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Home My WebLink AboutNC0000272_2014 Dioxin Fish Tissue Report_20150202 evergreerill. C Office packaging 175 Moin Stree • Canton, NC 26716 NMM#14-15 February 2,2015 CERTIFIED MAIL RETURN RECEIPT REQUESTED Landon Davidson 7099 3220 0007 0371 4644 Regional Supervisor Division of Water Resources Asheville Regional Office North Carolina Department of Environment and Natural Resources 2090 US Highway 70 Swannanoa,North Carolina 28778 Subject: 2014 Dioxin in Fish Tissue Report NPDES NC 0000272 Blue Ridge Paper Products Inc dba Evergreen Packaging Canton Mill Dear Mr. Davidson— Enclosed is the subject report with results of August 2014 dioxin in fish tissue for Waterville Lake as required by special condition I.A.(9.)of the May 2010 NPDES permit. In January 2007,the NC Department of Health and Human Services(DHHS) lifted the fish advisory for common carp in Waterville Lake and requested two additional years of fish tissue sampling and surveillance,which were completed in 2009. The May 2010 NPDES Permit for the Blue Ridge Canton Mill requires three(3)additional years of fish tissue sampling and surveillance in the summer of 2011,2013 and 2014. This report completes the 2014 surveillance. Very truly Nick McCracken EHS&S Water Supervisor 828-646-2874 nick.mccrackenna eveipack.com Enclosure—2014 Dioxin in Fish Tissue Report fresh by design / LIST OF TABLES Number Title Page 2-1 Pigeon River sampling station information . . . . . . . . . 3 4-1 Fish collection techniques and level of effort . . . . . . . . 8 4-2 Summary of fish composites collected at two stations in Waterville Lake, August 2014 . . . . . . . . . . . . . . . . . 9 6-1 Summary of Pigeon River fish tissue analysis results—2014 . . . . 17 6-2 Toxicity equivalence factors for CDD/F congeners . . . . . . . . 18 6-3 Summary of CDD/F isomer analyses, toxicity equivalent factors, and toxicity equivalent values for the 2014 Waterville Lake fish tissue composites . . . . . . . . . . . . . . . . 20 6-4 Blue Ridge Paper Canton Mill fish fillet tissue analysis results 2005—2014 . . . . . . . . . . . . . . . . 22 ii LIST OF FIGURES Number Title Page ES-1 TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2014 (Stations 4A and 4B) . . . . . . . . . . . . . . . . . v ES-2 TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2014 (Stations 4A and 4B) . . . . . . . . . . . . . . . . . . vi 2-1 Historical sampling station locations on the Pigeon River . 4 2-2 Sampling Stations 4A and 4B on the Pigeon River . . 5 4-1 a Lengths of fish collected from Waterville Lake for tissue analyses, 2004-2014 . . . . . . . . . . . . . . . . . . . . . . . 11 4-1b Weights of fish collected from Waterville Lake for tissue analyses,2004-2014 . . . . . . . . . . . . . . . . . . . . . 12 6-1 TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2014(Stations 4A and 4B) . . . . . . . . . . . 27 6-2 TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2014(Stations 4A and 4B) . . . . . . . . . . . . . . . . . . 28 iii EXECUTIVE SUMMARY The Blue Ridge Paper Products Inc., dba Evergreen Packaging, Canton Mill contracted the Department of Forestry, Wildlife and Fisheries of the University of Tennessee, Knoxville(UTK) to collect fish tissue samples for dioxin analysis from the Pigeon River during the summer of 2014 in accordance with NPDES permit conditions. UTK field personnel followed the March 2006 revision (Wilson 2006) to the December 2001 Fish Tissue Sampling Plan prepared by EA Engineering, Science and Technology, Inc., (EA Engineering 2001a) of Chicago, Illinois. UTK prepared this 2014 fish tissue sampling report using the revised protocol of 2006. Bottom feeding species (channel catfish and common carp) were collected in August 2014 from two locations (Stations 4A and 4B) in the Pigeon River (Waterville Lake) and analyzed for 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD), 2,3,7,8-tetrachlorodibenzofirran (TCDF), and other CDD and CDF congeners. Concentrations of 2,3,7,8-TCDD and 2,3,7,8-TCDF in channel catfish fillets were below detection level (DL) in Stations 4A and 4B (4A DL = 0.98 ppt for 2,3,7,8-TCDD and 0.98 ppt for 2,3,7,8-TCDF; 4B DL = 1.0 ppt for both 2,3,7,8-TCDD and 2,3,7,8-TCDF). In common carp, 2,3,7,8-TCDD was 1.5 ppt in fillet composites collected at Station 4A and was 2.1 ppt at Station 4B. For 2,3,7,8-TCDF the concentrations in common carp fillets were 2.5 ppt at Station 4A and 2.7 ppt at Station 4B. The concentration of 2,3,7,8-TCDF in the common carp whole body sample collected at Station 4A was 0.96 ppt and 1.4 ppt for 2,3,7,8-TCDD and 2,3,7,8- TCDF respectively(Table 6-1). The mean weights of common carp collected from Stations 4A and 4B (4.436 kg, Station 4A; 6.013 kg, Station B) were lower than those collected in 2007 (6.490 kg, Station 4A; 6.552 kg, Station 413),but consistent with weights of common carp collected in other previous years (2013, 5.052 kg, Station 4A; 4.364 kg, Station B; 2011, Station 4A, 4.144, Station 4B, 5.542; 2009, 4.303 kg, Station 4A; 4.848 kg, Station B; 2008, 4.727, Station 4A, 4.067, Station 413; 2006, 4.505 kg, Station 4A, 5.637 kg, Station 413; 2005, 3.857 kg - Station 4A, 4.695 kg - Station 413; 2004, 3.750 kg - Station 4A, 3.900 kg - Station 413; 1999-2003, 3.193 kg, Station 4A, 5.042 kg, Station 4B). Lipid concentrations in common carp fillets in 2014 were 15-17%. In January 2007, the NC DHHS lifted the fish advisory for common carp in Waterville Lake and requested two additional years of fish tissue sampling and surveillance,which was completed in 2009. The May 2010 NPDES Permit for the Blue Ridge Canton Mill required three (3) additional years of fish tissue sampling and surveillance. During the sampling years between 2008-2013 the concentrations in fish tissue fillets were below the NC DHHS 4 ppt TEQ action level for fish consumption advisory. In 2014, TEQ values were below detection for channel catfish for both sampling Stations; however, in common carp, TEQ values were 9.619 ppt for Station 4A and 2.928 for Station 4B. The TEQ results for common carp fillets in 2014 and 2007 could be anomalies, or could indicate that some fish are present in the population with relatively higher TEQ values. Lipid concentrations in common carp fillets were higher in 2014 (15% Station 4A, 17% Station 4B) than in 2013 (4.2-8.7%), and the higher concentration of lipids in 2014 could explain some of the elevation in TEQ values observed in 2014 for common carp. iv Figure ES-1. TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2014 (Stations 4A and 413) 70 60 t Station 4A 50 ` c ; i --t- Station 4B O 40 • a � 30 ' W a � C 20 ' 10 ' b 0 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 TIME b) TCDD concentrations at Station 4B were not detected, therefore, the values plotted represent the detection limit for those samples. The detection limit for 2,3,7,8-TCDD was elevated in the 2007 carp fillet for Station 4B because of a 10-fold dilution of the sample which was required to overcome sample matrix effects (high lipid concentration) during analysis. Consequently, reporting the detection limit for this sample can give a misleading impression that the concentration of 2,3,7,8-TCDD increased that year. v Figure ES-2. TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2014 (Stations 4A and 4B) 4.00 3.50 --*--Station 4A --4- Station 4B C 3.00 ._ 2.50 S. Y 2.00 c c 0 1.50 G F ' `� a 1.00 ` b 0.50 A a a ,� % : `. o.00 ----�I,_ _�_--- ---->•- a a a a b b 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 TIME a) TCDD concentrations were not detected at Station 4A, therefore the values plotted represent the detection limit for the sample. b) TCDD concentrations were not detected at Station 4B, therefore the values plotted represent the detection limit for the sample. c) The 2011 TCDD result for catfish fillets in 2011 at Station 4B was above detection limit at 1.7 ppt . The TEQ for the 2011 Station 4B catfish fillets remained below the 4 ppt action level of the NC DHHS. vi 1.INTRODUCTION The Blue Ridge Paper Products Inc., dba Evergreen Packaging, Canton Mill contracted the Department of Forestry, Wildlife and Fisheries of the University of Tennessee, Knoxville (UTK) to collect fish tissue samples for dioxin analysis from the Pigeon River during the summer of 2014 in accordance with NPDES permit conditions. UTK field personnel followed the March 2006 revision (Wilson 2006) to the December 2001 Fish Tissue Sampling Plan prepared by EA Engineering, Science and Technology, Inc. (EA Engineering 2001a) of Chicago, Illinois. This report details the results of a study conducted during August 2014 to determine the concentrations of 2,3,7,8-TCDD (dioxin) and 2,3,7,8-TCDF (furan) in bottom-feeding fish collected from the Pigeon River near Canton, North Carolina. The report follows the template developed by EA Engineering for prior reporting years. The 2014 fish tissue study is number 23 in a series of fish tissue surveys designed and conducted to be responsive to the requirements of A.(9.)Dioxin Monitoring Special Condition in Blue Ridge Paper's current NPDES permit for the Canton Mill (Permit No. NC0000272). Sampling locations, selection of target species, sampling methods, and sample preparation/preservation techniques are in accordance with the study plan. The approved study methods and scope detailed herein generally follow those used since 1990 (EA 1990, 1991, 1992, 1993a, 1993b, 1994, 1995, 1996, 1997, 1998, 2000, 2001b, 2001c, 2003, 2004, Wilson 2006, Henry and Wilson 2007, 2008, 2009, 2011, 2013). However, selected project details were modified to be responsive to the suggestions/recommendations of the North Carolina Department of Environment and Natural Resources (NCDENR), the Tennessee Wildlife Resources Agency, U.S. EPA Region IV, and the North Carolina Department of Health and Human Services (NC DHHS). The principal change in the program was that the collection and analysis of sportfish composite samples have not been required since 2000. In 2006,project details were modified again to be responsive to the North Carolina Division of Water Quality (NC DWQ) and these modifications were adhered to in the present investigation (i.e.,2014). The principal changes to the program in 2006 were the elimination of sampling of the main stem of the Pigeon River beginning in 2006 and the collection of at least one whole body bottom feeder sample from Waterville Lake (Stations 4A or 4B). These changes are included in more detail in Appendix D. The 2014 study was conducted during August, during which time biologists from UTK collected and prepared fish tissue samples from the two Waterville Lake sampling locations (Stations 4A and 4B) on the Pigeon River. Details relevant to the location of Pigeon River sampling stations and fish tissue sampling objectives follow in Sections 2 and 3, respectively. Fish collection techniques and level of effort are detailed in Section 4; methods of sample preparation and shipment are presented in Section 5. Analytical results are summarized in Section 6 and references are provided in Section 7. 1 2. SAMPLING LOCATIONS In accordance with the study plan (Wilson 2006) that was implemented in 2006, 2007, and 2008 (Henry and Wilson 2007, 2008, 2009, 2011, 2013), fish were collected from two sampling locations on the Pigeon River. For this sampling period two sites (Stations 4A and 4B) were sampled. Detailed sampling station information for both sites is provided in Table 2-1 and Figure 2-2. Monitoring Stations 4A and 4B are located in Waterville Lake at RM 41.5 and 39.0, respectively (Figure 2-1). Station 4A is located approximately 21.8 RM downstream from the Mill outfall, near the Messer Branch-Pigeon River confluence (Figure 2-2). Monitoring Station 4B is in the vicinity of the Wilkins Creek-Pigeon River confluence, approximately 24.3 RM downstream from the Canton Mill outfall (Figure 2-2). Appropriate habitats were sampled within each study reach in an effort to collect the desired complement of fishes. Fish sampling was conducted in the vicinity of each location described above; however, the distance or effort at each station depended on how difficult it was to collect fish at that station. The Station 4B study area consisted of an approximate 1.0 RM reach of Waterville Lake located from the dam to the confluence of Wilkins Creek. Sampling at Stations 4A and 4B included electrofishing and setting of trot lines near the shore along both the left and right banks of Waterville Lake. Reservoir water level in 2014 was approximately at full pool and was similar to water levels in 2006. Stations 4A and 4B sample areas covered approximately the same surface area as water levels in 2004-2006. 2 Table 2-1. Pigeon River sampling station information. Station Station Location and Site Description/Habitat Type Fish Community Number RM Distance from Outfall 4A 41.5 Upper Waterville Lake Characterized by deep-water lentic There are no dominant species. Bluegill,black (21.8 RM downstream from habitat with bedrock covered by crappie, flathead and channel catfish, small mouth the Canton Mill outfall) loose,unconsolidated bottom bass, and largemouth bass are common. Common sediments. Maximum depth carp are present but not common. sampled approximately 3 m. 4B 39.0 Lower Waterville Lake Characterized by deep-water lentic .There are no dominant species. Bluegill,black from the dam to confluence habitat,bedrock, and soft crappie, flathead and channel catfish, small mouth with Wilkins Creek(24.3 sediments. Maximum depth bass,and largemouth bass are common. Common RM downstream from the sampled approximately 12 in. Very carp are present but not common. Canton Mill outfall) steep banks with little cover. 3 Figure 2-1. Historical sampling station locations on the Pigeon River; fish tissues were collected from two sites (4A and 4B) for dioxin analyses in 2014. More precise geographical locations of each site are presented in Figure 2-2. tic aj TN Nwbvq TN Nw Mowr wNan wn TBprrEE R!R Hyry NOTE: R1wrmBw vi mtlSoon Sonoma b .or Mp) triWry moWP OhMnn M pmNhroo. G FM arq Bents SNnpiny 8letlon ■hRnn Don NSWW Ws rbbndbn 4B 4A a.r RMgib Iwa) + wv AftnnC AWSS �q py RW burro Do* 13711 aan pnnSon,moo. aon," non Aoo»cya. www. IM.q Iaw.Yn (mil ��sr ViSynonon +P AUS � G�nMr�NC wow. ; uA.NC 04 IMF 4 I \ Grassy Krwh �uy Op v WAIFRV Weacs oam r'i i4 "� DW 9Y Q ItLC L9E!( " � F 9 4' B U 17 ly — 4' '1347 n, 1347, Figure 2-2. Sampling Stations 4A(indicated by A) and 4B (indicated by B) on the Pigeon River. 