter, Alexander Craig, Ben Kearns, Adrian Moon, Dan Moore, and Maverick Raber D. All activity conducted under an Endangered Species Collection Permit must be .reported to the NC Wildlife Resources Commission via an online data entry web site to meet the reporting requirements (https://ncpaws.org/paws/). Some fields are required and are marked with an asterisk, but fill in as many of the remaining fields as you can. The report is due within 30 days of the expiration of this permit. Your user name is (first initial and last name) and the default password is "Aqu@tics01". The first time you log in you will be prompted to change your password and enter security questions. Once in the PAWS system click on the "+" before the Fisheries to view and click on the aquatics database link. Next add a new submission, then you will be able to click on the add/edit link to begin entering site data. Inside the data entry pages you can cursor over the green question marks for detailed information about a particular field. For some data entry boxes, we have provided specific examples of how we would like the data entered. Help documents are available online and additional questions can be sent to Ryan Heise (ryan.heise@ncwildlife.org). A ADDITIONAL CONDITIONS AND AUTHORIZATIONS ON REVERSE ALSO APPLY (PAGE 1 OF 1) 13. REPORTING REQUIREMENTS: • Within 15 days after expiration. VALID 30 DAYS AFTER EXPIRATION, IF RENEWAL REQUESTED. ISSUED BY: /4),47/ TITLE: Permits Supervisor DATE: 03/07/2011 DISTRIBUTION LIST: Division of Wildlife Enforcement U.S. Fish & Wildlife Service, Enf. Sect., Raleigh, NC; Todd Ewing eit'N fot) /1111 Idoft Oa) elet e1 talIPN North Carolina Division of Marine Fisheries Proof of Purchase UPDATE : Scientific or Educational Collection Permit : Permit Number 707778 Permit Number : 707778 Permit Year : 2011 NC Residency : Qualifying Product : Effective Date/I'imc : 01/14/2011 08:05 Expiration Date/1ime : 12/31/2011 23:59 Status : Active Issue Date/Time : 01/14/2011 08:05 Status Date : 01/14/2011 Sales Outlet : DMF Morehead City Office Terminal Numbcr : NI M0153 Fee : 0.00 Permit Holder : 730069 CZR, INC. Business Type: Physical Address : 4709 COLLEGE ACRES DRIVE M © m a V '.—\ �Iai i lddress : • SUITE 2, WILMINGTON, NC, 28403 United States County : New Hanover Race : ,f MAR 2 8 2011 Sjes : • Weight Gender : Date of Birth : CZR incorpora-ed Hair : Wilmington, NC : Height : ft. Inches Home Phone : (910) 799-3825 Primary Residence : NC Prior !Fames : Business Phone : (910) 392-9253 Secondary Residence : Fax : (910) 392-9139 Ids : E-Mail : czrwilm a czr-inc.com Business Agent : 730085 COOPER, SAMUEL Physical Address : 5425 ANDOVER ROAD, Mailing Address : . WILMINGTON, NC, 28403 United States County : New Hanover .County : Race : Caucasian Eyes : Brown Weight : 160 Gender : Male Date of Birth 03/12/1963 Hair : Brown Height-: 5 ft. 10 Inches Home Phone : (910) 799-3825 Primary Residence : NC Prior Names : Business Phone : (910) 392-9253 Secondary Residence : Fax : (910) 392-9139 Ids : E-Mail : Contact Information Contact Person Contact Person DOB Contact Person Telephone # SAMUEL COOPER 03/12/1963 (910) 799-3825 Purpose of Collection X Research Teaching Specimens Educational Display (Aquariums) Other (specify) SECTION 401 WQC MONITORING & DIOXIN SCANS Collectors Participantld Name DOB Contact Phone JULIA K. BERGER 02/02/1951 (910) 392-9253 SHERRY BANNER 07/21/1943 (910) 392-9253 JIM HUDGENS 09/17/1942 . (910) 392-9253 LORRIE LALIBERTE BOSWELL 06/29/1981 (910) 392-9253 KATHARINE BRALY 03/02/1984 • (910) 392-9253 NICOLE CARPENTER 05/14/1986 (910) 392-9253 RANDALL PULLEY 02/02/1978 (910) 392-9253 ALEXANDER CRAIG 10/1I/1983 (910) 392-9253 MICHAEL HUBBARD 05/24/1963 (910) 392-9253 MAVERICK RABER 08/28/1980 (910) 392-9253 BEN KEARNS 05/25/1986 (910) 392-9253 ADRIAN MOON 01/13/1974 (910) 392-9253 DAN MOORE 10/30/1971 (910) 392-9253 • JASON HALL 06/05/1973 (910) 392-9253 PATRICK AMICO 03/19/1985 (910) 392-9253 'Tinted : 3/25/2011 DMF Morehead City Office, 3441 Arendell St., PO Box 769, Morehead City NC., 28557-0769 SUEANN i3A' Page : North Carolina Division of Marine Fisheries peat, Proof of Purchase UPDATE : Scientific or Educational Collection Permit : Permit Number 707778 Pate Permit Number : 707778 NC Residency : Permit Year : 2011 Qualifying Product : tot1 Effective Date/Time : 01/14/2011 08:05 eAt1 Expiration Date/Time : 12/31/2011 23:59 Status : Active Issue DateTI'imc : 01/142011 08:05 Status Date : 01/14/2011 /1'a1 Owl Olt\ tot) I�1 Igeb f�1 /aq Sales Outlet : DMF Morehead City Office Terminal Number : N 1 M0153 Fee : 0.00 Restriction Information Restriction Type : Gear Code : Species Group : _ eWater Body : RESTRICT TO Gcar Quantity : Species Quantity : Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: GEARS OR METHODS: ELECTROFISHING; GILL NETS; FYKE NETS; TROT LINES; DIP NETS; TRAWL; SEINE; HOOK AND LINE; FISH TRAPS Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : Gear Units : Species Size : Time : Species Units : Start Time: End Time: . Comments: SPECIES: ALL EXCEPT THOSE LISTED AS ENDANGERED OR THREATENED. Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : 1201020204-W11ITEHU RST CREEK Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : 1900000000-CAPE FEAR RIVER Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : 0205010000-MUDDY CREEK Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : 0208000000-CHOWAN RIVER Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : 0200000000-ALBEMAR LE SOUND Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: WATER BODY: PCS PROJECT AREA I1 Restriction Type : Gear Code : Species Group : Water Body : RESTRICT TO Gear Quantity : Species Quantity : 0528070201-BAILEY CREEK Gear Units : Species Size : Time : Species Units : Start Time: End Time: Comments: ' Printed : 3/252011 DMF Morehead City Office. 3441 Arcade!! St.. PO Box 769, Morehead City NC., 28557-0769 SUEANN BA' Page : F�1 ANN /legitst egats OR1 f�1 North Carolina Division of Marine Fisheries Proof of Purchase UPDATE : Scientific or Educational Collection Permit : Permit Number 707778 Permit Number : 707778 Permit Year : 2011 NC Residency : Qualifying Product : Effective Date/Time : 01/14/2011 08:05 Expiration Date/Timc : 12/31/2011 23:59 Status : Active Issue Date/Time : 01/14/2011 08:05 Status Date : 01/14/2011 Sales Outlet : DMF Morehead City Office Terminal Number : NIM0153 Fee : 0.00 Restriction Type : RESTRICT TO Time : Start Time: Comments: End Time: Gear Code : Gear Quantity : Gear Units : Restriction Type : RESTRICT TO Time : Stara Time: Comments: End Time: Gear Code : Gear Quantity : Gear Units : Species Group : Species Quantity : Species Size : Species Units : Species Group : Species Quantity : Species Size : Species Units : Water Body : 0528370000-SOUTH CREEK 0528370100-TOOLEV CREEK Restriction Type : RESTRICT TO Time : Start Time: Comments: End Time: Gear Code : Gear Quantity : Gear Units : Species Group : Species Quantity : Species Size : Species Units : Water Body : 0528360000-HUDDLES GUT Restriction Type : Gear Code : RESTRICT TO Gear Quantity : Time : Start Time: Comments: End Time: Gear Units : 'Restriction Type : I-1 RESTRICT TO Time : Start Time: Comments: roiq Restriction Type : RESTRICT TO Time : Start Time: Comments: End Time: End Time: Gear Code : Gear Quantity : Gear Units : Gear Code: Gear Quantity : Gear Units : Species Group : Species Quantity : Species Size : Species Units : Water Body : 0528370300-JACKS CREEK Species Group : Species Quantity : Species Size : Species Units : Species Group : Species Quantity : Species Size : Species Units : Water Body : 0210000000-ROANOKE RIVER Water Body : 0210020000-W ELCH CREEK estN Restriction Type : RESTRICT TO tits eft► rime : Start Time: Astt, 3omments: testriction Type : 2ESTR1 CT TO egitN ime : toz1;tart Time: :omments: End Time: End Time: Gear Code : Gear Quantity : Gear Units : Gear Code : Gear Quantity : Gear Units : Species Group : Species Quantity : Species Size : Species Units : Species Group : Species Quantity : Species Size : Species Units : Water Body : 0528000000-PAMLICO RIVER Water Body : 0528370201-DRINKWA TER CREEK testriction Type : LESTRICT TO ,mad 'ime : :tart Time: elat :omments: ealiN Gear Code : Gear Quantity : Gear Units : End Time: Species Group : Species Quantity : Species Size : Species Units : Water Body : 0528370200-JACOBS CREEK DMF Morehead City Office, 3441 Mendell St., PO Box 769, Morehead City NC., 28557-0769 rinted : 3/25/2011 fsa1 SUEANN BA' Pagc tots North Carolina Division of Marine Fisheries Proof of Purchase UPDATE : Scientific or Educational Collection Permit : Permit Number 707778 !ten► Permit Number : 707778 NC Residency : - Sales Outlet : DMF Morehead City Office Permit Year : 2011 Qualifying Product : Terminal Number : N1M0153 Effective Date/Time : 01/14/2011 08:05 Fee : 0.00 E"t1 Expiration Date/Time : I2/312011 23:59 Status : Active Issue Date/me : 01/14/2011 08:05 Status Date : 01/14/2011 Restriction Type : Gear Code : RESTRICT TO Gear Quantity : Time : Start Time: Commcnts: End Time: Gear Units : Species Group : Water Body : Species Quantity : 0528350400-PORTER CREEK Species Size : Species Units : foit Restriction Type : RESTRICT TO , Time : Start Time: ▪ Comments: End Time: Gear Code : Gear Quantity : Gear Units : Species Group : Water Body : Species Quantity : 0528063302-SCOTT . CREEK Species Size : Species Units : Restriction Type : tms RESTRICT TO Time : Aq Start Time: Comments: r tati Gear Code : Gear Quantity : Gear Units : End Time: Species Group : Water Body : Species Quantity : 0535301000-SCOTI' CREEK Species Size : Species Units : Request To Sell? Issued By: evict Authorized to Sell? Li Issued Date: J'o '%I DMF Morehead City Office, 3441 Arendell St., PO Box 769, Morehead City NC., 28557-0769 esga1 Printed : 3/25/2011 SUEANN BA Page : APPENDIX C LETTER OF TRANSMITTAL/CHAIN OF CUSTODY ZR INCORPORATED ENVIRONMENTAL CONSULTANTS TO: SGS Environmental Services Attn: Amy Boehm 5500 Business Drive Wilmington, NC 28405 DATE: 6 October 2011 CHAIN OF CUSTODY 3110D1'75 4709 COLLEGE ACRES DRIVE SUITE 2 WILMINGTON, NORTH CAROLINA 28403-1725 TEL 910-392-9253 FAX 910-392-9139 czrwilm@czr-Inc,com FROM: Sam Cooper CZR Incorporated, Suite 2 4709 College Acres Drive Wilmington, NC 28403 scooper@czr-inc.com RE: International Paper Company, Inc., Annual Fish Project (IP 2011 PO# S-066125110 to SGS) Analysis of fish tissues for 2, 3, 7, 8 TCDD (Dioxin), 2, 3, 7, 8, TCDF (Furan), and lipids (%) ENCLOSED ITEMS: Thirteen (13) frozen composite fish tissue (fillets) samples, each fillet wrapped in aluminum foil (dull side toward fish) and enclosed in labeled "zip -lock" plastic bags. Composites are identified below. Composite # 1 2 3 4 5 6 7 8 9 10 11 12 13 COMMENTS: SAMPLE ID # Site Species (number of fish fillets) 1 1 1 1 2 2 2 2 3 3 3 3 1 Bluegill (10 "A" fillets) Flathead Catfish (1 "A" fillet) Blue Catfish smaller (8 "A" fillets) Blue Catfish larger (10 "A" fillets) Bluegill (11 "A" fillets) Flathead Catfish (4 "A" fillets) Blue Catfish (12 "A" fillets) Common Carp (8 "A" fillets) Bluegill smaller (10 "A" fillets) Bluegill larger (10 "A" fillets) Flathead Catfish (3 "A" fillets) Blue Catfish (10 "A" fillet) Blue Catfish large replicate (10 "B" fillets) - Send one digital version and two hard copies of the report to Sam Cooper/CZR at the above address. - Forward the invoice to Ms. Kim Fail International Paper Company John L. Riegel Road Riegelwood, NC 28456 (Kimberly.Fail@ipaper.com@ipaper.com) phone: 910 655-4753 fax: 910 655-9416 Relinquishef y. ___-----"Received by: loM( 13;1,r Date/time to I' 13:1tS ate/time CP #1340.19 } Nn s.ea 2151 Altemat6 A1A South • SUITE 2000 • JUPITER, FLORIDA 33477-3902 TEL 561-747-7455 • FAX 561-747-7576 • czrinc@czr-inc.com • www.CZRINC.com APPENDIX D LABORATORY DATA REPORTS Laboratory Report of Analysis To: Sam Cooper CZR Incorporated Suite 2 4709 College Acres Drive Wilmington, NC 28403 Report Number: 31102775 Client Project: Annual Fish Project 2011 Dear Sam Cooper, Enclosed are the results of the analytical services performed under the referenced project for the received samples and associated QC as applicable. The samples are certified to meet the requirements of the National Environmental Laboratory Accreditation Conference Standards. Copies of this report and supporting data will be retained in our files for a period of five years in the event they are required for future reference. All results are intended to be used in their entirety and SGS is not responsible for use of less than the complete report. Any samples submitted to our laboratory will be retained for a maximum of thirty (30) days from the date of this report unless other arrangements are requested. If there are any questions about the report or services performed during this project, please call Amy J. Boehm at (910) 350-1903. We will be happy to answer any questions or concerns which you may have. Thank you for using SGS North America Inc. for your analytical services. We look forward to working with you again on any additional analytical needs. Sincerely, SGS North America Inc. Amy J. Boehm Project Manager amy.boehm@sgs.com Date Print Date. 11/01/2011 N.C. Certification # 481 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com Member of SGS Group Page 1 of 149 SGS Laboratory Qualifiers J Report Definitions DL Method, Instrument, or Estimated Detection Limit per Analytical Method CL Control Limits for the recovery result of a parameter LOQ Reporting Limit DF Dilution Factor RPD Relative Percent Difference LCS(D) Laboratory Control Spike (Duplicate) MS(D) Matrix Spike (Duplicate) MB Method Blank Qualifier Definitions Recovery or RPD outside of control limits B Analyte was detected in the Lab Method Blank at a level above the LOQ U Undetected (Reported as ND or < DL) ✓ Recovery is below quality control limit. The data has been validated based on a favorable signal-to-noise and detection limit A Amount detected is less than the Lower Method Calibration Limit J Amount detected is between the Method Detection Limit and the Lower Calibration Limit O The recovery of this analyte in the OPR is above the Method QC Limits and the reported concentration in the sample may be biased high E Amount detected is greater than the Upper Calibration Limit S The amount of analyte present has saturated the detector. This situation results in an underestimation of the affected analyte(s) Q Indicates the presence of a quantitative interference. This situation may result in an underestimation of the affected analyte(s) I Indicates the presence of a qualitative interference that could cause a false positive or an overestimation of the affected analyte(s) DPE Indicates the presence of a peak in the polychlorinated diphenylether channel that could cause a false positive or an overestimation of the affected analyte(s) TIC Tentatively Identified Compound EMPC Estimated Maximum possible Concentration due to ion ratio failure ND Not Detected K Result is estimated due to ion ratio failure in High Resolution PCB Analysis P RPD > 40% between results of dual columns D Spike or surrogate was diluted out in order to achieve a parameter result within instrument calibration range Samples requiring manual integrations for various congeners and/or standards are marked and dated by the analyst. A code definition is provided below: M1 Mis-identified peak M2 Software did not integrate peak M3 Incorrect baseline construction (Le. not all of peak included; two peaks integrated as one) M4 Pattern integration required (i.e. DRO, GRO, PCB, Toxaphene and Technical Chlordane) M5 Other - Explained in case narrative Note Results pages that include a value for "Solids (%)" have been adjusted for moisture content. Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.G. Certification # 481 Member of SGS Group Page 2 of 149 ZR INCORPORATED ENVIRONMENTAL CONSULTANTS TO: SGS Environmental Services Attn: Amy Boehm 5500 Business Drive Wilmington, NC 28405 DATE: 6 October 2011 CHAIN OF CUSTODY 31 }0D1175 4709 COLLEGE ACRES DRIVE SUITE 2 WILMINGTON, NORTH CAROLINA 28403-1725 TEL 910-392-9253 FAX 910-392-9139 cuwilm@czrdnc.com FROM: Sam Cooper CZR Incorporated, Suite 2 4709 College Acres Drive Wilmington, NC 28403 scooper@czr-inc.com RE: International Paper Company, Inc., Annual Fish Project (IP 2011 PO# S-066125110 to SGS) Analysis of fish tissues for 2, 3, 7, 8 TCDD (Dioxin), 2, 3, 7, 8, TCDF (Furan), and lipids (%) ENCLOSED ITEMS: Thirteen (13) frozen composite fish tissue (fillets) samples, each fillet wrapped in aluminum foil (dull side toward fish) and enclosed in labeled "zip -lock" plastic bags. Composites are identified below. Composite # 1 2 3 4 5 6 7 8 9 10 11 12 13 COMMENTS: SAMPLE ID # Site Species (number of fish fillets) 1 1 1 1 2 2 2 2 3 3 3 3 1 Bluegill (10 "A" fillets) Flathead Catfish (1 "A" fillet) Blue Catfish smaller (8 "A" fillets) Blue Catfish larger (10 "A" fillets) Bluegill (11 "A" fillets) Flathead Catfish (4 "A" fillets) Blue Catfish (12 "A" fillets) Common Carp (8 "A" fillets) Bluegill smaller (10 "A" fillets) Bluegill Iarger (10 "A" fillets) Flathead Catfish (3 "A" fillets) Blue Catfish (10 "A" fillet) Blue Catfish large replicate (10 "B" fillets) - Send one digital version and two hard copies of the report to Sam Cooper/CZR at the above address. - Forward the invoice to Ms. Kim Fail International Paper Company John L. Riegel Road Riegelwood, NC 28456 (Kimberly.Fail@ipaper.com@ipaper.com) phone: 910 655-4753 fax: 910 655-9416 /Received by: Date/time !o 1' 13: iS ate/time . 5.eq 2151 Altemat6 A1A South • SUITE 2000 • JUPITER, FLORIDA 33477-3902 TEL 561-747-7455 • FAX 561-747-7576 • coin@czr-Inc.com • www.CZRINC.com �. 3C. CP #1340.19 Page 3 of 149 !^ !4"\ SGS North America Inc. Sample Receipt Checklist (SRC) Client: International Paper Work Order No.: 31102775 'd"\ 1. Shipped Notes: x Hand Delivered r4"b% 2. x COC Present on Receipt No COC Additional Transmittal Forms fAR's 3. Custody Tape on Container x No Custody Tape 4. x Samples Intact Samples Broken / Leaking r"N 5. x Chilled on Receipt Actual Temp.(s) in °C: 0.0, -2.1, -6.3 '^ Ambient on Receipt Walk-in on Ice; Coming down to temp. Received Outside of Temperature Specifications 6. x Sufficient Sample Submitted Insufficient Sample Submitted 7. Chlorine absent NA HNO3 < 2 !.`"N HCL < 2 elq Additional Preservatives verified (see notes) !mb` 8. x Received Within Holding Time Not Received Within Holding Time No sample collection date or time on COC or 9. No Discrepancies Noted bags. e., x Discrepancies Noted NCDENR notified of Descrepancies* /"t' 10. No Headspace present in VOC vials Headspace present in VOC vials >6mm Comments: roN eihN e.., etaN Inspected and Logged in by: TP r►, Date: Fri-10/7/11 00:00 Page 4 of 149 *NCDENR must be notified when collection, holding time or preservation requirements are not met. MI_11.6 r4"\ Sample Summary Client Sample ID Lab Sample ID Collected Received Matrix Comp#1 Site 1 Bluegill 31102775001 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#2 Site 1 Flathead Catfish 31102775002 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#3 Site 1 Blue Catfish sm 31102775003 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#4 Site 1 Blue Catfish Ig 31102775004 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#5 Site 2 Bluegill 31102775005 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#6 Site 2 Flathead Catfish 31102775006 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#7 Site 2 Blue Catfish 31102775007 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#8 Site 2 Common Carp 31102775008 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#9 Site 3 Bluegill sm 31102775009 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#10 Site 3 Bluegill Ig 31102775010 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#11 Site 3 FlatheadCatfish 31102775011 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#12 Site 3 Blue Catfish 31102775012 10/06/2011 00:00 10/06/2011 13:15 Tissue Comp#13 Site 1 Blue Catfish Ig 31102775013 10/06/2011 00:00 10/06/2011 13:15 Tissue Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sas.com N.C. Certification # 481 Member of SGS Group Page 5 of 149 Results of Comp#1 Site 1 Bluegill Client Sample ID: Comp#1 Site 1 Bluegill Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775001 Lab Project ID: 31102775 a }-{Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result EMPC Qual DL LOQ/CL Units RT Ratio 2,3,7,8-TCDD ND U 0.123 0.459 pg/g 2,3,7,8-TCDF ND U 0.0501 0.459 pglg \ J Print Date: 11/01/2011 N.C. Certification # 481 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903f 910.350.1557 www.us.sas.com Member of SGS Group Page 6 of 149 Results of Comp#1 Site 1 Bluegill Client Sample ID: Comp#1 Site 1 Bluegill Client Project ID: Annual Fish Project 2011 Lab Sample ID: 1102775001 Lab Project ID: 3 102775 >-LResults by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result 71.0 72.0 76.0 Batch Information Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/29/2011 21:07 Dilution: 1 EMPC L. DL LOQ/CL Units RT 40.0-135 40.0-135 40.0-135 Ratio Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt./Vol.: 10.9 g Prep Extract Vol: 20 uL Print Date: 11 /01 /2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903f 910.350.1557 www.us.sas.com N.C. Certification # 481 Member of SGS Group Page 7 of 149 e-LResults of Comp#1 Site 1 Bluegill Client Sample ID: Comp#1 Site 1 Bluegill Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775001-A Lab Project ID: 31102775 }{Results by Gravametric Parameter % Lipids r—lBatch Information Result 0.260 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): EMPC Qual DL LOQ/CL, Units RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 8 of 149 ))))))))))))))))))))))))))))))))))))))))))) Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:1MassLynx\Default.prolResultslb29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29octlla-4 Date: 29-Oct-2011 Time:21:07:59 J ID: 311027750011 Submitter: HRD1459 Task: MS Method Name: C:1MassLynxIDEFAULT.PROIACQUDBIdioxins_db5ms dw2.EXP Description: Comp#1 Site 1 Bluegill -fm 11')-II 1 2 3 4 5 6 7 :Name : Response. lon1Area: Ion2Area. RA .:RAFaiI?: RT; pg/pL. EDL; Heightl . Noisel; SN1. Height2::Noise2. SN2 ; M1 . M2. User RF 2378-TCDF - NO - 0.0273 591 552 1.004 ;2378-TCDD NO / - 0.0670 1072 - - 999 1.171 ES:13C-2378-TCDD 5.256e5 2.288e5 2.969e5 0.77 NO 27.24 0.739 0.0999 2.870e6 1844 1556.5 3.610e6 2074 1740.1 bb bb 1.026 .ES:13C-2378-TCDF 8.193e5 3.618e5 4.575e5 0.79 NO 26.35, 71.737 0.0659 4.598e6 1812 2537.2 5.882e6 2158 2725.6 bb bb 1.577 .JS:13C-1234-TCDD 7.242e5 3.206e5 4.036e5 0.79 NO 26.55/ 100.000 0.1025 4.229e6 1844 2293.5 5.355e6 2074 2581.6 bb bb 1.000 • CS:37C1-2378-TCDD 1.332e5 1.332e5 - - 27.26/ 15.100 0.0182 1.653e6 848 1949.7 - bb 1.218 •F1 Lock Mass - - 51073 - - Quantify Sample Report MassLynx 4.1 SCN640 ###TCOD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Method: C:IMassLynxIDEFAULT.PROIMethDB1db5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:lMas¢..ynx1DEFAULT.PRO1CurveDBImtetras-051611d new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-4, Date: 29-Oct-2011, Time: 21:07:59, ID: 31102775001, Submitter: HRD1459, Task: 2378-TCDD b29oct11 a-4 23.94 24.00:24.07 0 22.70 23.3923.69, �'AF\ 24.2024.4324.73 25.42 70 22.18 22.59 -..c 25.24 48- :� , sir-• - _ -1-----.- -^!. , .... , ... , i . ri ---- .7: �r-r � : s . i 1 :V-; - , ,-, i -r 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 2378-TCDD b29oct11 a-4 39- Voltage SIR,EI+ 319.8965 26.36 26.6427.49 27.90 6.272e+004 26.04 26.96 28.07 28.4428.68 29.05 29.38 .. .:"i 1-e= . , . �; �- r-r �, , ti , i -rr-s-r•-nrT?,-r-- . min 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 23.85 24.09.24.07 23.64�i 24.20 24.50 24.74 22.24 25.1925.42 25.93.26.01 26.44 26.96 27.23 27.36- - 28.76 22 00 ES-TCDD b29oct11 a-4 22.50 23.00 %]1 ."1" 1 22 00 22.50 23.00 ES-TCDD b29oct11a-4 23.50 24.00 24.50 25.00 25.50 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 26.55 ES:13C-2378-TCDD 27.24 26.00 26.50 27.00 27.50 26.55 I. ,. I I I . 1 1 , J 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 ES:13C-2378-TCDD 27.24 CS-TCDD b2 ,oct11 a-4 28.00 28.50 29.00 28.00 28.50 29.00 Voltage SIR,EI+ 321.8936 29.65 7.938e+004 min 29.50 30.00 Voltage SIR,EI+ 331.9368 4.286e+006 .., �...,� min 29.50 30.00 Voltage SIR,EI+ 333.9339 5.426e+006 min 27.50 28.00 28.50 29.00 29.50 30.00 CS:37CI-2378-TCDD 27.26 \, 22.00 Ff'Lock Mass b29oct11 a-4 e22.04 22.37 22.70 `\. •• 23.06 22.50 23.00 II 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 23.48 23.74 23.99 24.20 24 68 24.84 25 29 25.5025. 96 26.14 26.22 26.68 27.01 Voltage SIR,EI+ 327.8847 1.693e+006 i min 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 304.9824 27.87 28.0528 28 28.58 28.97 29.14 29 43 3.060e+006 min 22 00 22.50 23.00 23:50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Name: b29oct11a-4, Date: 29-Oct-2011, Time: 21:07:59, ID: 31102775001, Submitter: HRD1459, Task: 2378-TCDF b29oct11a-4 Voltage SIR,EI+ 24.73 303.9016 5.162e+004 % 22.0822.31.• .1\ .....97 2928 .298923.28 23.59 24.05 ..25.06 .26.01 26 45,26.54 27.51 28,36 28.44 �.'A_ ' A_ ,, .,. .,. .,. ,,, , min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11a-4 Voltage SIR,EI+ 28.68 305.8987 �� 4.392e+004 22.09 26.39 22.34 22.7022.8223.16 23.59 23.84 24.0224.36 24.71 25.07 25.48 25.86 26.22 /`26.72 ,26.82 27.38 5 28.03 28.48 28.74 29.30 r r w i 29.09 29.91 66, `. , , , ,min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11 a-4 ES:13C-2378-TCDF 26.36 1 ; ., , , .. , .•i, , , , ,,,1 . , , , 1 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 Voltage SIR,EI+ 315.9419 4.668e+006 ,,.,.,,.,,,,.,,,.,,.. ,,,, min 28.50 29.00 29.50 30.00 ES-TCDF b29oct11a-4 ES:13C-2378-TCDF Voltage SIR,EI+ 26.36 317.9389 i 5.962e+006 70- cV2 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 i T 27.50 28.00 28.50 29.00 29.50 30.00�n F'Lock Mass bZoct11 a-4 22.04 Ole Voltage SIR,EI+ 304.9824 3.060e+006 22.37 24.20 24.84 25.50 25.96 27.87 28.97 29.88 22.70 23.06 23.48 23.74 23.99 24.68 25.29 26.14 26.22 26.68 27.01 28.0528.28 28.58 29.14 29.43 35 , , , ; min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 SG$ Results of Comp#2 Site 1 Flathead Catfish Client Sample ID: Comp#2 Site 1 Flathead Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775002 Lab Project ID: 31102775 }-Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result EMPC gl& DL LOQ/CL Units RT Ratio 2,3,7,8-TCDD ND U 0.117 0.462 pg/g 2,3,7,8-TCDF ND U 0.0481 0.462 pg/g Print Date: 11/01/2011 N.C. Certification # 481 SGS North America Iic. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com Member of SGS Group Page 12 of 149 SG$ Results of Comp#2 Site 1 Flathead Catfish Client Sample ID: Comp#2 Site 1 Flathead Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775002 Lab Project ID: 3 102775 Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD e—IBatch Information Result EMPC 89.0 90.0 94.0 ual DL LOQ/CL Units RT 40.0-135 40.0-135 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/29/2011 21:44 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.NoI.: 10.82 g Prep Extract Vol: 20 uL Print Date: 11 /01/2011 SGS North America Inc. N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sas.com Member of SGS Group Page 13 of 149 SG$ Results of Comp#2 Site 1 Flathead Catfish Client Sample ID: Comp#2 Site 1 Flathead Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775002-A Lab Project ID: 31102775 }-{ Results by Gravametric Parameter % Lipids Batch Information Result EMPC 0.170 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Qual DL LOQ/CL Units 0/0 RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903f 910.350.1557 www.us.sgs.com N.G. Certification # 481 Member of SGS Group Page 14 of 149 ))))))))))))))))))))))))))))))))))))))))))) Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:IMassLynxlDefault.prolResults\b29octila-ltetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time lbl '-I-Ii Name: b29oct11a-54" Date: 29-Oct-20 )/ Time: 21:44:39 ID: 31102775002 Submitter: HRD1459 Task: MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins__db5ms_dw2.EXP Description: Comp#2 Site 1 Flathead Catfish 1 2 3 4 5 6 7 :Name : Response- Ion1Area: lon2Area: RA .:RAFaiI?: RT: pg/NL- EDL: Heightl - Noisel: SN1: Height2 :• Noise2 - SN2 : M1 : M2- User RF :2378-TCDF NO 0.0260 - 902 520 1.004 :2378-TCDD - NO -/ - 0.0633 1196 - - 1346 - - 1.171 :ES:13C-2378-TCDD 6.710e5 2.954e5 3.756e5 0.79 NO 27.24 88.867 0.0857 3.774e6 1747 2159.8 4.799e6 1695 2830.8 bb bb 1.026 : ES:13C-2378-TCDF 1.047e6 4.572e5 5.899e5 0.78 NO 26.36/ 90.225 0.0625 5.953e6 1926 3090.8 7.451e6 1931 3857.7 bb bb 1.577 •JS:13C-1234-TCDD 7.359e5 3.274e5 4.085e5 0.80 NO 26.55//100.000 0.0879 4.355e6 1747 2492.5 5.440e6 1695 3208.8 bb bb 1.000 • CS:37CI-2378-TCDD 1.680e5 1.660e5 - 27.26/ 18.744 0.0216 2.066e6 1030 2005.9 - bb 1.218 :F1 Lock Mass - - 55705 - 6b1. 1° 9 6 a6ed Quantify Sample Report ###TCDD TCDF Only ### Dataset: Untitled MassLynx 4.1 SCN640 Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Method: C:1MassLynxIDEFAULT.PROIMethOBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:IM7LynxxDEFAULT.PRO1CurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-5, Date: 29-Oct-2011, Time: 21:44:39, ID: 31102775002, Submitter: HRD1459, Task: 2378-TCDD b29oct11 a-5 24.00 23.23 23.74 24.10 24.73 26.16 26.34 26.49 26.70 27.26 27.7127.94 28.2328.46 28.84 44° : 22.5222.59 22.87 23.38���24.33- ,24.89 25.32 25.76 22 00 2378-TCDD b29oct11 a-5 22.50 23.00 23.50 24.00 24.50 25.00 23.97 24.04 °io 22.16 23.77. , \ 24.58 24.96 34- 22.00 22.50 23.00 23.50 ES-TCDD b29oct11 a-5 %1 22 00 22.50 23.00 ES-TCDD b29oct11 a-5 1 ...,,...I.,..,, 24.00 24.50 25.50 26.00 26.50 25.45 25.73 26.26.26.34 27.00 27.50 28.00 28.50 Voltage SIR,EI+ 319.8965 29.52 6.854e+004 29.00 27.26 27.71 27.97 28.71 29.17 25.00 25.50 26.00 26.50 27.00 27.50 ES:13C-2378-TCDD 26.55 27.24 28.00 28.50 29.00 29.50 min 30.00 Voltage SIR,EI+ 321.8936 8.927e+004 min 29.50 30.00 Voltage SIR,EI+ 331.9368 4.411 a+006 ,...,,.,r.,,,. .............. .... ,....,....� min 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 ES:13C-2378-TCDD 26.55 27.24 26.00 26.50 27.00 27.50 Voltage SIR,EI+ 333.9339 5.509e+006 .................... ..................4 min 28.00 28.50 29.00 29.50 30.00 CS-TCDD b2goct11 a-5 CS:37CI-2378-TCDD 27.26 11 A 2 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 F1 Lock Mass b29oc Voltage SIR,EI+ 327.8847 2.107e+006 t11a-5 Voltage SIR,EI+ `.22.04 22.37 22.62 22.90 23.58 24.05 25.3725.fi0 26.32 26.90 27.66 28,96 304.9824 23.36 24.27 24.73 24.96 ,25.06 26.11 27.08 27.8728.10 28.58 29.07 29.50 2.471e+006 41--� ... _ - . , ..__'.. . , � -, - ,-"�, ,min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Name: b29oct11a-5, Date: 29-Oct-2011, Time: 21:44:39, ID: 31102775002, Submitter: HRD1459, Task: 2378-TCDF b29oct11a-5 1 22.08 22.74 22.88 23.23 23.6223.85 24.27 24.91 25.06 I J� �/� 24 56/V \1\_�-•,...._ 25.52 25.90 26.41 26.57 26.82 27.10 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 Voltage SIR,EI+ 303.9016 3.562e+004 27.26 27.71 27.90 28.46 28.73 29.15 29.5629.68 ,.,,,,,, ,, min 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11a-5 Voltage SIR,EI+ 24.60 305.8987 22.0822.31 3.593e+004 24.51 26.37 23.72 23.$5 25.37 25.55 27.29 27.57 29.63 29.76 29.86 ;1 22.87 22.95 23.41 24•.68 25.04 !� 26.64 26.70,26.96 28.08 28.38.28.46 29.05 29.47 ^• 1.! :� r.�/ ' L� /�-J1 �n /`. r`� `�-. ^-� f J ' �� 2617 1 J� 1/ /` 11; �•- 1. . fJ �. , ,-_;. ,, ,,. , .-_.,..,.Aft._, 1! �' /1 `'�r`✓, .,��/l-' , f�_.%---- . �t 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11a-5 1 22 00 ES-TCDF b29oct11 a-5 22.50 23.00 23.50 24.00 24.50 25.00 R22 00 22.50 23.00 23.50 24.00 24.50 25.00 v F'eLock Mass b22oct11a-5 ES:13C-2378-TCDF 26.36 A I t T. .., .. .. min 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 315.9419 6.030e+006 ES:13C-2378-TCDF Voltage SIR,EI+ 26.36 317.9389 7.522e+006 .1 j, ,.,.r... ,ir,.,....,., , • .,.I,,. ....r. ,......I., i min 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 22.04 304.9824 2.471e+006 \ 22.23.58 24.05 25.3725.60 37 26.32 26.90 27.66 28.96 22;62 22.90 23.3624.27 24.7324.96...25.06 26.11 27.08 27.8728.10 28.58 29.07 29.50 29.88 41 ,. , , min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Results of Comp#3 Site 1 Blue Catfish sm Client Sample ID: Comp#3 Site 1 Blue Catfish sm Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775003 Lab Project ID: 31102775 >{Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result EMPC Qual DL LOQ/CL Units RT Ratio 2,3,7,8-TCDD 0.295 J 0.0983 0.459 pglg 27.26 0.62* 2,3,7,8-TCDF 0.277 J 0.0767 0.459 pglg 26.37 1.85* Print Date: 11/01/2011 SGS North America Inc. N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sas.com Member of SGS Group Page 18 of 149 e-LResults of Comp#3 Site 1 Blue Catfish sm Client Sample ID: Comp#3 Site 1 Blue Catfish sm Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775003 Lab Project ID: 31102775 }-Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD r-lBatch Information Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC 87.0 88.0 90.0 Qual DL LOQ/CL Units RT 40.0-135 40.0-135 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical DatefTime: 10/29/2011 22:21 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.NoI.: 10.9 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 19 of 149 c-LResults of Comp#3 Site 1 Blue Catfish sm Client Sample ID: Comp#3 Site 1 Blue Catfish sm Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775003-A Lab Project ID: 31102775 >-f Results by Gravametric Parameter % Lipids Batch Information Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC 2.44 Qual DL LOQ/CL Units RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sas.com N.C. Certification # 481 Member of SGS Group Page 20 of 149 Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only # /4 Dataset: C:IMassLynx1Default.prolResultslb29oct1 la-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29octlla-6 Date: 29-Oct-2011 Time:22:21:19 ID: 31102775003 4 Submitter: HRD1459 Task: MS Method Name: C:1MassLynx\DEFAULT.PROIACQUDBtdioxins_db5ms_dw2.EXP Description: Comp#3 Site 1 Blue Catfish sm 1 2 3 4 5 6 7 :Name :2378-TCDF 2378 TCDD : ES:13C-2378 TCDD : ES:13C-2378-TCDF •JS:13C-1234-TCDD • CS:37CI-2378-TCDD •F1 Lock Mass Response- Ion1Area: Ion2Area. RA .RAFait?• 1.310e3 8.505e2 4.593e2 1.85 YES 1.056e3 4.021e2 6.539e2 0.61 YES 5.593e5 2.478e5 3.115e5 0.80 NO 8.644e5 3.787e5 4.857e5 0.78 NO 6.230e5 2.807e5 3.424e5 0.82 NO 1.372e5 1.372e5 - RV pg!pL- 26.37/ 0.151 27.26' 0.161 27.23 87.496 26.36/ 87.978 26.54,z100.000 27.26, 18.077 EDL: Heightl - Noisel: SN1- Height2 :• Noise2 - SN2 : M1 : M2- User RF 0.0418 1.327e4 770 17.2 6.578e3 1082 6.1 bb bb 1.004 0.0536 5.400e3 872 6.2 9.121e3 905 10.1 MM MM 1.171 0.0978 3.134e6 1968 1592.8 4.003e6 1215 3294.8 bb bb 1.026 0.0746 4.829e6 1821 2652.3 6.164e6 1912 3223.6 bb bb 1.577 0.1003 3.574e6 1968 1816.0 4.317e6 1215 3553.3 bb bb 1.000 0.0288 1.748e6 1113 1570.5 - bb 1.218 57205 - C_TCbFi -, )' 3 /0e3 8'•G NttpS 6P1.10 I. 96ed 2ooOpJ /o q 3 1 i. aay/(, 0. X7-7-pi -f.,r, 11-I- ! I Quantify Sample Report ###TCDD TCDF Only ### Dataset: Untitled MassLynx 4.1 SCN640 Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Method: C:IMassLynxIDEFAULT.PRO1MethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:IMas LynxIDEFAULT.PRO1CurveDBlmtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-6, Date: 29-Oct-2011, Time: 22:21:19, ID: 31102775003, Submitter: HRD1459, Task: 2378-TCDD b29octl1a-6 Voltage SIR,EI+ 23.97 24.05319.8965 27.26 6.757e+004 22.23 23.11 --'� �,.24.30�24.5824.81 25.24_25.34 25.6826.03 26.34 26.62 28.61 28.97 29.22 29.55 45 T, T . , , ,-1=y , , , ,1-, . , , , .. , r, , . , -'riYrr -e. i i-rt , . =, . , ,' rr.,s-rr, . , ,--n--•frr.-, .. , . j , -1 , • . ri ... , .'r. -i min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11a-6 Voltage SIR,EI+ 23.9224.Q4 321.8936 25.42 26.54 27.05 7.535e+004 41� 22..14 23.38,23.48 - - - \,_ 24.33 ,24.43 24.91 25.22 25.80 26.11 26.36 i 27.24 27.99 29.25 --1, , , • , . , .,.-ip,i,�j ,f:'�' ,,,.r,1 , ,, , ,, • . , ,. r„ ,min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-6 ES:13C-2378-TCDO Voltage SIR,EI+ 26.54 27.23 331.9368 %- . ,.. . , .. 3.615e+006 ,,. ,. ,. ,. ,. ,. ;, ,, �,,.• . ,. ., ,. ,. ,. ,. 1 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11 a-6 22 00 22.50 23.00 23.50 24.00 24.50 ES:13C-2378-TCDD 26;,54 27.23 Voltage SIR,EI+ 333.9339 4.379e+006 ., , ..i ..i,... .,i min 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b2%octlla-6 CS:37CI-2378 TCDD Voltage SIR,EI+ cu 27.26 327.8847 11 .. n 1.788e+006 .. ,, ,. ,, ,. ,. ,. ,, ,, , ,. ,. .,. ,. .,. 1 min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 F1`°Lock Mass b29oct11a-6 Voltage SIR,EI+ 22.04 22.37 22.93 26.29 28.25 29.63 304.9824 cAl22.54 23.53 23.85 24.46 24.53 24.63 25.14 25.53 25.88 26.18 - _ 26.92 26.98 27.41 .27.51` ` 28.08 _; 28.38 28.48 29.15.29.42 2.572e+006 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ))))))))))))))))))))))))))))))))))))))))))) 879ar3$1 t+•6 Smeotn(S0,1x2) 41 23.97 24.05 24 30 24.58 24 01 25 24 35.34 elirtell 2378-TCDD 402.127260 0.16 o 4jL 25.66 28.326182634 2862 6` 2961 2897 -.1 2922 2955 Vollage SIR,EI• 319 8965 6757e•004 29 68 30.0Z min 829adi 1 a•6 Smoothr'S0.1,33 4t 23.9924 04 23.81 23.38 21.46Y^, Jrh 24 33 24.43 25.22 25.53 24.84 24.91 25.42 25.80 2811 28.38 26544 b:9asIt 18.8 8mcoth00,1 x2) b79ac111 a•6 Srnoctlt7S0,1 %2) 26.54 2854 2378-TCOD 27.24 653 93 27.05 1009 27.99 96 1 22.75 23.00 23.25 23.50 2375 24..00 24:25 24.50 24 75 25.00 2525 25:50 25.75 26.00 26.2S 25.50 26.75 I7.00 61' 610 £Z a6ed ES 13C-2370•T000 27.23 247785 23 87 50 pg$1L 1592 77 ES 13C•2378•TCDD_ 2123 31152013 3294 81 VO t7gv SIR,EI• 321.8936 7 535e•004 29 25 30 01 min Voltage SIR,EI• 3310388 3.6158.006 min Vgtlage EIR•E1• 333 8339 4.3708.008 27.25 min 21,50 27.75 28.00 28'75 28.50 28.75 • 29.00 29.25 29.50 29.75 30.00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Name: b29oct11a-6, Date: 29-Oct-2011, Time: 22:21:19, ID: 31102775003, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-6 25.68 2378-TCDF Voltage I 303.9016 22.32 25.62 1 26.37 4.643e+004 - 22.04/ 22.69 23.38 25.7625.99 28.08 28.46 22.75 23.62 23.87 24.25 24.38 25.12 25.29 ` /,r ^ Jt ��24.46 - _ , l 26.72 27.03 27.43 27.89 \ �` /28.54 29.14 29.50 29.71 22 00 22.50 23.00 23.50 24.00 24.50 25.00 i 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 i ' 29.50 30.00 2378-TCDF b29oct11a-6 22.34 22.041\ 22:74 \22.57 Voltage SIR,EI+ 305.8987 4.341 a+004 2637 3.05 23.25 23.59 23.84 24.20 24 46 26.i 1 26.95 28.05 28.43 28.79 �,�� - �� 25.02_. j! ,25y14� ; 2fi.73 27.46 �„ d1 ,\ 29.12 29.61 29.86 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF 25.09 25.47 25.67 28.23 ES-TCDF b29oct11a-6 ES:13C-2378-TCDF Voltage SIR,E1+ 26.36 315.9419 4.903e+006 ,.,..,., .,.,. ,.... ,,,..,...,�, ..,,... ,.1., ,,,,,.,. . ..,....... ,,.,. . ..... ........ min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11 a-6 %_ ES:13C-2378-TCDF 26.34 Voltage SIR,EI+ 317.9389 6.244e+006 ,.j,, .,,,.,. min 12 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 N A F19Lock Mass b2sDoct11 a-6 CO Voltage SIR,EI+ ,22.04 + 22.37 22.54 2.572e+006 \ -1 Jt•22.75 23.25 23.53 23.85 24.46 24.53 24.63 25.14 25.53 25.88 26.1826.29 26.92 26.98 27.41 27.51 28.0828.25 28.38 28.48 29.24 29.42 29.63 29.91 - ��_ -__- _ _._ _�•.Y r-..•w��.. �. ,, 1.= , min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 c-LResults of Comp#4 Site 1 Blue Catfish Ig Client Sample ID: Comp#4 Site 1 Blue Catfish Ig Client Project ID: Annual Fish Project 2011 Lab Sample ID: Z1102775004 Lab Project ID: 31102775 Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Result EMPC ND ND Qual DL LOQ/CL Units RT U 0.181 0.489 pg/g U 0.219 0.489 pg/g Ratio Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 25 of 149 e-LResults of Comp#4 Site 1 Blue Catfish Ig Client Sample ID: Comp#4 Site 1 Blue Catfish Ig Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775004 Lab Project ID: 31102775 }-)Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD rd Batch Information Result EMPC 69.0 69.0 71.0 Qual DL LOQ/CL Units RT 40.0-135 % 40.0-135 % 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/29/2011 22:58 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.NoI.: 10.22 g Prep Extract Vol: 20 uL Print Date: 11 /01!2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sos.com N.C. Certification # 481 Member of SGS Group Page 26 of 149 Results of Comp#4 Site 1 Blue Catfish !g Client Sample ID: Client Project ID: Lab Sample ID: 3 Comp#4 Site 1 Blue Catfish Ig Annual Fish Project 2011 1102775004-A Lab Project ID: 31102775 }-Results by Gravametric Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result % Lipids 3.69 Batch Information Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 EMPC ual DL LOQ/CL Units ok RT Ratio Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 27 of 149 Quantify Sample Summary Report ###TCDD TCDF Only ##1# MassLynx 4.1 SCN640 Dataset: C:1MassLynx\Default.prolResults1b29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11a-7/ Date: 29-Oct-20111 Time: 22:58:05 ID: 31102775004, Submitter: HRD1459 Task: MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins_db5ms_dw2.EXP Description: Comp#4 Site 1 Blue Catfish ig 1 2 3 4 5 8 7 :Name :2378-TCDF :2378-TCDD : ES:13C-2378-TCDD : ES:13C-2378-TCDF -JS:13C-1234-TCDD • CS:37C1-2378-TCDD • F1 Lock Mass • Response- Ion1Area• Ion2Area: RA .:RAFail?• NO NO 4.485e5 1.997e5 2.488e5 0.80 6.908e5 3.076e5 3.832e5 0.80 6.366e5 2.784e5 3.582e5 0.78 1.098e5 1.098e5 NO NO NO RT: pg/pL. EDL: Heightl: Noisel: 0.1121 - 1550 0.0925 - 1237 27.23f/ 68.676 0.0940 2.512e6 1781 26.34f 68.810 0.0809 3.786e6 1742 26.54�100.000 0.0965 3.510e6 1781 27.26/ 14.156 0.0466 1.341e6 1821 50792 1410.6 3.160e8 2173.1 4.777e6 1970.8 4.615e6 736.0 SN1: Height2 :. Noise2 - SN2 ; M1 2278 1207 1315 2402.8 bb 2351 2032.2 bb 1315 3508.8 bb - bb M2 User RF 1.004 1.171 bb 1.026 bb 1.577 bb 1.000 1.218 6t410 8Z e6ed Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Method: C:IMassLynxIDEFAULT.PROIMethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:IMassLynxIDEFAULT.PROICurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-t1', Date: 29-Oct-2011, Time: 22:58:05, ID: 31102775004, Submitter: HRD1459, Task: 2378-TCDD b29oct11a-7 22.11 23.81. 23.90 23.99 22.57 22.92 23.54 24.58 24.76 22.00 22.50 23.00 23.50 24.00 24.50 25.20 25.29 25.63 26.21 26.36 26.90.26.96 27.26 25.00 25.50 26.00 26.50 27.00 Voltage SIR.EI+ 319.8965 5.734e+004 27.79 28.03 28.31 28.82 28.9229.15 29.80�� min 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11 a-7 Voltage SIR.EI+ 24.00 321.8936 syd 22.09 23.6123.90. .^, 24.22 28.17 9.084e+004 33 _22.59 23.39., r ; J ` �� 25.14..25.24 25.63 26.3626.59 26.92 27.26 27.51 27.80 28.30 r'. r,-•r -1-, r-- 29.0T,-�. 29.fi0 ,..- 1�,-�- T ,,. r--�,-�,-�..