5 3. SAMPLING OBJECTIVES In accordance with the study plan (Wilson 2006), the goal of the fish collection effort was to collect one composite bottom feeder fillet sample at both sampling stations 4A and 4B. Each composite consisted of 3 to 5 similarly-sized (shortest specimen within 75% of the length of the longest) adult individuals of the target species. Common carp (Cyprtnus carpio) and channel catfish (Ictalurus punctatus) were the targeted species at sites 4A and 4B. In addition to fillet samples,one whole body common carp was collected from Station 4A. In summary fish were collected as follows: • Bottom feeder fillet composite--one sample at both locations • Catfish fillet composite—one sample at both locations • Common carp whole body composite—one sample from Station 4A Every reasonable effort was made to collect the desired size, species and/or number of fish; however, the outcome of the sampling effort each year is dependent on physical river conditions and the natural diversity and abundance of target fishes at each sampling location. The 2014 Pigeon River collections yielded the desired species at each location. In addition, the number of specimens collected made it possible to composite individuals of similar weight and length (with larger/adult specimens preferred), and the 75% rule was met for all samples. 6 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT Sampling was conducted during 6 August 2014. Notes were recorded at each sampling station with regard to the type of sampling gear, level of effort (time), and habitat(Tables 2-1 and 4-1). All fish submitted for tissue analysis (including whole body specimen) were measured to the nearest millimeter (total length) and weighed to the nearest gram (wet weight). These data are summarized in Table 4-2. For 2014, the mean total length of carp was 711 mm and fish ranged from 660-759 mm. In 2013, the mean total length for carp was 683 mm and fish ranged from 630-722 mm. Previously, fish collections were conducted by EA Engineering, Science, and Technology (see References), and the mean for carp total length was 618 mm for fish submitted for analysis between 1993 and 2003. The field investigators were equipped with an array of collecting gear, which enabled sampling of all habitats regardless of river conditions. U.S. EPA recommends active methods of fish collection in the Sampling Guidance Manual (Versar 1984), such as electrofishing, trawling, angling, or seining. These are preferred over passive methods (e.g., gill nets, trap nets, trot lines) because samples are collected from more definable areas (Versar 1984). A boat electrofishing unit(pulsed direct current) was used at both stations. The boat electrofisher was equipped with a Smith Root Type VIA electrofisher, and powered by a 240-volt, 5000-watt generator. Electrofishing techniques followed those described in the National Dioxin Study(Versar 1984). Fish collection techniques and level of effort (time) expended at both stations are summarized in Table 4-1. Total study effort for collection of fish at Stations 4A/413 was 1.8 hours electrofishing and trot lines were used for 48 hours. 7 Table 4-1. Fish collection techni ues and level of effort. Station Sampling Sampling Number I RM Dates Techniques Level of Effort Comments 4A 41.5 6 Aug 2014 Boat An approximate 1.0 RM reach of river was sampled and the entire electrofishing 0.8 hours area was electrofished. Trot line yielded capture of 11 channel Trot lines(one) 16 hours total catfish. 4B 39.0 6 Aug 2014 Boat 1 hours An approximate 1.4 RM reach was sampled by electrofishing. Trot electrofishing Hue yielded capture of 12 channel catfish and one largemouth bass. Trot lines(two) 33 hours total 8 Table 4-2. Summary of fish composites collected at two stations in Waterville Lake,August 2014. A composite sample was generated for each site and each composite consisted of the right-side fillet(R) from all five fish collected from the site. A whole body(WB) composite from a single common carp was obtained from site 4A. Total Total Length wholebody Date Station Species (mm) (9) Sample type Composite 6 Aug 14 4A Channel catfish 445 785 Fillet R (RM 41.5)Channel catfish 416 565 Fillet R Channel catfish 485 915 Fillet R Channel catfish 473 870 Fillet R Channel catfish 500 1135 Fillet R MEAN 464 854 4A Common carp 715 5580 Fillet R (RM 41.5)Common carp 680 4260 Fillet R Common carp 740 4760 Fillet R Common carp 660 3860 Fillet R Common carp 673 3720 Fillet R MEAN 694 4436 6 Aug 14 4B Channel catfish 537 1435 Fillet R (RM 39.0)Channel catfish 460 1030 Fillet R Channel catfish 487 915 Fillet R Channel catfish 463 815 Fillet R Channel catfish 452 775 Fillet R MEAN 480 994 6 Aug 14 4B Common carp 750 6100 Fillet R (RM 39.0)Common carp 756 6040 Fillet R Common carp 759 5900 Fillet R MEAN 755 6013 6 Aug 14 4A Common carp 664 4580 Whole body WB (RM 39.0) 9 Target species were collected at both sampling stations in 2014. Common carp, the target bottom feeder at Stations 4A, and 4B, were collected (and prepared for fillet and/or whole body analysis) at those stations. Because of the physiography of the Waterville Lake Stations 4A and 4B, trot lines were used in addition to the electrofishing gear for the collection of bottom feeding species. All trot lines were pulled and examined on a regular basis to reduce stress or specimen mortality. All specimens submitted for analysis appeared healthy and in good condition. Lengths and weights for each fish making up each composite are provided in Table 4-2. Bottom feeder fillet composites samples consisted of five channel catfish and five common carp at Station 4A, and five channel catfish and three common carp at Station 4B. A single bottom feeder whole body common carp from Station 4A was submitted for analysis (Table 4-2). All 18 composite fillets submitted for analysis in 2014 met the US EPA Region IV recommendation (Cunningham 1990) that the smallest specimen in each composite be equal to or greater than 75% of the total length of the largest specimen in that composite (Tables 4-2 and 6-4). Figure 4-la-b illustrates the length and weight distribution of fish collected for tissue analysis from Waterville Lake since 2004. The size distribution of catfish remained similar between 2004 and 2014. The size of the carp taken for whole body tissue analysis from Station 4A in 2014 was similar to size of whole body fish collected in previous years. 10 Max, Min and Mean of Lengths taken from Fish Tissue Samples 2004-2014 800 750 _ 700 ' E 650 ' t ■ ■ ■ E s 600 c 550 J 500 44 # 450 400 COf6 CO vm. 19 vm- f0 f0oU - U UU - oUmUU@� - o-� 0 mU mUmUU � �U�UmUU 4 Tr 3 ¢ �U coo moU UUm vC � � m �r 2004 2005 2006 2007 2008 2009 2011 2013 2014 Figure 4-la. Lengths of fish collected from Waterville Lake for tissue analyses, years 2004-2014. 11 Max, Min and Mean of Weights taken from Fish 9000 Tissue Samples 2004-2014 8000 7000 6000 5000 4000 ' 3000 2000 1000 T If O CO 075 �. N �� f�O �N �� f�O �.N �� N � N �� U U U �Ucv 0 C U �Uca0UmUmoUmU � O m CU U Ur U Ur U UL U Us U Ut U U U UrUUUUsUU CO UUs �r¢vm v¢vm v¢vm v¢vm v¢vm v¢vm v¢vm v¢vm v¢vn v v v �r v . v v v v v v v v v v v v 2004 2005 2006 2007 2008 2009 2011 2013 2014 Figure 4-lb. Weights of fish collected from Waterville Lake for tissue analyses, years 2004-2014. 12 5. SAMPLE PREPARATION All fish tissue samples were prepared in accordance with U.S. EPA Region IV recommendations (Cunningham 1990) as described in EA (2001a). To prevent cross-contamination between sampling stations, all sampling equipment likely to come into contact with the fish was rinsed with isopropanol and acetone then rinsed extensively with water filtered by reverse osmosis between stations. Specimens collected at each station were sorted by size and species, and target species were identified. The objective was to obtain a 3- to 5-fish composite sample for channel catfish and common carp at both 4A and 4B sample locations, as well as a common carp whole body sample from either station in Waterville Lake which met the species and size objectives discussed in Section 3. From the target fishes collected, specimens of similar length and weight were selected for each composite sample. All specimens retained were immediately placed on ice for later processing. For each fish retained, length and weight data were recorded on the appropriate fisheries data sheet. Following identification of target organisms, selection of composite samples, and collection of length/weight data, each specimen was prepared for shipment and analysis. Bottom feeder fillet samples consisted of epaxial muscle tissue and skin from one side of the fish. Bottom feeder whole body samples consisted of the entire fish. Fillet samples were prepared by removing scales (or removing the skin from catfishes) and then making an incision behind the opercula(on both sides of the fish) from the base of the spine (behind the skull) to just below the pectoral fin. Care was taken to cut through the epaxial muscle without puncturing the rib cage or gut lining. A second incision was made along the length of the spine to the caudal fin on both sides of the fish. The epaxial muscle was then gently cut away from the rib cage to obtain a fillet. In this fashion, all flesh and skin was obtained from head to tail on both sides of the fish. Fillet knives were solvent rinsed (hexane and acetone) between fish from different stations. Each composite sample was wrapped in aluminum foil (dull side toward sample), labeled, and placed on ice in the field. All individual specimens (fillets) composing a single composite sample were placed in a water- tight plastic bag labeled with the station name, sample number, and species identification. A chain-of-custody form was filled out for each cooler of samples submitted for analysis. Each form included composite specific information and instructions. All chain-of-custody forms had the following information: • sample location and station identification, • sampling team initials, • date of collection, • species name, • sample type (i.e., fillet or whole body) A copy of the chain-of-custody record is provided in Appendix A. 13 All samples were frozen solid prior to shipment to the analytical laboratory. The frozen samples were packed on dry ice and shipped via overnight delivery, where they arrived on 8/28/14 at TestAmerica West Sacramento. The back-up fillets were retained in a freezer at the Canton Mill until laboratory analytical results for the right side fillets were received and verified. 14 6. ANALYTICAL RESULTS The fish tissue samples were received in one shipment (828/14) at TestAmerica under chain-of- custody protocol. Once received at the laboratory, samples were compared to the chain-of- custody record to verify the content of each shipping container. Each individual fish or fillet within a composite was homogenized separately by TestAmerica personnel, and equal aliquots of the homogenate from each fish were removed to constitute the composite. Dioxin and furan analyses were performed using high resolution Gas Chromatography/Mass Spectrometry (GC/MS) as required by the U.S. EPA. Laboratory documentation of all chemical extractions and analyses are provided in Appendix B. All chemical analyses of the samples were conducted using EPA Method 8290 (U.S. EPA 1994) as specified in the Fish Tissue Sampling Study Plan (EA 2001 a). The quality of the analytical results was assured through reproducible calibration and testing of the extractions and GC/MS systems. A laboratory method blank was prepared along with each batch of samples. The laboratory also used precision and recovery standards for determination of initial and ongoing precision and accuracy. Laboratory reports for all 2014 Pigeon River fish tissue dioxin, furan, and lipid content analyses are provided in Appendix B. Each laboratory analysis report form lists the concentration of 2,3,7,8-tetrachlorodibenzo-p4oxin (TCDD), 2,3,7,8,-tetrachlorodibenzofuran (TCDF), and all other CDD/CDF congeners. Results of the dioxin, furan, and lipid content analyses are summarized in Table 6-1. Detection limits are reported parenthetically on a sample-specific basis. Only fillet results are discussed below because North Carolina Department of Health and Human Services(NC DHHS) considers only fillet results when issuing health advisories. Concentrations of 2,3,7,8-TCDD and 2,3,7,8-TCDF in channel catfish fillets were below detection limit(DL)in Station 4A(DL=0.98 ppt and 0.98 ppt respectively) and were also below DL at Station 4B (DL= 1.0 for both 2,3,7,8-TCDD and 2,3,7,8-TCDF (Table 6-1)). In common carp, the 2,3,7,8-TCDD concentration was 1.5 ppt at Station 4A and 2.1 ppt in fillet composites collected at Station 4B. For 2,3,7,8-TCDF,the concentrations in common carp fillets were 2.5 at Station 4A and 2.7 at Station 4B. The concentration of 2,3,7,8-TCDF in the common carp whole body sample collected at Station 4A was 0.96 and 1.4 for 2,3,7,8-TCDD and 2,3,7,8-TCDF respectively(Table 6-1). Examination of the data in Table 6-1 indicates that all fish collected during this study had body burdens well below the FDA dioxin health advisory level (25 ppt) for fish tissue [as established and presented in FDA (1981, 1983) and Cordle(1983)]. The NC DHHS recommends an average dioxin toxicity equivalent(TEQ) level of 3 ppt or less in fish tissue fillets. The NC DHHS issues dioxin fish tissue advisories at an average toxicity equivalent of 4 ppt or greater(e-mail correspondence with Dr. Luanne Williams 18 January 2005). The TEQ of each chlorodibenzodioxin and furan(CDD/F) isomer is based on the toxicity equivalence factor(TEF) (WHO 2005 and Table 6-2) as described in the 2001 Study Plan (EA 2001b). The TEQ value is calculated assuming additivity of effects for the individual congeners of dioxin and furans and is expressed as an"equivalent amount of 2,3,7,8-TCDD"(NC DEHNR 1991). The measured concentration of each CDD/F isomer,when multiplied by its appropriate TEF,yields the TEQ of that isomer(the toxic concentration of that isomer relative to the toxicity of 2,3,7,8-TCDD). In cases where concentrations were below the level of detection, a value of 15 zero was used in the TEQ calculation. Based on an advisory by the World Health Organization (e-mail correspondence with Dr. Luanne Williams 20 September 2006),new TER were developed in 2005 by the WHO and are now being used instead of the 1997 TEFs. 16 Table 6-1. Summary of the Pigeon River fish tissue analysis results 2014. Station Percent Number Sample ID Composite/Sample Type 2,3,7,8-TCDD(e) 2,3,7,8-TCDF(a) Lipid 4A SITE 4A channel catfish 5 fillet samples ND(DL=0.98) ND(DL=0.98) 9.3 SrM 4A common carp 5 fillet samples 1.5 2.5 15 SITE 4A common carp 1 whole body sample 0.96 1.4 12 4B S1TE 4B channel catfish 5 fillet sample ND(DL= 1.0) ND(DL= 1.0) 4.4 SITE 4B common carp 3 fillet samples 2.1 2.7 17 (a)Units=ppt(parts per trillion)or pg/g(picogram/gram) (ND)Not detected,concentrations below the instrument detection limit(DL). 