�............. T , j,. ••min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11 a-7 1• 26.54 ES:13C-2378-TCDD ;'\ 2A i,,,,T,,..,,.. ,,, .;.. t min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 n 26.50 27.00 27.50 28.00 28.50 29.00 29., 50 30.00 Voltage SIR.EI+ 331.9368 3.551e+006 ES-TCDD b29oct11 a-7 ES:13C-2378-TCDD Voltage SIR,EI+ 26.54 333.9339 01��27 23 n 4.669e+006 , 1,,, ,, 1 .1„.; T;i ,. ,; ,;„,, 1'= min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b29oct11 a-7 -v CS:37CI-2378-TCDD Voltage SIR.EI+ 23.61 27.26 327.8847 I 23.25 ; , 25.14 25.40 / `. 1.685e+006 = = i min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 F1`ci.ock Mass b29oct11a-7 Voltage SIR.EI+ 22.04 22.37 22.90 24.05 24.64 24.92 25.32 27.69 28.25 304.9824 % I mo_ 22.72 23.46 23.56 24.20 _ 25.11 25.6625.90.25.99 26.27 26.83 27.6127.67 28.07 28.86 -_28.96 29.55 2.485e+006 40 �,,..�. ,. ,, , , , . „1 .,1,.,,, i_..__ min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Name: b29oct11a-7, Date: 29-Oct-2011, Time: 22:58:05, ID: 31102775004, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-7 2807 Voltage SIR,EI+ . 25.66 28.20 303.9016 ',o y 11 \ �'y 1.026e+005 22.36 23.58 24.23 24.45 25.07 %! 25.98 26.37 27.43 27.77 � 29. i 5 29.76 29.89 ' : - 22.72 23.25 23.85 25.48/ \ 26.72 27.21 27.61 28.46 28.94 v1 r . .I.,r,�- `.i,�..;....i....�'.. Amin 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11 a-7 28.05 28.20 25.65 ill %- 22.32 24.25 25.09 �' 25.98 1 �t 22.74 23.23 23.58 23.87 :1 24.74 r-., 25.50 26.34 26.72 27.00 27.44 22 00 22.50 23.00 23.50 24.00 _ 24.50 1 25.00 25.50 26.00 26.50 27.00 27.50 27.77 i \i \ 28.43 ES-TCDF b29oct11 a-7 %- ES:13C-2378-TCDF 26.34 ' 22 00 22.50 23.00I 23.50 24.00 ' . T 24.50 25.00 I 25.50 26.00 ES-TCDF b29oct11 a-7 %- t 26.50 ES:13C-2378-TCDF 26.34 28.00 28.50 27.00 27.50 28.00 28.50 28.94 29.14 • 29.00 29.50 Voltage SIR.EI+ 305.8987 1.156e+005 29.89 29.63 ' , min 30.00 Voltage SIR,EI+ 315.9419 3.837e+006 29.00 29.50 , min 30.00 Voltage SIR,EI+ 317.9389 4.851e+006 ,, ,. ,. I. ,, ,. ,• I ,. I. ,'"i "r ri.rr., I min 2 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 F1.ock Mass b2ict11a-7 co .22.04 22.37 22.90 24 0 .05 24.64 24.92 25.32 28.25 28.86.28.96 29.55 29.81 I I �� 22.7223.46,23.56 24.20 25.11 25.6625.90.25.99-.26.27 26.83 27.5127.572769 ' - 28.07 40 , �...,,...... ,. , r min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 3-0.00 Voltage SIR,EI+ 304.9824 2.485e+006 r-LResults of Comp#5 Site 2 Bluegill Client Sample ID: Comp#5 Site 2 Bluegill Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775005 Lab Project ID: 31102775 8Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Result ND ND EMPC Qual DL U 0.184 U 0.0528 LOQ/CL 0.457 0.457 Units RT pg/g Pglg Ratio • Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sas.com N.C. Certification # 481 Member of SGS Group Page 31 of 149 ii,Results of Comp#5 Site 2 Bluegill Client Sample ID: Comp#5 Site 2 Bluegill Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775005 Lab Project ID: 31102775 }-I Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD Batch Information Result 96.0 97.0 106 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): EMPC Qual DL LOQ/CL Units RT 40.0-135 % 40.0-135 % 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/29/2011 23:34 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.Nol.: 10.95 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 32 of 149 /—[Results of Comp#5 Site 2 Bluegill Client Sample ID: Comp#5 Site 2 Bluegill Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775005-A Lab Project ID: 31102775 }-(Results by Gravametric Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result % Lipids 0.540 Batch Information Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 EMPC Qual DL LOQ/CL Units RT Ratio Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 33 of 149 Quantify Sample Summary Report ###TCDD TCDF Only Mt MassLynx 4.1 SCN640 Dataset: C:1MassLynx1Default.pro1Results1b29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11 a-8-, Date: 29-Oct-2011/ Time: 23:34:50 ID: 31102775005 / Submitter: HRD1459 Task: MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins db5ms_dw2.EXP Description: Comp#5 Site 2 Bluegill 1 2 3 4 5 6 7 :Name : Response: IonlArea: Ion2Area: RA . RAFaiI?: RT: pg/pL. EDL: Heightl . Noisel: SN1. Height2 :• Noise2: SN2 : M1 . M2: User RF :2378-TCDF NO - 0.0289 659 988 - 1.004 :2378-TCDD NO / ' - 0.1009 2520 - - 1649 1.171 : ES:13C-2378-TCDD 7.083e5 3.148e5 3.935e5 0.80 NO 27.21 95.580 0.0865 3.921e6 1604 2443.7 4.857e6 1701 2856.0 bb bb 1.026 .ES:13C-2378-TCDF 1.109e6 4.887e5 6.202e5 0.79 NO 26.32/ 97.351 0.0738 6.248e6 1948 3207.9 7.923e6 2384 3323.1 bb bb 1.577 •JS:13C-1234-TCDD 7.223e5 3.219e5 4.004e5 0.80 NO 26.52/ 100.000 0.0888 4.149e6 1604 2585.9 5.158e6 1701 3032.5 bb bb 1.000 • CS:37CI-2378-TCDD 1.863e5 1.863e5 27.25/ 21.178 0.0249 2.337e6 1131 2066.1 - bb 1.218 :F1 Lock Mass - 44009 - 61410 ti£ e6ed ))))))))))))))))))))))))))))))))))))))))))) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Method: C:1MassLynxIDEFAULT.PROIMethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:1Ma sLynADEFAULT.PRO1CurveDBlmtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-8, Date: 29-Oct-2011, Time: 23:34:50, ID: 31102775005, Submitter: HRD1459, Task: 2378-TCDD b29oct11a-8 Voltage SIR,EI+ 23.87.23.97 24.13 319.8965 6°/400 22.32 23.53 �� _ 26.32 26 55 - -- 28.53 - 4.803e+004 _„_ 22.7422.97 2_ _ j, ✓" ' "�.--� 24.53 25.19 25.25 25.88 25.98 26.82 27.24 27.52 27.89 28.31 29.04 29.33 i : .r'rr''i f. , ?'r min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11a-8 Voltage SIR.EI+ 2384 23.94 321.8936 . 22.09 22.41 22.88 ; \, 24.17 25.37 29.736.799e+004 %\. 23.08 23.58- _ _ _ \_ 24.84. 25.12_25.22 25.73 26.04 26.34 27.26 27.79 28.66 45, . ,-q , , ,< i r .. , , F , , , .. • r • .'r. T .'' - ; 1 ' . , , . t p--r, I --' ; - ,-r n (7, - , r i -.. ,_ ,.-r.. i rrrr rr-1-.-f- 1---r.- --.-.-ram min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11 a-8 ES:13C-2378-TCDD 26.52 27.21 ' 1 ., , i„ .i i ,. , 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 Voltage SIR,EI+ 331.9368 4.204e+006 , ..•imin 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29octlia-8 ES:13C-2378-TCDD Voltage SIR,EI+ 26.52 27.21 333.9339 r,/o A f 5.212e+006 ,.. =I== `i=. 'T,,.-,i,.,.i,,..i,,,.I .-,T,,,- 7,..,,.,,.,�,_ ,,,..I, ..,,..-.,. �',\ ,.,i.,, i,.,,i,.,.i,,., ._. I....,... i .,.i min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b29oct11a-8 CS:37CI-2378-TCDD Voltage SIR,EI+ 27.24 327.8847 al „ „ „ .. 2.390e+006 i i. .i, ., .i ; ., i i , i , , ,, , i min %2.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 A t0 F1 Lock Mass b29oct1'la-8 Voltage SIR,EI+ 22.0822,37 304.9824 ,/o 23.92 24.20 28.64 29.45 29.73g,g53e+006 22.80 23.31 23.74 24.71 25.01 25.34 25.68 26.16 26.46 26.92 27.64. 27.72 28.02 28.26 - 28.86 39 �`� ��-, Tom -iT - :- iT_._-.,_ ,,..,, --,1 , _ _-, :�- i-----i min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Name: b29oct11a-8, Date: 29-Oct-2011, Time: 23:34:50, ID: 31102775005, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-8 Voltage SIR,EI+ 29.98 23.36 303.9016 22.11 22.29 22.72 22.97 .., - • ,�_6.4 26.o i27.95 �...., ` _.. _ - ca.u�r 1b.4/ ) �. �w �. i .1S.I6 j 22 00 22.50 23.00 2378-TCDF b29oct11a-8 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 22.31 25.63 26.36 305.8987 P 4.186e+004 i' .� 23.08 23.49 24.00 24.13 24.30 � i � 26.55 27.48 28.02 28.22 28.46 29.24 �. i, 22.49 24.53 25.06 25.43125.80 26.11 i`26.70 27.13 27.8222.74 23 21 , 1 1 :1::�,..,,,, .,i...,i .. ..,,....i,,..,....i. r.,.i. i.,,.,....i...,,.... ..,,�,,.,,,,,,..... ...........i,. ,i.'..i ..,,-.. ...t min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30..0 ES-TCDF b29oct11a-8 %, 0 22 00 22.50 ES:13C-2378-TCDF 26.32 11\ ,,. , „ ,...,r,.. , ,,,, , min Voltage SIR,EI+ 315.9419 6.314e+006 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11a-8 ES:13C-2378-TCDF Voltage SIR,EI+ 26.32 317.9389 7.989e+006 %- O,, „ .,,,.,,,,..,i..,.., i ,.,..i.. , i ; , 1 . , i., ,.,..i. i ,..I ,. ..i .. , , 1 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 w 0) F'ILock Mass b22pct11a-8 Voltage SIR,EI+ 22.08 304.9824 2.853e+006 22.37 23.92 24.20 28.64 29.58 22.80 23.31 23.74 24.71 25.01 25.34 25.68 26.16 26.45 26.92 27.64 27.72 28.02 28.26 28.86 29.73 39---.,.; .� ._ ,.,, , ' -, ;.,•.i ,_.. -__ �- --,: min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ))))))))))))))))))))))))))))))))))))))))))) e-IResults of Comp#6 Site 2 Flathead Catfish Client Sample ID: Comp#6 Site 2 Flathead Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775006 Lab Project ID: 31102775 }-{Results by SW-846 8290A Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Result 0.439 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): EMPC 0.112 Qual DL LOQ/CL Units RT Ratio J 0.0955 0.457 pg/g 27.24 0.85 J 0.0467 0.457 pg/g 26.37 1.68* Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 37 of 149 SG$ Results of Comp#6 Site 2 Flathead Catfish Client Sample ID: Comp#6 Site 2 Flathead Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775006 Lab Project ID: 31102775 Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD Batch Information Result EMPC 101 104 106 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Qual DL LOQ/CL, Units RT 40.0-135 % 40.0-135 % 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/30/2011 00:11 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.Nol.: 10.93 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc. N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sus.com Member of SGS Group Page 38 of 149 Results of Comp#6 Site 2 Flathead Catfish Client Sample ID: Comp#6 Site 2 Flathead Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775006-A Lab Project ID: 31102775 }-[Results by Gravametric Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter % Lipids Batch Information Result EMPC 0.730 Qua! DL LOQICL Units RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc. N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.scis.com Member of SGS Group Page 39 of 149 Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:1MassLynxlDefault.pro\Results1b29oct11a-1tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11a-9 , Date: 30-Oct-2011 / Time: 00:11:31 ID: 31102775006 / Submitter: HRD1459 Task: MS Method Name: C:1MassLynxIDEFAULT.PROIACQUDBIdioxins db5ms_dw2.EXP Description: Comp#6 Site 2 Flathead Catfish 1 2 3 4 5 6 7 :F1 Lock Mass :Name Response: lon1Area:Ion2Area: :2378-TCDF 7.712e2 4.830e2 2.881e2 :2378-t.2D 2.2444e + 1.028e3 1.215e3 : ES:13C-2378-TCDD 7.984e5 3.530e5 4.453e5 .ES:13C-2378-TCDF 1.262e6 5.582e5 7.039e5 . JS:13C-1234-TCDD 7.707e5 3.397e5 4.310e5 • CS:37CI-2378-TCDD 1.999e5 1.999e5 - RA . RAFail?: 1.68 YES 0.85 NO 0.79 NO 0.79 NO 0.79 NO RT: pg/pL: 26.37/ 0.061 27.24/ 0.240 27.2100.963 26.34/ 103.846 26.54/ 100.000 27.26 / 21.290 EDL: Heightl . Noisel: SN1: Height2 :. Noise2 . SN2 : M1 - M2- User RF 0.0255 7.728e3 657 11.8 3.870e3 995 3.9 bb bb 1.004 0.0522 1.137e4 1142 10.0 1.611e4 1326 12.2 MM MM 1.171 0.0927 4.461e6 1881 2371.4 5.592e6 1894 2952.1 bb bb 1.026 0.0580 7.140e6 1776 4019.8 8.979e6 1853 4844.6 bb bb 1.577 0.0951 4.374e6 1881 2325.6 5.532e6 1894 2920.1 bb bb 1.000 0.0244 2.474e6 1180 2097.4 - bb 1.218 46844 - Ercbb3 �-?L {e3 - - ..r- ~ `Vosges- 10.939 1.171� 1 61410 Ott eBed Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Method: C:1MassLynx%DEFAULT.PROIMethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:IMas,Lynx10EFAULT.PROICurveDB%mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-9, Date: 30-Oct-2011, Time: 00:11:31, ID: 31102775006, Submitter: HRD1459, Task: 2378-TCDD b29oct11 a-9 22.28 23.3023.53 23.892, 3.95�24.05 24.33 2214 , 26 55 27 24 27.46 29.01 5.943e+004 22.65 23.10�� _ �24.5824.99 25.27 25.76 26A6 26.36 , ' 27.94 28.31 28.58 29.329.38 51 r� r � r . ^, �-t . , r �-; --r r,-z- r r 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11 a-9 23.84 23.97 24.12 ,�0 22.08 22 92 23.64 1. 24.94 25.25 _ 22.65 n :_.., 24.59 25.0626.36 43. - . ri- - 25.65 25 90 .ram_ - ..... .... _ -: 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 Voltage SIR,EI+ 319.8965 Voltage SIR,EI+ 321.8936 26.85 27.26 „_ ,.., 28.41 28.84 7.071e+004 28.63 min 28.00 28.50 29.00 29.50 30.00 27.00 27.50 ES-TCDD b29oct11a-9 ES:13C-2378 TCDD Voltage SIR,EI+ 26.54 27.23 331.9368 4.516e+006 1,.. , , ,. , , •, „ , .,I „ ,,,, „ , .. i '-, . , • , ., , , • . , „ ,. „ , . min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 ^ 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11 a-9 o0a_1 ES:13C-2378-TCDD 26.54 27.23 .., , , ..,.., ,. . ,. . , .., ,. ..,, , it min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 333.9339 5.641e+006 CS-TCDD b29 ct11a-9 CS:37CI-2378-TCDD Voltage SIR,EI+ co 27.26 327.8847 11 , , . , . , „ „ 2.529e+006 . ,. , , , ,, ,., , I I 'i' ,, L ;, i, .,,. .,. ,. i I ,, , min 32.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 it FI Lock Mass b29oct11a-9 Voltage SIR,EI+ .22.04 22.41 304.9824 ,�o'� 25.32 26.31 28.66 29.68 2.653e+006 f�____ 22.9723.20 23.44 23.82 24.15 24.46 24.78 25.17 25.73 26.13 26.96 27.43 27.72 28.18 28.26 29.09 39' .,...., -- • ' ,..,.I,,,.i -_.- - ..- ;___--,- --- T _�_ ,. ,... min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 0228111 a-9 StocothiS0.1 0) 96 51 2330 22 65 2310 !� 24.38 / 24.58 2173 24.99 L! `!V 4...-J252548 2576 26,05 26 35 26.55 26 98 Voltage SIR,EI• 319 89R5 5 9436.004 2378-TCDD 27.24 1028.31 0.74 WA_ 995 29.38 29.93 30 04 30.16 Z7 46 27.94 28.3 2 32} - 28 7� 0� !30 15 0290c11 t a•9 Smoom7S0,1 r2) 43 6ti 6 Jo Zb 86ed 23 97 23.84 2377 24.12 22.92 i 236\ tjI '�Isi 22 65 / 22.75 23.00 23.25 23.50 73.75 24:00 24:25 24.18 voltage SRO. 321.6938 7 0714.004 2370.TCDD 27.26 121530 1215 1 26.36 24.5� , 2, 8 25 5.6 26.09 1 28�89`��}36 28.41 28.63 78 84 3819 30./7 24 50 24 75 755.00 25.25 • 25.50 25:75 26 00 26.25 266 50�2�6:75 27 00 27.25 27:50 27'75 • 28.00 2825 28T50 28'75 29.00 29.25 29:50 29 75 30'80 30 25 30.50 ml„ Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Name: b29oct11a-9, Date; 30-Oct-2011, Time: 00:11:31, ID: 31102775006, Submitter: HRD1459, Task: 2378-TCDF b29oct11a-9 -1 70 . „•, ,..,.. „•,•.,•,, ,., „..1 ..'t • , , .,,, ...r--.•.••.•1••• •.•,•.,•,•,. „ •.•,,,,,1•, ,...,,••• r „ , ,. , ,. .. ..., ., , ,,,I min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 2378-TCDF 28.73 303.9016 26.37 '1 4.207e+004 22.28 22.69 23.38 25.50 25.91 26.09 26.72 26.93 28.07 28.46 i 29.20 \ 23.5623.79 24.08 24.45 24.69 25.0927.44 27.71 1 9 04 29.4229.65 29.96 2378-TCDF b29oct11a-9 22.31 25.48 2378 TCDF 28 A 2463 92 22.37 23.34 23.49 23.74 . 24.17 24.78 25.14 26.24 25.65 26.36 26.73 26.95 27.43 28.05 28.46 28.61 . 29.02 t.f� �` /\ 28.00• 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 ES-TCDF b29oct11 a-9 ofo 0 ES:13C-2378-TCDF 26.34 Voltage SIR,EI+ 305.8987 29.43 3.846e+004 29.71 29.81 29.50 30.00 Voltage SIR,EI+ 315.9419 7.233e+006 22 00 22.50 ES-TCDF b29oct11 a-9 ",, 23.00 23.50 24.00 i " ' I " 1 ' I 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 V2 00 22.50 F'S.Lock Mass b2 oct11a-9 �22.04 23.00 23.50 24.00 " o � .41 22.57 22.97 23.20 23.44 23.82 22 • 39 ,,,,., 22.00 22.50 23.00 23.50 24.50 25.00 25.50 24.15 24.46 24.78 25.17 25.32 25.73 ES:13C-2378-TCDF 26.34 III 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 317.9389 9.056e+006 26.00 26.50 27.00 27.50 28.00 28.50 29.00 291.50 30.00 min 26.13 26.31 26.96 24.00 24.50 25.00 25.50 26.00 26.50 27.00 Voltage SIR,EI+ 304.9824 2.653e+006 28.66 27.43 27.72 28.18-.28.26 29.09 29.58 29.68,:29 78 min 27.50 28.00 28.50 29.00 29.50 30.00 id Results of Comp#7 Site 2 Blue Catfish Client Sample ID: Comp#7 Site 2 Blue Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775007 Lab Project ID: 31102775 }Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result EMPC Qual DL LOQ/CL Units RT Ratio 2,3,7,8-TCDD ND U 0.200 0.473 pg/g 2,3,7,8-TCDF ND U 0.0853 0.473 pglg Print Date: 11/01/2011 N.C. Certification # 481 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com Member of SGS Group Page 44 of 149 r-LResults of Comp#7 Site 2 Blue Catfish Client Sample ID: Comp#7 Site 2 Blue Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 1102775007 Lab Project ID: 3 102775 > -R Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD Batch Information 111 Result 72.0 72.0 76.0 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): EMPC Qual DL LOQ/CL Units RT 40.0-135 40.0-135 40.0-135 OA % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Datemme: 10/30/2011 00:48 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt./Vol.: 10.57 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 45 of 149 Results of Comp#7 Site 2 Blue Catfish Client Sample ID: Comp#7 Site 2 Blue Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775007-A Lab Project ID: 31102775 Results by Gravametric Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result % Lipids 3.13 Batch Information EMPC Quai DL LOQ/CL Units % RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903f 910.350.1557 www.us.sas.com Member of SGS Group Page 46 of 149 Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:1MassLynx\Default.prolResults1b29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11 a-10/ Date: 30-Oct-2011 Time: 00:48:16 ID: 31102775007 Submitter: HRD1459 Task: `1 11-1-) MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins_db5ms_ Description: Comp#7 Site 2 Blue Catfish dw2.EXP 1 2 3 4 5 6 7 :Name :2378-TCDF 2378-TCDD : ES:13C-2378-TCDD : ES:13C-2378-TCDF .JS:13C-1234-TCDD • CS:37CI-2378-TCDD • F1 Lock Mass Response: Ion1Area: Ion2Area : 4.436e5 1.950e5 2.486e5 0.78 6.836e5 3.027e5 3.810e5 0.79 6.002e5 2.680e5 3.322e5 0.81 1.112e5 1.112e5 RA • RAFaiI?; NO NO NO NO NO RT: pg/pL- EDL: 0.0451 0.1059 27.2� 72.034 0.1242 26.34/ 72.234 0.0879 26.54/ 100.000 0.1274 27.24/ 15.208 0.0257 Heightl - Noisel; SN1. Height2 Noise2 . SN2 : M1 M2: User RF 592 973 1.004 1179 - - 1561 1.171 2.428e6 1669 1455.1 3.068e6 2276 1347.6 bb bb 1.026 3.827e6 2054 1863.5 4.876e6 2239 2177.5 bb bb 1.577 3.457e6 1669 2072.0 4.281e6 2276 1880.6 bb bb 1.000 1.422e6 970 1465.3 - bb 1.218 45074 6f'1. Jo Lb 96ed Quantify Sample Report ###TCDD TCDF Only ### Dataset: Untitled MassLynx 4.1 SCN640 Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Method: C:1MassLynxIDEFAULT.PROIMethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:lMassLynxIDEFAULT.PRO1CurveDBlmtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-10, Date: 30-Oct-2011, Time: 00:48:16, ID: 31102775007, Submitter: HRD1459, Task: 2378-TCDD b29oct11a-10 Voltage SIR.EI+ 22.39 23.62 23.87 24.00 319.8965 %,1 22.23 22.7422.97 23.10 -, - - `-' __`24.10 24.5824.69 25 20 25.68 26.2426.36 27.23 27.52 28.89 29.14 29.63 + %� 26.78 27.61 28.23 28.53 \ \ 29.28 •5.731 a 004 51 -? .. , , , . i 'i, .. . , i T , , . , 1 ' , , i � . . , , . ... ... „ , . .. T ". , " - ri-, T-r-rrrr, , 1 i T , 1 , .. 1 . , , I \ . i . . 1 miff 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11 a-10 36 23.8223.94 24.09 2,2.08 22.36 2458 22.74 23.36 24.28 .24.79 25.22 26.34 26.47 7"L 27.21,2 r.31 28.23 29.19 Voltage SIR,E1+ 321.8936 29.71 8.326e+004 22.00 ES-TCDD b29oct11 a-10 1, 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 26.54 ES:13C-2378-TCDD 27.21 min 28.00 28.50 29.00 29.50 30.00 22.00 22.50 23.00 23.50 ES-TCDD b29oct11 a-10 24.00 24.50 25.00 25.50 26.00 26.50 961 1 22 00 22.50 23.00 23.50 24.00 24.50 25.00 CS-TCDD b2soct11 a-10 w 27.00 27.50 28.00 26.54 ES:13C-2378-TCDD 27.21 �1 n, 25.50 26.00 26.50 27.00 27.50 28.00 CS:37CI-2378-TCDD 27.24 /`. °%2 00 22.50 23.00 23.50 24.00 co F1Lock Mass b29oct11 a-10 22.04 28 22.00 22.77 22.95 22.50 23.00 23.50 24.00 24.50 25.00 25.50 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.50 .29.00 1 29.50 Voltage SIR.EI+ 331.9368 3.512e+006 ,min 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 333.9339 4.320e+006 min 30.00 Voltage SIR.EI+ 327.8847 1.463e+006 , 1 min 28.00 28.50 29.00 29.50 30.00 23.56 23.94 24.25 24.56 24.69 25.12 25.52 25.78 26.2126.27 26.98 27.05 27.56 27.69 26.00 26:50 27.00 27.50 Voltage SIR.EI+ 304.9824 28.22 28.61 28.99 29.37 _ 2.804e+006 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11 a-10 Voltage SIR,EI+ 305.8987 22.34 26.42 3.945e+004 ' 22 5122.74 22.87 23.1123.46 23.90 24.3324.45 25;0 26.14 v' 26.72 26.96 27.44 28.00� 0? 28.33 28.71 28.87 29•6529.71 �,n� 1� , ,`� 24.92 25.22 25.78 i �! " ` 29.15 �'` ,. ,,, ,,,. .,,, ,. , , .,. .,. .,, .T .,. .,, r. ,. r,.-, ,.,,,,. ,..., ... ......:..... min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11 a-10 i 22 00 22.50 ES-TCDF b29oct11a-10 %_ 23.00 23.50 24.00 24.50 i 25.00 25.50 ES:13C-2378-TCDF 26.34 Voltage SIR,EI+ 315.9419 3.884e+006 ill 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES:13C-2378-TCDF 26.32 Voltage SIR,EI+ 317.9389 4.945e+006 ,,,,,,,,,,,,,,,.,,,,,,..,, ,,,..,,.:.,...,,., ,,,, ,.,..,..,,,. ,... , ,....,,..,,,,,.,.,,., min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 A CD F'FLock Mass b22oct11a-10 Voltage SIR,EI+ . 22.04 304.9824 2.804e+006 %22,77 22.95 23.56 23.94 24.25 24.56 24.69 25.12 25.52 25.78 26.2126.27 26.9827.05 27.56 27•69 28.22 28.61 28.99 29.37 29.6629'78 l ))))))))))))))))))))))))))))))))))))))))) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:44 Eastern Daylight Time Name: b29oct11a-10, Date: 30-Oct-2011, Time: 00:48:16, ID: 31102775007, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-10 Voltage SIR,EI+ 26.95 303.9016 22.36 23.87 4.818e+004 22.19 22.72 23.07 23.33 23.61 23.99 24.8825.11 25.48 25.7525.98 28.22 28.76 29.04 26.37 26.44 27 71 28.40 29.3329.56 29.63 29.81 -.11---� - �.r.�._�; •...,�..-.._/- �,_ _ - 24.43-•`-- .A v.,--� 27.47 .----�-- -^ `__ - --� 59 ,..,,, .................. ,,...,,1.. .,-..,,,,..,.. .,,,.,, ,.,, ..,..,., ,.,r ,., ,, ,....,,..,,. ,,,. ...,,,, ,...,,... ,... ,,...,, i min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 26.36 28 ,.,.., ,.. , ,. ,,... , ..T ,.,, ,.,,.. min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 SG$ c-LResults of Comp#8 Site 2 Common Carp Client Sample ID: Comp#8 Site 2 Common Carp Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775008 Lab Project ID: 31102775 Results by SW-846 8290A Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC 0.399 0.434 Qual DL LOQICL Units RT Ratio J 0.120 0.491 p9/9 27.25 0.66 J 0.0639 0.491 pg/g 26.36 0.74 Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 50 of 149 f—LResults of Comp#8 Site 2 Common Carp Client Sample ID: Comp#8 Site 2 Common Carp Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775008 Lab Project ID: 31102775 }-{ Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD ,e-lBatch Information J Result EMPC 96.0 97.0 105 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Qual DL LAQ/CL Units RT 40.0-135 % 40.0-135 % 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/30/2011 01:25 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.Nol.: 10.18 g Prep Extract Vol: 20 uL Print Date: 11 /01 /2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sos.com N.C. Certification # 481 Member of SGS Group Page 51 of 149 p-LResults of Comp#8 Site 2 Common Carp Client Sample ID: Comp#8 Site 2 Common Carp Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775008-A Lab Project ID: 31102775 }-Results by Gravametric Parameter % Lipids r—lBatch Information Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC 1.71 go! DL LOQ/CL Units RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.scts.com N.C. Certification # 481 Member of SGS Group Page 52 of 149 ))))))))))))))))))))))))))))))))))))))))))) Quantify Sample Summary Report MassLynx 4.1 SCN640 ####TCDD TCDF Only ### Dataset: C:IMassLynx\Default.prolResultslb29oct11a-ltetras.g1d Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11 a-11 Date: 30-Oct-2011 Time: 01:25:02 ID: 31102775008/ Submitter: HRD1459 Task: MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins_db5ms_dw2.EXP Description: Comp#8 Site 2 Common Carp -114N 11-1-11 :Name : Response. Ion1Area: Ion2Area. RA .:RAFai1?: RT: pglpL. EDL: Heightl . Noisel: SN1. Height2:.Noise2. SN2 : M1 : M2. User RF 1 :2378 TCDF 2.20,� _ 9.382e2 1.271e3 0.74 NO 26.36, 0.221 0.0325 1.578e4 861 18.3 1.611e4 841 19.2 bb bb 1.004 2 :2378- CDT D 1.524e3 6.059e2 9.182e2 0.66 NO 27.25// 0.203 0.0610 8.558e3 1035 8.3 1.211e4 1292 9.4 MM MM 1.171 3 : ES:13C-2378-TCDD 6.403e5 2.818e5 3.585e5 0.79 NO 27.23' 96.150 0.1242 3.584e6 2478 1446.1 4.559e6 1878 2427.7 bb bb 1.026 4 .ES:13C-2378-TCDF 9.948e5 4.382e5 5.567e5 0.79 NO 26.34/ 97.191 0.0745 5.742e6 1820 3154.7 7.375e6 2198 3354.5 bb bb 1.577 5 .JS:13C-1234-TCDD 6.491e5 2.881e5 3.610e5 0.80 NO 26.54 /100.000 0.1274 3.793e6 2478 1530.6 4.797e6 1878 2554.1 bb bb 1.000 6 • CS:37CI-2378-TCDD 1.657e5 1.657e5 - 27.25 20.964 0.0233 2.041e6 971 2101.6 - bb 1.218 7 • F1 Lock Mass 47722 - - Crn3F3 ; d. �•O9e3� 6171. Jo £5 a6ed 0.Lty.(6/ Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:45 Eastern Daylight Time Method: C:1MassLynxIDEFAULT.PRO1MethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:1MasstynxIDEFAULT.PRO1CurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-11, Date: 30-Oct-2011, Time: 01:25:02, ID: 31102775008, Submitter: HRD1459, Task: 2378-TC D D b29oct11a-11 Voltage SIR,EI+ 23.77 23.95 319.8965 701 22.36 22.42 22.83 23.13 23.61 �.04 2,4.35 24.58 24.94 2 4 25.52 25.73 26.36 26.44 2T.08 27.24 28.3Q.28.36 28.74 29.27 29.63 6.692e+004 46� Y, i i ; ; i _. r r,--r. , . , . r i �r, , , , . , , ,1 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29octl l a-11 23.74 23.90 23.97 24.36 ° 22.16 �''�-� 24.96 25.24 27.08 27.24 /° 22.24 22.52 22.97 23.56_ �~'" i t _ 24.73 25.63 2fi.32. 26.5,7 27.54 40 r.,;..r-�.,,.�r.,� -, 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 ES-TCDD b29oct11 a-11 °1°I 22 00 ES:13C-2378-TCDD 26.54 27.23 i i 27.99 28.00 28.61 29.4029.47 28.50 29.00 29.50 Voltage SIR,EI+ 321.8936 7.442e+004 min 30.00 Voltage SIR,EI+ 331.9368 3.838e+006 ES-TCDD b29oct11 a-11 %it 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 ES:13C-2378-TCDD 26.54 27.23 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 333.9339 4.847e+006 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b2$oct11a-11 CS:37C1-2378-TCDD Voltage SIR,EI+ `g 27.24 327.8847 �; `� 2.077e+006 ..,,,. , ;,,,,,,,,,,,,,,,,,,,;,, i, ,.i, „ ;,,., �„ ,.,,, ,,. ,,.,.,,,...,. ,,,,,i.,,,,.,,,�„ ,. min 12.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 F1 Lock Mass b29oct11 a-11 22.04 22.44 341 ,.�.... 22 00 22.50 Voltage SIR,EI+ 24.81 27.16 28.74 304.9824 -.._._- _ .. _......_. ___ .__ 3 27.77 2.7.84 28.20 28.8929.12 2.9.60 2.694e+006 23.00 23.2523.48.23.56 24.05 24.41 25.01 25.3925.80..25.90 26.27 26.6T 27. TTT 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 , ' . , , . , " i min 27.50 28.00 28.50 29.00 29.50 30.00 ))))))))))))I)))))))))))))))))))))))))))))) b29oi1114•I I Sn li53.112) 96 25.24 2.1t62458 2471 �.. / 24,94 25.01 t1 ti-1\,--'1/V 65 029 of t111.11 0 mc0mtS0.112) 55 614 10 55 abed 25 21 21.96 I4.46 / N4 56 2473� 25.34 25 52 25 732595 25.9426.11 25.63 25.63 26 01 26 36 26.32 2378-TCDD 27.24 605.92 020pg$14. 8 27 26.52 26.6926.8527-01 27.08 2370•TCDD 27.24 91823 9.38 28 57 26 61 27 DO 27 08 ,ry 1\ lo�j' 29.83 29.30 28.36 27.75 28.05 / 28.74 ?9 01 29 27 29.40 27.99 Voltage 3IR,E1• 319 S955 4.7822.004 29.99 min Vo'.1agv SIR,EI• 321.6936 5.4284.03s 27.54 29.4029 47 27.11 27 69 �` 2615 29 6128.73 9 0 29 4 • 29.66 29.94 27.48 27 6D 27.00 28.00 26.20 28.40 29.60 28.60 29,00 29.20 29 40 20,60 29.80 30 00 min 24:60 24.80 25.00 25.20 25110 25 60 25 80 26 OD 26:20 26 40 28 60 28.80 27.00 7 27.20 Quantify Sample Report ###TCDD TCDF Only ### MassLynx 4.1 SCN640 Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:45 Eastern Daylight Time Name: b29oct11a-11, Date: 30-Oct-2011, Time: 01:25:02, ID: 31102775008, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-11 2378-TCDF 26.36 Voltage SIR,EI+ 303.9016 4.794e+004 %22.3222.44 22.72 25.47 25.81 26.70 26.88 27.16 28.02 �� 23.33 23.41 23.87 24.2224.2824.69 25.04 28.41 28 48 29.14 29.57 �r�Y_.�--•�_- _... _ . r�, -� .._ ,1- _./\.. 26.19 ,..�. 27.72 29.76 64 , . , , , . , ... - .: ".. . .. ; . . - - _�n�--- �., �.. _,�. _._ ✓ '�, -�---� . �� 1 _ _ _�.- min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11a-11 2378-TCDF Voltage SIR,EI+ 26.37 305.8987 .\ 4.842e+004 22.32 22.70 23.13 2 25.50 25.57 25 67 2.72 27.06 28.05 29.14 29.71 29.91 ; 23.59 3.8423g�24.17 24.71 25.04 �� �� 26.08 \27.48 27.72 28.41�28.51 1 ,. .,,:, ,,..,,,,,,,, ,,,,, ,;,.:,....,....i... i' • i`••.,: :1....,.-.1•••• ,..,. ,-'-..,.(..1.,,.,....-,-•.-.-; .,1min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11 a-11 1 i min 22 00 22.50 1 23.00 i 23.50 24.00 i 24.50 25.00 25.50 26.00 26.50 27.00 r 27.50 28.00 i 28.50 , 29.00 29.50 30.00 ES:13C-2378-TCDF 26.34 Voltage SIR,EI+ 315.9419 5.807e+006 ES-TCDF b29oct11 a-11 %; .00 22.50 gin F1sL.ock Mass b29 ict11a-11 ..22.04 % 34 - 23.00 23.50 24.00 24.50 25.00 22.44 22.57 24.81 2716 28.74 29.75 23.00 23.2523.48 23.56 24.05 24.41 25.01 25.39 25.80.25.90 26.27 26.67 27.03 : ' 27.77 27.84 28.20 28.8929.12 29.60 �l ES:13C-2378-TCDF 26.34 l\ Voltage SIR,EI+ 317.9389 7.444e+006 ,....�..,,,..,,, , ,,,, ,,, I,..,.,,,,,.. . , min 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 • 22 00 22.50 23.00 23.50 Voltage SIR,EI+ 304.9824 2.694e+006 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 • min 30.00 ))))))))))))� Results of Comp#9 Site 3 Bluegill sm Client Sample ID: Comp#9 Site 3 Bluegill sm Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775009 Lab Project ID: 31102775 8Results by SW-846 8290A Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Result ND Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): EMPC g1.4 DL LOQ/CL Units RT Ratio U 0.107 0.495 pglg 0.140 J 0.0435 0.495 pg/g 26.36 0.98* Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 57 of 149 Results of Comp#9 Site 3 Bluegill sm Client Sample ID: Comp#9 Site 3 Bluegill sm Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775009 Lab Project ID: 31102775 }-Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD ,Batch Information Result 92.0 96.0 98.0 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): EMPC Qual DL LOQ/CL Units RT 40.0-135 40.0-135 40.0-135 OA Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/30/2011 02:01 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.NoI.: 10.11 g Prep Extract Vol: 20 uL Print Date: 11 /01 /2011 SGS North America Inc. N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sos.com Member of SGS Group Page 58 of 149 Results of Comp#9 Site 3 Bluegill sm Client Sample ID: Comp#9 Site 3 Bluegill sm Client Project ID: Annual Fish Project 2011 Lab Sample ID: 1102775009-A Lab Project ID: 3 102775 >-Results by Gravametric Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result EMPC Qual DL LOQ/CL Units % Lipids 0.520 °Ao riBatch Information 1 RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/me: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.NoI.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SCS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sc s.com N.C. Certification # 481 Member of SGS Group Page 59 of 149 Quantify Sample Summary Report ###TCDD TCDF Only ### MassLynx 4.1 SCN640 Dataset: C:IMassLynx\Default.prooResults1b29oct1 l a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11a-12/ Date: 30-Oct-2011 Time: 02:01:42 ID: 31102775009 I Submitter: HRD1459 Task: MS Method Name: C:1MassLynx1DEFAULT.PROIACQUDBIdioxins_db5ms_dw2.EXP Description: Comp#9 Site 3 Bluegill sm I 1 2 3 4 5 6 7 :Name :2378-TCDF :2378-TCDD : ES:13C-2378-TCDD . ES:13C-2378-TCDF • JS:13C-1234-TCDD • CS:370-2378-TCDD :F1 Lock Mass : Response. Ion1Area; Ion2Area. RA • RAFaiI?• 7.391e2 3.666e2 3.725e2 0.98 YES NO 6.469e5 2.835e5 3.634e5 0.78 NO 1.0�6 4.608e5 5.748e5 0.80 NO 6.821e5 3.080e5 3.741e5 0.82 NO 1.633e5 1.633e5 - RT:/ pgfpL. 26.36 0.071 27.21 j 92.428 26.34 96.272 26.54/ 100.000 27.24/ 19.659 EDL: Heightl - Noisel. SN1: Height2 ;. Noise2 . SN2 ; M1 : M2. User RF 0.0220 5.135e3 0.0539 0.1154 3.588e6 0.0776 6.049e6 0.1184 4.159e6 0.0238 2.052e6 525 1062 1919 1869.9 4.556e6 2180 2774.9 7.448e6 1919 2167.2 5.056e6 1069 1919.7 51260 - 9.8 5.928e3 674 8.8 bb 1006 2443 1865.0 bb 2331 3195.2 bb 2443 2069.6 bb - bb bb 1.004 1.171 bb 1.026 bb 1.577 bb 1.000 1.218 ( 0-o0T.237 I. 3(,/(5,j_ /-00q/1/ 6t76 to 09 abed ) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:45 Eastern Daylight Time Method: C:1MassLynxIDEFAULT.PROIMethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:1Mass ynx1DEFAULT.PRO1CurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-1 , Date: 30-Oct-2011, Time: 02:01:42, ID: 31102775009, Submitter: HRD1459, Task: 2378-TCDD b29oct11a-12 Voltage SIR,EI+ 23.77 23.92 319.8965 _ -,� 24.00 24.41 24.63 25.19 25.39 25.80 26.29.26.36 26.88 27.03 6.401e+004 °4 2 0 22.52 22.88 23.28 23 59, _- i 27.75 28.1528.38 29.14.29.22 29.51 46 '`-- - - r- , -1 - I . , ; r- -; -�-.•- . . r - r� .�., min �`i I r . . I . T . �-�,-_- I I I . I . ; . I I 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 • 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11a-12 Voltage SIR,EI+ 23.89 23.95.24.02 321.8936 722.04 22.24 23.00 • 24. .5123624.94 25.27 25.55,E. <2 26.22 6.34 26.64 27.24 27.69 28.10 28.36 28.89 7.976e+004 •.,� min39 rrr „I „I I i I 1 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-12 ES:13C-2378-TCDD Voltage SIR,EI+ 26.54 27.21 331.9368 070 /` ,1 4.207e+006 1 I I ; .,�., �, , ,,,• , I,., , ,, ,min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-12 ES:13C-2378-TCDD Voltage SIR,EI+ 26.54 27.21 333.9339 off° A A5.121 a+006 • „ ,,, ,,. ,i,r ,I .T, ,,, ,I, ,,, .I, ,I. .I, �� „ I•�I, .,,T.�.,..i,.,,I, .I, ,I,50,,,, .30.i 00min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29. CS-TCDD b2$oct11a-12 CS:37CI-2378-TCDD Voltage SIR,EI+ il 27.24 327.8847 6, , ,. ,, I •,, ,, �I I' ,, ,. ,. A , ,, ,, �. ,, min °%,2.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 • 28.00 28.50 29.00 29.50 30.00 co F1 Lock Mass b29oct11a-12 Voltage SIR,EI+ 22.04 22,39 304.9824 22.69 23,20 25.11 25.40 26.19 26.85 27.47 28.49 %1 23.33 23.64 23.97 24.33 24.60 24.94 25.98 27.03 27.6127.84 28.13 28,69 29.05 29.33 29.76? 666e+006 39 ----- - _ _T _ _ .._. . , min 22.00 22.50 23.00 _ 23.50 I 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 I 28.00 28.50 29.00 29.50 30.00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:45 Eastern Daylight Time Name: b29oct11a-12, Date: 30-Oct-2011, Time: 02:01:42, ID: 31102775009, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-12 2378-TCDF 26.36 26.88 24.12 25.47 26.52 22.31 23.77 24.27 25.06 25 81 25.90 22.41.22.65,.22.92 23.41 24.33 24.88 / , 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 --A/A.71 26.00 26.50 27.0 Voltage SIR,EI+ 303.9016 3.683e+004 28.96 27.16 27.62 27.95 28.4128,64 29.3829.50 29.88 IVJ-min 0 27.50 2/�8.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11a-12 2378-TCDF Voltage SIR,EI+ 26.36 305.8987 22.39 25.50 26.82 29.53 3.784e+004 23.53 23.77 23.84 24.94 25.04 25.35 25.83 ! 26.7227.15 28.43 28.76 29.14 /a ,J 2.52 22.90 . 24.23 24.30 l�, , ! " f \ . ,l il\ 27.41 27.74 28.36 !1N . A J�1 �.,.. _.,A 29.70 ,,, , " r� .,. .,. .1 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11a-12 ES:13C-2378-TCDF Voltage SIR,EI+ 26.34 315.9419 P 6.119e+006 %- ) 1 .T... ,. i : ,....i....,... , , 1 ,.. 1 ..; ..............................................min.,.1 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11 a-12 (22 00 22.50 0) FiLock Mass b*octll a-12 _ ,22.04 122.39 % - '*ts. 22.69 39 . 1 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 ES:13C-2378-TCDF 26.34 Voltage SIR,E1+ 317.9389 7.536e+006 i....,....I ..... .................... ...,.. ,},...,....i min 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 304.9824 2.666e+006 23.20 25.11 25.40 26.19 26.85 27.47 28.49 29.56 23.33 23.64 23.97 24.33 24.60 24.94 25.98 • 27.03 27.6127.84 28.13 28.69 29.05 29.76 •,., r.,,,1 min 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Results of Comp#10 Site 3 Bluegill Ig Client Sample ID Comp#10 Site 3 Bluegill ig Client Project ID: Annual Fish Project 2011 Lab Sample ID: 1102775010 Lab Project ID: 31102775 Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Result ND EMPC Qual DL LOQ/CL Units RT Ratio U 0.208 0.465 pg/g 0.149 J 0.0524 0.465 pg/g 26.37 0.54* Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 63 of 149 SG$ ii,Results of Comp#10 Site 3 Bluegill Ig Client Sample ID: Comp#10 Site 3 Bluegill Ig Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775010 Lab Project ID: 31102775 }-{Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD -1Batch Information 11 Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result 98.0 100 104 EMPC Qual DL LOQ/CL Units RT 40.0-135 % 40.0-135 % 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/30/2011 02:38 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.NoI.: 10.76 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc. N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com Member of SGS Group Page 64 of 149 ri,Results of Comp#10 Site 3 Bluegill Ig Client Sample lD1 Comp#10 Site 3 Bluegill Ig Client Project ID:l Annual Fish Project 2011 Lab Sample ID: 31102775010-A Lab Project ID: 31102775 ?--LResults by Gravametric Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result EMPC Qual DL LOQ/CL Units % Lipids 0.490 %a Batch Information RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sas.com N.C. Certification # 481 Member of SGS Group Page 65 of 149 Quantify Sample Summary Report ###TCDD TCDF Only ### MassLynx 4.1 SCN640 Dataset: C:lMassLynx\Default.prolResultslb29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11 a-13/ Date: 30-Oct-2011/ Time: 02:38:27 ID: 31102775010 Submitter: HRD1459 Task: MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins db5ms_dw2.EXP Description: Comp#10 Site 3 Bluegill Ig 1 2 3 4 5 6 7 :Name : Response: Ion1Area: Ion2Area- RA RAFaiI?: RT, pg/pL- EDL: Height1- Noised: SN1. Height2:. Noise2 SN2 : M1 : M2: User RF 2378-TCDF 8.986 3.145e2 5.841e2 0.54 YES 26.37' 0.080 0.0282 4.235e3 760 5.6 6.894e3 854 8.1 bb bb 1.004 :2378-TCDD NO - 0.1118 3007 - - 1802 1.171 : ES:13C-2378-TCDD 7.176e5 3.180e5 3.996e5 0.80 NO 27.2V98.452 0.0891 4.069e6 1715 2372.4 5.150e6 1701 3028.6 bb bb 1.026 : ES:13C-2378-TCDF 1.124e6 4.960e5 6.276e5 0.79 NO 26.32� 00.298 0.0707 6.286e6 2190 2870.2 8.063e6 1975 4081.9 bb bb 1.577 .JS:13C-1234-TCOD 7.104e5 3.143e5 3.962e5 0.79 NO 26.52 //100.000 0.0914 4.133e6 1715 2410.2 5.158e6 1701 3033.0 bb bb 1.000 • CS:37C1-2378-TCDD 1.797e5 1.797e5 - 27.25/ 20.772 0.0210 2.287e6 957 2390.4 - - bb 1.218 :F1 Lack Mass - 49131 - - ti--c„b6 617L 10 99 e6ed /O•7-65.. I• oog1 , 0. I 14 geil5 -rw,/, 1 Quantify Sample Report MassLynx 4.1 SCN-640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:45 Eastern Daylight Time Method: C:IMassLynx1DEFAULT.PRO1MethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:1MassLynx1DEFAULT.PRO1CurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-13, Date: 30-Oct-2011, Time: 02:38:27, ID: 31102775010, Submitter: HRD1459, Task: 2378-TCDD b29oct11a-13 Voltage SIR,EI+ 22.11 23.67 23.81.23.89 319.8965 a�o1 T c , 22.34 22.7422.97 23.21 . -/ . s' -- 4 �0 24.60 24.73 25.24 25.39 25.88 26.01 26.31 26.69 27.08 '21`27.43 28.15 28.74 28.99 29.38 29.56 5.683e+004 53 .,--,, : ,--- -- -r,, ;-.. - . i .. , 1-:--1; .. ; ..., .. i .. ,-.-.-r,-,�-- ., - 1 . T.ri:_, . , , .. , 7 1 ...., , , u.. , , ...... - .`, min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29octi 1a-13 22.08 22.39 22.92 42- .; :-. 22.00 22.50 23.00 ES-TCDD b29oct11 a-13 23.8123.92 23.74 24.18 _ - 24.66 23.50 24.00 24.50 25.20 25.60 25.00 25.50 26.32 26.83 _ 27.23 26.00 26.50 27.00 27.50 ES:13C-2378-TCDD 26.52 27.21 27.85 28.02 28.58 28.87 29.09 28.00 28.50 29.00 29.50 Voltage SIR,EI+ 321.8936 7.102e+004 min 30.00 Voltage SIR,EI+ 331.9368 4.196e+006 , ... , . I min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-13 %01 26.52 ES:13C-2378 TCDD 27.21 Voltage SIR,EI+ 333.9339 5.207e+006 ,,,. .;... , , ;,.t.�r .,�,,,. 1.. .,,1 .,,T .,.; ,... min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b22oct11a-13 CS:37CI-2378-TCDD Voltage SIR,EI+ 27.24 327.8847 2.337e+006 ,, ;,., ,. , , ,,..,� , �,.., ,n, , , ,.,, , f,?., , , , , , .. , 1min %2.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 A CO F1Lock Mass b29oct11a-13 Voltage SIR,EI+ ..22.08 22.87 23.18 24.97 25.25 26.92 28.10 28.69 29.40 29.65 304.9824 22.74 23.69 24.0424.27 24.60 25.11 25.42 26.08 , 27.13 27.4627.69 28.28 .28.8229.05 2.540e+006 o _ 28 1 , T . , . , , . , , . - .. , - --i - , .-_-------- -, ---•- -- - .-. _.:.. _ - -- � , �, . , , , , ; , .. -- --._,_ ' ._.._l , _..._.. _. • - min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11a-13 2378-TCDF Voltage SIR,EI+ 26.36 305.8987 1 3.932e+004 23.61 26.69 29.02 22.31 23,g1 2q,86 25.04 25.47 25.53 26.24 27 38 27.51 27.99 28.43 28.51 i 29.86 v` ji_ 22.74 22.80 23.23 , 24.2 24.30 25.86 27.00 /� 28.10 j 29.29 29.fi1 ES-TCDF b29oct11a-13 0 .. 22 00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only MN Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:45 Eastern Daylight Time Name: b29oct11a-13, Date: 30-Oct-2011, Time: 02:38:27, ID: 31102775010, Submitter: HRD1459, Task: 2378-TCDF b29oct11a-13 Voltage SIR.EI+ 23.34 303.9016 24.18 2378-TCDF 27.61 4.159e+004 .23237,1 ;:1 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 f , , i ' , , , , i T ,• min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES:13C-2378-TCDF 26.32 Voltage SIR,EI+ 315.9419 6.351e+006 r , . � � . . � I i . I .•, r , i r . ,•. , r• , r r . i . . , , , . . i .r , r r . , . r , , min 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDF b29oct11 a-13 ES:13C-2378-TCDF 26.32 Voltage SIR.EI+ 317.9389 8.132e+006 r ..... ..... ... , ...., , , ,,.rr,., c�2 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 rn co Ff-Lock Mass b2 ct11a-13 .22.08 % 28 Voltage SIR,EI+ 304.9824 2.540e+006 22.74 22.87 23.18 23.69 24.0424.27 24.60 24.97 25.11 25.2525.42 26.08 26.92 27.13 27.4627.69 28.10 28.28 28.69 28.8229.05 29.40 29.65 29.96 Tr T. r f. ,.. 