17 Table 6-2. Toxicity equivalence factors for CDD/F congeners. DIOXIN DIBENZOFURAN Isomeriel TEF(b) TEF(b) 2,3,7,8-TCDD 1 2,3,7,8-TCDF 0.1 1,2,3,7,8-PeCDD 1 1,2,3,7,8-PeCDF 0.03 2,3,4,7,8-PeCDF 0.3 1,2,3,4,7,8-HxCDD 0.1 1,2,3,4,7,8-HxCDF 0.1 1,2,3,7,8,9-HxCDD 0.1 1,2,3,7,8,9-HxCDF 0.1 1,2,3,6,7,8-HxCDD 0.1 1,2,3,6,7,8-HxCDF 0.1 2,3,4,6,7,8-HxCDF 0.1 1,2,3,4,6,7,8-HpCDD 0.01 1,2,3,4,6,7,8-HpCDF 0.01 1,2,3,4,7,8,9-HpCDF 0.01 OCDD 0.0003 OCDF 0.0003 (a) In each homologous group,the relative toxicity factor for the congeners not listed is 1/100 of the value listed for the other congeners in that homologous group. (b) TEF=toxic equivalence factor=relative toxicity assigned. 18 The TEQ calculation and summarization schemes presented in Table 6-3 followed methods used by NC DHHS (NC DEHNR 1991). All channel catfish analyzed bad TCDD and TCDF congeners below detection resulting in a TEQ of 0.000. The TEQ for common carp fillets was 9.619 ppt at Station 4A [value was above the NC DHHS advisory limit (4 ppt)], and 2.928 ppt at Station 4B. The values reported in years 2005-2011 for channel catfish are consistent with the results for 2013. Common carp TEQ results in 2007 were higher at Station 4A (13.44 ppt) and lower in Station 4B (1.263 ppt) than observed in 2014, and both 2007 and 2014 were higher than those observed in other years (2005- 2006, 2008-2009; 2009, Station 4A, 1.560 ppt; Station 4B, 1.496 ppt). The results for common carp in 2014 and 2007 could be anomalies, or could indicate that some (low frequency) fish are present in the population with relatively higher TEQ values. Whole body carp collected at Station 4A had TEQ of 2.017 ppt in 2014, whereas the 2013 whole body sample for common carp collected at Station 4B had a TEQ result of 3.196 ppt. Table 64 illustrates 2,3,7,8 TCDD concentrations in common carp fillet samples collected in 2005, 2006, 2007, 2008, 2009, 2011, 2013, 2014 and results for previous years (1990-2004) are in Appendix C. Between 1990 and 2006, 2,3,7,8-TCDD concentrations in carp fillets declined dramatically(94-99 %) at all sampling stations (Table 6-4, Appendix C, Figure 6-1). The 2014 mean weight of common carp collected from Station 4A was 4.436 kg (Station 4B, 6.013 kg) and consistent with previous years. In 2013, the mean weights of common carp collected from Stations 4A (5.052 kg) and Station 4B (4.364 kg) in 2013, were lower than those collected in 2007 (6.490 kg- Station 4A; 6.552 kg -, Station 4B),but consistent with weights of common carp collected in previous years (2008, 4.727- Station 4A, 4.067 Station 4B; 2006, 4.505 kg- Station 4A, 5.637 kg- Station 4B; 2005, 3.857 kg- Station 4A, 4.695 kg- Station 4B; 2004, 3.750 kg- Station 4A, 3.900 kg- Station 4B; 1999-2003, 3.193 kg- Station 4A, 5.042 kg- Station 4B). Lipid concentrations in common carp fillets were higher in 2014 (15% Station 4A, 17% Station 4B) than in 2013 (4.2-8.79/o), and the higher concentration of lipids in 2014 could explain some of the elevation in TEQ values observed in 2014 for common carp. 19 Table 6-3. Summary of CDD/F isomer analyses, toxicity equivalent factors, and toxicity equivalent values for the 2014 Waterville Lake fish tissue composites. STATION 4A Channel catfish fillet Common carp fillet Common carp whole bodv CDD/F congeners !W2 Resultsla) TEOro) Results(a) TEO b) Results"' TEOro> Dibenzodioxin 2,3,7,8-TCDD 1.0 ND 0.000 1.5 1.5 0.96d 0.96 1,2,3,7,8-PeCDD 1.0 ND 0.000 3.5d 3.5 ND 0.000 1,2,3,4,7,8-HxCDD 0.1 ND 0.000 4.0d 0.4 ND 0.000 1,2,3,6,7,8-HxCDD 0.1 ND 0.000 7.3 0.73 4.6d 0.46 1,2,3,7,8,9-HxCDD 0.1 ND 0.000 3.0d 0.3 ND 0.000 1,2,3,4,6,7,8-HpCDD 0.01 ND 0.000 21 0.21 16 0.160 OCDD 0.0003 ND 0.000 47 0.014 36 0.011 Dibenzofuran 2,3,7,8-TCDF 0.1 ND 0.000 2.5 0.25 1.4 0.14 1,2,3,7,8-PeCDF 0.03 ND 0.000 2.7' 0.081 ND 0.000 2,3,4,7,8-PeCDF 0.3 ND 0.000 3.6d 1.08 ND 0.000 1,2,3,4,7,8-HxCDF 0.1 ND 0.000 3.8d 0.38 ND 0.000 1,2,3,6,7,8-HxCDF 0.1 ND 0.000 4.9 0.49 2.6d 0.26 2,3,4,6,7,8-HxCDF 0.1 ND 0.000 3.5d 0.35 ND 0.000 1,2,3,7,8,9-HxCDF 0.1 ND 0.000 2.6d 0.26 ND 0.000 1,2,3,4,6,7,8-HpCDF 0.01 ND 0.000 4.5d` 0.045 2.6d` 0.026 1,2,3,4,7,8,9-HpCDF 0.01 ND 0.000 2.8' 0.028 ND 0.000 OCDF 0.0003 ND 0.000 6.4d 0.002 ND 0.000 Total TEQ 0.000 9.619 2.017 (a)Units=ppt(parts per trillion)or pg/g(picogram per gram) (b)Dioxin Equivalent Concentration using methodology from U.S.EPA(1989) (c)Toxicity Equivalent Factors from World Health Organization(WHO 2005) (d)Estimated result. Result is less than reporting limit,but greater than or equal to the method detection limit,concentration is approximate. (e)The reported result is the estimated maximum possible concentration of this analyte,quantitated using the theoretical ion ratio.The measured ion ratio does not meet qualitative identification criteria and indicates a possible interference. (f)The reported quantitation limit has been raised due to an exhibited elevated noise or matrix interference. 20 Table 6-3 (cont). Summary of CDD/F isomer analyses, toxicity equivalent factors, and toxicity equivalent values for the 2014 Waterville Lake fish tissue composites. STATION 4B Channel catfish fillet Common cart)fillet CDD/F congeners TEF101 Results(a) TEOroI Results() TEOro> Dibenzodioxin 2,3,7,8-TCDD 1.0 ND 0.000 2.1 2.1 1,2,3,7,8-PeCDD 1.0 ND 0.000 ND 0.000 1,2,3,4,7,8-HxCDD 0.1 ND 0.000 ND 0.000 1,2,3,6,7,8-HxCDD 0.1 ND 0.000 3.8° 0.38 1,2,3,7,8,9-HxCDD 0.1 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDD 0.01 ND 0.000 14 0.14 OCDD 0.0003 ND 0.000 34 0.010 Dibenzofuran 2,3,7,8-TCDF 0.1 ND 0.000 2.7 0.27 1,2,3,7,8-PeCDF 0.03 ND 0.000 NDr 0.000 2,3,4,7,8-PeCDF 0.3 ND 0.000 NDr 0.000 1,2,3,4,7,8-HxCDF 0.1 ND 0.000 ND 0.000 1,2,3,6,7,8-HxCDF 0.1 ND 0.000 ND 0.000 2,3,4,6,7,8-HxCDF 0.1 ND 0.000 ND 0.000 1,2,3,7,8,9-HxCDF 0.1 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDF 0.01 ND 0.000 2.8' 0.028 1,2,3,4,7,8,9-HpCDF 0.01 ND 0.000 ND 0.000 OCDF 0.0003 ND 0.000 ND 0.000 Total TEQ 0.000 2.928 (a)Units=ppt(parts per trillion)or pg/g(picogram per gram) (b)Dioxin Equivalent Concentration using methodology from U.S.EPA(1989) (c)Toxicity Equivalent Factors from World Health Organization(WHO 2005) (d)Estimated result. Result is less than reporting limit,but greater than or equal to the method detection limit,concentration is approximate. (e)The reported result is the estimated maximum possible concentration of this analyte,quantitated using the theoretical ion ratio.The measured ion ratio does not meet qualitative identification criteria and indicates a possible interference. (t)The reported quantitation limit has been raised due to an exhibited elevated noise or matrix interference. 21 Table 6-4. Blue Ridge Paper Canton Mill fish fillet tissue analysis results,2005—2014 2005 Results(d) 2006 Results(e) Number Length Range Number Length Range Station Species of fish (mm) 2,3,7,8-TC1313t�bl Station Species of fish (ab) P (mm) 2,3,7,8-TCDD I Black redhorse 5 359-384 ND(0.35) 4A Common carp 3 635-692 0.64(`) RM 64.5 RM 41.5 Channel catfish 5 430-500 ND(0.37) 2 Common carp 4 595-650 ND(0.45) 4B Common carp 3 650-745 0.73(`) RM 59.0 Channel catfish 3 443-460 ND(0.29) RM 39.0 Channel catfish 4 510-590 0.77(=) 3 Common carp 4 605-630 ND(0.46) RM 52.3 4A Common carp 3 601-665 1.3 RM 41.5 Channel catfish 5 464-508 ND(0.36) 4B Common carp 4 595-736 2.8 RM 39.0 Channel catfish 5 513-603 0.76(`) 5 Black redhorse 4 440-501 ND(0.41) RM 19.0 Total fish filleted= 37 Total fish filleted= 15 (a)Dioxin analyses conducted by TestAmerica(formerly Severn Trent Laboratories). (b)Units=ppt(parts per trillion)or pg/g(picogram/gram) (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August and September (e)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 23 Table 6-4 (cont). Blue Ridge Paper Canton Mill fish fillet tissue analysis results, 2005—2014 2007 Results(d) 2008 Results(e) Number Length Range Number Length Range Station Species of fish (mm) 2,3,7,8-TCDDt4bi Station Species of fish (mm) 2,3,7,8-TCDD(4b) 4A Common carp 4 680-775 6.4 4A Common carp 3 653-686 1.2 RM 41.5 Channel catfish 4 490-593 0.57(`) RM 41.5 Channel catfish 5 475-525 ND(0.29) 413 Common carp 5 672-762 ND(6.9) 4B Common carp 3 630-665 ND(0.36) RM 39.0 Channel catfish 5 505-670 0.67(`) RM 39.0 Channel catfish 5 459-595 ND(0.34) Total fish filleted= 18 Total fish filleted= 16 (a)Dioxin analyses conducted by TestAmerica(formerly Severn Trent Laboratories). (b)Units=ppt(parts per trillion)or pg/g(picogram/gram) (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August and September (c)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 24 Table 6-4 (cont). Blue Ridge Paper Canton Mill fish fillet tissue analysis results, 2005—2014 2009 Results(d) 2011 Results(e) Number Length Range Number Length Range Station Species of fish (min) 2,3,7,8-TCDD('b) Station Species of fish (mm) 2,3,7,8-TCDD(°'b) 4A Commoncarp 5 620-698 1.1 4A Common carp 5 625-710 0.83` RM 41.5 Channel catfish 3 493-578 0.52t`i RM 41.5 Channel catfish 5 435478 ND(0.24) 413 Common carp 5 647-696 0.93t`l 413 Common carp 5 625-740 1.1 RM 39.0 Channel catfish 5 467-574 ND(0.43) RM 39.0 Channel catfish 5 466-550 1.7 Total fish filleted= 18 Total fish filleted= 20 (a)Dioxin analyses conducted by TestAmerica(formerly Severn Trent Laboratories). (b)Units=ppt(parts per trillion)or pg/g(picogram/gram) (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August and September (e)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 25 Table 6-4 (cont). Blue Ridge Paper Canton Mill fish fillet tissue analysis results,2005—2014 2013 Results(d) Number Length Range Station Species offish (mm) 2,3,7,8-TCDD($h) 4A Common carp 5 631-722 1.8 RM 41.5 Channel catfish 5 391-511 ND(0.48) 4B Common carp 5 630-697 0.70t`l RM 39.0 Channel catfish 5 445-537 ND(0.49) Total fish filleted= 20 (a)Dioxin analyses conducted by TestAmerica(formerly Severn Trent Laboratories). (b)Units=ppt(parts per trillion)or.pg/g(picogram/grem) (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 26 Table 6-4 (cont). Blue Ridge Paper Canton Mill fish fillet tissue analysis results, 2005—2014 2014 Results(d) Number Length Range Station Species of fish (mm) 2,3,7,8-TCDD(Nb) 4A Common carp 5 660-740 1.5 RM 41.5 Channel catfish 5 416-500 ND(0.96) 4B Common carp 3 750-759 2.1 RM 39.0 Channel catfish 5 452-537 ND(1.0) Total fish filleted= 18 (a)Dioxin analyses conducted by TestAmerica(formerly Severn Trent Laboratories). (b)Units=ppt(parts per trillion)or pg/g(picogram/grem) (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 27 Figure 6-1. TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990-2014 (Stations 4A and 4B) 70 60 -♦—Station 4A SO � � � c ; --t- Station 4B 40 o. ` m 30 CL C ` G 20 ` G � V H � r 10 0 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 TIME b) TCDD concentrations at Station 4B were not detected, therefore, the values plotted represent the detection limit for those samples. The detection limit for 2,3,7,8-TCDD was elevated in the 2007 carp fillet for Station 4B because of a 10-fold dilution of the sample which was required to overcome sample matrix effects (high lipid concentration) during analysis. Consequently, reporting the detection limit for this sample can give a misleading impression that the concentration of 2,3,7,8-TCDD increased that year 28 Figure 6-2. TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2014 (Stations 4A and 413) 4.00 3.50 *--Station 4A --l- Station 4B e 3.00 0 2.50 2.00 a 1.50 A,. ~ 1.00 a b ' .� a b 0.50 A, aa a " b �._ b ----� a a a a b b 0.00 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 TIME a) TCDD concentrations were not detected at Station 4A, therefore the values plotted represent the detection limit for the sample. b) TCDD concentrations were not detected at Station 4B, therefore the values plotted represent the detection limit for the sample. c) The 2011 TCDD result for catfish fillets in 2011 at Station 4B was above detection limit at 1.7 ppt . The TEQ for the 2011 Station 4B catfish fillets remained below the 4 ppt action level of the NC DHHS. 29 7. REFERENCES Cordle, F. 1983. Use of epidemiology in the regulation of dioxins in the food supply, in Accidental Exposure to Dioxins: Human Health Aspects (F. Coulston and F. Pocchiara, eds.),pp 245-256. Academic Press,New York. Cunningham,W.R. 1990. Letter to Paul Wiegand. 30 January. EA Engineering, Science, and Technology Inc. 1990. Study Plan for the Monitoring of Dioxin in Fish Tissue. EA Report No. 11370.01,prepared for Champion International Corporation, Canton,North Carolina. EA Engineering, Science, and Technology Inc. 1991. Results of the 1990 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.02, prepared for Champion International Corporation, Canton,North Carolina. EA Engineering, Science, and Technology Inc. 1992. Results of the 1991 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.03, prepared for Champion International Corporation, Canton,North Carolina. EA Engineering, Science, and Technology Inc. 1993a. Results of the 1992 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.05,prepared for Champion International Corporation, Canton,North Carolina. April. EA Engineering, Science, and Technology Inc. 1993b. Results of the 1993 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.06, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1994. Results of the 1994 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.07, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1995. Results of the 1995 Dioxin Monitoring in Fish Tissue. EA Report No. 13043.01, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1996. Results of the 1996 Dioxin Monitoring in Fish Tissue. EA Report No. 13176.01, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1997. Results of the 1997 Dioxin Monitoring in Fish Tissue. EA Report No. 13353.01, prepared for Champion International Corporation, Canton,North Carolina. November. 30 EA Engineering, Science, and Technology Inc. 1998. Results of the 1998 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2000. Results of the 1999 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01, prepared for Champion International Corporation, Canton,North Carolina. January. EA Engineering, Science, and Technology Inc. 2001a. Study Plan for Pigeon River Dioxin Monitoring in Fish tissue. Prepared for Blue Ridge Paper Products Inc., Canton, North Carolina. November. EA Engineering, Science, and Technology Inc. 2001b. Results of the 2000 Dioxin Monitoring in Fish Tissue. EA Report No. 13745.01, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2001c. Results of the 2001 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.01, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2003. Results of the 2002 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.02, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2004. Results of the 2003 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.03, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. January. Food and Drug Administration. 1981. FDA advises Great Lakes States to monitor dioxin- contaminated fish. FDA Talk Paper dated 28 August, in Food Drug Cosmetic Law Reports,paragraph 41, 321. Commerce Clearing House, Inc. 8 September. Food and Drug Administration. 