22 00 22.50 23.00 23.50 24.00 24.50 ,.., , .,,,.., ,., ,..r,,r r.,, f....i min 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Results of Comp#11 Site 3 FlatheadCatfish MR. Client Sample ID: Comp#11 Site 3 FlatheadCatfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775011 Lab Project ID: 31102775 }-I Results by SW-846 8290A Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Collection Date: 10/06/2011 00'.00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC ND 0.147 Qual DL LOQ/CL Units RT Ratio U 0.156 0.490 pg/g J 0.0588 0.490 pg/g 26.35 0.70 Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 69 of 149 Results of Comp#11 Site 3 FlatheadCatfish Client Sample ID: Comp#11 Site 3 FlatheadCatfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775011 Lab Project ID: 31102775 >d Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD Batch Information Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC 97.0 100 103 Qual DL LOQ/CL Units RT 40.0-135 40.0-135 40.0-135 Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/30/2011 03:15 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.Nol.: 10.21 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 70 of 149 e-LResults of Comp#11 Site 3 FlatheadCatfish Client Sample ID: Comp#11 Site 3 FlatheadCatfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775011-A Lab Project ID: 31102775 Results by Gravametric Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter % Lipids Batch Information Result EMPC 0.320 ual DL LOQ/CL Units RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.NoI.: 1 mL Prep Extract Vol: 1 mL Print Date: 11/01/2011 SGS North America Inc 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 71 of 149 Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:IMassLynxlDefault.prolResults1b29oct1 l a-1 tetras.gld Last Altered: 01-November-11 8:13:12 AM Eastern Daylight Time Printed: 01-November-11 8:43:40 AM Eastern Daylight Time Method: Untitled 31 Oct 2011 09:53:18 Calibration: C:IMassLynnxxDEFAULT.PROtCurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-14 Date: 30-Oct-2011 Time: 03:15:08 / ID: 31102775011 Submitter: HRD1459 Task: Description: Comp#11 Site 3 FlatheadCatfish 1 2 3 4 5 6 :Name 2378-TCDF� 2378-TCDD ES:13C-2378-TCDD ES:13C-2378-TCDF . JS:13C-1234-TCDD • CS:37CI-2378-TCDO 7 . F1 Lock Mass Response. Ion1Area; Ion2Area. RA • RAFaii?; 8.739e2 3.611e2 5.128e2 0.70 NO NO 7.271e5 3.199e5 4.072e5 0.79 NO 115.115e5 6.435e5 0.80 NO 7.340e5 3.260e5 4.080e5 0.80 NO 1.843e5 1.843e5 - RT pg/NL. 26.35 / 0.075 27.23/j 96.555 26.34� 99.786 26.54/ 00.000 27.24 / 20.614 EDL; Heightl. Noisel; 0.0300 6.709e3 1200 0.0798 0.0906 4.076e6 0.0598 6.670e6 0.0930 4.356e6 0.0224 2.407e6 SN1: Height2:. Noise2 : SN2 ; M1 : M2- User RF 5.6 6.656e3 618 10.8 MM MM 1.004 1877 - 1586 - 1.171 2159 1887.6 5.173e6 1487 3478.7 bb bb 1.026 1707 3908.3 8.392e6 1995 4206.3 bb bb 1.577 2159 2017.3 5.420e6 1487 3644.9 bb bb 1.000 1068 2253.6 - - bb 1.218 43913 •- EFC ij Pi - • /. SSec 6176 J0 ZL 96ed aC7UUpC J ro.ata -ion i -1- If )))))))))))))))))))))))))))))))))i))))) ))) ) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:46 Eastern Daylight Time Method: C:IMassLynxIDEFAULT.PRO1MethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:lMass ynx1DEFAULT.PRO1CurveDBlmtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-14, Date: 30-Oct-2011, Time: 03:15:08, ID: 31102775011, Submitter: HRD1459, Task: 2378-TCDD b29oct11 a-14 % 52 22 00 22.36 23.79 24.02 23.90 25.29 23.25 24.17 23.05•57 ;� r r •����24.40 25.45 25.75 2378-TCDD b29oct11a-14 %l 22.18 43 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 ES-TCDD b29oct11a-14 01 ., .. , ., 1 .. IT. ,. 1 „ , .. 1 , 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 ES-TCDD b29oct1 l a-14 22.50 23.00 23.50 24.00 24.50 25.00 25.50 Voltage SIR.EI+ 319.8965 26.2126.32 26.49 28.30 28.69 29.27 5.860e+004 26.95 27.26 27.54 28.10 28.51 29.45 min 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 23.64 23.8423.95 22.69 23.25 \ < 224.10 24.53 24.91 25.24\ 25.43 25.88 26.36 26.49 27.24 27.54 28.13 28.56 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 in ES:13C-2378-TCOD 26.54 27.23 Voltage SIR,E1+ 321.8936 7.097e+004 Voltage SIR,E1+ 331.9368 4.407e+006 I" , �,,. , , ,• ,,.. min 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 %1 I� / \ 5.468e+006 1Amin 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b2%octl 1a-14 ca w - ES:13C-2378-TCDD Voltage SIR,E1+ 26.54 27.23 333.9339 CS:37CI-2378-TCDD 27.24 22.00 22.50 23.00 23.50 m F1 Lock Mass b29oct11 a-14 24.00 24.50 25.00 25.50 26.00 26.50 11 �., , .,, i min 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,E1+ 327.8847 2.448e+006 Voltage SIR,E1+ 22.04 22.42 304.9824 o �`23.74 25.91 26.17 26.90 27.80 - 28.56 28.84 2.596e+006 /, 22.85 23.30 23,54 24.15 24.46 24.78 25.1225.35 25.76 . 26.70 27.05 27.59. 28.02 28.72 29.23 29.56 37- , ,.,'� ,... r,.,.,, ,,..., -�� `.T,.. ,.'� min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:46 Eastern Daylight Time Name: b29octlla-14, Date: 30-Oct-2011, Time: 03:15:08, ID: 31102775011, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-14 2378-TCDF 22.26.22.34 ..2.26.36 26.60 26.93 .34 22.95 2315 2438 5.47 2555 23.53 23.92 24.22 25.02.25.10 27.57 28.02 28.36 22 00 22.50 2378-TCDF b29oct11 a-14 23.00 23.50 24.00 24.50 Voltage SIR,EI+ 29.60 303.9016 A 5.228e+004 28.87 29.45� �9.73 29.79 25.00 , ... .. , , , , , . ; ; i - ^--�. , . , `, ... ,.. ,�, . ;, min 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 22.04 22.51 Atc..2 22.72 23.62 24.8724.99 .80 23.21 23.92 24.41.24.66, 2378-TCOF 26.36 25.45 26.29 ;` . f 26.5926.70 27.44 27.52 2 j 25.6625.89 27.70 r r tw„ • A`�� 22.00 22.50 23.00 23.50 24.00 24.50 25.00 ES-TCDF b29oct11 a-14 °Jo 0. 25.50 26.00 26.50 ES:13C-2378-TCDF 26.34 27.00 27.50 22.00 22.50 23.00 ES-TCDF b29oct11a-14 23.50 .,,, .�.. ; ..,,. ,I .,, (12 00 22.50 23.00 23.50 v F1 Lock Mass b2toct1la-14 m 22.04 Ok 24.00 24.50 ir 24.00 24.50 25.00 ,i,, i,,,.,, „f, 25.00 25.50 26.00 26.50 27.00 27.50 ES:13C-2378-TCDF 26.34 I !' 1 25.50 26.00 26.50 Voltage SIR,EI+ 29.61 305.8987 A 3.866e+004 7.95 29.53 29.88 f) 28.20 28.44 28.72 29.35. A,.,.•1min 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 315.9419 6.740e+006 .1...,, T,,,.I,..,I,,,,,...,I,..,i m1n 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 317.9389 8.481e+006 .,,.. �.r,,,. ,,, ........... ....... ...... ,.,,.I min 27.00 27.50 28.00 28.50 29.00 29.50 30.00 22.42 54 23 22.85 23.30 2325.91 26.17 26.90 27.80 ..7424.46 24.15 24.78 25.1225.35 25.76 _ -26.70. 27.05 27.59 - 37 :/, , ... , 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 Voltage SIR,EI+ 304.9824 2.596e+006 28.02 28.56 28.7228.84 29.23 29.8829.94 26.50 27.00 27.50 28.00 1 I , r, It, l min 28.50 29.00 29.50 30.00 3))))))) ))) ))))))))T)))))))))))))))))) ) ))))))))) ))))))))))))) 1))))))))))))))))) ) b29oct1 t a-14 Smooth(S0,1x2) 83 b29act11a•14 Smooth(S0,1x2) 25.27 96 5.75 25 86 25 93 26.04 25.45 2378•TCDF;26.36;361.14;0.08 pg/p1.45.59 25.3: 25.55 25.60 25.66 25.76 25.81 25.89 25.96 26.09 26.21 b29oct11 a•14 Smooth(SO,1 x2) b29oct11 a-14 Smooth(S0,1 x2) 96- 25.20 25.30 25.40 25.50 25.60 25.70 25.60 25 90 26.00 26.10 26.20 26.30 26.40 26.50 26.60 26.70 26.80 26.90 27.00 2378-TCDF;26.36;512.81;10.77 26.29 26.52 26.49 ES:13C•2378-TCDF;26.34,511482.13;99.79 pg/1L;3908.31 E S:13 C-2378-TCDF;26.34;643524.69;4206.32 26.60 26.59 26.70 26.70 28.82 Voltage SIR,EI• 303.9016 3.775e+004 26.93 27.00 26.80 28.91 min Voltage SIR,EI+ 305.8987 3 787e•004 min Voltage SIRE!. 315.9419 6 740e'005 min Voltage SIR.EI+ 317.9389 8 481 a+006 6ti6 !a SL a6ad id Results of Comp#12 Site 3 Blue Catfish Client Sample ID: Comp#12 Site 3 Blue Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775012 Lab Project ID: 31102775 Results by SW-846 8290A Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF 1 Result EMPC ND ND Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): ual DL LOQ!CL Units RT U 0.256 0.478 pglg U 0.0825 0.478 pg/g Ratio Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 76 of 149 f-LResults of Comp#12 Site 3 Blue Catfish Client Sample ID: Comp#12 Site 3 Blue Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 1102775012 Lab Project ID: 3 102775 >-1Results by SW-846 8290A Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD Batch Information Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC 83.0 84.0 86.0 Qual DL LOQ/CL Units RT 40.0-135 40.0-135 40.0-135 Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/3012011 03:51 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.Nol.: 10.47 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 77 of 149 Results of Comp#12 Site 3 Blue Catfish Client Sample ID: Comp#12 Site 3 Blue Catfish Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775012-A Lab Project ID: 31102775 >id Results by Gravametric Parameter Result % Lipids 1.18 Batch Information Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): EMPC Qual DL LOQ/CL Units RT 0/0 Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL J Print Date: 11/01/2011 SGS North America Inc 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 78 of 149 ))))) :))) )))))) ))))))))) ))) )))) )))))))) )) ) ) Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:1MassLynxlDefault.pro1Resultslb29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11 a-15 Date: 30-Oct-2011 Time:03:51:49 ID: 31102775012/ Submitter: HRD1459 Task: MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins_db5ms_ Description: Comp#12 Site 3 Blue Catfish dw2.EXP 1 2 3 4 5 6 7 :Name :2378-TCDF : 2378-TCDD ES:13C-2378-TCDD : ES:13C-2378-TCDF • JS:13C-1234-TCDD • CS:370-2378-TCDD :F1 Lock Mass Response: lonlArea: Ion2Area: RA •:RAFaiI?• NO • NO 3.856e5 1.700e5 2.156e5 0.79 NO 6.035e5 2.655e5 3.380e5 0.79 NO 4.551e5 2.003e5 2.548e5 0.79 NO 9.574e4 9.574e4 - - RT pglpL- 27.21'/ 82.568 26.32+ 84.085 26.52 /100.000 27.24J 17.272 EDL: 0.0432 0.1342 0.1086 0.1003 0.1114 0.0395 Heightl: Noisel: 668 - 1308 - 2.168e6 1389 1561.0 2.769e6 3.305e6 1571 2103.2 4.235e6 2.597e6 1389 1869.2 3.309e6 1.166e6 1136 1026.3 48794 SN1: Heightl :. Noise2 : 636 1784 1241 2162 1241 SN2 • M1 •, M2- User RF 1.004 1.171 2231.3 bb bb 1.026 1959.0 bb bb 1.577 2667.0 bb bb 1.000 - bb 1.218 6b1. Jo 6L abed Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:46 Eastern Daylight Time Method: C:IMassLynxIDEFAULT.PRO1MethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:lMassLynxIDEFAULT.PRO1CurveDBlmtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-15, Date: 30-Oct-2011, Time: 03:51:49, ID: 31102775012, Submitter: HRD1459, Task: 2378-TCDD b29oct11a-15 Voltage SIR,EI+ 23.81 23.9424.00 319.8965 Vol 22.29 ' �� 24.17 24.92 25.24 25.3225.4325.78 25.85 26.3626.47 27.00 27.24 5.653e+004 22.16 22.82 23.08 23.61 . - 27.72 28.22 28.7628.99 29.43 �_ 54 . .,,�;,-,��f�-,�..i---„,, _ _ min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11a-15 23.89 Voltage SIR,EI+ 23.64 24.00 321.8936 ° w - 24.13 25.3825.62 26.21 28.94 7.602e+004 40 22.3222.55 23.11 ,... .24.32,24.56 25.25 26.09 26.67 26.95 27.26 27.69 27.94 28.23:.28.3328.74 29.30 22 00 22 �50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 in ES-TCDD b29oct11a-15 % ES:13C-2378-TCDD 26.52 27.21 \ n Voltage SIR,EI+ 331.9368 2.643e+006 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 in ES-TCDD b29oct11 a-15 0421 i 4 ES:13C-2378-TCDD 26.52 27.21 ` Voltage SIR,EI+ 333.9339 3.353e+006 .,..,h,.,,.j.. .,..,,1„ 1 ,.,,,I..,.,,,,.T,..., ,,,,,,,.,,,I ,.,,,,, .,.. 1„ , ,..,.l 1 1 ,,,,.,,',.,.,, l,,.,1. ,.,..,. ,.,.� min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b29oct11a-15 CS:37CI-2378-TCDD 27.24 Voltage SIR,EI+ 327.8847 1.201e+006 , ,,.,.,.• ,,,,,,,,,,,,,,,,,,,,, , ,,,,,,....,.,,,,..,, ,, ,,.r. r,..,,, ;...., ,.,.,,...., .,, min (22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 F'f Lock Mass b29oct11 a-15 Voltage SIR,EI+ 22.08 22.37 22.60 23.43 23.69 25.47 27.05 27.51 28.10 29.24 304.9824 /°1 __, .22.80 23.25 24.12 24.50 24.78 25.25. 25.66 25.98 26.26 26.7026.93. 27.64 27.74 .28.31 28.81 29.38 2.742e+006 ;r r,r T:;-,; -',: '�., ,min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00� 29.50 30.00 �� )))))�)�))�))�))�)� )))) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:46 Eastern Daylight Time Name: b29oct11a-15, Date: 30-Oct-2011, Time: 03:51:49, ID: 31102775012, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-15 22.21 .22.31 ..22.57 23.23 23.62 23.76 24.46 25.17 ,'! 24,00 24.6324.69 25.53 25.81,25.88 ►7 . 22 00 " 22.50 Voltage SIR,EI+ 26.36 7 29.75 303.9016 �.881e+004 26.57 26.65 27.18 27.62 28.00 2- -28.51 29.09 29.3729.60`! �+\ _ /���^•^V-. .___A____ �•1_ i� %�r".ti .._ �" ,., .�f•/'\ �/1�_ i'�-�/ ,....,.. �.•.., , ,,., ,.., ,.. , v\-.. , i ., ,,..v,•., Amin 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11a-15 22.32 /0 22.13 ti 22.74 23.72 24.23 24.38 24.79 �4 22.80 23.26 23.85 82 , ..,.r.i. ,..r.� ...,. ..... 22 00 22.50 23.00 23.50 24.00 24.50 25.00 ES-TCDF b29oct11 a-15 1• r. 22 00 22.50 23.00 25.12 I 1 25.01 1 25.63 26.31 26.93 27.11 27.41 28.03 28.45 25.725 96 26.52 27.97 25.50 26.00 26.50 27.00 27.50 28.00r 28.50 ES:13C-2378-TCDF 26.32 Voltage SIR,EI+ 305.8987 3.692e+004 28.82 29.00 29.60 29.40 min 29.00 29.50 T 30.00 Voltage SIR,EI+ 315.9419 4.151e+006 ES-TCDF b29oct11 a-15 23.50 24.00 24.50 25.00 25.50 25.01 i 26.00 26.50 ES:13C-2378-TCDF 26.32 27.00 27.50 28.00 28.50 ,i , ,, min 29.00 29.50 30.00 Voltage SIR,E1+ 317.9389 5.098e+006 00 22.50 m 00 F1 �.ock Mass b29Rct11 a-15 co �22.08 22.37 `4 22.60 22.80 23.25 43 .. 23.00 23.50 24.00 23.43 23.69 24.12 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 24.50 24.78 25.25. 25.47 25.66 25.98 26.26 26.7026.9327'0527.51 27.64 27.74 28.10 28.31 T 1min 29.00 29.50 30.00 Voltage SIR,EI+ 304.9824 2.742e+006 28.81 29.24 29.38 29.81 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 i........., min 29.00 29.50 30.00 Results of Comp#13 Site 1 Blue Catfish Ig Client Sample ID: Comp#13 Site 1 Blue Catfish Ig Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775013 Lab Project ID: 31102775 }-IResults by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Result EMPC Qual DL. L OQ/CL. Units RT Ratio 2,3,7,8-TCDD ND U 0.205 0.491 pg/g 2,3,7,8-TCDF 0.234 J 0.119 0.491 pg/g 26.34 0.68 J Print Date: 11/01/2011 N.C. Certification # 481 SGS North America Inc 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sQs.com Member of SGS Group Page 82 of 149 Results of Comp#13 Site 1 Blue Catfish Ig Client Sample ID: Comp#13 Site 1 Blue Catfish Ig Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775013 Lab Project ID: 3 102775 Results by SW-846 8290A Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Parameter Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD HBatch Information Result EMPC 95.0 99.0 101 Qua! DL LOQ/CL Units RT 40.0-135 % 40.0-135 % 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/30/2011 04:28 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.Nol.: 10.18 g Prep Extract Vol: 20 uL Print Date: 11 /01 /2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 83 of 149 e-LResults of Comp#13 Site 1 Blue Catfish Ig Client Sample ID: Comp#13 Site 1 Blue Catfish Ig Client Project ID: Annual Fish Project 2011 Lab Sample ID: 31102775013-A Lab Project ID: 31102775 > {Results by Gravametric Parameter % Lipids te—lBatch Information Collection Date: 10/06/2011 00:00 Received Date: 10/06/2011 13:15 Matrix: Tissue Solids (%): Result EMPC 1.38 Qual DL LOQ/CL Units aka RT Ratio Analytical Batch: HXX1347 Analytical Method: Gravametric Instrument: BAL10 Analyst: RSS Analytical Date/Time: 10/24/2011 17:00 Dilution: 1 Prep Batch: HXX1347 Prep Method: Gravametric Prep Date/Time: 10/24/2011 17:00 Prep Initial Wt.Nol.: 1 mL Prep Extract Vol: 1 mL ♦ Print Date: 11/01/2011 SGS North America Inc. N.C. Certification # 481 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sos.com Member of SGS Group Page 84 of 149 ))))))))))))))))))))))))))))))))))))))))))) Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:1MassLynx\Default.prolResultslb29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11a-16 Date: 30-Oct-201 y Time: 04:28:36 ID: 31102775013 Submitter: HRD1459 Task: MS Method Name: C:IMassLynxIDEFAULT.PROIACQUDBIdioxins_db5ms_dw2.EXP Description: Comp#13 Site 1 Blue Catfish Ig 1 2 3 4 5 6 7 :Name 237� -TCDF : 2378-TCDD ES:13C-2378-TCDD ES:13C-2378-TCDF • JS:13C-1234-TCDD • CS:37CI-2378-TCDD :F1 Lock Mass Response. Ion1Area: ton2Area. RA • RAFaiI?: 7.5 65e2 3.065e2 4.500e2 0.68 NO NO 3.925e5 1.740e5 2.185e5 0.80 NO 6.321e5 2.804e5 3.517e5 0.80 NO 4.049e5 1.779e5 2.270e5 0.78 NO 9.946e4 9.946e4 - - RT:/ pg/pL: EDL: Heightl : Noisel; SN1- Height2 :. Noise2 . SN2 : M1 . M2. User RF 26.34 0.119 0.0605 5.664e3 1260 4.5 6.584e3 677 9.7 bb bb 1.004 0.1044 823 - - 1587 1.171 27.21/ 94.501 0.1449 2.185e6 1473 1482.8 2.773e6 1642 1689.1 bb bb 1.026 26.32/ 99.012 0.1086 3.534e6 1842 1918.7 4.443e6 1747 2543.8 bb bb 1.577 26.52/100.000 0.1486 2.302e6 1473 1562.3 2.913e6 1642 1774.1 bb bb 1.000 27.23/ 20.170 0.0337 1.225e6 861 1423.2 - bb 1.218 - 46910 - - ITCbq -r- 1..565e 2. �.3aItes 61'610 59 96ed o qc5A. 060,0 Quantify Sample Report MassLynx 4.1 SCN640 DD TCDF Only ### 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 ES-TCDD b29oct11 a-16 Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:46 Eastern Daylight Time Method: C:lMassLynxIDEFAULT,PRO1MethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:1MassynxlDEFAULT.PRO1CurveDBlmtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29octlla-16, Date: 30-Oct-2011, Time: 04:28:36, ID: 31102775013, Submitter: HRD1459, Task: 2378-TCDD b29oct11 a-16 Voltage SIR,EI+ 22.60 23.15 ,' 319.8965 701 22.21 22.31 . 23.46 r- 24.35 24.63 24.84 26.54 27.06 4.815e 004 - l _,_-_• _ 25�19 25�48 25.91 26.32 27.21 4�27.33 28.05,28.15 28.50 28.86 29.25 29.80 + 22 00 .. 22�50 , •, `�- n • -(� • , .: ; . , , r, .-- i-----_-..-. , i i . , i r, �-r r� j-7�.7-: r ce'. ; i , ?-r ,-r---ri"'"r �-i min 23.00 23.50 24.00 i 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11 a-16 23.71 23.81 23.95 23 82 23 92 Voltage SIR,EI+ 321.8936 90- -22.19 y2,49 22.74 2.88 r 23.56 . ,_..� 24.17 24.69 25:17 25.45,25.55 25.94 26.32 26.72226.80 27.23 27.77 28.02 28.31 28.79 29.24 29.56 6.094e+004 i ,--,Li i T" - - -- -- *�-� min 30.00 28.50 29.00 29.50 ES:13C-2378-TCDD Voltage SIR,EI+ 26.52 27.21 n 331.9368 1 ; 22 00 22.50 " 23.00T23.50 24.00 24.50 „ 25j00 25�50 l min 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-16 ES:13C-2378-TCDD Voltage SIR,EI+ 10 , . „ 26 52 27.21 333.9339 2.952e+006 22.00 22.50 i 23.00 23.50 24.00 i 24�50 i 25.00 i i j J 25.50 f 26.00 26i50 27.00 i j 27.50 T 28.00 28.50 i , i 29.00 i r J 29.50 30.00 in CS-TCDD b29oct11 a-16 0 CS:37CI-2378-TCDD 27.23 I i „ 1 „ i i,, . i ,, i .00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 Voltage SIR,EI+ 327.8847 1.263e+006 27.50�n j 28.00 28.50 , i 29.00 29.50 30.00 F1 tock Mass b29oct11a-16 22.04 22.37 •Voltage SIR,EI+ 304.9824 22.64 22.88 23.99 24.79 26.01 26.67 26.97 27.67 28.51 2.690e+006 44 j - - 23.39 23.77 24.4524.79 25.63 25.88 26.82 2T.31 27.87 28.40 29.01 29.78 22.00 22 .50 * J 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 in )))))))))))))))i))))))))))))))) )))))) ))))) ) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only NM Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:46 Eastern Daylight Time Name: b29oct11a-16, Date: 30-Oct-2011, Time: 04:28:36, ID: 31102775013, Submitter: HRD1459, Task: 2378-TCDF b29oct11 a-16 22.32 Voltage SIKH+ 303.9016 0/ 24.68 2378-TCDF 4.738e+004 22.26 22.72 24.2024.524.68 .20 26.34 22.8323.07 23.56 23.87 24.09, 26.70 27.18 -.r�� 24 5 25.01 .47 2611,27297272840 L_-_.-5'\.r, . _ 2874 29.04293329562980 i".,.I.,,.I....I...,I.. .1 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF b29oct11 a-16 I 22 29 Voltage SIR,EI+ `� 2378-TCOF 305.8987 4.483s+004 %o 0 l 22.70 22.83 23.23 23.49 23.58 23.89 24.45 24.71 226.37 -IV/ 5.07 L_o& 3 2547 28'83 25,91 _,'S �- y I .. I `. "'�'1� /I I � -i _'� 1 I 1/`'�r�/ i `• ,. �'I 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00min 29.50 30.00 ES-TCDF b29oct11a-16 22 00 22.50 ES-TCDF b29oct11a-16 %- y I I . I .. I" I I i I I 'I I .. 'I I r l 1 min 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 w F1Lock Mass b2tct11a-16 'O �22.04 ‘-'\` 22.37 44 .. I?,., 22 00 22.50 ES:13C-2378-TCDF 26.32 Voltage SIR,EI+ 315.9419 3.585e+006 23.00 23.50 I 24.00 i 24.50 25.00 I 25.50 26.00 26.50 i 27.00 27.50 28.00 28.50 29.00 I 29.50 r 30.00 in ES:13C-2378-TCDF 26.32 Voltage SIR,EI+ 317.9389 4.503e+006 Voltage SIR,EI+ 304.9824 2.690e+006 22.64 22.88 26.01 26.67 26.97 27.67 28.51 23.39 23.77 23.99 24.4524.79 24.9225.16 25.63 25.88 26.82 27.31 , • 27.87 28.40 29.01 29.78 29.86 ; ;. T . �- _-- 29.7 . -. _ ..