1983. Statement by Stanford A. Miller, Director, Bureau of Foods, FDA before the Subcommittee on Natural Resources, Agriculture Research and Environment, U.S. House of Representatives. 30 June. Henry, T.B., and J.L. Wilson. 2006. Results of 2005 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc., Canton Mill, Canton,North Carolina. January 2006. Henry, T.B., and J.L. Wilson. 2006. Results of 2006 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc., Canton Mill, Canton,North Carolina. December 2006. Henry,T.B., and J. L. Wilson. 2008. Results of 2007 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc., Canton Mill, Canton,North Carolina. April 2008. 31 Henry,T.B., and J. L. Wilson. 2008. Results of 2008 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc., Canton Mill, Canton,North Carolina. November 2008. Henry, T.B., and J. L.Wilson. 2009. Results of 2009 Dioxin Monitoring in Fish Tissue.Final Report to Blue Ridge Paper Products, Inc., dba Evergreen Packaging. December 2009. 29 pp- Henry, T.B., and J. L.Wilson. 2011. Results of 2011 Dioxin Monitoring in Fish Tissue. Final Report to Blue Ridge Paper Products, Inc., dba Evergreen Packaging. December 2011. 29 PP. Henry, T.B., and J. L. Wilson. 2013. Results of 2013 Dioxin Monitoring in Fish Tissue. Final Report to Blue Ridge Paper Products, Inc., dba Evergreen Packaging. December 2011. 29 pp. North Carolina Department of Environment, Health, and Natural Resources. 1991. Fish Tissue Dioxin levels in North Carolina: 1990 update. Division of Environmental Management, Water Quality Section. U.S. Environmental Protection Agency (U.S. EPA). 1994. Analytical procedures and Quality Assurance for Multimedia Analysis of Polychlorinated Dibenzo-para-dioxins and Polychlorinated Dibenzofurans by High-Resolution Gas Chromatography/High-Resolution Mass Spectrometry(Method 8290). U.S. Environmental Protection Agency (U.S. EPA). 1989. Interim Procedures for Estimating Risk Associated with Exposures to Mixtures of Chlorinated Dibenzo-p-dioxins and Dibenzofurans (CDDs and CDFs) and 1989 Update Report No. EPA/625/3-89/016, U.S. EPA, Risk Assessment Forum, Washington,D.C. Versar, Inc. 1984. Sampling Guidance Manual for the National Dioxin Study. U.S. Environmental Protection Agency. EPA Contract 68-01-6160. Work Order Number 8.7. Office of Water Regulations and Standards, Monitoring and Data Support Division, Washington, D.C. Final Draft. July. Wilson, J.L. 2006. Study plan revision: Dioxin monitoring in fish tissue, Waterville Lake. Prepared for Blue Ridge Paper Products, Inc. Canton Mill, Canton, North Carolina. March 2006. World Health Organization (WHO). 1997. Exposure and Human Health Reassessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) and Related Compounds: Part 11: Health Assessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) and Related Compounds. 32 APPENDIX A: CHAIN OF CUSTODY FORM APPENDIX B: TESTAMERICA WEST SACRAMENTO APPENDIX C: BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS 1990-2004 APPENDIX D: 2006 REVISIONS TO DIOXIN MONITORING PLAN 33 APPENDIX A CHAIN OF CUSTODY FORM 34 Custody ■ A4 THE LEADER IN ENVIRONMENTAL TESTING PMJOaAbfmww r : •_ • • u ` IAl! ' i Q S&qmb D.ft.and 0vwrp&r qtit, .t...� 7 ••117��■■■■I.\I.l■■■■■■I.l■■IJ■■■■■■■■ + r J ■■■■■■■■■■■■■■■■■■■■■■■■■ .a. -_■■■■■■■■■■■■■■■■■■■■■■■■■ ■■■■■■■■■■■■■■■■■■■■■■■■ , , _.; ■■■■■cL■■■■■■c�■■I-■■■■■■■■r t c ■■■■r�r�■■■■■■■■■■■■■■■■■■ ' PPIAA.i, �■�■■■■■■■■■■■■■■■■■■■■■■■■■ ■■■■■■■■■■■■■■■■■■■■■■■■■■■■ ■■■■■■■■■■■■■■■■■■■■■■■■■■■■■ ■ , ■ El .... ♦. APPENDIX B TESTAMERICA WEST SACRAMENTO ANALYTICAL REPORT 35 TestAmedca THE LEADER IN ENVIRONMENTAL TESTING _ ANALYTICAL REPORT Job Niliriber. 320=9127A Job Description:Tissue For. Evergreen Packageing.FKABlue Ridge Paper PO BOX 1546 Canton,NC 28716 Attention: Nick McCracken jw Ali = . a0MM Jill Kellmann., Manager of Project.Management U0 Riverside Parkway, West Sacramento, CA,;95605 (910A74-4402 jill.kellmann@testomericainc;com 1,6/0612014 Revision; 1 TestAmerlm Laboratories,Ina TeslAmerim Sacramento 880 Rivemide Parkway.West Sddamento,CA 95605 Tel(916)373-5600 Fax(916)372-1059 s wlestamerimlrmmm Page 1 of 934 10/06/2014 Table of Contents Cover Title Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Data Summaries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 Definitions . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . 4 CaseNarrative . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Detection Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Client Sample Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 Default Detection Limits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Isotope Dilution Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 qC Sample Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 QCAssociation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 Chronicle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . _ . . . 19 Certifieation Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . I . . . . . . . 21 Method Summary.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 Sample Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 Manual Integration Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24 Reagent Traceability. . . . . . . . . . . . : . . . . . : . . . . . : . . . . . . . . . . . . . . . . . . . . 29 COAs. . . .. . .. .. :. . :.... . .. . .. . . . . . . . : . . .. ... . . . . . . .. .. . . . .. . .. . . .. .. . . ... 43 Organic Sample Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 240 Dioxin . . . . . . . . . . . . . . . . . . . . . . . . . . _ . . _ . . . . . . . . . . 240 Method 8290.. . . . . .... .. .. . ... .. .. .. . . . . . . . .. . .. . . . . . .. . . .. .. .. . .... . . .. 240 Method 8290'Q.0 Summary.............................................I................ 241 Method 8290 Sample Data...................................::.:..............:...:..... 246 Standards Data..:.................................................................... 456 Method 8290ICAL Data....................::...................................... 456 Method 6290 Resolution Data.................................................:..... 625 Method 8290-CCAL Data........................................................... 633 Page 2 of 934 10/06/2014 Table of Contents RawDG Data............................................................................. 756 Method 8290 Tune Data..............:............:.......1....::................... 756 Method 8298 Blank Data,:............................................................ 812 Method 8290 LCS(LCSD Data.. ....................................:.::....::...:. 843 Method 8290 Run Logs.....:.......:..........................:.:..:................... 871 Method 8290 Prep.Date.................................................................... 875 Inorganic Sample Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 919 General Ch@mistry Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . 919 Gen Chem Cover Page. .. .. .. . . ..... . .. . . .. . . .. . . . . . . .. . . . 920 Gen Chem Sample Data. . .. . . . .. .... . .. . ... . . . .. .. . ... .. . . .. . .. . . . . . . ..... . 921 . GenChem MDL. . .. . . . . . ..... ... . . . . .. . . . . . . ... . .. . . . . . . . . ... . .. . . . . ... .. • 926 Gen Chem Preparation Lo 928 9• Gen Chem Ahalysi6 Run Log.... . . .. . . . . . . . . . ... ... . . . . . . .. . .. ... . . . . .. . . . . 920 Gen Chem Prep Data. . . . ... .. .. . . . . . . .. . .. . ... . . . . .. . . . . .. . . ... . : . .. . . . . : 930 Shipping;and Receiving Documents . . . . . . . . . . . . . . . . . . . . . . . . . . . 932 Client Chain of Custody . . . . . . . . . . . . . . . . . 933 Sample Receipt Checklist. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ... . . . 934 Page 3 of 934 10/06/2014 Definitions/Glossary Client:Evergreen Padcageing FKAB1ue Ridge Paper TestAmerica Jab 1D:32"127-1 ProjecUSite:'Tissue. Qualifiers _. Dioxin Qualifier Qrnillier Description J Resuh Is less_than ihe;RL but Ipeare_r,tlhan or equal.to t1heMDL end the wncentretion N,an appro>omata value, q The repotted result is the estimated madmurn possible concentration of this enatyte,,quantllated using tre theorotical bn ratio.The measuredton rebo does not meet quafdative Identification cdtenend a indieetes a possible imerieheaoe: G The reported quantitation rimd has been raised due to an e>dubited elevated noise or monx interference ' isotope 1JUA n analyze exceeds contrgt tiinits I Ion R260_au64c limits,value is E RC. Glossary Abbravlation These commonly used abbreviation may or may not be Present in this report q Listed under the'D'column to designate that)he result is reported an a dry weight basis .AR Percerd Recovery CFL Conteins Free Liquid CNF Comems no Free Liquid DER Duplicate error ratio(nonnalbed absolute tltference) Dar Fac DIIWort Factor DL,RA,RE;IN Indicates a Dilution,Reanalysis,Re exbaction,oradgitional initial metalslenion analysis of the sample DLC Decision level concentration MDA Minimum detectable activity EDL Estimated Detection Clink MDC Minimum detectable concentration MDL Method Detection Limit ML Minimum Level(Diman) NG Not CaRirmted ND Not detected at to imparting limit(or MDL m EDL0 shown) PQL Practical Quantitaten Limn QC Quality Control RER Relativeemoijato RL Reporting Urmt or Requested Limit(Radwchamisty) RPD Relative Percent Differancei a measure of the relative difference behveen two points TEF Toxicity Equivalent Factor(Dioidn) TEQ Toxicity Equivalent Quotient(Dloxin) TeslAmerica Sacramento Page 4 of 934 10/06/2014 Revision-October G.2414 Revision created to correct calculation error for the percent lipids. Receipt The samples were received on 812812014.9:45 AM;the samples arrived in good condition,properly preserved and,where required,on ice. The temperature of the Cooler at receipt was-37.90 C. Dtorin-Method 8290 The ending bracketing continuing calibration verification.(CC�associated with analytical batch 51,996 has thwan4le t 3;4,7,8-HxCDD with percentdif�e2ncevalues that are between the method criteria d2A to 251E deviation from the initial calibration'burve. Per method guidelines,an average relaEve,response fdctor('RRF)fs_dalaGated,from ihebeginrung and ending bracketing CCV's and is used to quantitateLany-positive results in the associated samples forihe affected analyse. The follaMhg.sample exhibited elevated n'Oise.or matrix Interference for one or more analytes requiring the detection limits(EDL)to be raised abomthe reporting Emit(RL):SITE 4B COMMON CARP R RLLETS(320-9127.5)., These analytes were ilaggep with the"G° g6iiliher. No additional analytical or quafdy issues were noted.,otherthen those descrbed above orinthe Defipdions/Glossary page., Dioxin Piep No analytical or quality issues were noted„other than those described in the DefuulionslGlossary page. Page 5 of 934 10/06/2014 O.t: 1- 0 o S :4 9) p A 5 O a El O 37 ol pu lu In rn kD P- P; Cl) 0 p 0 P S{ p p p b p P. E R'fS R R411 R R t ow; S 0. S S S gnIA a 'g a sor a Er ' ' z Z: lj il 'ff- EY Detection Summary Client EvergreenPackageing FKABlue Ridge Paper TestAmerica Job ID:320-9121-1 Project/Site:Tissue. Client Sample ID:SITE 4A COMMON CARP WB WHOLE BODY Lab,Sample ID:320-91273 (Continued). pnalyts Result Qualfer RL EDL Unit DIIFac: D Method Prop ryps 2,378-TCDF RA ._.. 1.4, .... 0.99 . 019 porg 1 8280 . . TotaVNA ..........:...:.................. _.. _. .... .... ....... :.....:. Analog Result 'Quallfrer RL MDL Unit D9 Faa U ,Method prop Type Percent lipids 12 000 0.10 % 1 Lipids Totam Client San_iple IDi SITE 4B CHANNEL CAT R FILLETS, , Lab,Sarriple ID:320 9127-4 [Analyre Result Qualiflor .RL MDL Unii DIIFao U Melllod Prep Type Percent lipids 4:4 0.10 0.10 % 1 Upids .TotaVNA Client SamplelD: SITE 4B,COMMON CARP R FILLETS Lab Sample ID:320-9127-5 Awyla kesult Quajiflar RL EDL Unit Uil Fac D Method Prep Type 2,3,7,87TCDD- 2.1 0.99 0.94 Pw9 1 8290 ' TotaM dcD0 34 9.9 '-1A PgIg 1 8290 TotaVNA Total TCDD 2.1 0,99 0.94 pglg 1 8290 TotaVNA 1,2;3,9;7,9-itKCOD 3,9 '4.9 176-pp/g. 1 8290 ToteY1JA Total Hx&!) 3.8 J 4:o 0.99 pg/g 1 8290 Totam 1,2,3,4,6,7,9-HpCDD 14 4.9 D.95 pgig. 1 8290 TotatINA .. .. ... .. . .. .. .. .. .. .. Tata111pCDD 14 4.9 9,95, pgrg 7 9290 Total/NA Total TCDF' 3.3, G 2.0 20 4a 1 8290 Total/NA 1,2,3,4,6,7,84pCDF 2-8 J 4,9 1.8 pgig 1 8290 Totam, .. ... .. ............ ...... . TareI HpCDF -' �� 28 J 4.9. 2.0 P9rg ....1 9290 ��TotaVNA 2,3,7,8-7CDF-RA 2:7 6.99 0.21 pgig 1 B290 ToraVNA AcaW Result Qtialifler. RL MDL Unit DIIFac D MaMud Prep Type Pvrdent Lipids - 17 0.10 0,10 % 1. Lipids TotaVNA This Detection Summary does not include radlocherjical lest results. TestAmerica Sacramento Page 7 of 9.34 10/06/2014 Client Sample Results Client;Evergreen Packageing FKABlue Ridge Paper Te9tAmerica Job ID:320-9127-1 Project/Site:Tissue, Client Sample ID: SITE 4A CHANNEL CAT R-FILLETS Lab'Sample, ID:326-6-W-1 Date Collected:,08/06114 11:02 Matrix:Tissue Date Received:081W14 WAS Method:'8296-Dioxins and Furans(HRG(J11iRMS)• "Wte :Re 11 CWalieer. RL EDL Unit D Prepared. A**l zM DII Fac Z,3,7,8-TCD0 ND 0;98 0.47 p918 0910511417:19 09'10911422:15 1 OCDD 5.3 J as 02D pofg 09I0511417:19 010911422:15 1 To1aITCDD ....NO 098 047 P9/8 091=1417% 09M91142215 1 ....... .. .: 1 Z3,7,B;Pet1DD..•......... .. .::.... NO . •-�.4_9 0.79 polo ... 0=51141719 '09109l142215.,.,...,9 To4lPeCDD ND 4.9 1.4 p9/9 Gap!S!1417:19 09/09/142Z15 1 1;2,3,4,7,11 tkxCDD ND 4.9 0.69 p91g 0 9/0914 1 7:19 09/09/1422:15 1 12,3,6,7,&HxCDD NO 4.9 1,5 p9!9 09/05/1417.19 09/0911422.15 1 1,2,3,7,8,9-HzCDD ND 4.9 0.61 p91g o9105/1417:19 OW0911422.15 1 Total HxGDO ND 4,9 1.5 pg/g 09105114-17i19 09/0911422:15 1 1,2,3,4,6,7,84ipCDD ND 4.9 2:3 pglg 09N5/144719 09/09N4221_5 1 Toter HpCDD NO 4.0 2:3 Pgrg 091V1417.10 OSAMU 22:15 1 Z3,7,e-TCDF NO d_98 0.22 P919 091WI417:19 09=114'22:15 1 TofaI TCDF � NO. 0,99 0;22 polo OB/0511,4f171g OBM911422;15 1 1,2,3,7,e6.17jeCOF NO 4.9 o57 P919 0910511417,1g 69/0911422:15 1 2,3,4,7,8-PeCD0 ND 4.9 0.59 pglg 09105tl4.17.19 09N9A42215 1 ._ .. ... .. ... ... ... Told PeCDF ND. � 4.9 3.4 polo 09/05ry4 17:19 0E.009/14.7215 1 1,2,3,4,7,8:HxbDF ND 49. 0.45 Pg/g 09JD511417.19 991D904MIS 1 1,Z3,6,7,B,HxCOF NO 4A 6.95 P" 0.BIW1417:19 091091142215 1 ZiAii.7;&HxCDF.. ND 4.9 0..19 pg/o 091061f417:19 6910911,4 M15 1 1,213,7.g.!). xCDF ND 4.9 0.311 ,pg%g D9M&14 W.19 09M8/142215 1 Total HxCDF NO 4.9 0,85 P919 091051141789 0910911422ns 1 1,2,3,bi9;7,f1-HpCDF ND 4.9 0.69 polo 09/05M417:19 091091142215 1 1A3,4,7,8,gdipCDF NO 4.0 0,48 Pd19 W10511417:19 09111gA42215 1 Total HPCDF ND 4.9 0.89 polo 09/0511417:19 09M911422:15 1 OCOF No 9.6 1.1 pglg 0"5/1417i19 OWW1422:15 1 isotope Dilution %Recovery QualKler umtta Prepared Analyzed D/1Fae 13G$3,7,8-TCOD 77 40.-135 09ASH417.'19 -09M/142Z15 1 13G7,2.3,7,8-PeCDD 74 40-135 09AS1417..19 0"9H42ZI5 1 13G1;2,$6,7,8HxCOD 90 40:135 0965H417.'19 09rDeH422'15 •1 .. .. ._ .. .. .. . .. ,.. - f3G1,Z3r4r6;7,e�11pCDD • �76 40-135 09iD5K417.'19 09r09H42215 1 13CLOCDD 77 40.135 094W417:19 091DW42215 1 13GZ3,76-TCDF 77 40.135 09;o51417..19 09MI42215 1 13G7;2,3,7,8-PeCDF 73" 40-735 09,'2&1417,'111 01W9l1422 15 .... 1 13G1,Z3;4784,[zCDF .66 40-135 ORIM417.19 09AY"422'15 1 13C4.Z3,4.6,7,8-H0CDF 76 40-135 09,0511417119 09ID911422:15 1 [General Chemistry - Anaiyb Result Qualifier RL MDL Unit D Pispaiod Analyaid oil Fes Percent Lipids 9.3 0.10 0.10 % 09/08/1415:38 0910811415:38 1 Client Sample ID: SITE 4A COMMON CARP R-FILLETS Lab Sample ID: M-9127-2 Date Collected:061bli/14 11:48 Matrix:Tissue Date Received:.08129/14 09:45 Method:8290-.Dioxins and Furans(HRGC/HRMS) Anatyte Result Qualieer RL EDL Unit D Prepared AnatyzW DII Fac 2,3,7,8-TCDD 1.6 0.09 0.065 •iglg 09/0511417:19 091091142258 1 OCOD 47 9.0 0.87 P9/9 '=0511417:19 091091142259 1 Total TCOD 1.5 0.99 0.065 p9/9 09M511417.19 09MR1142258 1 Testgmddca Sacramento, Page 8 of 934 10/06/2014 Client Sample Results Client Evergreen 0adtageing FKABlue Ridge Paper TestArnerica Job ID:320-9127-1 Pmject/S te'.Tissue Client Sample ib-Sim 4A COMMON CARP R-FILLETS Lab'Sample ID:320-9127-2 Data Collected;09106/14 17:48 Matrix;Tissue Date Received:08/28114 09AS Method:8290-Dioxins and Furans(HRGCIHRMS)(Continued) Aeaw Result Qualifier RL EDL Unit D Prepared Analyzed oil Fie 1;2,3,7;8-PaCDD .3.5 J- - -- 4.9 0.37 pgfg 09/05/1417:19 09/08/142258 1 1..,.:,-._.........................................................................:.......�.�.,..,...... Total PeCDD 3:5 J 4.9 0:37 ..iarbbi ...... P01B 081D51141Ta9 OB/09114 22:58• 1 Y;2,3;1;7,8-HaCOD 4.0 J 4.9 0.17 p0/9 091OW14.17.19 091091142ZSB 1 :..... ... .... .. ............. ............... .... ..... - - 3 67184Y1iCOD 7.3'- 4.9' 0:18 �pglg •- O9/OS/141719 09l09f1422:58-• ••....1 4,23,7,8,944XCDD 3.0 J 4.9 0.13 p9/9 O9/DSH417:19 09AM44258 1 Total HxCDD 14 4.9 0.15 pg/g 09/05114 17:19 09/09/14 ZZ58 1 1,2,3r4;6,7,8-HPCDD 21 4.9 0.38 pg/g 09/05/1417.19 09109/142258 1 Total HpCDD 21 4.9 0.38 pg/g 09M14 17:19 09/09/14 M58 1 Total TCDF 3.1 0.99 0.27 p9/g 0 9/0 5114 1 7:19 09/09/14 2256 1 ......... .. .. . .. -.:.. 1,2,3,7,E-PeCOF 27 J 4.9 0.37 1`9/g 09/05/14 17:19 09l09/14 2258 1 2,3,4,7;8-PeCDF 3.6 J 4.9 0.38 pg/g 09105/141719 09109/142258 1 Total PeCDF 6J 4.9 0.37 pg/g 09MW1417.19 09M91142258 1 .. . . ... ... .. ......I....I.,... 1 ,,4,7,8 0iCDF 3.8 J 4.9 - 0.29,2,, p9/9' 08/05/7417:19 09109/142258 '1 IA3,6;7;84HxCDF 45 4.9 D.26 P919 D9/0511417:19 09109/142258 '1 2,3,4,6,7.s4ixCDF 35 J 4.9 0.28 pg/g 09/05/1417:19 09/091142258 1 -. .. .. .. . .., ..-4i .. •-•� 09/OS11417d 9 09/09l14 2258 1 Yotal HiCDF 15 4.9 0.28 p09 09MS 1417:19 09=114 2258 1 I.Z3;4,6,7;8:HPCDF 45 Jq 4.9 0.66 pg/g 09M5/1417:19 09/091142258 1 IA3,4,7,6,9;HpCDF 2.8 J 4.9 0.81' Pglg 091051141719 091091147268 1 Total HPCDF 7.3 q 4.9, 0.74 jW9 0SW14 17.19 09109114 ZT58 1 OCDF 6A J 9.9 0.18 pg/g 0910511417.19 091091142258 1 Isotope Dilution %RwaVaW Orcfdni Limits Prepared Mdb-,d D4Fae /3C-Z3,7,_5:7'CDD 97 40_135 09,03`1417.79 091091142Z58 1 13G143;7,aFeCDD 97 40.435 OWS1417:'19 OM91142258 '1 13C4,2,3;8j7,84*CDD 112 40-135 DA41417,•19 09r09(142258 1 13G123,4,6,T,"pCD0 98 40-435 09)DY141719 09N9/1422'S8 1 13C-OWD 96 40.135 09=0417..19 09M§/140.68 1 1392,J,7,8-7CDF 98 40.135 "OSM1417:19 02,190422.59 1 f3C-1,23,7,8PeCDF 95 406135 09ib5!14,1T;fa 09N9(14 M-59 1 13G12,$4,7,&teQOF 87 40-135 0SPW411,19 09,OV142258, 1 Y3G12,$4fi,7,XHpCDF 96 40-135 69105(1417:19 09ba/14225a, i Method:6290-Dioxins and Furans t1iRGC/HR AS)-RA Anarjla Result Qualifier RL EDL Unit q Prepared Analyzad Del*Be 2,3,7,6•TCOF 25 0,99 0,25 p919 09/05H417:19 09113/140529 1 lsafopa Dlluillon 76Reenvery Quallrler LJmlts. Prepared Analyzed Oil Fec. 13GZ,3,7,&7CDF 93 40-135 OMY1417-19 09/13N40&29 / [General Chemistry Anayte Rosult QuallBer RL MDL Unit Prepared Analyzed oil Fie Percent Llplds 15 0:10 0.10 % 09108H4 15:38 09108/14 15:38 1 Client Sample ID: SITE 4A COMMON CARP WB WHOLE BODY Lab Sample ID: 320-9127-3 Date Collected:08/06/14 10:00 Matrix:Tissue Date Received:08128114 09:45 Method:8290-Dioxins and Furans(HRGC/HRMS) Analyte Result Ouali ler RL EDL Unit D Prepared Analyzed oil Fee 2A7,8-TCDD 0.96 J 0.99 O.D69 pg/g - 09/05/1417:19 09109/14 Z3:41 1 OCDD 36 9.9 0.53 pgfg- 09M5/1417:19 091=1423.41 1 TestAmerica Sacramento Page 9 of 934 10/06/203:4 Client Sample Results Client.Evergreen Packageing FKABlue Ridge Paper TestAmerica Job.ID:320 9127-1 PrcjectlSite:Tissue Client Sample IDi SITE 4A COMMON CARP WB WHOLE BODY Lab Sample ID:320.91273 Date'Collectsti:OV0611410:OD Matrix:tissue Date Received:00/28/14 09:45 , Method::8290-Dioxins and Furans(HRGC/HRMS)(Continued) Mtlyte. Penult Qualifier RL EDL Unit D Prepared Anatynd DD Fac Total TCDD. ,..0.96 J 099 0.069 12.3r7,8•PeCDD .. ND - Pg/g 09/D514 17 19 09/09/14 2A1 1 f. ,,, .....,.. 5.0 fig . O9OS/141719 0901423AI 1 Total PeCDD ND 5;e 1,0 Pg/g gVW1417.'19 09/09/1423:41 1 1,23,4,7.s-HxCDD NO 5,0 1.8 ;PoIg 06165/141118 691691142141 1 1,2,3,67.8-HiCDD.�... .._..4.6..J ... -:.1. ..:....•.5.0 0.i6 pg/g D&D5r141719 OBI09/142341 1 1,23,7,8,9-HxCDD ND: 5.0 1.6 pl 09/D511477:19 01SM1423:41 1 Total HxCDD 4.6 J 5,0 13, P;Ig 09/os/14 17:19 09f09114 23:41 1 1A3,4,6,7,8.HpCDD 16 5.0 0.39, Pg1g D9105r1417:10 0916§11423:41 1 Total HpCDO 16 5.0 0.30 pglg 0Q/05/14 17;19 09/09/14 M li 1 Total TCDF 21 0.99' 0,30 Pg/a 09/0X14 17:19 69/09114 23:41 1 . .. ._,,. 1,23,T8-PeCDF - NO io - 1.8 W9 ..,..... O9/a5H417a9 OB10911423td1 '1 2,3,4,7,8-PeCDF ND 5.0 2.3 pg/g 0910id141Z16 69/09/1423.41 1 Total POCDF ND 5.0 2.3 pg/g 09/05f1417:19 09109/1423:41 1 1,2,3,4,7;8-HzCDF ... . . . . "ND � � .... 5.0 2:2 palg .0 9/05114 17,19 09/09/1123:41 1 1,2,3,6,7,84-biCDF 2.6 J 5.0 0.19 pp%g 09105/1417.19 09/69i1423.41 1 2,3,4,6,7.5HR !F ND 5.0 1.6 Pg/g 091051141719 09/091142341 1 .......:..... ... . .... ....:... ��ND ��. .. ��5,0� ��D:87 pg/g �08/05/14 17�19 09/09/14 23:4P 1 Total H%CDF 2.6 J 5.0 1,2 ^pg/g 09f05/1417:19 0910911423:41 1 1,2,3,4,6,7,8,.HPCDF 2.6 Jq 5.0 051 pg/g 0910511417:19 091OW1423:41 1 1,2,3,4,7,0,9-HpCDF ND * * , , . .5.0 /1.88 pg%g '09IM1,417:10 '09f09/1423:41 1 TOW HPCDF 2.6 J q 5.0 0.57 pg/g 0910511417:19 09/09114.23:41 1 OCOF ND 9.9 1.9 Pg/g 091051141719 0910911423.41 1 isotope DlNNon. %Necovety QualMler UM& Prepared Analyzed DIIFac 73G2,3,7,B-TC00 72 40.135. 09105W 17;19 09AM423i41 1 13G1,2,3,7,BwPeQDD 70 40.135 DEW1417.779 D9X911423:41 1 13G1,2,3;6;7,8-}iCCOD 80 40-135 09R157417:19 09N9/1423:41 1 13G1,g3,4,8,754HpCDD 73 40-135 O9N0417919 OW911423:41 1 13GOCDD 73 40.135 09)W1417:19 09MV1423:41 1 13G2;3,7. -TCO,F 73 40.'135 .ORMSI41719 D910911423:41 1 13GL2,3,7,8-PCCDF 08 40,.135 OROW4 17!19 O&W1423:41 1 13GL33.4,TB=MtCOF fit 40-135 'O9N.5H417.19 09MI1423:41 1 13G1A3,4,6,7,"pCDF 72 40-135 0"W1417:16 09)WI42541 1 Method:8290-Dioxins and Furans(HRGC%HRMS)-RA Mely(e Result Qualifier RL EDL Unit D Prepared Analyzed Oil Fee 2,3,7,8-TCDF 1A '0.99 019 p0/9 09105/1417:19 09113/1406.00 1 Isotope DluOon. %6gceVvy OuaNRer Unrlts Prepared Analyzed DIIFee 13C-Z3,7,8-TCDF 65 40.135 09MS'1417:19 OM3H40606 1 General Chemistry Analytn Result Qualer RL MOL DnR 0 Propared' _ May+m nil Fee Percent Lipids 12 0.10 0.1D % 0 9/0 811 4 1 6:38 09MB11415:38 1 Client Sample ID: SITE 4B CHANNEL CAT R FILLETS Lab Sample ID:'320-9127.4 Date Collected'08/06/14 09:38 Matrix:Tissue Date Received:08/28/14 09:45 r I Method:8290-Dioxins and Furans(HRGC/HRMS) - Analyte Result Qualifier RL EDL Unit U Prepared Analyzed oil Fee 2,3,7{9-TCDD NO 1.0 0.47 p9/g 09/D5/1417:19 09/1011400:23 1 TestAmerica Sacramento Page 10 of 934 10/06/2014 Client.Sample Results Client Evergreen Pa&ageing FKABlue Ridge Paper TestAme_rice Job ID:'320-9127r-0 Project Site:Tissue Clien4.9ample IDc SITE4B CHANNEL CAT R FILLETS Lab Sample ID: 320-0127 4 -Date Collected:08f06/14 09:38 Matrix:Tissue. Date Received:08/28/14 09:45 Method:8290•Dioxins and Furans(HRGCfHRMS)(Continued) Analyle Result Qualifier RL EDL Unit D :Prepared Analyzed DII Fee ,OCDD. - ND 10 ,3.9 pgf9 090511417:19 09/10/1400:23 1 Total TCDD NO 1:0 0.47 pglg 09105/1417t19 0911011400:23 1 1;2,3,7,8-PeCDD ND 5.0 0.26 p9l9 09/05/1417:18 09110/14 0023........1 Total PecbD ND SA 0.28 p9/9 DSMW14'17.19 D9/10/14'.0023 1 1,2,3,4;7,S4ixCDD ND 5.0 0.31 p9/9 ORW1417:19 '09/10/140023 1 1A3,6,7,B4tXCDD NO 5.0 0.65 ;g DRM511417:19 09110/1400:23 1 1,2,3;7,8,9-HxCDD, NO 5.0 0.24 P9/g 09105/14,17:19 09110/14 D023 1 Total HxCDD No 5.0 0.65 P919 09M5/1417.19 09110/140g23 1 1, 3.A6;7,8-HpCDD ND '5.0 1.4 p919 0SW1417;18 08110/140023 1 Total HpCDD ND 5.0 1A pgfg D9M511417:19 09110/14.0023 1 2,3:7,8_TCOF ND 1.0 021 p9/9 09M5M417:10 091101140023 1 Total TCOF NO 1.0 021 p0i9 09/05/14 17:19 09/10114,0023 1 1,Z3,7."eCDF ND 6.0 0.37 pg/9 D9105/141719 09/10/140023 1 2,3.4,7,8-PeCDF ND 5.0 0.39 P0 oamf1417:19 0911011400:23 1 Total PeCDF ND 5.0 0.39 P919 09M511417N9 09/101140023 1 1,2,3,4_7,8-HZCOF ND 5.0 0,19 pp7g 09105/1417:19 09/10/14 OD:23 1 1;2,3,6,7;8-HiCOF No '5.0 0.26 pg/9 09105/1417:19 09/101140023 1 2,3,4,817,8-HZCOF ND 5.0 0.17 p9/9 �� O WWI 417.19 09/70/14 0023 1 1.Z3,7,8,9-HiCDF ND 5.0 0.48 P9/9 O9M50417:19 09110/1400i23 1 Total HiCDF ND 5.0 0.48 pgrg '09/05/1417:19 091101140023 1 1,2,3,4,8,7,&HpCDF No 5.0 0.38 pglg r09/OS%1417,'.1,0 09A0/140023 1 1,Z3,4,7,6,9-HpCDF NO 5.0 022 pglg 08/051141719 09/10/140023 1. Total HpCDF ND 6.0 0.38 p'g/g -09105114'17,'19, 09/101140023, 1 OCOF ND 10 0,40 pg/g 09l051141T19 09110114 6P.23 "woe DIMM %Reeovery, Qual/fier Palms Prepared Analyzed b11Fee 13GZ3;7,8-TCDD '75 40_135 09M(i11417:19 09110H400.23 1 13G7,$3,7,8-PeCDD 72 49�135 09MV1417;99 09/iMf460:23 1 13p1;Z'3,6,76-WOD 88 40_135 0&1%"417:19 09/10/140623 1 }3G7-z3,4:6,7r&HpCOD 73 40_135 09iOy140:19 09ry0!14 pk23 1 13G0CDD 72 40_135 09R251117.19 0"mf40223 1 13G2;3i7,8-TCDF 77 401135 09,0s'141.7.19 091101400:23 1 f3Gi z3,78_FeCDF 71 40_'135 aril Yi11Y. 09/iD<1400:23 1 13G1,2,3;4,7,8-f iCDF 65 40_M QW15*4 Mill 09/1(Vf460.23 1 13G1,Z3,4,,8,7,8-HpCDF 74 40_f35 09N51417.18 09/f0/140023 1 [General Chemistry _ Analyte Result Qualifier RL IdbL Unit D Prepared Analyzed. DD Fee Percent Llpids 4.4 0.1.0 0:10 % 09/08/1415:38 09W1415:38 - 1 Client Sadiple ID: SITE 4B COMMON CARP R FILLETS Lab Sample ID:'320-91275 Date Collected:08/06/14 13:20 Matrix:Tissue Date Received:08128/14 09:45 Method:8290•Dioxins and Furans(HRGCIHRMS) Anatyta Result Qualifier RL EDL Unit D Prepared Arialyrad oil Fee 2,3,7,8-TCDD 2.1 0.99 0.94 P9/9 09105114 17.19 09/10/14 01:06 1 OCODI 34 9.9 1:8 P9/9 0910511417:19 0911011401:06 1 Total TCDD 2.1 0.99 0.94 p919 09/05/1417.19 D9/10114 01:06 1 1,2,3,7,8-PeCDD ND 4.9 4.1 pg/g 0910511417:19 WHIM 01:08 '1 Total PeCDD No 4.9 4.1 p9/9 0910511417.19 09/1U/1401:06 '1 TestAmerice Sacramento Page 11 of 934 10/06/2014 Client Sample Results Client,Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320.91VA PlojecVSite:Issue C)ient Sample ID: SITE 46 COMAAON CARP R FILLETS Lab Sample ID:320-91275 Date.Cuhected:D8(06(141320 Matrix:Tissue Date Recelvedi OW28114 09:45 Method:8200-Dioxins and Furans(HRGC(HRMS)(Continued) Anatyte Result Qual8ler RL EDL Unit D Prepared. Analyzed DII Fac 12,347,B�HxCDD ND ,...4.9 1.1 pg1g `_... ORM14:1719 091101140108. 1 i'........... .. ... ... ....... ......, 1236,7;8•H1cCDD 3.8 J 4;9 1.0 PC/g 09A5H4'1719 .0911W1401:06 1;2A,7,8,&HxCDD No 4:0 0.8,5 pgfg q6MU1411.19 09116M401:08 1 Total HKcDD 3.8 J 4.9 0.99 P919 09rO5n417 9 filHO1,401:06 1 - -. .. ...w... ..-;...._ ..... 1,23467;8-HpCDD ..... 14 ....................4.9j. .0.95 pglg.•....... 09/05/1417,19.. .09HW7401*Os........1 Total HpCOD 14 4.9 0.e5 pgfg 09l0511417.19 09/1011461:06 1 Total TCDF' 3.3 G 2,0 2.6 pg(g 6005/14.17:19 09/10-11401:08 1 1,2,3,7,8-PeCDF ND G 5.7 5.7 pgtg 06/0511417:18 09A0%1401:06 1 213,4;7,8-PeCDF ND G 6.0 6.0 p9/g &A)511417:19 0911011401:06 1 Total PeCDF ND G BA 6.0 p0/g 09/05H41I:19 0911011401:06 1 .. ........ .... ... .... .... ....:...... .. . t2,3;4;7,eaHzCOF ND' 4.9 1.4 pg/g 09iD5H4.17:19 09/10I1481:08. 1 1.2.3,6,7,8-H%CDF ND 4.9 1,2 pgf0 09705f1417.19 0011OR401:06 1 2,3,4,8;7;8&H%CDF ND 4,9 1.3 pglg 09106M417:19 09110/1401:06 1 1;2,3;7,B,B�HxCDF. NO 4.9 1.3 'pgfg 09/05f141719 09/1011401:08 1 Total HxCDF ND 4.9 4.1 P9f9 OWSM417:19 0911011401:06 1 1,2,3,4,6,7,8-HPCDF .,. 7-6 J .4.9 1.6 P91g 091D5M417:19 0911W14.01:06 1 ._.. ..- .;7,8,&HpCDF ND 4.8 22 p01a 09/05/1417:10 0911011 401:08 1 Total HpCDF 2.8 J 4.0 2.0 P919 09105114.17:19 09HO114 01:08 1 OCDF ND 9.9 1.1 P819 09105114 1719 09110114 01:06 1 Isotope Diloflon %Reeomy Qualdter Units .Prepared Anabwed DifFae 13G2,3,78-7COD 73 40-135 09MWI417.19 09VIO1401:06 1 13W,3378-PeCDD 58 40_135 ORDS1417:19 0911011401:06 1 13G1;2,3;678-1lrCDb 93 40-135 09)M417;19 091107401:05 1 .. ... .. 13Gf Z34,fi7,9-HpCDD 67 40_Y35 09iD594.77:19 09%fN14.D1[OB 1 13GVCOD 61 40.135 09i0W1417.'19 0911W1401:06 1 13G23;YB-7CIIF 74 40-135 02D50417.•19 091100401:06 1 13G-1;2,3,'78-PBCDF .60 40-135 09)OWN41719 09N017401.05 '1 13C-,1,43,t;78-1kCDF 66 40.135 09MW417:19 091101401:06 1 13G1,2,'3;4;5;78-F1pCOF 66 40-135 09IM417.'19 0911Wf401i06 "1 Method:8290-Dioxins and Furans(HRGtIHRMS)-RA Angie Rasa Du2181x RL EDL Unit D Pmpzred Analyzed D11Fae '2,3,7,8-TCDF 2.7 0.89 021 p919 00105/1417:19 09113/14 DB:44 1 Isotope.Dllu6on %Recovery Qua08er tlmin Prepared Anabwd glFec 13C-$3;78-TODF - 66 40-135 09,D"917..19 00113N406.44 1 General Chemistry AnayM Result QuaOrter RL 6ADL Unit D' Prepared Analyzed DII Fae PercentUpids- 17 010 0.10 % 09/08(1415:38 ORMW415:38 1 TestAmerica Sacramento Page 12 of 934 10/06/2014 Default Detection Limits 9 g 9 P TestAmerica Job ID:320.9127-1 Client Evergreen Parka efn FKABIue Wd a Paper Phijewsite Issue Method:8290 -Dioxins and Furans(HRGC/HRMS) MaW RL UnfW Method 1,2,3,4,6,7,8-HPCDD 5.0 P0/9 8290 1:2,3.4.87,8-HPCDF '5.0 ;;rg 82DO 1;2,3,4,7,8,9-HPCDF 5.0 pglg 8290 1,2,3,4,79-HZCDD .. .. .... .......5.0 •.. .... e. :.8290 1,2,3,4.7S4UcCDF 5.0 0919 8290 1;2,3,6;7A-HaCDD 5.0 pg/g am ..::.............................................. -............................�.................,-8290....... ....... ....... 5:0 1;2,3,7,8;9-HXCDD 5.0 P9/9 8290 1,2,3;7,D;D-HiCOF 5.0 pp/D 8290 :: :........ .............................................................._.. a.....:....._ . ...................... 1;2.3,7:8-PeCDD ...... 5:0 / .....82D0 1,2.3;7,8-PeCDF 5.0 09/9 8200 2,3,4;6,7,8-HxCDF 5.0 pp/g 8290 -r ................ .............................. 2,3,4.7.BfeCDF. ... ... 5.0................... ....................6910 . 2,3;7,8.TCDD '1:0 Iig/g 8219.0 2;3.7,8-TCDF 1.0 pg/g 82.90 OCDD 10 P0/0 8290 OCDF 10 OGO 829D Total HpCDD 5.0 P09 9290 Total HPCDF S.D pg/g 8296 Tofu]HiCDD 5.0 FD/9 828o Total HXCOF 5.0 pg/g 6299 ToW PeCOO 5.0 .. :..... 