� min 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 ~~~ 28.50 29.00 ` 29.50 30.00 SG$ ri!,:tatch Summary Analytical Method: SW-846 8290A Prep Method: SW-846 3540C/HRMS Prep Batch: HXX1337 Prep Date: 10/28/2011 17:00 Client Sample ID OPR for HBN 14044 [HXX11337] LMB for HBN 14044 [HXX/1337] Comp#1 Site 1 Bluegill Comp#2 Site 1 Flathead Catfish Comp#3 Site 1 Blue Catfish sm Comp#4 Site 1 Blue Catfish Ig Comp#5 Site 2 Bluegill Comp#6 Site 2 Flathead Catfish Comp#7 Site 2 Blue Catfish Comp#8 Site 2 Common Carp Comp#9 Site 3 Bluegill sm Comp#10 Site 3 Bluegill Ig Comp#11 Site 3 FlatheadCatfish Comp#12 Site 3 Blue Catfish Comp#13 Site 1 Blue Catfish Ig Lab Sample ID Analysis Date 46213 10/29/2011 19:36 46212 10/29/2011 20:32 31102775001 10/29/2011 21:07 31102775002 10/29/2011 21:44 31102775003 10/29/2011 22:21 31102775004 10/29/2011 22:58 31102775005 10/29/2011 23:34 31102775006 10/30/2011 00:11 31102775007 10/30/2011 00:48 31102775008 10/30/2011 01:25 31102775009 10/30/2011 02:01 31102775010 10/30/2011 02:38 31102775011 10/30/2011 03:15 31102775012 10/30/2011 03:51 31102775013 10/30/2011 04:28 Analytical Batch Instrument Analyst HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HR01459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL HRD1459 HRMS2 JHL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 88 of 149 ri, Method Blank Summary Blank ID: LMB for HBN 14044 [HXX11337] Matra: Tissue Blank Lab ID: 46212 QC for Samples: 31102775001, 31102775002, 31102775003, 31102775004, 31102775005, 31102775006, 31102775007, 31102775008, 31102775009, 31102775010, 31102775011, 31102775012, 31102775013 > Results by SW-846 8290A Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Labeled Standards 13C-2378-TCDD Result ND ND 99.0 13C-2378-TCDF 98.0 37CI-2378-TCDD 102 Batch Information EMPC ual DL LOQ/CL Units RT U 0.0902 0.500 pglg U 0.0438 0.500 pg/g 40.0-135 % 40.0-135 % 40.0-135 % Ratio Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Analytical Date/Time: 10/29/2011 20:32 Dilution: 1 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Prep Initial Wt.Nol.: 10 g Prep Extract Vol: 20 uL Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 89 of 149 Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:IMassLynx\Default.prolResultslb29oct11a-1tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11 a-3 Date: 29-Oct-2011/ Time: 20:32:14 �/ iD:46212 Submitter: HRD1459 Task: MS Method Name: C:1MassLynxIDEFAULT.PROIACQUDBIdioxins__db5ms_dw2.EXP Description: LMB for HBN 14044 [HXX11337] -ri 1 1-1-11 1 3 4 5 6 7 :Name : Response. IonlArea: Ion2Area. RA . RAFaiI?: RT: pg/pL. EDL: Heights . Noisel: SN1: Height2 :• Noise2 - SN2 : M1 - M2. User RF :2378-TCDF - NO - 0.0219 504 - 603 1.004 :2378-TCDD - - NO / - 0.0451 961 - - 735 1.171 : ES:13C-2378-TCDD 6.570e5 2.893e5 3.677e5 0.79 NO 27.23� 98.639 0.1001 3.533e6 1597 2211.9 4.566e6 1839 2482.7 bb bb 1.026 .ES:13C-2378-TCDF 1.006e6 4.444e5 5.620e5 0.79 NO 26.36/98.301 0.0664 5.554e6 1706 3255.8 7.074e6 1800 3929.9 bb bb 1.577 .JS:13C-1234-TCDD 6.492e5 2.813e5 3.679e5 0.76 NO 26.54/ 100.000 0.1027 3.625e6 1597 2269.5 4.765e6 1839 2591.0 bb bb 1.000 • CS:37C1-2378-TCOD 1.618e5 1.618e5 - 27.26/ 20.464 0.0192 2.042e6 782 2611.0 - bb 1.218 • F1 Lock Mass - - - 50713 ' - 617110 06 a6ed Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Method: C:1MassLynxIDEFAULT.PROIMethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:IMasfynxIDEFAULT.PROICurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29octlla-3, Date: 29-Oct-2011, Time: 20:32:14, ID: 46212, Submitter: HRD1459, Task: 2378-TCDD b29octl la-3 Voltage SIR,EI+ 23.69 �...,�..2S,36 319.8965 22 08 23.24..7,1 2u 29124 29.434.065e+00422.47 22.54 23.28..', r23.7424.25 25.39 25.90;25.99 26.59 26.83 2739 27.66 28.22 28.69=1, i, IT ,. I, I i �, 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11a-3 Voltage SIR,EI+ 25.19 27.61 321.8936 j 22.14 22.32 22.97 23.4323.54 24.02 24.43 '.2_24_.8_9 �' �25.34 25.7825.90 26.32 26.6 26.75 27.26 t ` 27.67 28.28�28.38 _ 28.8929.12 29.45 4.390e+004 . , I ' I . �' i i , , i'S., i •I- 4 i , i , I i•, i , , . I i . 1 , i� ,' T. i 77 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-3 ES:13C-2378-TCDD Voltage S1R,EI+ 26.54 27.23 331.9368 n 3.673e+006 01� ,, I 1 1 i . i i I I ., I I i ri ,, I ` I i ,•, i I ,min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-3 22.00 22.50 23.00 ES:13C-2378-TCDD 26.54 27.23 /'� Voltage SIR,EI+ 333.9339 4.812e+006 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b299octlla-3 CS:37CI-2378-TCDD Voltage SIR,EI+ CD 27.26 327.8847 IT . , T i I 1 I I I...I 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 A F1` Lock Mass b29oct11 a-3 o K22.04 22.70 22.83 23.08 /0 23.53 23.99 24.38 24.83 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 26.78 27.13 27.61 27.94 28.26 28.76 29.04 304.9824 25.88 25.34 25.67 - . 26.24 26.95 27.77 29.24 29.55 3.109e+006 -- - - t- i , , . ; .. ..._.._�; 1 ....�_.l min Quantify Sample Report ###TCDD TCDF Only ### Dataset: Untitled MassLynx 4.1 SCN640 Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:43 Eastern Daylight Time Name: b29oct11a-3, Date: 29-Oct-2011, Time: 20:32:14, ID: 46212, Submitter: HRD1459, Task: 2378-TCDF b29oct11a-3 22.16 22.31 22.9023.20 23.26 23.39 22.00 22.50 23.00 2378-TCDF b29oct11a-3 OA 23.94 / 24.40 24.84 24^t91 25.22 \! \ J _ t / �r ! 1^ n f 1 23.50 24.00 24.50 25.00 25.47 26.39 I 27.13 . 25.8125.90 27r24 27.56 2807 28.46 pf\e_26.45 25.50 26.00 26.50 27.00 27.50 28.00 28.50 Voltage SIR,EI+ 303.9016 3.481e+004 29.01 29.55 29 65 29.00 29.50 30.00 Voltage SIR,EI+ 22.08 305.8987 24.56 26.37 3.96`! a+004 23 28 23.53 24.91 25.47 26;82 27.52 27.72 28.31 28.40 29.0T 29.48 I' 22 52 22.93 23.76_ 23.84 24.40 • 25.04 25.91 / ` ' ^ -_/ t.Il 'p^ /,,. 26.21/ i l 27.11 n 0 28.46 - 29.63 11 78 , i i.., ,.,. , ,- „ i, , , .., i,,. i ;,.. , ,i min 23.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 22 00 22.50 23.00 ES-TCDF b29oct11 a-3 22.00 22.50 23.00 ES-TCDF b29oct11 a-3 24.00 24.50 25.00 23.50 24.00 i 24.50 25.00 25.50 26.00 26.50 ES:13C-2378-TCDF 26.36 �1 T 25.50 26.00 26.50 ES:13C-2378-TCDF 26.34 i �` i i .. , 27.00 27.50 28.00 Voltage SIR,EI+ 315.9419 5.635e+006 , , •i , i min 28.50 29.00 29.50 30.00 Voltage SIR,E1+ 317.9389 7.143e+006 (12.00 22.50 23.00 23.50 c° N FtJock Mass b2,ct11a-3 4° 22.04 29 24.00 24.50 25.00 22.70 22.83 23.08 23.53 23.99 24.38 24.83 25.50 26.00 26.50 25.34 25.67 25.88 26.24 27.00 T 27.50 i 28.00 , min 28.50 29.00 29.50 30.00 Voltage SIR,EI+ 304.9824 3.109e+006 26.78 26.95 27.13 27.61 27.77 27.94 28.26 28.76 29.04 29.24 29.55 29.80 22.00 22.50 23.00 23.50 24:00 24.50 25.00 , ,..,,;,. , min 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 I ) ) ))))))))��) SG$ ii,Blank Spike Summary Blank Spike ID: CPR for HBN 14044 [HXX/1337] Blank Spike Lab ID: 46213 Date Analyzed: ' 0/29/2011 19:36 Matrix: Tissue QC for Samples: 31102775001, 31102775002, 31102775003, 31102775004, 31102775005, 31102775006, 31102775007, 131102775008, 31102775009, 31102775010, 31102775011, 31102775012, 31102775013 }-1Results by SW-846 8290A Parameter 2,3,7,8-TCDD 2,3,7,8-TCDF Labeled Standards 13C-2378-TCDD 13C-2378-TCDF 37CI-2378-TCDD Batch Information Analytical Batch: HRD1459 Analytical Method: SW-846 8290A Instrument: HRMS2 Analyst: JHL Blank Spike (pg/g) Spike Result Rec (%) 20.0 20.2 101 20.0 21.1 105 88 92 96 CL 40.0-135 40.0-135 40.0-135 Prep Batch: HXX1337 Prep Method: SW-846 3540C/HRMS Prep Date/Time: 10/28/2011 17:00 Spike Init Wt.NoI.: 10 g Extract Vol: 20 uL Pnnt Date: 1170 t72011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 93 of 149 Quantify Sample Summary Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:IMassLynx\Default.pro1Results1b29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:03:37 PM Eastern Daylight Time Name: b29oct11 a-2 Date: 29-Oct-2011/ Time: 19:36:51 ./ ID: 46213✓ Submitter: Task: MS Method Name: C:IMassLynx\DEFAULT.PROIACQUDBIdioxins_db5ms.EXP Description: OPR `7-1/,l 11 __ l' /l :Name :2378-TCDF 2 ; 2378-TCDD 3 : ES:13C-2378-TCDD 4 : ES:13C-2378-TCDF 5 • JS:13C-1234-TCDD 6 - CS:37C1-2378-TCDD 7 :F1 Lock Mass Response: IonlArea: lon2Area:: RA . RAFaiI?; 6.065e4 2.708e4 3.358e4 0.81 NO 4.267e4 1.791e4 2.476e4 0.72 NO 3.603e5 1.589e5 2.014e5 0.79 NO 5.736e5 2.514e5 3.222e5 0.78 NO 3.970e5 1.772e5 2.198e5 0.81 NO 9.324e4 9.324e4 - RT: pg/pL. 26.35, 10.531 27.24/ 10.110 27.22, 88.460 26.33/ 91.617 26.53/ 100.000 27.24/ 19.284 EDL; Height1 • Noisel; SN1- Height2;-Noise2 . SN2 : M1 M2- User RF 0.0408 3.421e5 527 648.7 4.404e5 681 646.8 bb bb 1.004 0.0476 2.347e5 507 462.6 3.182e5 492 647.1 MM MM 1.171 0.1137 1.975e6 830 2378.8 2.495e6 1620 1540.3 bb bb 1.026 0.0979 3.230e6 1416 2280.5 4.141e6 1828 2265.5 bb bb 1.577 0.1166 2.345e6 830 2824.0 2.945e6 1620 1817.6 bb bb 1.000 0.0317 1.193e6 812 1469.2 - bb 1.218 53495 61410 t 6 abed ))))))))))))))))))))))))))))))))))))))))))) Quantify Sample Report ###TCDD TCDF Only #1## Dataset: Untitled MassLynx 4.1 SCN640 Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:42 Eastern Daylight Time Method: C:1MassLynxIDEFAULT.PRO1MethDBldb5ms-tetrascurve.mdb 31 Oct 2011 09:53:18 Calibration: C:1MassLynxIDEFAULT.PROICurveDB%mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-2, Date: 29-Oct-2011, Time: 19:36:51, ID: 46213, Submitter: , Task: 2378-TCDD b29oct11a-2 F1:Voltage SIR,EI+ 27.24 319.8965 /O A +11 22r.70 . 24.97„ .: , „ : , . , . 28.26 „ , , , . 2.6fi . 1 min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDD b29oct11a-2 F1:Voltage SIR,EI+ 27.24 321.8936 3.493e+005 9 ,,..:r.....! min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 26.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11 a-2 °/a-1 ES:13C-2378-TCDD 26.53 27.22 \ f ,. , ., r,.,,T,,,.� .. �.,,,,r. ; „ , , , {,,.,` .,, r .. r....r ,. ,. {,:.., ,. ! min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 ES-TCDD b29oct11a-2 ES:13C-2378-TCDD 26.53 27.22 F1:Voltage SIR,EI+ 331.9368 2.389e+006 F1:Voltage SIR,E1+ 333.9339 2.991e+006 r „ !., r I .I .,,{ {,..,1 ,..,,.r,{.,.,r .,,r,.,,r..............r....r .,.r..,.r. ..r , ,r .r .. r,"'r. ....! min 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 CS-TCDD b299octlla-2 CS:37CI-2378-TCDD F1:Voltage SIR,EI+ i 27.24 327.8847 i r r' r ! min $,2 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 j F'ftock Mass b29oct11a-2 F1:Voltage SIR,EI+ ,,22.04 22.95 24.7124.94 28.42 304.9824 1 \ 22.39 22.75 23.44 23.85.23.94 24.33 25.14 25.63 _ __ 26.06 26.47 26.86 27.1927.6027.85.27.95 28.23 3.303e+006 26 . , ', . 1 • _ _-� .- , • „ , min 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 b294t1113-2 SmcctP CSG,1 .7) 96 11 22.70 2497 2378•TCDD 27.24 17908.54 10.13DVA. 462.64 929ott11a4 Sn:cct1 SG,14.2) I 2378•TCDD 27.24 24761.92 647.09 F1-Vo-tage SIR,EI. 319 6995 2 668e•005 28.26 • man F1 Voltage SIR,FI• 321 E938 3-4934.005 22.25 22.50 22.75 23 00 23.25 23.50 23.75 24.00 24 25 24.50 24 75 25.00 25 25 25.50 25 75 26.00 26 25 26.50 26.75 27.00 27.25 27.50 27.75 28 00 28.25 I8 50 6ti6 10 96 abed min Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Untitled Last Altered: Monday, October 31, 2011 10:04:49 Eastern Daylight Time Printed: Monday, October 31, 2011 10:05:42 Eastern Daylight Time Name: b29oct11a-2, Date: 29-Oct-2011, Time: 19:36:51, ID: 46213, Submitter: , Task: 2378-TCDF b29oct11 a-2 22.00 2378-TCDF b29oct11 a-2 %- 6 22.50 23.00 I I 23.50 2378-TCDF F1:Voltage S1R,E1+ 26.35 303.9016 (' 3.751e+005 J I i I i ir, , , I .,.,,,.,r.,. , ,.,,,,,.I I [ r T 1. min 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 2378-TCDF 26.35 F1:Voltage SIR,EI+ 305.8987 4.742e+005 22 00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 ES-TCDF b29oct11 a-2 1 25.00 r \ ES:13C-2378-TCDF 26.34 27.00 27.50 28.00 28.50 29.00 29.50 ,.., min 30.00 F1:Voltage SIR.EI+ 315.9419 3.464e+006 22.00 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 ES-TCDF b29oct11 a-2 • 22 00 CD V F>~,Lock Mass b4goct11 a-2 CO 22.04 25.00 A ES:13C-2378-TCDF 26.34 11 27.50 28.00 28.50 29.00 29.50 ...i min 30.00 F1:Voltage SIR,EI+ 317.9389 4.408e+006 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 min 28.50 29.00 29.50 30.00 F1:Voltage SIR,EI+ 304.9824 3.303e+006 22 39 22 75 22.95 23.4423.85.23.94 24.33 24.7124.94 25.14 25.63 26.06 26.47 26.86 27.1927.60.27.85 27.95 28.23 28.42 26 22.00 min 22.50 23.00 23.50 24.00 24.50 25.00 25.50 26.00 26.50 27.00 27.50 28.00 28.50 29.00 29.50 30.00 617l 10 86 abed Analytical Method' 829 1613 8280 1 668A DLM Other: QC Date Prev. WGv. I PreWG Workgroup* Logbook# 19 Page# 1337 ' 28-Oct-11 N/A - Extraction by Modified Method s� 3540C (Soxhlet Extraction) — Dean -Stark? L re•Sox? Extract Cleanup by Method 3630/3620 (Silica/Florisil) Modified injection Prep. Sample Identification Client Sample ID SGS Sample ID* Sample Matrix Sample Weight* ES Amt.* (pL) MX Amt. (pL) CS Amt.*mt (pL) PCU Analyst PCU # / Train JS A * (pL) i. 46212 LMB1337 Tissue 10.00 _ 40 N/A 40 HHJ Z 1 20 Comp#1 Site 1 Bluegill 31102775001 Tissue 18,9 0 40 - N/A 40 , HHJ Z 2 20 Comp#2 Site 1 Flathead Catfish 31102775002 , Tissue tok ta 40 N/A 40 HHJ 7. 3 20 Comp#3 Site 1 Blue Catfish sm 31102775003 Tissue 'Di 90 40 N/A 40 HHJ 2. ti-- 20 Comp#4 Site 1 Blue Catfish Ig 31102775004 Tissue l a q a 40 N/A 40 HHJ 2 '5 20 Camp#5 Site 2 Bluegill 31102775005 Tissue i 0, 5 40 N/A 40 HHJ 2 cc, 20Comp#6 Site 2 Flathead Catfish 31102775006 Tissue j0A 3 40 N/A 40 " HHJ Z .7 20 Comp#7 Site 2 Blue Catfish 31102775007 Tissue to , 5 40 N/A 40 HHJ Z 20 Comp#8 Site 2 Common Carp 31102775008 Tissue pi g 40 N/A 40 HHJ 'L 9 20 Comp#9 Site 3 Bluegill sm 31102775009 Tissue r0, j 40 N/A 40 HHJ j. j (1 20 Comp#10 Site 3 Bluegill Ig 31102775010 Tissue f p,-7 6 40 N/A 40 HHJ 'L (1 20 Comp#11 Site 3 FlatheadCatfish 31102775011 Tissue _ ID, 1.1 40 N/A 40 HHJ Z t z 20 Comp#12 Site 3 Blue Catfish 31102775012 Tissue 1014 40 N/A 40 HHJ 2. j 20 Com #13 Site 1 Blue Catfish Ig p 31102775013 Tissue (j), l4 40 N/A 40 HHJ 2. 2. 20 46213 OPR Tissue 10.00 40 40 40 HHJ 'L. 20 Dioxin Standards Lot # Conc. Ina/uL) Analyst Witness Items Lot # Extraction Std. s39•15pa. D.cS . /7f5 Toluene STL1-1 Matrix Spike 539.149 Q;005 $5• 7%,' Tridecane - Cleanup Std. 541-I(2'v _01 qA fi P_I. McCI STL1-2 Injection Std. Salt SPL2-237 PCB Standards Hexane DD787 Extraction Std. Acid Silica SPL3-7 - Matrix Spike Base Silica SPL3-7 Cleanup Std. Silica 22-22 - Injection Std. �� Fiorisil SPL3-6 • _ _ Balance Refers ce: WB1 w1B1 Extraction Da e/Time Start: c Finish: Extraction alyst: !./6ata in prep table? Cleanup Dat Imo: Comments: *or ty \()(& \ -c-r) nalyvela - -u4PS f0(Zel(ll .- To"be entered in the Prep Table. odata in prep to DC_308.8 Batch Summary Analytical Method: Gravimetric Prep Method: Gravimetric Prep Batch: HXX1347 Prep Date: 10/24/2011 17:00 Client Sample ID Comp#1 Site 1 Bluegill Comp#2 Site 1 Flathead Catfish Comp#3 Site 1 Blue Catfish sm Comp#4 Site 1 Blue Catfish lg Comp#5 Site 2 Bluegill Comp#6 Site 2 Flathead Catfish Comp#7 Site 2 Blue Catfish Comp#8 Site 2 Common Carp Comp#9 Site 3 Bluegill sm Comp#10 Site 3 Bluegill Ig Comp#11 Site 3 FlatheadCatfish Comp#12 Site 3 Blue Catfish Comp#13 Site 1 Blue Catfish lg Lab Sample ID Analysis Date 31102775001 10/24/2011 17:00 31102775002 10/24/2011 17:00 31102775003 10/24/2011 17:00 31102775004 10/24/2011 17:00 31102775005 10/24/2011 17:00 31102775006 10/24/2011 17:00 31102775007 10/24/2011 17:00 31102775008 10/24/2011 17:00 31102775009 10/24/2011 17:00 31102775010 10/24/2011 17:00 31102775011 10/24/2011 17:00 31102775012 10/24/2011 17:00 31102775013 10/24/2011 17:00 Analytical Batch Instrument Analyst HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS HXX1347 BAL10 RSS Print Date: 11/01/2011 SGS North America Inc. 5500 Business Drive, Wilmington, NC 28405 t 910.350.1903 f 910.350.1557 www.us.sgs.com N.C. Certification # 481 Member of SGS Group Page 99 of 149 Lipid SGS Project: 31102775 Sample ID Client ID Sample Weight Initial Weight Final Weight % Lipid ('h 1 2775-001 10.50 32.7123 32.7392 0.26 / 2 2775-002 10.57 32.6063 32.6242 0.17 ✓ 3 2775-003 10.02 32.5531 32.7971 2.44 4 2775-004 11.46 32.5091 32.9321 3.69 5 2775-005 10.42 32.5534 32.6098 0.54 6 2775-006 11.28 32.5343 32.6162 0.73 7 2775-007 10.04 32.5608 32.8755 3.13 ,/ 8 2775-008 10.96 32.5338 32.7208 1.71 9 2775-009 10.65 32.5507 32.6057 0.52 10 2775-010 10.81 32.5205 32.5732 0.49 11 2775-011 10.71 32.5955 32.6298 0.32 12 2775-012 10.65 32.5225 32.6487 1.18 13 2775-013 10.87 32.4688 32.6183 1.38 #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DiV/0! #DIV/0! 14'1! Initials: etN P"N r'L'N raN Page 100 of 149 SoN EARN r rmk, Sample ID % Lipid SGS Project: 31102775 Client ID Sample Weight Initial Weight Final Weight % Lipid 1 2775-001 10.50 32 i 23 _ 3.17. % 0.00 2 2775-002 10.57 3). 6063 3 a.4.1`ix 0.00 3 2775-003 10.02 13. 5.$31 3. 797I 0.00 4 2775-004 11.46 32 . 5a 91 32. M ( 0.00 5 2775-005 10.42 32. SS 3 LJ- 3 d 44 951 0.00 6 2775-006 11.28 3�, 62043 3a. 16 0.00 7 2775-007 10.04 "TaL5gtst 3 , $7S3 0.00 8 2775-008 10.96 3a . 5.3343 32. --go--goi 0.00 9 2775-009 10.65 3a. 5S'O ) 32 . Lac? 0.00 10 2775-010 10.81 3.Q. gaits 3e.I .71x 0.00 11 2775-011 10.71 -9Sr 2. 9 0.00 12 2775-012 10.65 5 )5 _ a ,$1 0.00 13 2775-013 10.87 39. L� oZ • ClIt 3 0.00 #DIV/0! #DIV/0! #DIV/0! #DIV/01 #DIV/0! #DIV/oi #DIV/01 #DIV/01 , Initials: e•At► Page 101 of 149 Quantify Compound Summary Report MassLynx 4.1 SCN640 ### !CAL Summary ### Dataset: Y:IDefault.prolCurved blb 16may11 d-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:10:56 Eastern Daylight Time YYl a-k-vctS n 5 i t I kn-e_LO Method: Untitled 31 Oct 2011 09:53:18 Calibration: 31 Oct 2011 14:10:32 Compound name: 2378-TCpF Response Factor: 1.00416 J RRF SD: 0.0464143, Relative SD: 4.62219 Response type: Internal Std ( Ref 4 ), Area * ( IS Conc. / IS Area ) Curve type: RF Filename Sample ID Std. Conc. RRF / IS# 1 bl6maylld-2 CS0.5_S37-4... 0.25 1.084/ 4 2 bl6maylld-3 CS1_S37-40... 0.50 1.024 4 3 bl6maylld-4 CS2_S37-401J 2.00 1.012 4 4 bl6maylld-5 CS3 S36-206J 10.00 0.968 4 5 bl6mayl 1d-6 CS4_S37-401L 40.00 0.976 4 6 bl6mayl ld-7 CS5_S37-40... 200.00 0.961/ 4 Compound name: 2378-TpDD Response Factor: 1.1714 v/ RRF SD: 0.116561, Relative SD: 9.95056 Response type: Internal Std ( Ref 3 ), Area * ( IS Conc. / IS Area ) Curve type: RF Filename Sample ID Std. Conc. RRF IS# 1 bl6may11 d-2 CS0.5 537-4... 0.25 1.396 3 2 bl6maylld-3 CS1_S37-40... 0.50 1:153/ 3 3 bl6maylld-4 CS2_S37-401J 2.00 1.181 3 4 bl6maylld-5 CS3_S36-206J 10.00 1.130 3 501 bl6mayl 1 d-6 CS4_S37-401L 40.00 1.070 3 6 bl6maylld-7 CS5_S37-40... 200.00 1.099 3 N O co J eINA I )))))))))))))))))))))))))))) )).)) )..) )J.) ).).) ) ) ) Quantify Compound Summary Report MassLynx 4.1 SCNG40 ### ICAL Summary M# Dataset: Y:lDefault.prolCurvedblb16may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:10:56 Eastern Daylight Time Compound name: ES:13C-,2378-TCDD Response Factor: 1.02637 RRF SD: 0.0375477, Relative SD: 3.65829 Response type: Internal Std ( Ref 5 ), Area * ( IS Conc. / IS Area ) Curve type: RF Filename Sample ID Std. Conc. RRF IS# 1 bl6may11d-2 CS0.5 S37-4... 100.00 1.028 5 2 bl6may11d-3 CS1_S37-40... 100.00 0.990 5 3 bl6maylld-4 CS2_S37-401J 100.00 1.017✓ 5 4 b16may11d-5 CS3_S36-206J 100.00 0.994 5 5 1316may11d-6 CS4_S37-401L 100.00 1.035 5 6 bl6may11d-7 CS5_S37-40... 100.00 1.094 5 Compound name: ES:13C-2378-TCDF Response Factor: 1.5771 / RRF SD: 0.0366419, Relative SD: 2.32338 Response type: Internal Std ( Ref 5 ), Area * ( IS Conc. / IS Area ) Curve type: RF Filename Sample ID Std. Conc. RRF IS# 1 bl6may11d-2 CS0.5_S37-4... 100.00 1.600 5 2 b16may11d-3 CS1 S37-40... 100.00 1.543 5 3 bl6may11d-4 CS2 S37-401J 100.00 1.598 / 5 4 bl6mayl ld-5 CS3 S36-206J 100.00 1.523 ✓ 5 5 bl6may11 d-6 CS4_S37-401L 100.00 1.582 5 6 bl6may11d-7 CS5_S37-40... 100.00 1.617 5 Compound name: JS:13C-1234-TCDD Response Factor. 1 RRF SD: 0, Relative SD: 0 R6ponse type: Internal Std ( Ref 5 ), Area * ( IS Conc. / IS Area ) Cave type: RF Filename Sample ID Std. Conc. RRF IS# 1 . bl6mayl 1d-2 CS0.5 S37-4... 100.00 1.000 5 2 bl6mayl1d-3 CS1 S37-40... 100.00 1.000 5 J Quantify Compound Summary Report ### ICAL Summary ### MassLynx 4.1 SCN640 Dataset: Y:IDefault.prolCurvedblb16may11 d-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:10:56 Eastern Daylight Time Compound name: JS:13C-1234-TCDD Filename Sample ID Std. Conc. RRF IS# 3 bl6may11 d-4 CS2_S37-401J 100.00 1.000 5 4 b16may11d-5 CS3_S36-206J 100.00 1.000 5 5 bl6may11 d-6 CS4_S37-401L 100.00 1.000 5 6 bl6may11 d-7 CS5_S37-40... 100.00 1.000 5 Compound name: CS:37C12378-TCDD Response Factor: 1.21831 RRF SD: 0.0703355, Relative SD: 5.77319 Response type: Internal Std ( Ref 5 ), Area * (IS Conc. / IS Area ) Curve type: RF Filename Sample ID Std. Conc. RRF IS# 1. bl6maylld-2 CSO.5 S37-4... 0.25 1.315 5 2 bl6may11d-3 CS1_S37-40... 0.50 1.263 5 3 bl6mayl1d-4 CS2_S37-401J 2.00 1.179 5 4 bl6mayl 1 d-5 CS3_S36-206J 10.00 1.128 5 5 bl6mayl 1 d-6 CS4_S37-401L 40.00 1.170 5 6 bl6may11d-7 CS5_S37-40... 200.00 1.255 5 6VL Jo VOL abed )))))))))))))))))))))))))))))))) .) ) ) 10. Quantify Sample Summary Report MassLynx 4.1 SCN640 ### ICAL Summary### Dataset: Y:1Default.prolCurvedb1b16may11d-tetras.g1d Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:12:40 Eastern Daylight Time Method: Untitled 31 Oct 2011 09:53:18 Calibration: 31 Oct 2011 14:10:32 Na e: 16may11 d-2 ID C . _S37-401G D .1 -May-2011 Time: 18:05:48 User: JLJ Submitter: Task: 1 Name Response Ion1Area lon2Area RT }A RAFaiI? RRF MRRF %RSD IS# Heightl Noisel SN1 Height2 Noise2 SN2 M 1 2378-TCD 1.0 48e4 4.909e3 5.570e3 30.97 9.88 NO 1.084. 1.004 4.6 4 6.872e4 894 76.9 6.796e4 838 81.1 MM 2 2378-TCDD 8.671e3 3.962e3 4.709e3 31.56/ .84 NO 1.396, 1.171 10.0 3 6.343e4 820 77.4 7.063e4 1176 60.0 MM 3 ES:13C-2378-TCDD 2.485e6 1.091e6 1.394e6 31.54/9.78 NO 1.028, 1.026 3.7 5 1.681e7 1043 16116.9 2.123e7 1413 15024.4 bb 4 ES:13C-2378-TCDF 3.867e6 1.714e6 2.153e6 30.95/ 0 0 NO 1.600. 1.577 2.3 5 2.129e7 1693 12574.7 2.654e7 1946 13637.9 bb 5 JS:13C-1234-TCDD 2.417e6 1.075e6 1.342e6 31.11 p.80 NO 1.000. 1.000 0.0 5 1.446e7 1043 13870.9 1.782e7 1413 12614.8 bb 6 CS:37C1-2378-TCDD 7.946e3 7.946e3 - 31.54/ - 1.315, 1.218 5.8 5 1.194e5 704 169.6 - bb ao pj,4 .2 3 .W (v7 et, O. c; 57 4 . 6bl. Jo 50L a6ad /.os TO , v-314 I F1:Voltage SIR,EI+ 331.9368 0 { , , . , i 1 i . I , - 1 i , . . 4 , { . . , 1 i , 1 ! T 1 1 , I ! { 1 1 1 { ! 1 1 I 1 { { . I { { I i { { , l 1 { ( { I T . { { ' { ' { { I , '1.689e+007 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 311.00 31.25 31.50 T 31.75 32.00 32.25 32.501n ES-TCDD bl6may11d-2 ES:13C-2378-TCDD F1:Voltage SIR,EI+ 100- 31.54 333.9339 n 2.133e+007 -01 { i.{,.. 1 1 r T. I i ,. I i i T i,- I i. i I.. i I- I i T. l{, T r . i T T I l, I 1 i I 1 i I min 28.00 28.25 28.150 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 CS-TCDD b16mayl 1d-2 4131 1 rI , Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:1Default.prolCurvedb1b16may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Method: Untitled 31 Oct 2011 09:53:18 Calibration: 31 Oct 2011 14:04:30 Name: bl6may11d-2, Date: 16-May-2011, Time: 18:05:48, ID: CS0.5_S37-401G, Submitter: , Task: 2378-TCDD bl6may11d-2 28.30 28.43 29.90 30.211 (3/0.29 30.57 30.93 31.10 32 . 1 I 1 i 1 I I i . ' { i , i , 1 I r 1 T 1 1 i 1 T .low- 1 , •. 1 { I 1 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 2378-TCDD bl6may11d-2 F1:Voltage SIR,EI+ 319.8965 31.80 32.17 32.26 9.528e+004 {�{ F{ i . 