2 P8/9 829U ' Total PeCDF 8,0 W9 8290 TotsI TWO '1.0 Pg/g 8290 Tota1TCCF 1.0 •� .. P8/0 8280 .. . General Chemis" [Analyfe _ RL MD,L units Method Per cent UPlds 0.10 0d0 % Llpids TestAmerica Sacramento Page 13 of 934 10/06/2014 Isotope Dilution Summaiy Client Evergreen Pac4geing FMplue Ridge Paper TestAmerica Job ID:320-9127-1 Pfpl&oSite:Tissue Method:8290-Dioxins and Furaos(HRGC/HRMS) Matrix:Tissue Prep Type:Tolat)NA Pecent Isotope Dilution Recovery(Acceptance L:snBs) TCOD PeCDD HxCD132 HpCDD OCDD TCOF PecOF1 HXCOFI Lab Sample ID Client Sample ID (40436) (40436) (IO-135) (40.135) (40.1351 (40:135) (40-135) (40-135) 32D.9127=1 SITE 4A CHANNEL CAT.R-FILLETf 77 _74 - 90 .79, - 77 77" 73 - 68 320-9127-2 SITE 4A COMMON CARP R;FILLE- 97 97 i 12 l99 Be 68 95 97 320-9127-2-RA SITE 4A COMMON CARP R-FILLE 93 ._kff............».. .....__.. .................._.........................._._.-a .._.. 32o-91273 - SRE`4A COMMON CARP WB WHG727D 84 73 -73 73 '66-- ` 62 320-91273-RA SITE 4A COMMON CARP WB WHC 65 320-9127-4 SITE413 CHANNEL CAT R FILLET.- 75 72 Be 73 72 77 71 85 320-91Z7-5 SITE 413 COMMON CARP R FILLET 73 58 93 67 61 74 6o Be 320-9177.5-RA SITE4B COMMON'.CARP R FILLEI 66 LCS 3205170=-A Lab Control Sample 76 75 90 77 81 70 75 68 Me 32D51700H-A McMod Blank 69 68 78 69 72 69 66 69 Percent lsotcpeDilution Recovery(Acceptance Umfta) HpCDF1 Lab Sample lO CnerRSample,l0L (40.135) 320-9127-1 SITE'4A CHANNEL CAT R-FILLET: 76 320-9127-2 SITE 4A COMMON CARP R-FILLE 96 32049127.2-RA SrrE'4A COMMON CARP R-MLLE _ - . . . . . .... . . .. . . . E 4 .. .. 320-9127-3 SITE COMMON CARP WB WHC. 72 32 9127-3-11A SITE 49 COMMON CARP WB WHC 329791274 SITE 4B CHANNEL CAT R FILLET; 74 32(F9127-5 SITE 0DOMMON CARP R FIL1E1 68 320;8127S-R(v SITE 40 COMMON CARP R FILLE1 LCS 320-5170012-A Lab CwrWl Sam'a 78 W MB'320-6 ... ...17BW1-A Me6i0p Blank, 71 Surrogate Legoml TCDD=13C..2,3,7,8-TCDD PeCDD=13C=1,2.3,T9-PeCDD HxCDD2.=,i 0,0,dxe;H CDD HpCDD=13G•1,2,3,4,6;7;&)1pCOD oDDD='lic-OCpO TCDF=f c-j,3,7;B,-TCDF PeoDFi=1riA3,7."s DF HxCDF{-13G1,2,3,4,7.15-HxCOF HpCDF1=ur l,2,3,4,6,7,0-HpCDF TestAmedca Sacramento Page 14 of 934 10/66/2014 QC Sample Results ClientEve7green Packageing FKABIue Ridge Paper T,estAnierica Job ID:320-9127-1 Broj@Wl Ae:Tissue Method:'S260=Dioxins and Furans (HRGC/HRMS) Lab Simple ID:MB 320-51700117A Client Sample ID:Method Blank Matrix:'TIISeoe Prep Type:TotabNA Analysis Batch:.51998 Prep Batch:51700 Me Ma Anatyto Result Qualifier RL EDL Drill D Pnlpued Anaymd Oil Fac 2,3,7.8SCDD ND 1.0 0.13 p910 9R/W 1417,:18 09/D9114t20:50 1 'OCDD ND 10 u pp/0 09/0611417:19 09109/14205D 1 Total TCDD, ND 1.0 0.21 pg10 09/0511417:19 .. . .. . .. . . .. .............. .. �. .� .. . z¢ 0 1 1;2,3,7,9&PeCDD �-� �� ND 5.0� �� 0.24 p9/9 O9/0,5/14A7:19 09/0911120;50. 1 Total PeCDD NO 5.0 024 pglg OB/QSb417:79 09I09/1420:50. 1 1;2,3,4,7,8-HxCDD ND 5.0 0,13 pg/0 00/05114'17:19 09/00/1420:50 1 1,2;3,6,7,8-HxCDD NO 5.0 0.12 'owl; 09/05/.'14 it.19 00100/1420;50 1 1,2;3,7,8,9-H*CDD ND 5.0 0,098 pg/g 09/a5/14:1709 091001142C56 1 Total HiwD" ND 5.0 0i13 pg/g 0 9/0511 4 17.19 09 i.1420:50 1 1;2,3;4,8;7;8-HpCDD ND 5.0 025 pe/g 091105/14'-17:18 O910e114.20:5D 1 Total HPCDD ND 5.0 0.25 pg/0 09/05114 T7:m9 6WWI420:50 1 2;3,7;8-TCDF ND 1J0. 0.'22 P.910 08/05/1417.19 Q91W1420:50 1 ... .... N .. .,..... ..:...... .. Total TCDF ND �� - 1:0 022 - -pg/g, 09/05l1417;19 08/09/1'4 2050 1 1,2,3,7,8-PeCDF ND 5.0 0.81 p9/g 09/D5A417:19 OM911420.50 1 2,3,4;7,8-PeCDF ND 5:0 0:53 P0/9 09105/1417:19 OSIW1420:50 1 . ............... .... .__I............... ... - .., Total PeCDF NO �� 5.0 0,53 P9/g, �� 09/05/14 17,19 09%09n4 2D;SD�� 1 IA;4;7,8.H.xCDF ND 5.0 0.12 P919 6916511417:19 09/09i1420:50 1 1,Z3678-HxCDF NO 50. 011 pg/g 69/0511417-19 09/6g11420:50 1 34......zCDF.. ... .:.....:...NO. ........::... 5.0 0... ....._... z, pg1e ow9s14 n 1s `oeloeild2¢so 1 1;2,3,7,0,9-NfCDF ND 5.6 0.12 pg/g 09105/1417:19 08709/1420:50 1 Total HxCDF NO 5.0 0.12 �p91g O9/OS/1417.19 09/09/1420:50 1 ...... ................................ ..,.............._.._......_......................... 1,Z3,4,6,7,8-HpCDF ND 5.0 025 pi g '09/0511417'19 09/0911420:50 1 1,2,3,4,7,8,"pCDF ND So 0.094 p9_19 091W1417:19 OGIDD11420:50 1 Total HpCOF NO 5,0 0.25 pglg 09M511417.19 09/09/1420:50 1 OCOF ND 10 0.33 pglg 09105/1417:19 ORMI1420:50 1 Ma MB !so"Dilution _ Y.Reeovory 4ualiffor UmMa Prepared AnsVzed oil Fec 13GZ3,7,&7CDD 69 404;15' 09/05'l417.19 0"911420'50 4 13G7,Z3;7,SPeWD .85 40.AS5 09/051417.19 •.02,021142050 1 13C-/,Z3,67,84-&C,DD 78 40-135 09105%417:19 09MI1420:50 1 j3GL2,34,S,48-HpCDD 69 40_135 09N91417.19 09i0911420:50 1 Isc-oaDD. 72 40.135. OM5114'77:19 DAW14205D 1 136 Z3,78-TCDF 69 40_135 '09NSY7417.19 09 M42050 7 73G1,2,3,7,8-PeCDF 66 40_l35 I `09N5�149Tf9 '02D9H42050 1 13G4,Z3,4,7,8-1raCDF 59 40-135 0M5H4 M19 o9jW1420:50 1 13F1,ZA4,6,7,847pWF 71 40.135 09105H417.19 09A9/1420.'50 1 Lab Sample ID:LCS 320-51700/2-A Client Sample iD:Lab Control Sample Matrix:Tissue Prep Type:TotatlNA Analysis Batch:61998 Prep Batch:51700 Spike LCS LCS SRec. Anslyta Added Result Qualifier unit D %.Rae Units Z3,7,8-TCDD - 20.0 21.1 pg/g 105 50_150 OCDD 2DO 212 pe/9 Ica 50-150 1,$3,7,8-PeCDD 100 105 pg/g 105 50_15D 1,2,3,4,7;8-HaCDD 100 1D3 pi/i 103 50.166 1,2,3,6,7,8-HxCDD 100 104 pg/g 104 50.150 1,2,3,7,8,9-HXCDD 100 89.0 pg19' 89 50_150 TestAmeriaa Sacramento Page 15 of 934 10/96/2014 QG$ample Results Client:Evergreen Packegeing FKABlue Ridge Paper TestAmedca Job ID:320-9121-1 Pcoject/S.he:Tissue Method:8290 -Dioxins and Furans(HRGC/HRMS),(Codtinued) Lab Sample ID:LCS 320-51700/2-A •Client Sample ID:Lab Control Sample Matrix:Tissue 'Prep Type:TotaUNA Analysis WON 51998 Prep Batch:51700 Spike LCS LC$ %RK. Anaiyb Added .Result Qaa05er _ Una D, %k= _ Llmks_ 1;2,3,4,s,7,8-HpCDD - - '100. -1.14 P919 11,4 50-150 — — 2,31 7;6-TCDF 26.0 19.7 p919 Be 50,180 112,3,7,8-PeCDF 1d0 103 pgtg 10j 50-150 ....... .... .. ...... .. 100 108 PgrB 708 50_150 1,2,3,4,7,8-HKCDF 100 108 P919 168 50-150 1,2,3,6,7,"XCDF 100 129 pglg 129 50_450 $3;4,6,7,8-HzCDF 180 420 pg/g 120 50.150 1,2,3,7,8,9-HxCDF 100 110 pg/g 110 50.15D 1,2,3,4,8,718-HpGDF 100 106 Pori; 7D6 50,.150 1,2,3,4,7,8,9=FIpCDF 100 '107��' "50_15D OCDF 200 206 pWg 103 50_150 LCs Lcs laerope Weir ;%Rwwery Qwfifier Lrmfta 13C-2,3,48•TCOD - 76 40_135 13GL2,3,7,8&PeCDD 75 40.135 130.1;23,6,7,0-WCDD. 90 "40_135 .:.s..r.::......:........ . 1361,2;3,4,6,7,8-HpCDD "77 '4dLY35 13C-CMD 81 40.135 130-Z3,7,8-TCDF 78 40.135- 13G7;23,78-PeCDF 75 40.135' 13C-1,2,3,4,7,S*CDF 68 40_135 136L2,3,$6;7,XtOMF 78 40_135 TestAmedca Sacramento Page 16 of 934 10/06/2614 QC Association Summary Client Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-9127-1 .Project/Site Tissue Specialty Organics Analysis Batch:4.68,97 [Lab"Bampleto Client Semplel0 Prep Type Matrix Method "prep Batch CPS320-4689711 CPS Time 8290 Analysis Batch:49055 Lab Sam Samoa rep ple l0 Client Saal P Tyq� Matrix Llethod. Prep Batch [CPS 320-4905W CPS Time 8290 Prep Batch:51700 Lab Sample 10 CBent Sample l0 Prep TyPo Matrix Method Prep Batch 320-9127-1 SITE 4A CHANNEL CAT R-FILLETS 'TotaVNA Tissue 8280 320.9127-2-RA SUE 4A COMMON CARP R--FILLETS Totallm Time 8290 320-9127-2 SITE 4A COMMON CARP R-FILLETS Totam Time 8290 320.91273-RA SITE 4A COMMON CARP WB WHOLE BODY T6tepNA ...... .. Tissue . 69 0 320-91273 SITE 4A COMMON CARP 4VB WHOLE BODY TotaVNA Tissue 8290 320.81274 SITE 4B.CHANNEL CAT R FILLETS TctaVNA Tissue 8290 . .,. .. .. 320.9127,5-RA AW SfTE°4B COMMON CARP R FILLETS �7otaUNA �� Tissue �� 8280 . ... . ...... . 320-91775 SITE 48 COMMON CARP R FILLETS TctaVNA Tissue 8290 LCS 320-517002A Lab Control'Sample TolaVNA Time 8280 ... Me 32 0.517 0 0/1-A Mathes Blanii TomVtU Tissue 8290 Anatysis batch:.51998 Lab Sample ID Client Sempie,ID Prop Type _ Mama Method Prep Belch 320.9127-1 SITE 4A CHANNEL CAT R-FILLETS TctaVNA Time 8290 51700 32D-9127-2 SITEAA COMMON CARP R-FILLETS TctaVNA Time 9280 51790 320-9127-3 SRE4A COMMON CARP WB WHOLE BODY Teta9NA -Tissue 8290 51799 320-.91274 SITE4B CHANNEL CAT R FILLETS TctaVNA Tissue 8200 51700 320-91275 SITE 48 COMMON CARP R FILLETS TotaUNA Time 8290 51700 CPS320-5199VI CPS T'Beue 8290 . ._. . LOS3170U/2-A CebCordml Sample. ToteVNA Time 8290 51700 Me 1351700/1-A Method Blank TOMWA Time 0280 51700 Analysis Batch:62309: Lab3amplelD Client SamplelD Prep.Type Matrix. Method Prop Batch 32t19127-2-RA SITE 4A'COMMON.CARP R-FILLETS TotaVNA Time am 51700 3249127-3-RA SITE bA COMMON CARP WB WHOLE BODY TotatINA Tissue 6290 61700 ,320.91275 RA SITE 4B COMMON CARP R FILLETS Totem Tissue 9290 51700 CPS 3205230911. ....... CPS....... ..... ..:...... ......... Time 8290 General Chemistry Prep Batch:52229 Lab Sample l0 Client Sample l0 Prep Type Mabia Method Prep Batch 320-9127-1 SUE 4A CHANNEL CAT R-FILLETS TotaVNA Tissue HRMS-Sox 320-9127-2 SITE 4A'COMMON CARP R-FILLETS TetaVNA Time HRMSSox 320.9127.3 SUE 4A COMMON CARP We WHOLE BOGY TotaVNA Time HRMS-Sox 320.8127-4, SITE 4B CHANNEL CATR FILLETS TotaUNA HRMSSox 32 0.912 7-5 SRE4B COMMON CARP R FILLETS ToMMA Time HRMSSox Analysis Batch:62231 rLab Sample ID Client Sample ID Prep Type Matrix Method Prep Balch 3 20-91 27-1 SUE 4A CHANNEL CAT R-FILLETS TotaVNA. Time Lipids 52229 TeslArnerica Sacramento' Page 17 of 934 10/06/2014 W Association Summary Client Evergreen Packageing FKABlue Ridge Paper TestAmerica Jab ID:320-91274 ProjeoUSite:Tissue General`Chem(stly(Contlnlied) Analysis batch:62231 (Continued). Lab Sample0 Client Sample ID Prop Type Uatdx _ Method Pwp Batch 320-9127.2: SITE 4A COMMON CARP Ft-FILLETS TetalWA Tissue Lipids 52229 320-9127-3 :SITE 4A COMMON CARP M MoLE BODY 7O12MA Tissue Upids 52229 ........._ -....-.... .• .. . ....rt ................. 320.9727.4 SITE46 GFIANNEL.OAT'.REILLETS TohiVNA Trssue Lipids 52229 320-9177-5 SITE 4B.COMMON CARP R FILLETS Totam Tissue Upfds, 52229 TestAm erica.Sacramento Page 1S of 934 10/06/2014 Lab Chronicle .Client Evergreen P.ackageing FKABlue Ridge.Paper TestfyRerica Jots ID:320-9127-1 ProjectiSite:Tissue Client,Sample ID!SITE 4A CHANNEL CAT RrFILLETS Lab Samplell) 320=9127=1 Date'Coliected:.08106114 11:02 Matrix:Tissue Date Received:00iii8/4 09;45 Bate Batch Dilution Batch Prepared Prep Type Type Method Run Factor Number _ or}Mayzed Analyst LA TomVNA Prep 82RO 51700 09/05/1417:19 GDB TAL90 TotaVNA AMWS 829D 1 51996 W091142215 JRB_ TALSAC T0t3VNA Anaysis Gpids 1 52261, 0910811415:98 ELK TALSAC Totalim Frep HRMSSox 5=0 09/a8/141538 ELK TALSAC Client Sample ID:SITE 4A COMMON CARP R-FILLETS Lab Sample 1D:320-9127-2 Date Collected:6EV0611411:48 Matrix:Tissue Date Received:08/28H409:46 Batch Balch DHAon Batch Prepared Prep Type Type Melbod Run Factor Number or Ana"d Analyst, Lab TotaVNA Prep 4290 RA 51700 09/0 1417:19 GDB TALSAC TotaVNA Analysis 6180 RA 1 52309 091IM405:28 SMA 'TALSAC TotaVNA Prep 8280 51706 69MI141T19 GDB TALSAC TotaVNA Ana s am 1 51898 09/09/1422:58 JRB TALSAC TotalMA Anaws Lipids 1 62231 ,69108/1415.39 ELK TALSAC TotaVNA Prep HRM6-86x 52229 ,OB(00(1415:96 ELK TALSAC, Client'Sample ID:_SITE 4A COMMON CARP WB WHOLE BODY Lab.Sample ID:320-91273 Data Collected:08106M4 10:00 Matrix:Tissue Date Received;08/28N4 09:45... .. . ,... _.. . . �__ Batch Batch Dilution Batch Prepared Prep Type Type Method_ Run Factor Number -or Analyzed Anayat Lab TotaVNA Prep am RA 51700 ORMSh1417:19 GDB TALSAC Toia*A Analysis E296 RA 1 andii d9/13/14 08:06 SfAA TAL SAC Toia*A Prep -6266 s1700 ,WOS71417:19 GDB TALSAC TutamA .Analysis 8290 1 51698 d90a/14'23.41 JRB TALSAC, Toiam Analysis Lipids 1 52231 09/d9/.1415:38 13.K TALSAC Tot-m Prep FIRA15Sox 52228 d9%08/1415:38 ELK TALSAC Client Sample ID:SITE 4B CHANNEL CAT R FILLETS Lab Sample ID: 320-9127-4 Date Collected:08/06/14 09:38 Matrix:Tissue Date Received:.08/28/14'09:45 Batch Batch Dilution Batch Prepared Prep Type Type Method Run Factor Number orAnayud Amyst Lab TOtaVNA 'Prep 829.0 - 51700 090/1417:19 GDB TALSAC TOLANA Amysia 8290 1 51998 08/10/14D0:23 JRB TALSAC TOta*A A—Wm Lipids 1 52231 08%OW1415:38 ELK TALSAC ToteVNA Prep HRMSSox 52229 09/0811415:38 ELK TALSAC TestAmerica Sacramento Page 19 of 934 10/06/2014 Lab Chronicle Client Evergreen-Packageing FKABlue Ridge Paper TestAmerica Job ID:320-91274 PFbject/Site:Tissue Client Samp eb: SITE 413 COMMON CARP R FILLETS Lab Sam le ID: 32M127-5 Date collected::08106114 1 3:20, Matrix:Tissue Date Received:08128/14 09:45 -_ . . .. .. Batch Balch D114M Batch .Prepared Prep Type: Type MOMDd Run Factor Wumhar "AnalyzW. Analyst Lpb TotaVNA Prep 829A RA 51700 '00/05/1417.19 GDB TAL SAC TcWVNA Analysis 8290 RA 1 62369 09/1314 06;44 SMA TAL SAC TGUM Prep a290 51700. 0_9165/1417.19 DOB TAL$AC TotaVNA Analysis 8290 1 51998 09716/1461:66 JRB TAL.SAC TOMM Analysis Lipids. 1 52231' W/08/lOUI0 ELK TAL SAC T=VNA Pn:p HRMS.Soc 52229 19103%141535 ELK TAL SAC Laboratory Rotimences: TAL SAC=TesiAmerica Sacramento,880 Mi slde.Pa*wdy,West Sa=Mnto,CA MOS.TEL(Q15)3735460 TestAmerira Sacramento Page 20 of 934 10/06/2014 Certiftation Summary Client Evergreen'Packageing FKABlue Ridge,Paper TestAmedca Job ID:320-9127-1 ProjecUSite.Tissue Laboratory.TestAmerica Sacramento All eer58611on4 held by this laboratory are listed Not a0 cerii Mt6ris are applicable to ttifs report Auft ty Program EPA Reglon Cer06lat1w IO Eaprretton Date A2LA - DgD.P_1AP - 2928-01 01-31-16 Aiaske(UST) State Pmgrsnl 1g UST-U55 92-1&13• Arizma. ,State ProDram 9 Azg7w 06-1,1-75 bib . .. ....... .................. Arka.nsa.e-s.DEO •. .... ........ .. ..StateProgram - ..:•........ ...8..6..... 8.-0691 ...... 0&17-15 Caliromia State Program g 2897 01c31.15 Colorado State Program 8 WA 06-31-15 Connecticut State Program 1 P""I 06-30-15 Fladda NELAP 4 E87570 0630-15 Hewett State.Program 9 WA 01-29-15 118nols NELAP 5 200060 03-17-15 Kansas NELAP 7 E,10375 1031-14 Louisiana NELAP 6 30612 0630-15' M1Wgen Stale Program --5 9847 01-31.15 Nebraska State Program 7 NE-OS-22-13 01-29-15 Nevada State Program 9 -CA44 0731-15 . . . .... ,. . ... .. . . New Jersey .. . . .. ..NELAP ....... . ...� .2 ... .CA005. ._06-74T6 New York NELAP 2 11665 04-01-15 Oregon NELAP 10 CA2DOODS 01-29-15 Oregon 10 E97570 06-30'15 Pennsylvania NELAP 3 9947 03-31-15 Terns NELAP 6 T104704389.06-TX 0"1.15 US Fish 8 W4dINe Federal LE14838&0 12-31=14 USDA Federal P330.11-0D435 12.3044 USEPAUCMR Federal 1 CADD044 11-08-18 Utah NELAP 8 QUAN1 02-28-15 Washingt0h State Pfograrn 10 C581 0595.15 West Vlrginla(DW) state pmgr 3 9930C 1231-14 wimbig state Program a UTMS-Q 01-2&15 Certification renewal pending-pertlfication considered valid. TestAmerica Sacramento Page 21 of 934 10/06/2014 Method:Summary Client E 6i0treen Pa6kageing FKABIue Ridge:Paper TesfAmerica Job ID:M2 giV-1 PrajeoSite:ll-sWe Method Udthud Description _ . Protocol .Laboratory 8280 Dimdns and Furans(HRGC/HRMS) SW848 TAL SAC upidsPercent Liplde TestAmeri*SOP TALSAC Protocol References: SWB48- rest Mettads For Evaluating Slid Wasle,PtryslraVChemical Methods',Third FAltlon,yovember,7908 And Its Updates: TestAmerica SOP.=TestA oica,Inc.,Standard Operating Procedure, Laboratory References: TAL SAC=TadMwira Sacramento,080 Riverside ParbM,West Sactamento,'CA 85005,TEL(618)373560b TestAme&a Sacramento Page 22 of 034 10/06/2D14 Sample Summary Client Eyergieerl Packageing FKABlUe Ridge Paper TestAmerica Job ID:320-912Z PiOJecusas'Tissue Leb's.mgaID CMiHsw*841) Malfc: calk-dw. Ret.iv.a 320-91274 SITE4A CHANNELCAT R-FILLETS Tissue wout141192 oB/2B14'08:45 320-9127.2 SITE 4A:COMMON CARP R-FILLETS Time 04*h4 i 1;46 O jWf4 60,45 320.8127-3 SITE 4A COMMON.CARP We WHOLE BODY Tribe bwwi4i6:od 6aas7l4dg:4B 32051274 SffE 4B CHANNEL CAT R FILLETS Tissue paWI4 053a 0a12B114 Qa:45. 32"127-5 SITE 4B COMMON CARP FILLETS Tissue OB/0671913:20 OBJ29%14 DB:A.S TestAmerica Sacramento Page 23 of 934 10/06/2014 'DIOXIN ,MANUAL INTEGRATION, SUMMARY Lab Name: TestAmerica Sacramento Job No.: 32D-912:7-1 SDG go.s Instrument ID: 502 Analysis, Hatch ,Number.: 49055 Lab Sample ID: IC 320-4'9055/4 Cient. ,Sample ID: Date, Analyzed: 08/03/14 11:32 Lab F le::ID: 05AU145D2_004.fl GC. Column: DE-225 ID! 0,32',(mm)' COMPOUND NAME RETENTION MANUAL. INTEGRATION. 'TIME. REASON ANALYST 'DATE' 37C14-2.,3,7,8-TCDD 1;4.:77 Peak Tai-1 stephensk O8�/08/1:4' 161-48 2,3,7,8-TCDF - '16„-11. Haserine' stephensk 08'/05/1;,4 16:48 8290 Page 14 of 93,4 10/06112014 DIOXIN MANUAL INTEGRATION.:SUMMARY Lab .Name: TestAmerica Sacramento Job No.: :320-912741 SDG No. : Instrument ID: SDZ Analysis, Batch :Number-: 52$09 Lab Sample ID: 320-9127-2 RA Client Sample ID: 'SITE 4A COMMON CARP R-FILLETS RA Date Analyzed: 09/13/14 05:29 Lab Vile-ID:- 1i25B14A5D2_011,d G6 Column: DB-225 ID: 0.,32(mm) COMPOUND NAME. RETENTION 'MANUAL INTEGRATION, -'DIME REASON ANALYST DATE 2,3,7,:8-TEDF 16..1-1. 'Poor chYom"at'og aphy hernandezz 09/.1'S/14, .14:28 1 8290 Page 25 of 934 10/06/2014 DIOXIN MANUAL INTEGRATION SUMMARY Lab Name: TestAmerica Sacramento Uob,lb'.. 320-91:27-1 SDG No.: Instrument ID:. 9D5- Analysis Batch Number: 469§7 Lab. Sample ID: IC 320-4'6897/3 Client, Sample;.ID: Date• Analyzed: 07/09/14 13.38 Lab File ID: :0'9jLl4A9DS_003,d'. .GC, Column3 DB=5 ID' 0:32(mm) COMPOUND NAME - RETENTION - - ;MANUAL INTEGRATION TIME REASON ANALYST DATE 2,3,7,8-TCDF 1 17,40 -Peak-Tail sYephensk 07/I0/14. ,12:4:7 8290 Page. 16: of: 934 ..10/06/ZO14, DIOXIN MANUAL INTEGRATION SUMMARY Lab Name: TestAmerica Sacramento. .Job No.: 320-9127=1 SDG No.: Instrument ID: '9D5 'Analysis .Batch Number;: 5199B 'Lab Sample ID: CCV 32.0-,51:998/2 .Client Sample ID: Date Analyzed: 09/09714 17:42 Lab File. ID; 09SE14B9D5..002.d GC Column: DB-5 COMPOUND NAME RETENTION MANUAL INTEGRATION TIME REASON I ANALYST I DATE 11,2,3,4,7.,B-HxCDD 31.76 Poor bhromatography barnettj: 09/10/19t 10:24 13C-1,.2.,3,6,7,8-HxCDD 31.83 Poor -chromatography barnettj_ 09/.10/I9 10:24 1,2,3,6,7,E-HxCDD 31..89 Poor ahromato ra h g P.y barnettj. 09L10/14 10:,24 Lab Sample ID: 320-912.7-2 :Client Sample ID: SITE 4A COMMON CARPIR-FILLETS Date Analyzed: 0910YI14 22:.58 .Dab File 1D, 09SE14B9D5_009vd GC Column: DB-5 ID: 0.327(um) COMPOUND NAME RETENTION MANUAL INTEGRATION TIME REASON I ANALYST DATE 13C-1,2,3,.6,7,B-HxCDD 31,'.83' .Split Peak hernandez 09/15/14� 16:46 1 Lab Sample ID: 320-9127-3 ClieAt :Sample ID: SITE 4A;COMMON CARP' WH WHOLE BODY Date Analyzed: 09/09/14 231-41 .Lab File„ID: .09SE14B9D5_010..d GC-'Column:: DB-S- ID: 0..32.(=) COMPOUND NAME RETENTION MANUAL INTEGRATION. TIME REASON ANALYST DATE L,2,3,6,7,8-HxCDF -Split Peak ,hern'andez 69/15/14, 16r52 1. 13C-1,2,.3,6,7,8-HxCDD 31..84 :Split Peak hernandez 09/15/14; ;16:52 1,2,3,6,7,E-HxCDD i' 31,85 'Split .Peak bernandez. 09/15/14. Y6:.52 1. 8290 Page 27 of :934 10/06/-20.14 DIOXIN .MANUAL INTEGRATION SUMMMY Lab Name: TestAmerica 'Sacramento, Job,No. : 320-9127-1 SDG No. : Instrument ID; 965 Analysis Batdh, Number: 51.998 Lab Sample ID: 320-9127-5 Client Sample ID: SITE 4B COMMON CARP R FILLETS Date Analyzed: 09/10/14 01.:Ofi Lab File ID: '09SE14B9D5_0122.d GC Column* DB-5 ID 0:32(mm) COMPOUND NAME', RETENTION MANVAL INTEGRATION TIME - REASON ANALYST DATE 13C-1,2,3,6,7,,8-HXCDD 31.86: Split Peak 'hernandez•. 09/15/14; 13:00 1. 1,2,3,6, 1,8-HBCDD 31.B8' Split Peak Fernandez 09/15/1'4 17.-00 1 1,2,3,4,6;7,8-HpCDF 33.71 Unspecified 8290 'Page 2B' of 034 10/06/2014, :REAGENT TRACEABILITY SUMMARY Lab Name: TestAmerica Sacramento .Job No.. : 320-9127-1 SDG No. : Reagent Parent Reagent' Exp Prep Dilutent Final Volume Reagent ID Date Date Used Volume. Reagent,ID Added 'Analyte Concentration, HREOWM 00023 01/24/17 O6/24/13 C14, Lot•STHC2541V -0 mD, NRDXNCP_00022 0.04:mL 13C-2,3,7,8-TCDF. 0.01 uq/mL 2,.3,7,8-TCDF O A5 u /mL I . XRD%NCP_00022 OS/24/21 CIL,_ Lot 'R663: (Purchased.Reagent) 13C52,3,7.,,8-TCDF 7 u 7mL 2,3,7,8-TCDF :5 u /mti BRDxHCP 00025 1'1/13/14. 11/13/13 C14; Lot STBC2591V ' 5 mL HRDXNCP_00024 1'mL 19C=2,3,7,8-TCDD 40 pq/uL 13C-2,3,1,8-TCDF 40 pg/uL 2,3,7,8-TCDD 40 q/uL" OB/O1/17 2,3;7,B-TCDF 40 . /uL .HRDXNCP 00024 CIL, Lot ;ER082007-OS (Purchased Reagent) 13C-2,3,7,8-TCDD 200 13C-2,3,7,8-TCDF 200 ng/mL .2,3,7 8-TCDD 200 nq/mL' 2,3,7,8-TCDF 200 na/mL HRmuiiC 00022 11/21/14 02/26/141 C14, Lot STRC2541V '0:5 to1. HRDXNIDA 00146. 0:25 mL 13G-1,2,3,4,6,7,Ce HpCDD' 100' ng/mV 13C-1;2,8,7.,8-PeCDD 100 ng/mL 13C-1,.2,3,6;74B-HXCDD 300 'ng/mL 13C-1;2,3,7,8-PeCDF 100 .ng/mL 13C-OCDD 200 nq/mL 13C-1,2,3,4;6f7 8-H CDF 100 nq mL 13C-.2,3, ,,B-TCDD 300 n /mL 13C-2,3;7,8-TCDF .300 nq/mL NRDXNIDA00156 0.125 mL '13C-1,2,3,4,7,8-HxCDF 100 n /mL KRDXNSP_00032 0;01 ML 1,2;.3,4;6,7;8-HpLDD 25' ng mL 7.,NRCDF' 25 ng n,L 9-N CDF 25 ng/mL 1';2;.3;4,7,B-XxCDo 25 ng ,nI, I•,2,3,4,7,8-HxCDP` 25 ng/mL 1'.2,3;fi,7;8-HxCDD 25'. n /mli .1;2,3,6,7.,8-HxCDF 25: n /mL :1,2,3,7,6,9-HxCDD '25 ng/mL .1,2,3,7,8,9-HXCDF 1,2,.3,7,8-PeCDD 25' ng/mL 1l2,.3,7,B-PeCDF ,25: ng/mL 2,'3,4,6,7,'B-HxCDF '25'.n /mL '2,d;4,7,:8-PeCDF .25, n /mL 2,3,,7,B=TCDD 10 ng/mL. 1,3,7,8=TCDF '10n /mL OCDD 50 ng/mL. OCDF 50 ng mL HRDXNSU 00077 ,0:025 mL .37C1"4-2 3;7,8-TCDD .HRDY.NIDA_00146 03/09/l7, 02/03/14 Isooctane;..Lot 250.mL HRDXNIDA 00136 10"ng/mL 0000026263 1 mL 113C-1,'2,.3;4,16,'7,8-NpCDD O',2'uq mL HRDXNIDA.00137 1 mL 13C-1/2,:3,1,1-PeCDD 0.2.uq/mL HRDXNIDA 00138 1 mL .13C-1,2,3,:6,7,8-HXCDD 0.2[ug/m1, HRDXNIDA 00139 1 mL 13C-1;2,3,7,B-PeCDF NRDXNIDA,00140 10 mL T33C-OCOD, HRDXNIDA=00142 1 mL 13C-1,2,3,4',6,7,8-H CDF OS2iu /mL HRD%NIDA-00143 1. mL- 13C-2;3,7;8-TCDD' 0.2 ug/mL Page 29 of `934 10/06/2014 ,REAGENT TRACEABILITY SUMMARY Lab' Name: TestAmesica 'Sacramento Job No. : 320-9127=1 SDG No.: Reagent Parent Reagent' Exp prep Dilutant Final Volume Reagent ID Date Date Used ad Volume Reagent' ID 'Added Analyta , 'Concentration NRDXNIDA 00149. 3imL 19C-.2,3,7,6-TCDF..HRDXNIDA 00135 03/09/17 CIL, Lot ER111030-01 (Purchased Reagent) 13C-1,2,3,4,.5;7,.8-H CDD' S0 ug/mL'..HRDXNIDA 00137 03/09/17 CIL, Lot' ER030907-02 (Purchased Reagent) 13C-1,2>.3,.7,8-PeCDD: SO ug/mL ..NRD%NIDA'00138 01731/19 CIL,. LotER010209r03 (Pt)LCNaaed Reagent) 13C=1,2,3.6',•7,8-HxCDD 50 u /mL ..HRDXNIDA 00139 01/01/21 ,CIL, Lot. ER01211-01 (:Purchasetl Aea-ent) 13C-L,2,3,7,8-PeCDF 50.Uq/mL ..NRD%NIDA 00140 D7/33720 CIL, Lot ERD7.3 S10=01 (Purchasetl Reagent) 13C-0CDD 10:u /ml ..HRDXNIDA 001:42 11/30 21 CIL, 'Lot,ER102711'-02 (Purchased'.Rea ent) L3C-1,2,3,4,6;J.8-N CDF 50:ug/mL ..HRDXNIDA-00143 06/30/17 CIL, Lot •ER060407-01 (PUrchased,Reagent) 13C-2,3,7;8-TCDD 50 u /mL ,.HRDXNIDA 00144 09/25/: CIL,�Lot ER092507-01 (Purchased Reagent) 13C-2,3,7,8-TCDF 50 .0 /mL NRDXNIDA_00156 OS/30/17, 02/20/14 Ieooetana, lot IOU,mL HRDXNIDA 00152 0:8 mL 13C-1,2,3,4;7,8-HXCDF �0,4 ug/mL '0000026263' ..HRDXNIDA 00152 07/3120 CIL, Lot ER072810-02 ;Purchased Reagent) 13C-1,.2,3,.4,7,.8=HxCDF 50 ug7mL .HRDXNSP_00032 02/27/15 02/27.14: Acetone, Lot. 0000059687 5 mL HRUAWNSTA OD005 1 ML 11213 6;?,8-HpCDD'. 1.25.Uq/mt 1,2,3;4,.65.7,8-,,HpCDF' 1:25-ug/mL 1,2,3;A,7,8,9-HPCDF 1.25 ug/mL I' 1,.2,3)A n7,8-HxCDD' 1.25 u /mL 1,H;3 4,7-,8=HxCDF .1.25 ug/mL 1,2,3,.6,.7.,8,HXCDD 1..25 u /mL b,,,U-HxCDF 1c25,U /mL L,2}3;.7,8y9-NXCDD' 1.25 u /mL 1,2,3;.7,8'9-HxCDF 1,25•ug/mL 1,2;3;7,8-PeCDD 1.25 u /mL 1,2;..3,7 .8-PeCDF 1.25 ug/mL 2,3,4,6,7„8-RxCDF 4.25 pug/mL 2i3,4,7}8-PeCDF 1..25 u m1 2131.7',S-TCDD 'O.5,ug/mL 2,3)7,.8:-TCDF 0.5 ug/mL GCOD 2:5 .u9 m1 OCDF. 2.5 'u9/mL ,.HR8280SNSTA 00005' 09/30 19 CIL, Lot'ER091409-01 (Purchased Reagent) 1,2,3;A,6'.7,.8-HpCDD 6.-25 u /mL 1,2,3p4,6,-7�U-HpCDF 6.25 pug/mL 1,2;3,4,.1,8,9-HpCDF 6'.25•ug/mL 112L3,407d-HxCDD- 6.25:Ug/mL 1,2,3;.4,7iO-HxCDF '6'.25.ug/mL . 1,2;3;6;.7.,.6-HxCDD. 6.25 ,u /mL 1,2,3p6;1;8'-HxCDF 6.25,u /mL 1,2g3;7,.8,9-HxCDD' 6'.25'ug/mL 1,2,3,9;es9-HxCDF 6.25',u /mL 1,213;7p8-PeCDD, b'.25:u /mL 1,2;37,8-PeCDF 6.25 v /mL 2).3,4,.6,7,.8-HxCDF' 6.25 Ug/mL 2;3,4;1,8-PeCDF bs25'U /mL 2,3;7;8-TCDD '21 5-un' 9;3, O TCDF H ,ug/mL CDD 12;5 u mL OCDF 12..5.0 /mL .HRD%NSU_00077 11/22/14. 11-22/13 I00002626 Lot 25 mL .HRDXNSU=00076 1,mL 37C14-2,3,7,8-TCDD -0.2 ug/mL 0000026263' - Page 30' o£ 934 10/06/2014 REAGENT TRACEABILITY SUMMARY' Lab Name: TestAmerica Sacramento Job -No.: ,320-9127-1 SDG No.: Reagent Parent, Reagent Exp Prep Dilutant Final Volume. Reagent ID Date Date Used Volume Reagent ID Added Analyte 'Concesttation..HRDXNSU_00076 OS 31/20 11/22/13 Isooctane, Lot. 12 mL. HRDXNSU-00075 1.2 ML 37C14-2,3,7,E-TCDD 0000026263 - 5 ug/mt ..:HRDXNSU 00075 OS/31/20 CIL,. Lot ER052010 (Purchased Rea ent) 37C14-2;3,.7y B-TCDD 50 ug/mL KRIONIDA 00166 OS/14/15 OBZ14'/14 Acetone, Lot 0000062T48 •500-mL HRDXNIDA_00146 5 mL 13C-1;.2,3,7;8 9-NxCDF 2 P9/uL 13C-1;2;3,4i6,7,8-HpCDD' 2 g/uL 13C-152,3,7,B-PeCDD• 2 p 7ul; 13C-1,2,3,6,7;8-HXCDD' 2 g/uL 13C-1,2,3,7.,8-PeCDF 2 /uE 13C-OCDD 4'- /uti 13C-2,3,4;6,7,8-HpCDF' 2 /uL 136-1,2,3,4,6,.7,8-H CDF 2 /uL 13C-2;3,7,8-TCDD 2 g/uL 13C-2,3,7,E-TCDF. 2p /uL 13C-1,.2,.3,6,7,:B-NxCDF. 2 pg/uL HRDXNIDA 00162 2-5 ML 13C-1,2,.3,9,,7.,.8=3NCDF 2 pg•uL 13C-1,2,3,4,7,8-HXCDD; 2, g/uE, 13C-1;2,3,4,7,.8,9-HpCDF' 2' g/uL ' .HRDXNIDA 13C-.2,3,4,7.,B-PeCDF 2 /uL 00143 03/09/17 02/03/14 .Isooctane, Lot '250—ML HRDXNIDA 1 ML 13C-1,2,3,7,B,9-N%CDF � 0000026263 0.2 ug/mL 'HRDXNIDA 00136 '1 ML Y3C-1;2,3,4,6,7,.B-H CDD 0.2 ug/mE HRDXNIDA 00137' '1 ML .13C-1.;2,3,1,8-PeCDD 0-2 u /mL HRDXNIDA 00138. 1;mL.'13C-1,2,3,6;J,BvHzCDD' 0.2 u 7mE .HRDXNIDA 00139 1 ,ML :13C-1,2p.3,7,8-PeCDF 0.2 ug/mL HRDXNIDA 551459 10 ML 13C-OCOD 0.4' u /ml HRDXNIDA 00141 '1 MI; '13C-2;.3,4,6,7,8-HXCDF 0.2,ug/mL: HRDXNIDA 00142- 2 ML :13C-192,3,4,6,7,8-HpCDF 0.2 ug/mE HRDXNIDA 001431 :1 ML. ,13C-2,3;7,8-TCOD 0.2 u /mE: HRDXNIDA-.00144. 1 •mL .13C-2,3,7,8-TCDF 0.2 u /m1 •HRDXNIDA-00145 .1.mL 13C-1,2,3,6 '7,B-HzCDF 0.2 ug/mL ..HRDXNIDA 00135 30/07/17 CIL, LOt ER020705-01 (Purchasetl Reagent) 13C-1;2,.3,7,8,9-NxCDF SOug/mL ..HRDXNIDA 0013fi I1/30/20! 'CIL, LOt.ER111010-01 (Purchased Reagent) 13C-1,2r3,-4,'6 78-X CDD •50 ug/mL .-HRDXNIDA 00137 03/09/17 'CILr Lot ER030907-02' (Purchased Reagent)- 13C-.1';2,3;7,8-PeCDD ,SOuq/mL .:HRDXNIDA'00138 O1/31 19 CIL, Lot EA030209-01 (Purchasetl' Reagentl '13C=1,2,3,.6,7,:8-HxCDD 50, ug/mL ..HRDXNIDA 00139 O1gO1Z21. CIL, Lot.ER01211-01 (Purchased Reagent) 13C-1,2,:3;7;B-PeCDF 50 u /mL ...HRDXNIDA 00140 ,07/31/20 'CIE, L'ot ERD73610-.01 (Purchased'.Red Reagent) IX-0CDD 10' ug/mL: HRDXNIDA OOldl 03/31/l, .CIL, Lot ERD31507.-03 (PDLCna6etl Reagent)' '13C-2r3,4,6;7;8-NxCDF 50 ug/mL ..HROxNIDA 00142 : 11/30l21. CIL, Lot, ER1027.11c 02. (Purchased Reagent) 13C-1,2,3i4;6;1.;8=HpCDF SOug7mL ..HRDXNIDA 00143 'O6/30/17 'CIL, Lot. ER060407-01 (Purchased Reagentl: -13C-2,3,7;0=TCDD '50u ..HRDXNIDA g0144 09/25717 CIL, Lot ER092507-01 (Purchased Reagent) 13C-2,3 7,8-TCDF' 30 u /mL' :.HRDXNIDA 00145 06/30/17 'CIL, Lot!ER053107-03' _ (Purchased Reagent) '13C-1;2 3;6,7,8-NxCDF SOu /mL .HRDXNIDA 00162 05/30/I7 07./1OZ14 I00002626 lot 25 ML RRD%NIDA_00152 0.2 ML 33C-1,2,3,4,7,8-HzCDF 0.4 ug/mL 0000026263 HRDXNIOA,00153 0:2 mL '13C-1,.2,3r4,7,B-HxCDD HRDXNIDA 00154 0.2 mL..13C-1,2,3,4,7,.B,9-HpCDF 0.4 ugJmL HRDXNIDA.UU155 0.2 mL 13C-2,3,4,7,8-PeCDF 0:4•ug/m1 ..xROXNIDA' 00152' 07/31/20 CIL, Lot,EA072810-02 (Purchased Rea ent)! 13C-1,;2,3,4;7;8-HzCDF 50 u /mL ..HRDXNIDA 00153 30/31/21 ,CIL, Lot ER102711-01 (Purchased Reagentp 13C-1,2,3,4,7,8-HxCDD 50 uq/mL Page 31 of 934 10/06/2014 REAGENT TRACEABILITY SUMMARY Lab Name: TestAmerica Sacramento Job. No.-: 320-9127-1 SDG No.: Reagent parent Reagent Exp Prep •Dilutant Final_ Volume Reagent ID Date, Date• 'Used Volume Reagent ID Added Analyte. Concentration .:HRDXNIDA 00154, 05130/111 CIL, Rea 13C-1 10l3 oE1060:.HRDXNIDA 00155 Ped' ee ;2,3;9;T,8;9-HpCDF 50'ug/mL ent)' ,13C-2,3,4;7,9-PeCDF 50 uq/mL ll ®tD=8_00049 05/071,15, 05/07/14 C14, Lot STEC7287V 100 ML HRDXNIS 00048 2 ML, 13C-1,2,3;7.,8,9-N1CDD 0.1 ug/E 13C-1,2 3,4-TCDD 0,:I,ug/mL .HRDXNIS 00048 . '05/07/15 OS/0?/14 .Isooctane, .Lot i"3?59 10.mL. NRDXNI5 00046 1 mL.i13C-1,2 .3,7;8,9-HXCDD 5'u9/mL .HRDXNIS '00047 1ML 13C-1,2,.3,4-TCDD 5u /mL ..HRDXNIS 00046 OB/20/1B 'CIL, Lot ER082508-01. (purchasedReagent) 13C-1„2,3;7,8;9-NXCDD 50 uq/mL ..HRDXNIS 00047 O6/O1/20' CIL', LOt.ER06071001 pPu rchased Rea ent( '13C-1;.2,3.4-TCDD 50 ug/m eRDXNL2_OD013 ,11/21/,14 02/24/14. C14; Lot;STBC2541Y 1 mL 'HRDXNIDA-00146' 0.5 ML, 13C-1,:2, 6,7,B-H CDD .100 ng/mL 13C-1;2,3,7,B-PeCDD. 200 n /mL 13C-1;2;3,6,7,8-RxCDD. 100 n /mL --13C-1,:2;3,7,8=PeCDF 100 n /mL 13C-OCDD: .200 ng/mli '13C-1,2;3,4,6,7.8-11 CDF 100 n /mli 13C-2,3,7,8-TCDD '100 ng/mL '13C-2;3,7:,8-TCDF '100 n /mL 'HRDXNIDA 0015C 0.25'mL 13C-1,2,3,-0;7,8-R%COF' :100 ng/mE HRDXNIS_00053 'SImL '13C-1,2,.3;7,8,9-NXCDD 100 ng/mL 13Cc1,2,3,4-TCDD 100 n /mL HRDXNSU_00079 '0.3125'.'37014-2,3,7.,8-TCDD 0.25 ng/mL mL HRDXNTA 00038 -Y.125.mL, 1)2,3,4,G, 'a -HPCDD 2..5 Tg/mE- 1;2,.3,4,6,7,8-HpCDF 2:5 n9/mE 1,2,3,4,7,8,9-HpCDF 2.5 ng/mL 1;2,3,4;7,8-HxCDD: 2.5 ng/mL 1,2,3,4,7,8-HxCDF' 2.5"n /mL 1,2,3,6,7,8-HxCDD. :2.5 n /mL 1,2,3,6,7.,8=NxCDF 2.5 n /mL 1,2,3;7,8,9-NXCDD 2:5 ng/mL. 1,2,3,7,9,9-HXCDF 2.5 ng/mL L,2,3,7,8-PeCDD• 2.5 n /mL' 1J2.3,7,8-PeCDF 2.5 ng/mL 2,3,4,6,7.,8-HXCDF 2.5 n /mti .2,3,4,7,8-PeCDF 2.5 n /mU .2,3,7,8-TCDD O.:s:ng/mE 2,3;7,8-TCDF 0.5 ng/mL OCDD ,5 ng/mL' OCDF 5 ng/mL .HRDXNIDA 00146- 03/09/17 02/03/14 Isooctane, Sot 250 ML, HRDXNIDA-OD136 '4'mL 13C-1,2,3,4,6,7,,8-HpCDD' 22 ug/mL' 0000026263 '.HRDXNIDA' 00137 1 :ML 13C-1,2,3,7,8-PeCDD ,0.,p.0 /mL ARDXNIDA'00138' '1'ML '33C-1,2,3,6;7,8-HxCDD'. 0:2 a /mL:• 'HRDXNLDA 00139 '1 'mt .13C-1,2,3,7:,8-PeCDF 0:2 ug/mL' HRDXNIDA 00140 10.mL 1dC-0CD5 04 ug/mU '.HRDXNIDA 00142t -1 ML :13C-1,2,3,4,6;7,8-H CDF 0:7 u /mL HRDXNIDA 00143' 1-ML 13C-2y3,7,8-TCDD U.2 u /mL HRDXNIDA 00144. '1 ML 13C-2,3,1,8-TCDF 0:2 u /mli Page ;3Z of;.934 10%061201'4 REAGENT TRACEABILITYSUMMARY Lab Name: TestAmerica .Sacramento Job No.: '320-9127-1 SDG No.: Reagent Parent Reagent Exp Prep Dilutant Final Volume Reagent ID Date Date Used Volume. Reagent. ID Added Anal to ..HRDXNIDA 00136 11/30/20 CIL, Lot ,ER11.1010-01 Y 'Concentration ..HRDXNIDA 00137 03/09/1T CIL;.;Lot ER030907-02 (Purchased Reagent) 13C-1,2,3,d,6,?,8-N CDD 50 u /mL ..HRDXNIDA 00138 01/31/19 CIL; Lot ER010209-01 (Purchased Reagent) 13C-3,2,3,J,.8-PeCDo- 50 'ug/mL ..HRDXNIDA 00139 01/01/21 CIL, Lot:ER01211-01 (Purchased.Reagent) 13C-1,.2,3,6,-1,8-HxCDD, 50'ug/mL (Purchased Reagent) 19C-1,2,3,.7,8-PeCDF 50 ug/mli ..NRDXNIDA-00140 07/31/20 CIL, Lot ER071630-01 jPurchased'Reagent) 13C-OCDD 10 �u /mD. ..HRDXNIDA-00142 11/30/21: CIL, LotiER102711-02 (Purchased'Reagent) 13C-1,2.3 4,6;7,.6-H CDF 50 'uq/mL .:RRDXNIDA 00143 06/30/11 CIL;-Lot'ER060407-01 (Purcnased,ReaOent) 13C-2,3,7,8-TCDD 50 u /mli ..HRDXNIDA 00144 09/25/17 CIL, Lot �ER092507-01 (Purchased Aeagertt) 13C-2,],7,8-TCDF 50 .0 /mD .HRDXNIDA_00156- OS/30/11 02/20/14 Isooctane, Lot.. 100 mL :HADXNIDA_00152 O.B 4nL 13G-1,2,3,4,7,8-HXCDF 0.4 •u /mL 0000026263+ 9 ..HRDXNIDA'00152 07/31/20 CIL, LbLER072830-02 (Purchased Reagent)- 13C-1,2,3,4,.7,8-HXCDF 50 u /mL; .HRDXNIS_00053 11/21/14 11/21/13 C14, Lot STBC72B7V' 100 mL HRDXNI9 00052 •2;mL, 13C-1.,2,3,.7,8,9-HxCDD, 0.1•ug/mL 13C-1,2,3,4-TCDD 0.1`ug/mL ..HRDXNIE 00052 31/21/14� 11/21 13 .Isooctane, Lot 10 mD .XRDXNIS..00050 1:mL 13C-1,2,3,7,.8,9-HxCDD. 