1min 31.75 32.00 32.25 32.50 F1:Voltage SIR,EI+ 321.8936 28.43 30.21 30.90 31.38 - 1.028e+005 - . I - I r T I . . { . I , . . I I . I { - , r l . l , - „ I - _ min 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD bl6mayl 1 d-2 ES:13C-2378-TCDD 31.11 3� 31.56 31.50 31.56 31.54 CS:37CI-2378-TCDD 31.54 { I I I 1 i I r r . . I 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 F1a.ock Mass bl6may11d-2 28'20 28.33 29.43 29.63 30 32 28.121 , 28.58 28.79 28.99 29.17 29 55� ' �29.75 30.01 - 30 26 3 ' 30.52 30.65 30.85 31.01 89 '. I 28 00 28.25 28.50 28.75 29.00 31.39 31 48 31.24 F1:Voltage SIR,EI+ 327:8847 32.25 1 '514e+005 r{ { . { i min F1:Voltage SIR,EI+ 31.87 31'99 32.20 32.28 304.9824 +006 min 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 )J))))) )1))) )) ))))))))))))))))))))))) ) ) ) .) ) ).__) b 1 &may11 d• 2 Smooth(SG,1 x2) CSO.5_537.401 O 26.08 30.93 27.58 28.30 28.43 29.90 30.21 � '29 30.57 I 31.10 2378-TCDD 31.56 F1 voltage SIR,EI+ 319.8965 9.528e+004 31.80 32.17 32 26 bl6mayl 1d•2 Smooth(SG,1x2) CS0.5_837-4010 30 6176 10 LOI. abed 6.04 26.37 26.52 26.88 27.87 28.43 30.21 30.90 31.38 .min 26.25 26.50 26.75 27.00 27 25 27.50 27.75 28.00 28.25 28.50 28.75 29 00 29.25 29.50 29.75 3000 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDD 31.56 F1-Voltage SIR,EI• 321.8936 1.028e •005 Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:1Default.prolCurvedb1b16may11 d-tetras.gtd Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6mayll d-2, Date: 16-May-2011, Time: 18:05:48, ID: CS0.5_S37-401 G, Submitter: , Task: 2378-TCDF bl6may11 d-2 30 28.45 28.88 28 00 28.25 2378-TCDF bl6may11 d-2 28.50 28.60 31� ,1--rTT.T, i 28.75 28 00 28.25 28.50 28.75 ES-TCDF blCmayl ld-2 %. 0 28 00 29.00 29.25 29.50 29.65 29.75 29.29 29.70 29.00 29.25 29.50 29.75 30.00 r 30.00 30.25 30.25 30.60 30.75 30.50 30.50 30.75 30.75 2378-TCDF 30.97 31.00 2378-TCDF 30.97 31.00 ES:13C-2378-TCDF 30.95 31.25 31.25 31.50 31.52 31.50 31.75 31.75 F1:Voltage SIR,Et+ 303.9016 1.005e+005 31.89 32.36 32.00 32.00 32.25 min 32.50 F1:Voltage StR,EI+ 305.8987 1.002e+005 32.25 min 32.50 F1:Vo!tage SIR,EI+ 315.9419 2.142e+007 ,,rr ES-TCDF bl6may11d-2 7. 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES:13C-2378-TCDF 30.95 F1:Voltage SIR,EI+ 317.9389 2.670e+007 - r r r.. r r r.. r,. r t r, r. r r -r . r r r i r, r,... .. , r r r r r r, r r r r r r r r r r,; r. r r min c8 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 F'.ock Mass blfirnay11d-2 co_ 89 28.20 28.58 29.43 29.55 29.63 28.12 28.33 28.79 28.99 29.17 29.75 30.01 28 00 30.2630.32 30.5230.65 30.85 31.01 31.24 31.39 31.48 F1:Voltage SIR,EI+ 31.99 32.20 32.28 304.9824 31.87 :7 +006 . . . r . r , , r , , , , , , , , , , , , , . , , , , , , , . , , r . T r , r r 1 min 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ) ) ) ) �)) ... .. ..�1._ �l ) ). ._l ...�. ) bt 6may11 d.2 Sm14th0G.1x2) CS0 5 S37.401O 96 26.79 30 bl 6mayl td-2 Smooth(SG,1x2) C90.5_837-4010 96 2378•TCDF 30.97 27.59 28.45 28.88 29.65 30.60 30.75 28.60 29 29 _� 9.70 31.52 31 s", 1 1 minr 26.25 26.50 26.75 27.00 27.25 27.50 27.75 28.00 28.25 28.50 26., 75' 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 lab 2378-TCDF 30.97 F1:VOltage SIR,EI* 303.9016 1.005e•005 31.89 32.36 min F1 Voltage SIR.EI+ 305.8987 1.002e•005 6176 Jo 601. 962d 26.08 Quantify Sample Summary Report MassLynx 4.1 SCN640 ##f# ICAL Summary### Dataset: Y:lDefault.prolCurvedb1b16may11 d-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:12:40 Eastern Daylight Time Na e: b 6may11 d-3 ID: CS1 S37-401H Da -May-2011 Time: 18:52:44 User: JLJ Submitter: Task: J 1 Name Response Ion1Area Ion2Area RT 5A RAFaiI7 RRF MRRF %RSD IS# Heightl Noise1 SN1 Height2 Noise2 SN2 M 1 2378-TCDF 1.690e4 7.528e3 9.369e3 30.96'' .80 NO 1.024 • 1.004 4.6 4 1.082e5 563 192.3 1.374e5 677 203.0 bb 2 2378-TCDD 1.221e4 5.368e3 6.846e3 31.56'.78 NO 1.153. 1.171 10.0 3 8.948e4 734 121.8 1.210e5 1102 109.7 MM 3 ES:13C 78-TCDD 2.11 6 9.327e5 1.186e6 31.54".79 NO 0.990. 1.026 3.7 5 1.645e7 1036 15873.7 2.124e7 1269 16742.1 bb 4 ES:13C-2378-TCDF 3.301e6 1.454e6 1.847e6 30.95�79 NO 1.543. 1.577 2.3 5 2.030e7 1299 15625.3 2.595e7 1903 13631.7 bb 5 - JS:13C-1234-TCDD 2.139e6 9.418e5 1.197e6 31.11�79 NO 1.000• 1.000 0.0 5 1.446e7 1036 13958.6 1.850e7 1269 14578.2 bb 6 CS:37CI-2378-TCDD 1.351e4 1.351e4 - 31.56 " - - 1.263 • 1.218 5.8 5 2.513e5 715 351.5 - - bb --rc:042-1= 1. -)-al -ti-I 61410 013 a6ed j.i53 : 3►-1 J ))))))))))))))))))))))) .) ) ..)) )... j.))) ...) )..) ..)))))) ) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:1Default.prolCurvedb1b16may11d-tetras.g1d Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-3, Date: 16-May-2011, Time: 18:52:44, ID: CS1_S37-401H, Submitter: , Task: 2378-TCDD bl6may11d-3 %_ 26 28 00 28.61 28.86 29.32 29.73 30.95 31.56 F1:Voltage SIR,EI+ 319.8965 1.204e+005 28.25 2378-TCDD bl6may11 d-3 20 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 min 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 31.56 F1:Voltage SIR,EI+ 321.8936 1.536e+005 30.93 31.36 32.18 min 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD bl6mayl ld-3 31.11 ES:13C-2378-TCDD 31.54 I 1 f r 1 T . r r 1 1 . T 1 1 1 1 1 i . . . T 1 I . T . . . I { ' . T T r T 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 ES-TCDD bl6may11 d-3 100 31.11 31.25 31.50 l I 1 1 31.75 32.00 ES:13C-2378-TCDD 31.54 F1:Voltage SIR,EI+ 331.9368 1.652e+007 . . , { min 32.25 32.50 F1:Voltage SIR,EI+ 333.9339 2.132e+007 •0- . , 1 . . . 1 T 1 1 . T i , T T i . . . 1 . 1 { 1 . 1 . . 1 . . 1 1 . , 1 1 . , , . . . , i i 1 T I 1 i . , i , 1 f >� I 1 . 1 , 1 1 { 1 I min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.1 75 30.00 30.. T 25 30.50 30.75 31.If 31.25 31.50 31.75 32.00 32.25 32.50 CS-TCDD bl6may11d-3 13 �° 1 I.4 _ `y 1 . 1 . I 1 . , . I 1 T 1 1 1 I 1 1 t I I 1 1 1 1 i 1 1 1 i { 1 I i I { I 1 1 I 1 1 1 1 I ! T i T I i i l i I i . I 1 . T 1 1 S 1 r 1 . 1 1 1 I • T I r i i . T r I i 1 1 1 I min 8.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 0 FiLock Mass bl6may11d-3 F1:Voltage SIR,EI+ 28.02 28.25 28.61 28.66 28.86 28.97 29.24 29.43 29.50 29.70 29.88 30.08 30.22 30.32 30.45 30.75 30.83 31.01 31.06 31.3131.44 31.67 31.80 31.90 32.20 32.38 304.+006 9824 % CS:37CI-2378-TCDD 31.56 88y 28 00 28.25 F1:Voltage SIR,EI+ 327.8847 2.822e+005 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 min 31.25 31.50 31.75 32.00 32.25 32.50 bt dmayl l d-3 Smooth(SG.1 x2) CS1 S37-401H 96 26.09 26 82 28.86 29.32 / 26 7 .• bl 6may11 d-3 Smodin(S3,1 x2) CS7 S37-441H 30.95 29.73 2378-TCDD 31.56 2378•TC00 31.56 F1:Vottage SIR,EI• 319.8965 1.204e+005 .. , .... ,min F1:Voltage SRO. 321.8936 1.536e+005 32.18 20 min 26.25 26.50 26.75 27.00 27.25 27.50 f 27.75 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 6t 4 Jo Z 61. abed )))))) .))))))))).))))))A. .:1.))...))...)._.j)) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only### Dataset: Y:1Default.prolCurvedb1b16may1ld-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: blfimaylld-3, Date: 16-May-2011, Time: 18:52:44, ID: CS1_S37-401H, Submitter: , Task: 2378-TCDF bl6may11d-3 2378-TCDF F1:Voltage SIR,EI+ 30.96 303.9016 1.400e+005 %: 22 . 30.16 . . . . . , , . . . . , . � � � 1.. �, I I� I I . t,� 1 I I I I ., 11.. , � . 1 r 1 P I . 1 . 1 , I min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDF bl6may11d-3 %: 29.66 18 , 1 . 1 . I 1 , ram. 1 . , . 1 1 . . ( r r 1 . . . i . . . 1 , . i , . . 1 , , 1 min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDF F1:Voltage SIR,El+ 30.96 305.8987 1.714e+005 ES-TCDF bl6mayl ld-3 ES:13C-2378-TCDF 30.95 F1:Voltage SIR,EI+ 315.9419 2.044e+007 •. . 1 , 1 , I . . ( min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDF bl6may11d-3 ES:13C-2378-TCDF 30.95 F1:Voltage SIR, El+ 317.9389 2.614e+007 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 Fl -ock Mass b11tnay11d-3 co 28.02 28.25 28 00 28.25 28.61 28.66 28.86 28.97 Amin 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 29.24 29.88 30.08 30.22 30.32 29.4329.80 29.70 30.45 30.75 30.83 31 3131.44 31.01 31.06 F1:Voltage SIR,EI+ 3190 32.20 32.38 304.9824 31.67 31.80.27 +006 . . . 1 . . 1 . 1 . 1 , 1 1 . I . . 1 T I „ 1 , 1 1 1 . • min 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 Quantify Sample Summary Report ### ICAL Summary ### MassLynx 4.1 SCN640 Dataset Y:\Default.prolCurvedb\b16may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:12:40 Eastern Daylight Time Na e: 16may11 d-4 ID CS2 S37-401J D te: -May-2011 Ti .19:42:50 User: JLJ Submitter: Task: Name Response Ion1Area Ion2Area RT 5A RAFaii't RRF MRRF %RSD IS# Heightl Noise1 SN1 Height2 Noise2 SN2 M 1 2378-TCDF 6.080e4 2.701e4 3.379e4 30.97/0.80 NO 1.012• 1.004 4.6 4 3.449e5 613 562.7 4.314e5 822 524.9 bb 2 2378-TCDD 4.515e4 1.995e4 2.520e4 31.56/0.79 NO 1.181 • 1.171 10.0 3 3.280e5 604 542.8 4.121e5 747 551.8 MM 3 ES:13C-2378-TCDD 1.91� 8.410e5 1.070e6 31.54/ .79 NO 1.0� 7. 1.026 3.7 5 1.369e7 1119 12236.6 1.740e7 755 23031.4 bb 4 ES:13C-2378-TCDF 3.003e6 1.317e6 1.686e6 30.95 0.78 NO 1.598• 1.577 2.3 5 1.642e7 1653 9934.3 2.126e7 1967 10807.7 bb 5 ' JS:13C-1234-TCDD 1.880e6 8.313e5 1.048e6 31.114.79 NO 1.000 • 1.000 0.0 5 1.128e7 1119 10078.6 1.440e7 755 19061.2 bb 6 CS:37C1-2378-TCDD 4.432e4 4.432e4 - 31.561 - - 1.179 • 1.218 5.8 5 7.198e5 802 897.3 - bb I_gisuee ►oop,5r6,4 6P1. 10 PR a62d 1. 01(,S -7,/0 31- 1) ) ) ) ) ) ) ) ) ) ). ) ) ) ) 1 ) ) ) ) ) ) ) ). ).. Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:1Default.prolCurvedblb16may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-4, Date: 16-May-2011, Time: 19:42:50, ID: CS2_S37-401J, Submitter: , Task: 2378-TCDD bl6may11d-4 31.56 0/01 9 28 00 28.25 28.50 28.75 29.00 29.25 , 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDD bl6may11 d-4 31.56 F1:Voltage SIR,EI+ 319.8965 3.613e+005 1 7 , , , . , , . , , , , . , , ( min 14 28 00 28.25 28.50 28.75 29.00 29., 25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD bl6may11d-4 100 14 31.11 ES:13C-2378-TCDD 31.54 F1:Voltage SIR,EI+ 321.8936 4.443e+005 F1:Voltage SIR,EI+ 331.9368 1.378e+007 0 , . , . ▪ , + , , , , , , . , , . . , , , . , 14 , , , , , , , min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD bl6may11 d-4 100 -0 . . , . , T , , . . , 28 00 28.25 28.50 28.75 29.00 CS-TCDD bl6mayl 1d-4 Zt▪ 8 00 28.25 28.50 28.75 29.00 0 FiLock Mass bl6may11 d-4 - 28.13 ^ono -288428.97 89 28 00 28.25 28.50 31.11 . , , , , . . ,T " . , . . 1 min 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 29.25 29.50 29.75 ES:13C-2378-TCDD 31.54 CS:37C1-2378-TCDD 31.56 F1:Voltage SIR,EI+ 333.9339 1.748e+007 F1:Voltage SIR,EI+ 327.8847 7.537e+005 , , , . . , , . , . i . ? . . , , , , , , min 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 29.19 29.45 29.57 29.85 29.93 30.14 F1:Voltage SIR,EI+ 30.47 30.57 30.6730.80 31.28 1.31 31.49 31.69 31.95 32.00 32.30 304.9824 31.03 +006 ,..,..,.imin 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 b1 amay1 ld-4 Smootf(S0,1x2) C82_537-401 J 9 ;1r r r -1 i . �", 7 77. S'^,,"'. �--Y, bl6maylld-4 Smootb(S0,1x2) CSZ 537-401J 2378•TCDD 31.56 Ft:Voltage SIR,EI• 319.8965 3.613e•005 - min 2378-TCOD 31.56 F1 :Voltage SIR,EI. 321.8936 4.443e.005 •. , •r• � r .T1 � min 26.25 f 26.50 26.75 27.00 27.25 27.50 27.75 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00T 31.25, 31.50 31.75 32.00 32.25 32.50 6til 10 91.I. e68d ))))))))))))))))) MY) )))))))))))))T))))3 )))))))))))1*))))))))))))))))))))_))))))))))) Quantify Sample Report MassLynx 4.1 SCN640 #k##TCDD TCDF Only ### Dataset: Y:\Default.pro1Curvedblbl6may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-4, Date:16-May-2011, Time: 19:42:50, ID: CS2_S37-401J, Submitter: , Task: 2378-TCDF bl6may11d-4 2378-TCDF F1:Voltage SIR,EI+ 30.96 303.9016 /1 3.794e+005 min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDF bl6mayl ld-4 ° 2378-TCDF F1:Voltage SIR,EI+ 30.96 305.8987 /1 4.652e+005 /a 7 . I . . . . . . . . i . . . . . . . . . ( . . . . . . . . r j . . . . . 1 . . . . . . . . r i r . . r r . . . min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES TCDF b l6mayl l d-4 %- ES:13C-2378-TCDF 30.95 0 2800 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 F1:Voltage SIR,EI+ 315.9419 1.651e+007 ES-TCDF bl6mayl 1d-4 %y T - D- 1 1 1 ( 1 . . . . 1 / j , 1 r . 1 . . , . 1 l . . I~ T . 1 . . . . . . . . 1 . . . . 1 . . . . 1 . . . . I min (28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES:13C-2378-TCDF 30.95 min F1:Voltage SIR,EI+ 317.9389 2.136e+007 -1 F'FLock Mass b1 may11d-4 28.13 28.38 28.48 28.66 28.8428.97 29.19 29.45 29.57 29.85 29.93 30.14 F1:Voltage SIR,EI+ 31.95 32.00 32.30 304.9824 30.47 30.57 30.67 30.80 31.28 1.31 31.49 31.69 - • +006 31.0331.10 89 - , i j , . , . i , . . , � . , . , . , . . , i min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 Quantify Sample Summary Report MassLynx 4.1 SCN640 ### iCAL Summary ### Dataset: Y:(Default.prolCurvedblbl6may1ld-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:12:40 Eastern Daylight Time Na ► e:' 16may11d-5 ID: CS3 - 36-206J Da e: 1 May-2011 Tim •.20:32:51 User: JLJ Submitter: Task: Name Response IonlArea Ion2Area RT RAFaiI? RRF MRRF %RSD IS# Heightl Noisel SN1 Height2 Noise2 SN2 M 1 2378-TCDF 4.735e5 2.057e5 2.678e5 30.977 0.77 NO 0.968- 1.004 4.6 4 2.683e6 663 4045.0 3.576e6 2181 1639.6 bb 2 2378-TCDD 3.609e5 1.592e5 2.017e5 31.56.479 NO 1.130. 1.171 10.0 3 2.637e6 996 2648.8 3.318e6 890 3726.4 MM 3 ES:13C-2378-TCDD 3.195e6 1.407e6 1.788e6 31.54 99 NO 0.994. 1.026 3.7 5 2.389e7 1245 19189.5 3.038e7 1044 29089.3 bb 4 ES:13C-2378-TCDF 4.893e6 _ 2.153e6 2.740e6 30.95700.79 NO 1.523- 1.577 2.3 5 2.862e7 1763 16232.6 3.630e7 1457 24910.8 bb 5 JS:13C-1234-TCDD 3.214e6 1.426e6 1.788e6 31.11480 NO 1.000- a 1.000 0.0 5 2.097e7 1245 16846.0 2.603e7 1044 24927.8 bb 6 CS:37C1-2378-TCDD 3.625e5 3.625e5 - 31.56/ - - 1.128. 1.218 5.8 5 6.029e6 603 10000.3 - - bb 6ti1. 10 91.1. abed E5 -1i1 b � $4- 793P 5 /00 I. 5D. - -rrr»bo-31- 1/ ))))))))))))))))))))))) ) ) ) ). ).. ) ) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:IDefault.pro\Curvedb\b16may11d-tetras.g1d Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-5, Date: 16-May-2011, Time: 20:32:51, ID: CS3_S36-206J, Submitter: , Task: 2378-TCDD bl6may11d-5 31.56 F1:Voltage SIR,EI+ 319.8965 2.668e+006 , ; , r . , . . . . ; , I, r r ; r ; . . . ; , , r . . . . • . . , , . , . r , ; , , , min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDD bl6may11d-5 31.56 F1:Voltage SIR,EI+ 321.8936 3.350e+006 %- 1- ..,•;,..;rrrF,,..;r.r; .;.• min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD bl6may11d-5 100- oIo 28.00 28.25 ES-TCDD bl6may11d-5 31.11 ES:13C-2378-TCDD 31.54 F1:Voltage SIR,EI+ 331.9368 2.403e+007 , , . . r , . ; r . r r . . . ; , , ; , , . . r . r . ; . , , . . , , r ; . . . , ; , . . l c , . r ; . 1 r . . r . . . r . r . ; , . . . 1 min 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 31.11 ES:13C-2378-TCDO 31.54 1001 OA -O • I • . ; . . r . •, r ; r , , i r i . i , , . ; ; r , r „ r j min 28 00 28.25 28., 50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 CS-TCDD bl6may11d-5 v Z88 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 0 FiJ Lock Mass bl6may11d-5 28.15 28.3628.43 28.64 28.83 29.04 29.24 29.34 29.53 29.78 29.98 30.26 30.41 30.57 30.77 �o 85 30.00 30.25 30.50 30.75 31.00 31.25 CS:37CI-2378-TCDD 31.56 F1:Voltage SIR,EI+ 333.9339 3.056e+007 F1:Voltage SIR,EI+ 327.8847 6.080e+006 . . r . i . . •i r ; . min 31.50 31.75 32.00 32.25 32.50 F1:Voltage SIR,EI+ 31.11 31.23 31.39 31.47 31.74 31.85 32.1332.20 30 .824 9824 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 bThmay11 d•5 Smaoth(SG,1 x2) CS3_836.206J 1 blOmay11 d-5 8mooth(S0,1x2) CS3_S36.206J 2378•TCDD 31.58 2378•TCDD 31.56 F1:Vottago SIR,EI 319.8985 2.668e•006 min F1:Vottage SIR,EI• 321.8936 3.350e•006 min 26.25 26.50 26.75 27.00 27.25 27.50 27.75 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 6P1, Jo OZ6 a68d )))))) )))))))))))))))).).. ..... ........ )) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:1Default.prolCurvedblbl6may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-5, Date:16-May-2011, Time: 20:32:51, 1D: CS3_S36-206J, Submitter: , Task: 2378-TCDF bl6may11d-5 %L: 2378-TCDF F1:Voltage SIR,EI+ 30.96 303.9016 /1 2.728e+006 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDF bl6may11d-5 %-] 1 1 . . . . 1 . . r . 1 . . . . 1 . . 1 . T 1 . I . . . 1 . r . . I . . . I I . l i i I . I . r I . I . i I . . . 1 min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 2'9.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDF bl6may11d-5 0 . . . . I . . . I . . , I . 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 ES-TCDF bl6mayl 1 d-5 "0_- 8 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 Fi.Lock Mass b'lmay11 d-5 30.00 2378-TCDF F1:Voltage SIR,EI+ 30.96 305.8987 3.629e+006 ES:13C-2378-TCDF 30.95 F1:Voltage SIR,EI+ 315.9419 2.885e+007 i min 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES:13C-2378-TCDF 30.95 F1:Voltage SIR,EI+ 317.9389 3.656e+007 85 28 00 28.15 28.3628.43 28.64 28.83 29.04 29.24 29.34 29.53 29.78 29.98 30.26 0.41 30.57 30.77 ,.I.I.,,..II..Imin 31.23 31.39 31.47 31.74 31.85 31.11 F1:Voltage SIR,EI+ 32.1332.20 304.9824 2. 89e+006 I . . . . I . . . . I . . . I . . . . I . . I , , . . . I I I . I r . . . I . . . .1 min 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 Quantify Sample Summary Report MassLynx 4.1 SCN640 ### ICAL Summary ### Dataset: Y:(Default.prolCurvedblb16may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:12:40 Eastern Daylight Time Na c bl6may11 d-6 ID: S4 = 37-401L Da - : 1 'May-2011 Time: 21:22:53 User: JLJ Submitter: Task: Name Response Ion1Area Ion2Area RT RA RAFaiI? RRF MRRF %RSD IS# Heightl Noisel SN1 Height2 Noise2 SN2 M 1 2378-TCDF 1.808e6 7.916e5 1.016e6 30.96/9.78 NO 0.976 • 1.004 4.6 4 1.191e7 762 15630.5 1.550e7 1083 14318.8 bb 2 2378-TCDD 1.297e6 5.735e5 7.235e5 31.56.79 NO 1.070, 1.171 10.0 3 1.078e7 1233 8744.4 1.364e7 1452 9391.6 MM 3 ES:13C-2378-TCDD 3.030e6 1.333e6 1.697e6 31.54/.79 NO 1.035. 1.026 3.7 5 2.501e7 916 27285.9 3.206e7 1708 18776.5 bb 4 ES:13C-2378-TCDF 4.632e6 2.045e6 2.586e6 30.95' 0 79 NO 1.582. 1.577 2.3 5 3.021e7 1723 17528.8 3.850e7 1882 20459.9 bb 5 JS:13C-1234-TCDD 2.928e6 1.281e6 1.647e6 31.11 �78 NO 1.000- 1.000 0.0 5 2.082e7 916 22719.8 2.660e7 1708 15578.9 bb 6 CS:37C1-2378-TCDD 1.370e6 1.370e6 - 31.56/ - 1.170, 1.218 5.8 5 2.599e7 723 35926.5 - bb CS-i- b =_1, 1 60 6b6 Jo ZZI. abed i 00 i /04 I, 11-9_, ,a-31-)1 ))))))))))))))))))))))))))) ._ ) i),)))))) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:1Default.pro\Curvedblbl6may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-6, Date: 16-May-2011, Time: 21:22:53, ID: CS4_S37-401L, Submitter: , Task: 2378-TCDD bl6may11d-6 31.56 F1:Voltage SIR,El+ 319.8965 1.081 a+007 r , i . r . , I . r , , ' . . , , ' . , , , . . , + . , . , . . r . , ( , . , , . , ' . . , , . i , , 1 min 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDD bl6may11d-6 31.56 F1:Voltage SIR,EI+ 321.8936 1.368e+007 0 = . . . I . . , . , . . , . . . , . , . , r . , , . , . , . . , , . . . . I . . , I . . . . . . . . . . . . . . . . . . . . . . . . , , . , . . , , , . . . min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD bl6may11d-6 100- , r , , , I i , . . I r . . . I . . . , min 28.00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD bl6mayl 1 d-6 100 -0 , . , 28 00 28.25 CS-TCDD bl6may11d-6 1c y 31.11 31.11 ES:13C-2378-TCDD 31.54 ES:13C-2378-TCDD 31.54 F1:Voltage SIR,EI+ 331.9368 2.507e+007 F1:Voltage SIR,EI+ 333.9339 3.224e+007 :28.50 28.75 . r I , , r j . . . . . . . 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 CS:37CI-2378-TCDD 31.56 32.00 . . i min 32.25 32.50 Fl:Voltage SIR,EI+ 327.8847 2.604e+007 min /8 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 FiLock Mass bl6may11 d-6 88 28 00 28.69 28.81 28.9629.25 28.20 28.45 8.5829.20 28.25 F1:Voltage SIR.EI+ 29.75 29.93 30.75 31.05 31.34 31.42 31.6731.77 31.85 32.03 32.38 304 9824 024 29.48 29 63 0.04 30.29 30.49 30 82 31.24 min 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 b16may11(1.6 Smoolh(S0,1 x2) CS4_S37.401L %• 0 2378-TCDD 31.58 F1:Votiage SIR,E1+ 319.8955 1.091 a+007 bl6may11d-6 Smooth(S0,1x2) CS4_S37•401L 96- 6b 6 Jo bZ 6 abed 1 2378-TCDD 31.56 min Fi VotiageSIR,EI• 321.8936 1.368e+007 min 26.25 28.50 26.75 27.00 27.25 27.50 27.75 28.00 20.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ))))))))))))))))))))))))))))))))))))))))))) Quantify Sample Report ###TCDD TCDF Only ### MassLynx 4.1 SCN640 Dataset: Y:1Default.pro1Curvedblb16may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-6, Date: 16-May-2011, Time: 21:22:53, ID: CS4_S37-401L, Submitter: , Task: 2378-TCDF bl6maylld-6 2378-TCDF F1:Voltage SIR,EI+ 30.96 303.9016 Il 1.201e+007 0 I r r „ i t r i, c r r , r, r i r r, r( r . r r, r, r r r 1 r r r 1, r r r 1 r r r r r „ i „ r, i r r r, i min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDF bl6may11d-6 % o• 28 00 28.25 ES-TCDF bl6mayl ld-6 2378-TCDF Fi :Voltage SIR,EI+ 30.96 305.8987 /l 1.561e+007 r , i „ r r Ir r , r i „ r , . r , i r r r , r r , r i, , , i r „ r i r , r r r r r i r r, l „ r , i , r r r i r , r r i r r „ i „ r , 1 min 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES:13C-2378-TCDF 30.95 F1:Voltage SIR,EI+ 315.9419 3.039e+007 0 r , r r , , . , , , , , i, r r r i r r , r i r „ r r „ r i r r r , , , , r , r r r r r , r i , rr r r „ i „ , r „ , i r r r r r r , i r r , r min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDF bl6mayl ld-6 ES:13C-2378-TCDF F1:Voltage SIR,EI+ 30.95 317.9389 3.871e+007 r i, r,,, r r r r r r, I r r r, r r, r i „ r. i r r i „ r i r r c r i, r, , r, r i,,,, i, r r, i,., r, r r, i r r r min V8 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 N F..ock Mass b1anayl1d-6 F1:Voltage SIR,EI+ 30.75 31.34 31,42 31.77 31.85 32.03 32.38� 304.982440� 28.69 28.81 28.96 29.25 29.63 29.75 29.93 30.29 30.82 31.05 31.67 "�O 28.20 28.45 8.58 29.20 29.48 30.04 30.49 31.24 r, r r, r i min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 Quantify Sample Summary Report MassLynx 4.1 SCN640 ### ICAL Summary ### Dataset: Y:1Default.pro\Curvedblb16may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:10:32 Eastern Daylight Time Printed: Monday, October 31, 2011 14:12:40 Eastern Daylight Time Na . 16may11d-7 ID* CS5 37-401M D te: ay-2011 Ti e: :13:00 User: JLJ Submitter: Task: Name Response IonlArea Ion2Area RT RA RAFaiI7 RRF MRRF %RSD IS# Heightl Noisel SN1 Height2 Noise2 SN2 M 1 2378-TCDF 5.788e6 2.520e6 3.268e6 30.971 .77 NO 0.96 1 1.004 4.6 4 3.836e7 1269 30226.8 4.955e7 970 51086.4 bb 2 2378-TCDD 4.473e6 1.970e6 2.503e6 31.56,9.79 NO 1.099 • 1.171 10.0 3 3.702e7 843 43905.5 4.714e7 1060 44452.7 MM 3 ES:13C-2378-TCDD 2.036e6 8.957e5 1.140e6 31.54,9.79 NO 1.094• 1.026 3.7 5 1.604e7 983 16322.2 2.072e7 835 24808.1 bb 4 ES:13C-2378-TCDF 3.010e6 1.327e6 1.683e6 30.95( 0.79 NO . 1.617. 1.577 2.3 5 1.962e7 1072 18304.8 2.463e7 1075 22897.9 bb ..r- 5 JS:13C-1234-TCDD 1.861e6 8.211e5 1.040e6 31.114.79 NO 1.000. 1.000 0.0 5 1.271e7 983 12936.5 1.625e7 835 19462.4 bb 6 CS:37CI-2378-TCDD 4.671e6 4.671e6 - 31.56/ - 1.255, 1.218 5.8 5 8.776e7 1125 77979.3 - - bb 2!- 3.0(Oe.-t gOdi),,k 6t►L 10 9Z1. abed D •q� -Fyn to- 3►-/ Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only #1## Dataset: Y:(Default.prolCurvedblblfimaylld-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-7, Date: 16-May-2011, Time: 22:13:00, ID: CS5_S37-401M, Submitter: , Task: 2378-TCDD bl6may11d-7 F1:Voltage SIR,EI+ 31.56 319.8965 100 3.711e+007 -Q00 . „`, . , 1 , 1 . , , . , , 1 , , , . 1 , y min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDD bl6may11d-7 100 -�/ . 1 , 1 1 , , , 1 , 1 , , 1 . , . 1 , 1 , . . 1 . 1 , 1 , , min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 31.56 ES-TCDD bl6mayl 1d-7 31.11 ES:13C-2378-TCDD 31.54 0 0°1 „ , . , . , 1 . , 1 , , . , 1 , 1 , , 1� 1 ,, l , , 1 1 „ l , min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDD b 16may11 d-7 31.11 ES:13C-2378-TCDD 31.54 F1:Voltage SIR,EI+ 321.8936 4.726e+007 F1:Voltage SIR,E1+ 331.9368 1.607e+007 F1:Voltage SIR,EI+ 333.9339 2.077e+007 , min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 0 CS-TCDD bl6may11 d-7 1- CS:37CI-2378-TCDD 31.56 0 8 00 28.25 FiLock Mass bl6may11d-7 % I , F1:Voltage SIR,EI+ 327.8847 8.788e+007 1 . min 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 28.10 28.30 28.43 28.5128.74 28.79 28.89 29.1529.22 83 1.,.,1 28 00 28.25 28.50 28.75 29.00 29.43 29.58 29.80 30.1630.22 30.37 30.64 30.70 30.78 31.34 31.44 31.74 31.0631.20 F1:Voltage SIR,EI+ 31.87 32.05 32.30 304.9824 8. +006 m 29.25 29.50 29.75 30.001n 30.25 30.50 30.75 31 .00 31 .25 31 .50 31 .75 32.00 32.25 32.50 b1 bmay11 d•7 Smooth(SG,1x2) C85_537.401M 100 -0... .., .j. bl6may11d•7 Smooth(30,1x2) CS5_537-401141 100 -0 6v410 9ZL axed • 2378-TCDD 31.56 Ft :Voltage SIRE • 319.8965 3.711e•007 4=? tmin 2378-TCDD 31.56 1.1 F1:Voltape SIR,EI• 321.8930 4.726e•007 • 26.25 26.50 26.75 27.00 27.25 f 27.50 27.75 28.00 28 25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31 00 31.25 31.50 31.75 32.00 32.25 32.50 min ) )_) ) ) )_,) .) Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: Y:1Default.prolCurvedblbl6may11d-tetras.gld Last Altered: Monday, October 31, 2011 14:05:07 Eastern Daylight Time Printed: Monday, October 31, 2011 14:06:18 Eastern Daylight Time Name: bl6may11d-7, Date: 16-May-2011, Time: 22:13:00, ID: CS5 S37-401 M, Submitter: , Task: 2378-TCDF bl6may11 d-7 2378-TCDF F1:Voltage SIR,EI+ 30.97 303.9016 n 3.859e+007 0 . . i r r . r . . . . . . r , r , . I" , . r . min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 2378-TCDF bl6may11d-7 0' . i . . . . i . i , i r , . . , . . . . i i . r i . . , , ,i , i min 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 ES-TCDF bl6may11 d-7 2378-TCDF F1:Voltage SIR,E1+ 30.97 305.8987 4.984e+007 ES:13C-2378-TCDF 30.95 0 " . . i , r i . . , i . . . , i , ,• 28 00 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 F1:Voltage SIR,EI+ 315.9419 1.972e+007 ES-TCDF bl6may11d-7 ES:13C-2378-TCDF 30.95 i min F1:Voltage SIR,EI+ 317.9389 2.475e+007 % -.p�: a - . , . . , , . i . . , , , , , , . . , . , , . , , , . . . 1 min 1800 28.25 28.50 28.75 29.00 29.25 29.50 29.75' 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 N cD F1R...ock Mass bltnay11d-7 28.10 28.30 28.43 28.5128.74 28.79 28.89 29.15 29.22 29.43 29.58 29.80 83 , 28 00 30.1630.22 30.37 30.6430.70 30.78 31.0631.20 31.34 31.44 31.74 F1:Voltage SIR,EI+ . 3205 304.9824 31.87 32.30 1.98 +006 , . . , i . . . . ,• , . r , ,•, . r , . . , . . i , . . ,•i i , , r . , . min 28.25 28.50 28.75 29.00 29.25 29.50 29.75 30.00 30.25 30.50 30.75 31.00 31.25 31.50 31.75 32.00 32.25 32.50 614 io 0£ 6 a6ed Instrument: Data File b29octlla-1 b29octlla-2 b29octlla-3 b29octlla-4 b29octlla-5 b29octlla-6 b29octlla-7 b29octlla-8 b29octlla-9 b29octlla-10 b29octlla-11 b29octlla-12 b29octlla-13 b29octlla-14 b29octlla-15 b29octlla-16 b29octlla-17 SGS North America, Inc. HRMS2 Sample ID Retcon_S39 -59D 46213 46212 31102775001 31102775002 31102775003 31102775004 31102775005 31102775006 31102775007 31102775008 31102775009 31102775010 31102775011 31102775012 31102775013 Retcon_S39 -59D JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL JHL An alyst Acquisition Date/Time Inj.Vol 2011-10-29 18:44:55 1 uL 2011 -10-29 19:36:51 1 uL 2011 -10-29 20:32:14 1 uL 2011 -10-29 21:07:59 1 uL 2011 -10-29 21:44:39 1 uL 2011 -10-29 22:21:19 1 uL 2011 -10-29 22:58:05 1 uL 2011 -10-29 23:34:50 1 uL 2011 -10-30 00:11:31 1 uL 2011 -10-30 00:48:16 1 uL 2011 -10-30 01:25:02 1 uL 2011 -10-30 02:01:42 1 uL 2011 -10-30 02:38:27 1 uL 2011 -10-30 03:15:08 1 uL 2011 -10-30 03:51:49 1 uL 2011 -10-30 04:28:36 1 uL 2011-10-30 05:05:18 1 uL Iwc03\- Page 1 of 1 ))))))))))))))))))))))))))))))))) ))))))))))))))))))))))))))))))))))))))))))) Sample List Report MassLynx 4.1 SCN640 Sample List: Last Modified: Printed: C:1MassLynxlDefault.prolSampledblb29oct11 a.SPL Saturday, October 29, 2011 20:05:54 Eastern Daylight Time Saturday, October 29, 2011 20:05:59 Eastem Daylight Time File Name Bottle HRD(Batch) Lab Sample ID 1 b29oct11a-1 1 2 b29oct11 a-2 4 HRD1459 3 b29oct11a-3 5 HRD1459 4 b29oct11a-4 6 HRD1459 5 b29oct11a-5 7 HRD1459 6 b29oct11a-6 8 HRD1459 7 b29oct11a-7 9 HRD1459 8 b29oct11a-8 10 HR01459 9 b29oct11 a-9 11 HRD1459 10 b29oct11 a-10 12 HRD1459 11 b29oct11a-11 13 HRD1459 12 b29oct11 a-12 14 HRD1459 13 b29oct11a-13 15 HRD1459 14 b29oct11 a-14 16 HRD1459 15 b29oct11 a-15 17 HRD1459 16 b29oct11 a-16 18 HRD1459 17 b29oct11 a-17 1 -- 6i4 10 6£6 abed Retcon_539-59D 46213 46212 31102775001 31102775002 31102775003 31102775004 31102775005 31102775006 31102775007 31102775008 31102775009 31102775010 31102775011 31102775012 31102775013 Retcon_S39-59D Customer Sample ID OPR for HBN 14044 [HXX/1337J LMB for HBN 14044 [HXX/1337J Comp#1 Site 1 Bluegill Comp#2 Site 1 Flathead Catfish Comp#3 Site 1 Blue Catfish sm Comp#4 Site 1 Blue Catfish Ig Comp#5 Site 2 Bluegill Comp#6 Site 2 Flathead Catfish Comp#7 Site 2 Blue Catfish Comp#8 Site 2 Common Carp Comp#9 Site 3 Bluegill sm Comp#10 Site 3 Bluegill Ig Comp#11 Site 3 FlatheadCatfish Comp#12 Site 3 Blue Catfish Comp#13 Site 1 Blue Catfish Ig Page 1 of 2 Page Position (1, 1) Sample Type MS File Inlet File QC dioxins_db5ms dioxin_db5ms Analyte dioxins db5ms dioxin_db5ms Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins db5ms dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 Analyte dioxins_db5ms_dw2 dioxin_db5ms_dw2 QC dioxins db5ms dioxin_db5ms Experiment Calibration Report File: Printed: MassLynx 4.1 SCN640 Experiment: dioxins_db5ms.exp Refe ence: pfk.ref Function: 1 @ 200 (ppm) Saturday, October 29, 2011 18:39:5 Eastern Daylight Time M 292.9824 R 10917 M 342.9792 R 10728 I 41 I i l i E= �P I — -- _ - -- 11'04 6b 610 Z£ 6 96Bd M 304.9824 R 11159 M 318.9792 R 13017 M 354.9792 R 10122 M 366.9792 R 10869 r` Page 1 of 1 M 330.9792 R 10588 M 380.9760 R 11630 Z ))))))))))))))))))))))))))))))))))))))))))) Experiment Calibration Report MassLynx 4.1 SCN640 File: Experiment: dioxins_db5ms.exp Refer7e: pfk.ref Function: 2 @ 200 (ppm) Printed: Saturday, October 29, 2011 18:40:11 Eastern Daylight Time M 330.9792 R 11261 �N r 6.) M _ i. Dili 111. . 4111 ill M 380.9760 R 11626 / 614 Jo eel abed M 342.9792 R 11519 66. 146 1111, S;,I M 392.9760 R 11207 .64 Page 1 of 1 M 354.9792 R 11014 M 404.9760 R 11961 • M 366.9792 R 10822 IM 10' Ji M 416.9760 R 12197 r�. Experiment Calibration Report MassLynx 4.1 SCN640 File: Experiment: dioxins_db5ms.exp Ref ence: pfk.ref Function: 3 @ 200 (ppm) Printed: Saturday, October 29, 2011 18:40:36 astern Daylight Time M 366.9792 R 12689 M 416.9760 R 12373 6P 6 Jo PEI. abed M 380.9760 R 10681 Page 1 of 1 M 430.9728 R 11312 .ra• .1 1f. 1 M 392.9760 R 10917 )tiv 011 M 442.9728 R 11012 140 1/)i M 404.9760 R 12018 1)0 AR M 454.9728 R11112 ➢))➢)))))))➢))))))))))))))))))))))))))))))) Experiment Calibration Report MassLynx 4.1 SCN640 File: Experiment: dioxins_db5ms.exp Ref ence: pfk.ref Function: 4 © 200 (ppm) Printed: Saturday, October 29, 2011 18:42:3 Eastern Daylight Time M 404.9760 R 10967 M 454.9728 R 11905 6IL 10 9£6 abed Page 1 of 1 M 430.9728 R 11961 IIM 416.9760 R 11683 M 466.9728 R 12952 • M 442.9728 R 12693 Experiment Calibration Report MassLynx 4.1 SCN640 File: Experiment: dioxins_db5ms.exp Refer nce: pfk.ref Function: 5 @ 200 (ppm) Printed: Saturday, October 29, 2011 18:42:58 astern Daylight Time Page 1 of 1 M 430.9728 R 12256 M 480.9696 R 12820 M 442.9728 R 11792 2.9696 R 11994 1111 AI? 617l 10 9E6 abed M 454.9728 R 10778 M 504.9696 R 12195 M 466.9728 R 12016 1or iw liliiJ"y' M 516.9697 R 11061 )))))))))))))))))))))))))))))))))))))))) Resolution Check Report MassLynx 4.1 SCN640 Printed: Sunday, October 30, 2011 06:00:01 Eastern Daylight Time Page 1 of 4 M 292.9824 R 12261 M 342.9792 R 12196 6I'I Jo LEI abed M 304.9824 R 13111 M 354.9792 R 13459 11 1..-- , ,11.11 L_ __.`, i --1 {{ _ M 342.9792 R 11859 — - 1—--- L_. ,�---- LI 'I—L I _ �, ��1� - i 1441,11I ,�- — - M 318.9792 R 16080 - ----------- - 1- _____ (ri M 366.9792 R 13640 M 354.9792 R 13851 M 330.9792 R 11829 M 380.9760 R 12490 M 366.9792 R 13297 Resolution Check Report MassLynx 4.1 SCN640 Printed: Sunday, October 30, 2011 06:00: 1 Eastern Daylight Time Page 2 of 4 M 380.9760 R 12872 Ij ! II id H 41_ L _ . - - ,„ M 366.9792 R 12828 I It 1 � lilI - I-• -- f- ;i I tiril JI L .- .1 .�,rr t� - Ivy {li JI_., M416.9760 R 14631 1 IN IIII, I 1 1 th 1 6b 610 9£ I. a6ed M 392.9760 R 12627 � 1 I I ---I---- t—.--_ Li, 1 14i/ M 380.9760 R 11905 M 430.9728 R 12239 M 416.9760 R 14730 M 404.9760 R 12890 --—f--——t-- —- lj��'—i'rl'--I—•— M 404.9760 R 14426 1 I 1 1 1 ----t-- 1T—r-- w I ��' j - I-- - al 1 I I �'I 1 --L l I- .��. �-- —- Ij I _kph_ __:__ __1 v Ij , ... ... M 392.9760 R 14264 M 442.9728 R 13370 ))))))))))))))))))))))))))))))))))))))))))) Resolution Check Report MassLynx 4.1 SCN640 Printed: Sunday, October 30, 2011 06:00: Eastern Daylight Time Page 3 of 4 M 404.9760 R 14651 I Hilbf I ; I LI L ' I 140 I M 454.9728 R 13592 10 6116 10 M 442.9728 R 13899 r•� 61110 6£1 abed M 416.9760 R 15437 , I i : 1 I --1-- ;ih-; -t- - -- n I 1 [:-. _ _ __ _ ji i L I1I ijj itii. M 466.9728 R 16929 06 t: 60 M 454.9728 R 13321 I— -- — — I — -114 M 430.9728 R 14060 110, L — L— al --1 :41I M 480.9696 R 14893 • M 466.9728 R 15389 : 1- I 1 1 - L _ . �� ri t Lt..T M 442.9728 R 13670 106 1101 ---1- Y. M 430.9728 R 14285 M 480.9696 R 14244 Resolution Check Report / MassLynx 4.1 SCN640 Printed: Sunday, October 30, 2011 06:00:01 Eastern Daylight Time Page 4 of 4 M 492.9696 R 13232 ..—__,__ . - 1 _ -- ti `'I a� 1_--. II - __ , 6b610 OI' abed M 504.9696 R 13481 �r M 516.9697 R 16790 ����)3) -1)))) )))))))))))i)))))))))))))))))) ) ) ) ) ) ) 6171. Jo 141. abed b29octi 1a-1 Sb (1,1.00 ) 100- 0 26.40 26.58 1;\ 27.09 /1 I \ 26.96 Retcon_S39-59D 27.27 29-Oct-20111 18:44:55 1: Voltage SIR 16 Channels El+ 319.8965 6.06e5 1---._.-- . ,-- ---ij ----. .... __..-_. ..___ _ _ 26.60 26.80 27.00 27.20 27.40 27.60 27.80 28.00 28.20 _28.40 .. 28.31 Time Quantify Sample Summary Report MassLynx 4.1 SCN640 ### 8299 CCAL Summary ### Dataset✓✓: C:IMassLynx\Default.prolResults1b29oct1 l a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:10:27 PM Eastern Daylight Time Method: Untitled 31 Oct 2011 09:53:18 J Calibration: C:IMassLynADEFAULT.PRO1CurveDB1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-1 Date: 29-Oct-2011 Time: 18:44:55 ID: Retcon_S39-59D Instrument: User: JHL 1 2 3 4 5 6 7 :Name Response:. Ion1Area: Ion2Area : RT:A :RAFaiI?. pg/pL. %Der1,. RRF:. Height1.: Noisel:: SN1.: Height2 - Noise2 : SN2 • M :User RF :2378-TCDF 1.632e5 7.044e4 9.273e4 26.30.76 NO 9.762 -2.4 0.980 8.959e5 1172 764.3 1.177e6 1048 1123.9 bb 1.00 :2378-TCDD 1.072e5 4.643e4 6.078e4 27.27/0.76 NO 9.977 -0.2 1.169 5.841e5 786 743.5 7.499e5 972 771.6 MM 1.17 : ES:13C-2378-TCDD 9.173e5 4.106e5 5.066e5 27.24,,0,81 NO 86.074 -13.9 0.883 5.145e6 1418 3629.3 6.319e6 1258 5024.6 bb 1.03 : ES:13C-2378-TCDF 1.664e6 7.308e5 9.337e5 26.371)0.78 NO 101.617 1.6 1.602 9.124e6 966 9448.5 1.161e7 1302 8917.2 bb 1.58 •JS:13C-1234-TCDD 1.039e6 4.614e5 5.773e5 26.57.80 NO 100.000 0.0 1.000 5.810e6 1418 4098.3 7.312e6 1258 5813.9 bb 1.00 • CS:37CI-2378-TCDD 1.065e5 1.065e5 - 27.27' - - 8.415 -15.9 1.025 1.349e6 923 1462.2 - bb 1.22 • F1 Lock Mass 55328 6b L Jo Zb 6 abed Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:1MassLynx\Default.pro\Resultslb29oct11 a-1 tetras.gld Last Altered: 01-November-11 8:13:12 AM Eastern Daylight Time Printed: 01-November-11 8:16:14 AM Eastern Daylight Time Method: Untitled 31 Oct 2011 09:53:18 Calibration: C:1MassLynxIDEFAULT.PRO1Curve0B1mtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct'l1a-1, Date: 29-Oct-2011, Time: 18:44:55, ID: Retcon_S39-59D, Submitter: , Task: 2378-TCDD b29oct11a-1 2378-TCDD F1:Voltage SIR.EI+ 23.95 26.58 26.96 27.27 28.31 319.8965 6.915e+005 > > 1 ( S 1 1 ` r r i min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 2378-TCDD b29oct11a-1 2378-TCDD F1:Voltage SIR.EI+ 23.95 26.58 26.94 27.27 28.31 321.8936 % 5 , 25.48 /\ , '`f\ t \ A8.424e+00 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 2'7.5 28.0 28.5 29.0 29.5 30.0 ES-TCDD b29oct11a-1 ES:13C-2378-TCDD F1:Voltage SIR.EI+ 26.57 27.24 331.9368 5.867e+006 1 1/.1.,,�• ; �• , min 20.0 20.0 20.5 21i.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 ES-TCDD b29oct11 a-1 ES:13C-2378-TCDD 26.55 27.24 ,, .,,,� �..� ,,�1 �,, ..1min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 F1:Voltage SIR,EI+ 333.9339 7.378e+006 CS-TCDD b2ioct11a-1 CS:37C1-2378-TCDD F1:Voltage SIR,EI+ 27.27 327.8847 Gt► _ A 1.392e+006 t7` i , , , , , , , . , , , , 1 min 0.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 co F1 Lock Mass b29octlla-1 F1:Voltage SIR,EI+ 22.04 24.13 25.97 304.9824 % 1 22.37 22.75 23.33 23.89 24.31 24.89 24.9725.48 25.79 26.20 27.04 27.35 27.81 27.93 28.57 3.319e+006 27 - - __.._. . min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 929ot111:-1 Smootn(S3.1x2) 520v111a•1 SrnoathiSO 1i21 22.25 6I1-Jotiti1-a6ed 22.50 22 75 23 03 23 25 23 50 23 75 23 95 1 23 95 24 00 24 25 24.50 24'75 25.00 25.40 25 25 25.50 25 75 28 00 25 25 26 50 28.58 26.58 27 09 2696 2709 28.94 2575 2700 2378-TCOD 27.27 44737.42 9 72 pghl 732.53 2378-TCDO 27.27 59172.55 764.39 F1:vatage SlR,EI• 319 6465 6915e•005 28 31 J Ft:Ve33g? 0IR.0 )21 8436 203f 8424e•005 i 27 25 27 50 27.75 28.00 28.25 min 28.50 Quantify Sample Report ###TCDD TCDF Only ### MassLynx 4.1 SCN640 Dataset: C:1MassLynx\Default.prolResults1b29oct1l a-1 tetras.gld Last Altered: 01-November-11 8:13:12 AM Eastern Daylight Time Printed: 01-November-11 8:16:14 AM Eastern Daylight Time Name: b29oct11a-1, Date: 29-Oct-2011, Time: 18:44:55, ID: Retcon_S39-59D, Submitter: , Task: 2378-TCDF b29oct11a-1 2378-TCDF Fi:Voltage SIR,EI+ 22.34 26.39 303.9016 o j i 28.44 1.057e+006 To; � 25.50 1` ,. 3 ,�.� ,.,.� �.,;, ,,, ` �., , , ,min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 2378-TCDF b29oct11a-1 2378-TCDF F1:Voltage SIR,EI+ 22.34 26.39 305.8987 111 ,; 28.44 1.259e+006 25.50 I 1 2,.., . ,r , 1min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 ES-TCDF b29oct11 a-1 ES:13C-2378-TCDF F1:Voltage SIR,EI+ 26.37 315.9419 9.252e+006 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 ES-TCDF b29oct11 a-1 ES:13C-2378-TCDF F1:Voltage SIR,EI+ 26.35 317.9389 1.169e+007 min 7420.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 oi FELock Mass b29oct11a-1 F1:Voltage SIR,EI+ 22.04 304.9824 3.319e+006 22.37 22.75 23.33 23 89 24.13 24 31 24.89 24.9725.48 25.79 25.97 26.20 27.04 27.35 27.81..27.93 _ 28.57 27 . , , min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 ova Quantify Sample Summary Report MassLynx 4.1 SCN640 ### 8290 C YAL Summary### Dataset: C:1MassLynxlDefault.pro\Resultslb29oct11 a-1 tetras.gld Last Altered: 31-October-11 5:03:18 PM Eastern Daylight Time Printed: 31-October-11 5:10:45 PM Eastern Daylight Time Method: Untitled 31 Oct 2011 09:53:18 Calibration: C:IMassLynxIDEFAULT.PROICurveDBlmtetras-051611d_new.cdb 31 Oct 2011 10:04:21 Name: b29oct11a-17/ Date: 30-Oct-2011 Time: 05:05:18 / ID: Retcon_S39-59D Instrument: User: JHL 1 2 3 4 5 6 7 :Name :2378-TCDF :2378-TCDD : ES:13C-2378-TCDD : ES:13c-2378-TCDF . JS:13C-1234-TCDD • CS:37CI-2378-TCOD :F1 Lock Mass J Response:. IonlArea• Ion2Area . RT• RA •RAFai1?- pg/µL- %Dev. RRF:. Heightl. Noisel.: SN1•: Height2 - Noise2 • SN2 - M ; User RF 1.271e5 5.603e4 7.107e4 26.334.79 NO 10.066 0.7 1.011 7.038e5 942 746.9 9.468e5 1237 765.4 bb 1.00 9.038e4 3.989e4 5.048e4 27.22.1.79 NO 9.753 -2.5 1.142 4.800e5 783 613.1 6.460e5 2118 305.0 MM 1.17 7.911e5 3.457e5 4.454e5 27.21/9.78 NO 94.097 -5.9 0.965 4.459e6 1118 3989.9 5.791e6 1226 4721.5 bb 1.03 1.257e6 5.578e5 6.997e5 26.32�.80 NO 97.308 -2.7 1.535 7.470e6 1605 4654.8 9.288e6 1266 7337.4 bb 1.58 8.194e5 3.692e5 4.502e5 26.5e 0.82 NO 100.000 0.0 1.000 4.854e6 1118 4342.5 5.962e6 1226 4861.5 bb 1.00 9.465e4 9.465e4 - 27.22/ - - 9.484 -5.2 1.155 1.231e6 833 1477.6 - bb 1.22 39571 6t410 9171. eBed Quantify Sample Report MassLynx 4.1 SCN640 ###TCDD TCDF Only ### Dataset: C:1MassLynx\Default.pro\Resultslb29oct11 a-1 tetras.gld Last Altered: 01-November-11 8:13:12 AM Eastern Daylight Time Printed: 01-November-11 8:16:14 AM Eastern Daylight Time Name: b29oct11a-17, Date: 30-Oct-2011, Time: 05:05:18, ID: Retcon_S39-59D, Submitter: , Task: 2378-TCDD b29oct11 a-17 23.92 26.55 27.04 2378-TCDD 28.26 �6.91 27.22 f 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 F1:Voltage SIR.EI+ 319.8965 5.871e+005 2378-TCDD b29oct11a-17 2378-TCDD F1:Voltage SIR,EI+ 23.90 26.91 27.22 28.26 321.8936 26.53 7.780e+005 °70 A 25.41 (\.... 1 . i min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 ES-TCDD b29oct11a-17 ES:13C-2378-TCDD F1:Voltage SIR,EI+ 26.52 27.21 331.9368 i\ 4.907e+006 1 i _ 1 _ i 1 _ i . . _ , _ . . i . . r , T _ I , . . . . , , 1 min) 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 ES-TCDD b29oct11a-17 ES:13C-2378-TCDD 26.52 27.21 %-i 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 F1:Voltage SIR,EI+ 333.9339 6.019e+006 .. . ....,. ..,....min 28.0 28.5 29.0 29.5 30.0 CS-TCDD b29oct11a-17 CS:37C1-2378-TCDD F1:Voltage SIR,EI+ 27.22 327.8847 IT r 1 1.267e+006 ,,- �.-; ,, r �.,. ', min ;20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 .A F1'Lock Mass b29oct11a-17 F1:Voltage SIR,EI+ 22.04 304.9824 24.87 25.66 26.02 28.34 2.413e+006 %] 1 22.4923.00.23.13 ` 23.56 24.0824.17 24.61^� 25.48 26.73 _27.09 27.49 28.08.28.182 .__.� 25 , , � , . 1 , f , 1 min 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 6t4Jo8b696ed 679of.t11 a-17 Smoot1;S0.14) 0290 Dia-17 Smco040.1.22) 2392 23 93 J 25 41 22.25 22 50 22.75 23 00 23.25 23 50 23 75 24.00 24.25 24.50 24.75 25 00 25.25 25.50 25.75 28.00 26 25 20 26 55 26.53 26.91 ti-----"-- -----ice 27.n04 • 2378-TCDD 27 77 41707.66 1015 09MU1- 623 60 2378-TCDD 27.22 51912.99 309.56 27.04 75 2700 21.25 7750 2775 29 26 29-26 F1:VoDa9a SIR,EI• 319 8955 5 871 e•035 71:Vota;o COUP, 321 6936 7 7800.005 3)))))))�)���))))))���� j ))))) I. )._. i))))))))))))))) )__ ) )) _))))))))))))))) ) Quantify Sample Report MassLynx 4.1 SCN640 ####TCDD TCDF Only ### Dataset: C:1MassLynx\Default.pro\Resultslb29oct1la-ltetras.gld Last Altered: 01-November-11 8:13:12 AM Eastern Daylight Time Printed: 01-November-11 8:16:14 AM Eastern Daylight Time Name: b29oct11a-17, Date: 30-Oct-2011, Time: 05:05:18, ID: Retcon_S39-59D, Submitter: , Task: 2378-TCDF b29oct11 a-17 %- 3 20.0 r I r (. I- r. . r.. r, r . r r, 20.5 21.0 21.5 •22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 �n 2378-TCDF b29oct11 a-17 2 20.0 20.5 ES-TCDF b29oct11a-17 22.31 2378-TCDF F1:Voltage 303SI 90116 !\, 26.33 28.41 ssi � 25.46 t 22.31 2378-TCDF F1:Voltage SIR,EI+ 305.8987 26.33 28.39 1.236e+006 , ,fi \ 25.46 1\ A , , 21.0 21.5 ..., 22.0 22.5 23.0 23.5 24.0 24.5 25.0 26.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30, min .0 ES:13C-2378-TCDF F1:Voltage SIR,EI+ 26.32 315.9419 /,_ t 7.551e+006 0' r 20.0 20.5 21r.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0min ES-TCDF b29oct11a-17 ES:13C-2378-TCDF 26.32 30.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0• in m F1 t.ock Mass b2Act11 a-17 22.04 F1:Voltage SIR,EI+ 304.9824 2.413e+006 o/Q 25 24.87 25.66 26.02 22.4923.00.23.13 23.56 24.0824.17 24.61 4 25.48 26.73 27.09 27.49 28.08 28.18 28.34 F1:Voltage SIR.EI+ 317.9389 9.384e+006 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 in