3 uQ/mL 0000026663 '.HRDXNIS 00051 1mL' 13C-1;2-,3',:4-TCDD 'S ug/mL ...HRDXNIS 00050 02/28/21 CIL,-Lot ER020141-02 (Purchased Reagent) 13C-1,2,3;7,B,9-HxCDD 50 ug/mL ...XRD%HIS 00051 11/22/14 CIL, Lot ER06013001 iPurchased Reagent) 13C-1,2,3,4-TCDD" 50 ug/mL .HRD%NSU_OOD79 11/22/14' 01/10/1'4' Isooctane, Lot '500 mL 'HRDXNSU_00077 2;mli 37C1/-2,3,7,8-TCDD O'.0050 ug/mL 0000026263. ,,HRD%NSU_00077 11/22/34' '11/22/13 1,1sooctane, Lot, 25 mL NRDXNSU_09076 IL .37C14-2,3,0,8-TCDD 0.2 og/mt .NRDXNSU_00076 05/31/20 11/22/13 0000026263 Isooctane, Lot 12 ML HRDXNSU 00075 1:2.mL 37C14-2,3,7:,8-TCDD 5 ug/mL - ...HRD%NSU 00075 05/31/20 CIL; Lot iER05201'0 - (Purchased Reagent) 37C14-2,3,7,8-TCDD 50 ug/mL. :HRD%NTA 00038 11/22/14. 11/22/13 Isooctane, I:bC 25 mL :HRD%NTA_0003.7 0.25 ML 1,2;3,4,6,7,.8-HpCDD: 20 ng/mL 0000026263 - 1,2,3,4,6,7.,8-HPCDF 20 ng/mL 1,2y 3y4,1,Bi 9-HPCDF 20 ng/mL 1,2,3,4',7,8-HXCDD 20 n /mL L,2,3,4;7,8-HXCDF- 20 .ng/mL 1,2,3,6,7;8-H%CDD 20 ng/mL 1,2;3,6,7,8-HXCDF Y0 m jmU 1,2,3;7„H,9-HxCDD 20 n /mL•. 'l;2,:3,7,8,9-HXCDF 20 ng/mL ,.3,7,8-PeCDD 20 n' /mD .1,2,3,7,8-PeCDF 20 ng/mL, 3`3:Q,6,7,8-HXCDF 20 nq/mL 2;'3,4,7,8-PeCDF 20 n /mL 2„3,7,8-TCDD 4. ng/mL 2,:3,'1,B-TCDF 4 n /mL OCDD 40n /mL ..HRO%NTA 00037 03%31/20C IL, Lot EA031010-01 OEDF 40' n mL (Purchased Reagent) 1,2,3 , ,7.,.8-H CDD 2' a /mL -NpCDF 2 u mL1,2,3467,.8 -1,2,.3,4;7,8,9-NpCDF 2 u /mL 1;2,3,4,7,8-HxCDD 2' u mL ,1,2,3,4,7,8-HXCDF 2. ug/mL 1,2,.3,6,7,8-.HxCDD 2:ug/mL Page 33 of 934: 10/0'6/2014 REAGENT TRACEABILITY SUMMARY Lab Name: TestAmerica Sacramento Job. No. : 320-9127=1 SDG No. : Parent Reagent Reagent Exp Prep oilutant Final. Volume, Reagent ID Date •Date Osad' Volume Reagent ID Added Analyte Concentration 1,2r3;6;7.,8-HxCDF 2 u /mL 1,2,3,-7,8,9-HXCDD 2 u9/mL 1,2,3,7.,8,9=HxCDF 2 uq/mL '1;2r3;7,.8-PeCDD 2 u 7mL; 1,:2;3,9,8=PaCOF- 2 u /mL 4,'.6,7,8=HxCDF 21 u /mL 2,,3,E' 8=PeCDF 2 ug/ML. 2,3,7,:8-TCDD1 0.4 u /mL 2,3,7;8-TCDF 0.1, OCDD 1 u /mL OCDF A, u /mL aRDxNL3_00011 11/21 14 02/24/14 C14, "Lot:STSC2541V' 0.5 mL .HRDXNIDA 00146' - 0.25 mL AW-.1,2,3,4,6,7{B-HpCDO 1 00 ng/mt. :33C=1;2,:3,7,8'.PeCDD' 100 ng/mL 8-HxCDD- 300 ng/mli 13C-1,2,3,7;8-PeCDF' 100 ng/mli '33C-OCDD 200 ng/mL 13C-1,.2;9,4,6;7,8-N CDF '100 ,ng/mL 43C-2,3,7,8-TCDD 100 ng/mD. 13C-2,3,7•,8-TCDF 100 ng/mL, HRDXNIDA 00156 '0:125 mL :b3C-1p2,3,4,7.,8-HxCDF 100 ng mL HRDXNIS_00053 0,5 mL 13C-1,.2,3,7,8,9-HxCDD. '100 n /ML '13C-Iy 2,3 4-TCDD 100 n 'mL ,HRDXNSU]00079 D,625 mL .37C14i2,3,7,8-TCDD 1:ng/mL. HRDXNTA_00038 0,25 mL 1,2,3,4,6 7,8-HPCDD 16 n /mL 1,2,3,4,6,7,8=HpC F' 10 ng/mL. 1,2,3,4,7,8,9-HpCDF 10'.ng7-L' 1;2;3,4,7,8-HxCDD+ 10 n /mL 1,2,3,4;7,8-HxCDF 10 ng/mE 1,2,3,6;7.,8-HxCDD 10 n /mli 1,2,31 6,7;8-HxCDF' 10 nq/mL "1,;2,3;7,8,9-HxCDD" - 10 ng/mL 1,2,.3,7.,8,9-HxCDF 77 10 ng/mv 1,2,3,7,8-PeCDD' - 10 ng/mL' b;.2,3,7;8-PeCDF 10 no/mL 2,3,4y6,778-HxCDF 30 ng/mL 2,.3;4,7,8-PeCDF 10 ng/mL 2,3,7;8-TCDD ;2 ng'/mL' :OCDD :BCOF 2 ng/mL OCDD 20 n /mL. .HRDXNIDA 00146 ACD£ 20 n /mL 03709/17 02/03/14- Isooctane; 'Lot 250 mL..HRDXNIDA-06136• '1�mL'd3C-1,2,3,4,6,7,8-HpCDD 0.2 ug/mL 0000026263 HRDXNIDA OD137 :1 mL 13C-1;2,3,7,8-PeCDD HRDXNIDA D013B' '1 mL, 13C-1,'2,3,6;7,8-HxCDD' 0.2 ug/mL HRDXNIDA 00139 '1 mli :13C-1`;2>.3,7;8-PeCDF HRDXNIDA.00140 .10 mL 33C-uuuD, RROXNIDA 00442' .1•mLI13C-1,2,3,4,6r 7,8-HpCDF ;0.2 ug/mL HRDXNIDA 00343' 1mD "13C-2y 3,1,8-TCDD '0:2 ug/mL .Page,34 :of 034 10/.06/2014 REAGENT TAACEABILITY. SUMMARY Lab Name.: TestAmerica Sacramento Job No.:r 320-.9127-1, SDG No. : Reagent Parent Reagent EXp. Prep Di'lutant Final Volume Reagent ID Date Date •Used Volume Reagent ID Added% Analyte. Concentration HRDXNIDA'0014d - 4 ML 13C-,2,3,7,8-TCDF 0.2:u /mL ..HRDXNIDA 00137 11/30/20 CIL,.LOG ER11301D-01 _ (Purchased Reagent) 13C-L2,3,.4;6,7,8-R CDD 50'u /mL ..HRDXNIDA 00137 D3/09217 CIL, Lot ER030907-0Y (Purchassd.Rsagent) 136-112,.3,7y8-PeCDD 50.ug/mL ..HRDXNIDA 0013B -01/31/19 CIL',, Lot ER010209-01 (Purchased Reagent). 13C-1,2,3,6,I.,B-HzCOD .50'u9/1L ..HRDXNIDA 00132 01/01/21 OIL, +Lot'ER01211-01. (Purchased Reagenth 13C-1�2,3,4rrB-PeCDF DSO uq/mL ..HRDXNIDA 00140 07/3T/20 CIL, LOt:ER071610-01 (Purchased'Rea ent): 13C-OCOD 50:u /mL ..HRUXNIDA OU142, 11/30/21 CIL; Lot.ER102711-02 (Purchased.Reag ent)! 13C-1,-2 3 (d',�8,7;8'HpCDF 'SO':u /mL ..HRDXNIDA 00143' 06/30/17 CIL, Lot. ERO60407-01 (Furchased Reagont) 13C-2,3,7,B-TCDD, SOIu /mL ..HRDXNIDA 00144. 09/25717. CIL, Lot.ER092507-01 (Purchased Reagentl 13C-2,3,7,8-TCDF SO.0 mL. .HRDXNIDA 0015E 'OS/30/.17 02/20 14 Isooc[ane, :Lot 160 mL HRDXNIDA.00152 ,0.8 mL '13C-.1,2,3,4';7,8-HXCDF 0,4 ug/mL 0000026263 - .:NRDXNIDA 00152 07.31/20, .CIL, Lot ER032810-02' (Purchased Reagent), 13C-.1;.2;.3,4,W,8-HXCDE 50,uq mL .XRDXNIS-00053 11/21/14 11/21/13 C14,. 'Lot iSTRC7287V IOU ML HRMNIS_UO052 2: mL 13C-1;2,3,7,9;9-HxCDD 0'.1,uq/mL. 13C-;1,23;4-TCDD' 0.1..uq/mL ..XRDXNIS OOD52 11/2P/14 11/21/13 Isooctane; Lot :30-mL XRDXNIS 00050 1 mt 13C-1,7 3,7,:8;9-HxCDD 5ruq/mL. 0000025663 XRDXNIS. 00051 1 mL ,13C-1',2,3�4-TCDD 5 uq/mL ...HROXNIS.00050 02/28121 CIL, Lot ER020111-02'. (PuzchasedRea ent): 13C-1',2,3,7;8,9-HxCDD .50 u /mL' ...HRDXNIS' 00051 06/61/20 CIL, Lot 'ER06071001 (Purchased Reagent)'. -'.13C-1,2 9,4-TCDD.HRDXNSU 00079 11/22/14 01/10/14 Isooctane,, Lo 50 XRDNIU 00077. 2' mL� B- u ,SO,UV/mL 0000026263 . ,Ug/mL, ..HRDXNSU-00077 11722/14 .11/22113 Isooctane;.,Lot 25'mC HRDXNSU' 00076- 1.ML 37C14-2;,3,7,B-TCDD' 0.2 ug%mL. oob0026263 - ....HRDXNSU_00076 05/31/20 11/22/13 Isooetanep'Lot 12 mL HRDXNSU_00075 1.2 mL,97C14-2,3,7,8=TCDD, 5 u9/mL. 0000026263 ....HRDXNSU 00075 DS/31/20 CIL, Lot ER052010 (Purchased'Reagent). 37C14-2;3;7,'B-TCDD; 5O'u /mL .HRDXNTA_00038 11/22/14 11/22-d3. Isooctane,. Lot '25 ML HRDXNTA 00037 0,.25 mL 1;2,3,4,6,7}6-11PCDD !20 ng/mL 0000026263 1,2,3,4,6,7,8-HPCDF '20. n mL 1,2,3,4,7;B,I9-H CDE ,20 nq/mL, 1,2,3y4,7,B-HxCDD .20'ng/mL 1,Zp3,4;7,-B-HXCDE 20 ng/mL xCDD .20 n /mL 1,2j3p6,7;8-HXCDF .20 ng/mL 1,2,3,7,8,9-HxCDD 20 no/mL 7,.8-p9-11XCDF 20 ng/mt ,7,8-PeCDD 20 ng/mL 1,2;3,7,8-PeCDF 20 n /mL 2,3;4,6,7,8-HXCDF 20 n /mL 2,3;AL;7',8-PeCDF 20 no/ 253,7,8-TCDD 4 no YMI. 2;3,;I,8-TCDF 4 n /mL OCDD 40'n mL HRDXNTA-00037 D3/31/20 CIL„ Lot ER031010-01 (Purchased Reagent) 1c2e3,4,6,T,8-N GOD 40 n /mL P 2 ug/mL 1,.2,33,4,6,.7',8-N CDB 2 v mL 3,40,8,9-HPCDF ,2•u /mL, 1,2,3,.4,16 UB HXGVD 2'u /mL,. 1.,.2,3,4,],.8-HxCDF 2 vq/mI. Page 15 of 934 10/06/2014'. REAGENT TRACEABILITY .SUMMARY Lab Name.: TestAmerica Sacramento Job No.: 320-9121-1, SDG No. : Reagent Parent Reagent ' T Exp. Prep- Dilutant Final Volume' Reagent ID ➢ate Date Used' Volume :Reagent ID Added' Analyte Concentration 1,2,3,6,7,8-HxCDD 2, U -ML 1,2,3,6,7.,8-HxC5F 2 u /mL L,2,3,1,8;9-HxCDD 2: ug/mL 1,2,3,.7.,8,.9-HxCDF y u /mL 1,2,3,7,.8-PeCDD- 2%u YmL 1,'.2;3,7,:8-PeCDF 2•U /mL 2,.3,4,6,7,8-HxCDF 2:u' /mL 2,3,4,7,E-PeCDF 2, ug/mL 2,3,7,8--TCDD 0'.:4 u /mL '2,3,7,.8-TCDF 0.4' Ug/mL OC➢➢' 4'.ug'mL OCDF '4 u /mL HP➢XNt4_00026 11'/21/14 06/19/14 C14 p:,Lot S1'.BC2541V 1. ML HRDXNIDA 00146 0.5 ML "13C=1;2;3,A,.6,7,:B-HpCDD 100. n4/mL 130>1,.2,3,7;B-PeCDD 200- ng/mL 13C-1,2r3{6;7;B-HxCDD 100 nq/mL 13C51,2,3,7.,8-PeCDF. 100:nq/mL ,I3C-0CDD 200'ng/mL 13C71;2,3,.4;6,7.,8-NPCDF 100 ng/mL 13C=2,3;7;8-TCDD 100ng/mL •13C-2,3,7,;8-TCDF •.1m ng mL HRDXNIDA.00156, 0.25 ML ,136+1;2,3,�4,7;B-HxCDF 100n mL HRDXNIS 00049 .1 ML- '13C-1;2,3;7{8,'9-HxCDD 100 ng/mL :13C-1j.2;3,4-TCDD 100 n /mL. HRDXNSU.-00083 '.0.025 ML.37C14=2,3,7-,8-TCDD 5' n /mL NRD%NTA 00040 0.025 ML 1,2,,, !4L ;7y 8=NpCDn '50: n /mL 1.,2,3,.4j6;7y8-H CDF 50. n /mL 1,2„3,.4,7;8,9-N CDF SQ n /mL. •1',&�3L4;7y'B=HXCDD '50. ng/mL, '1;2,3;4,7;0225 5an /mL ,1;2,3;6;7,.8-HxCDD ,50. ng/mL 1;2';3-,,16,7,8-HxCDF 50 nq/mL 1;2;3,7,8;9-HxCDD 50. n /mL .1,2,3,7,8,.9-HxCDF 50 ng/mL 1,8-PeCDD .50'n mt 1 2p:3,7,8-PeCDF 50' ng/mL '2;'3;4;.6,7,�B-HxCDF .50n /mL 2,3;4,7;8-PeCDF 50 n /mt. 2,3,7,8-TC➢D, 10 ng/mL. 2,3;7,8-TCDF OCDD. 100 n /mL .NRDXNIDA_00146 03/09L17 02 03 14. I0000260026263 ML 2e OCDF 100.n /mL 000 ,. Lot 250'mL HRDXNIDA_00136 .1. 13C-1;2,.3,41.61718-HpCDD 0.2'ug/mL HRDXNIDA.00137 1 ML 13C-.1+.2',3,7;.6=PeCDD 0.2' u /mL HRDXNIDA 00130 1 1 mL. 13Ci3,6,7y'8-NXCDD 0.2' uq/mL HRDXNIDA._00139 :1 mL :13C-1;2,.3,7y'B-PeCDF 0.D u /mL HRDXNIDA.00140 10 mL :13C-OCDD 0.4 Ug/InL HROXNIDA_00142 1 mL,.13C-1;.2,3,4,'0,778-NPCDF O'.2'ug/mL Page .36 of 934 10/0.6/2014 REAGENT TRACEABILITY SUMMARY Lab Name: TestAmerica Sacramento :Job No. : 320-9127-'1 SDG No:: Reagent Parent Reagent Exp Prep Dllutant Final Volume Reagent ID Date Date Used Volume; Reagent ID Atlded 'Analyte 'Cdncentration HRDXNTDA 00143. 1 m➢ 13C-2,3,9,E=TCDD 0.2 u /mL HRDXNIDA 00144 limli OC-2,3,7,8=TCDF ...HRDXNIDA 00136 03Y30/20 CIL,-.Dot ER113010-01 '0:2 u /mL (Purchasetl'Reagent) 13C-1,2,3,4,6',.7,.8-NpCDD. 50 a /mL -..HRDXNIDA 00138 03/.09/19 CIL;-•Dot:ER010207-02 gPurchased'Reagant) 13C-1,2,3',1,8-PeCDD 50 u /mL ..HRDXNIDA 00138 O1/31/19 CIL;'Lot ER010209-01 (Purchasec!Reagent) 1'3C-1, 6',7,.B-HzCDD' S0 uq/mL.-HRDXNIDA 00139 OI/O1/21 CIL, Lot.RR01211-01 (Puzchased•Reagent) 13C-1,2,3,.7,8-PeCDF 50 u /mL ..HRDXNIDA 00140 07/31/20 CIL;'Lot ER071610-01 (Purchased Reagent) 13C-0CDD 10 a /mL ..HRDXNIDA 00142 11/30/21 CIIr-Lot ER102711-02 (Pumhasetl:Reagent) 13C-1,2y 3,4,6;7 8-H CDF 50.. /mL..HRDXNIDA 00143 06/30/17 CIL, 'Lot ER060407-01 (PurchasedReagent) 13C-2,3,7,8-TCDD 50 u /mL..HRDXNIDA 00144 69/25/17 CIL, Lot 'ER092507-01 (Puzchasatl Ro3gent) 13C-2,3,7,8-TCDF 50 ug/mL.HRDXNIDA 00156 05/30/17 02/20 14 Isooctane, Lot '100'mL HRDXNIDA_00152 0.8 mL 13C-1,2,3,4m xCDF •,0,4 ug/mL 0000026263. ..HRDXNIDA,00152 07/31/20 CIL, :Lot ER072610-02 (Purchased.Reagent) 19C-1,2,3,4XCDF 50 mg/mL.HRDXNIS_00049 05707/1'S 05 07/14 C14, Lot.STBC7211V .IUU mL HRDXNIS_0004B 2'mL 13C-1,2,3,7xCDD 0.1 uq/mL 13C-1.,2,.3,40:1 Ug/mL..HRDXNIS_0004B 05/07/15' 05/07/24 Isooctane, Lot.53799 10'mL HRDXNIS-00046 1 mL 13C-1,.2,3,7xCDD 5 ug/mL NRDXNIS"00047 1,mL P3G-1,2,3,45 uq mL..HRD%NIS 00046 08720/18 CIL, LotiER00250B-01 -(Purchased'Reagent9 13C-1,2,.3,7zCDD 50 ug/mL.HRDXNSNIE 00047 O6/01120 CIL, Lot' ER06071001 .(.Purchased.Reagent) 13C-1,2,.3,450 a /mL..XRDXNSU 00083 11/22/1'4' O6/11/14 Isooctane, Lot 2$ mL .HROXNSU_00076 1-mL 37C14-2,3,7D 0;2 ug/mL 0000026263� ..HRD%NSU_00076' OS/31/20 11/22/13 .Isooctane, LOD 12 mL .HRDXNSU 000.75 1.2.mL 37C14-2,3,7DD '5 ug/mL 0000026263` - ...NRDXNSU 00075 05131120 CIL', Lot'ER052030. '(Yumnased Aeagent) 37C14-2,3,7,8-TCDD 50 u /mL.HRDXNTA 00040 11/30/22. - CIL Lot�ER111212-01 (Purchased Reagent) 1;2,3;4;6,7,8-HPCDD 2 u /mL' 1,2;361,B-H CDFDF' Z u /mL 1,2,9,4p7,8,9-HxC '2 u /mL. L,2;3,4- 7,8-HXCDD' 2 ug/mL. 1,2,3,4,7y8-HXCDF 1,2,3;67;8-HXCDD 2 ug/mL 1;2;3,6;7.,B-HxCDF 2 ug/mL. 1;2;3;7;8,9-H%CDD 2 ug/mL 1,2,3,7,8,9-HxCDF 2, u /mL .1',2,3i7,8-PoCDD- 2 ug/mL :1,2,3;7;8-PeCDF 2 ug/mL 2i3,4;6,7,8-HxCDF" 2 ug/mL �2;3;4•,7„8-PeCDF 2 ug/mL 2;3,7,B-TCDD 0.4'•uq/mt '2,3,7;8-TCDF 0.4-u /mL OCDD 4�u /mL OCOF � u /mt' BRD%NL4_00027 11/21/T40T/10/14 C1 , Lot 8TBC2541V 1 mL !NRDXNIDn 001-060:5 mt 13C-2,.3,7,E-TC➢D 4 100.n LmL. 136-2,3(7,:B-TCDF 300 ng mL 'HRD%HIS 00049 '1 m& 13C-1,2,3,4-TCD➢ 100 ng/m1 HRDXNSU 90083 ;0.025 mH 37C14-2,3,7,8-TCDD 5' n /mL' NRDXNTA_00040 ,0.D25 mL, 2;3,7,:8-TCDD 30. ng/mL 2'3j7,8-TCDF l0.nq mL Page; 37 oV 934, 10/06/2014 REAGENT TRACEABILITY SUMMARY Lab Name: TestAmerica Sacramento Job: No. 320-9127-1 SDG No.: :Parent Reagent. Reagent Exp 'Prep Dilutant Final Volume; Reagent ID 'Date. 'Date Used` Volume Reagent. ID Added Analyte Concentration :HRDXNIDA 00146 03/09/17 :02/03/14 I9coctane, :Lot 250. mL, NRD%NIDA_00143� 1 mL' 13F2,3,7,8-TCDD 0:2 uq 00000261263 HRDXNIDA,.00144 1 mL-:13C-2;3,7y8-TCDF 0.2 u /mli ...HRDXNIDA'00143 06/30/17 'CIL, Lot ER060407-01 (Purchased Reagent) :13C-YT3,7;0-TCDD 50 ug/mL ..HRDXNIDA 00144 .09/25/17 CIL,. Lot ER092507-01 (Purchased Reagent) 13C-2,3-798=TCDF '50 ug/mL' .HRDXNIS 00049 -05/07/15. . oocae, 7 2587 m . 13C-1;2,3y4-TD 05/07/ 9 e 0 :,NRDXNIS 00048 135/07/15 14Is tn3'& 379 10 mL :HRDXNIS 00047. mL 13C-1,2;3;4-TCDD :0.1 u /mti 5 u /mL ...HRDXNIS 00047 '06/01/20 CIL; Lot:ER06071001 (PnrCna9eO Reagent) :13C-1;2,3,4-TCDD- 50 u /mL' .HRDXNSU_00003 11/22/14. '06/11/14. Isooctane,+Lot 25 mL HRDXNSU_00076 I'mL..37C14-2,3,7,8-TCDD .0.2 ug/mL 0000026263 ..NRDxNSU_00076 .OSX31/20 11/22/13 Isooctane, Lot 12 ML. HRDXNSU_00075 1.2 mL 37C14-2;3, 0000026 7,,8-TCDD 5 ug/mL 263 - ....HRDXNSUT0075 05/31/20 CIL; Lot'ER052010 (PU Co aged Reagent) 37C14-2,3/7.,8-TCDD 50 ug/mL' .NRD%NTA_00040 ,11/30/22. CIL, Lot ER111212-01 (Purchased Reagent) '.2,3;7,8-TCDD 0.4 uq mL 2,3,7,8-TCDF MU)X N5 00015 111,21114, 02/21/14' C14, .Lot STBC2541V' 0.2 ;ML,'.HRDXNIDA 00146 0.1 mL 13C-1,.2,3,4,6,.7,8-HpCDD- KIOOng/mL /mL 13C-1,2'3,7,87 CDD' /mti13C-1:,2,3,6,7,.8:HxCDD: /mL13C-1,2,3,.7,82;ECOF /mL13C-0CDD g'/mL13C-1,2,3,A,6y7,8-HpCDD /mL13C-2,3,7,8-TCDD /mL13C-2,3,7,8-TCDF /mLHRDXNIDA 00156 0.05•mL' 13C-1,2,3,4,7,B-HXCDF /mL:HRDXNIS 00053 0.2:mL 13C-1,2,3,.7,.8;9-HpCDD` ML 13C-1,2,3,4-TCDD 100:nq/mL •HRDXNSU,00077 0,02`mli 37C14-2-,3,7,8-TCDD 20 •nq/mti NROXNTA_00040 0:,02`MI; 1,2,3,4,6p7,B-N CDD' ,200,n /mL 1,2,3,4,6)7,8-HxCDF 300.n /mL 1,2;3,4 7.,8;9-N CDF I200:n /mL 1,20,40,;O-HxCDD '200 .n /mli 1,2,3,477,E-HxCDF :200,n /mL 1,2,3,6,•7,8-HxCDD 200 .ng/mL 1,2,3,6,7.,8-HxCDF 200 mq/mL . 1,2,J0-,8,9-HxCM 1200 ,ng/mL 1',2;3,7,8,9-HxCDF' 200 ng/mL 1,2,3,7y 8-PeCOD' 200'ng/mL 1,2,3;.1,U-PeCDF ,200'n /mL 2,3,4,6;7:,8-HxCDF 200.n /mL 2,3l400-PeCDF 200 ng/mL 2,3,.7,8-TCDD 4-0—'nq7mL 273,7,.8-TCDF AO n mL 0CDD 400 'nq/mL OCDF400 no/mL .HRDXNIDA 00146 03/09/17 02/03/14 Isooctane, Lot :250 mL :HRDXNIDA_00136 1•mL 13C-1,2,3,4.,M,8-HpCDD 0.2 ug/mL 0000026263: :HRDXNIDA 00137. 1'mL 13C-:L,2,3,Jy8-PQCDD- 0.2,ug/mL HRDXNIDA 00138 I IMLI 13C-1,2,3,6,7,8-HxCD0' 0;2 yg/mL Page. 3.81of 93:4 10/06/•2014 REAGENT 'TRACEABILITY SUMMARY' Lab Name':. TestAmerica Sacramento Job No. : 320-9127-i SDG No.: Reagent Parent Reagent �Exp Prep Dilutant Final Volume 'Reagent ID Date Date Used Volume. Reagent ID Added 'Analyte Concentration HRDXNIDA. 00139 InL 13C-1,2,3,7,8-PeCDF •0.2 u /mL �HRD%NIDA 00140 10ImL 1JC-OCOD '0.4 u /mL' .HRDXNIDA 0014D 1 ML, 13C'1,2,3,4.,617,G-HpCDF 0.2 U. /mL 'HRDXNIDA 00143'. 1 OL 13C-2.,3,7;8-TCDD :0 2 uq/mL- ..XROXNIDA.00136 11/30/20 CIL„ Lot ERIIIO10-01. 'HRDXNIDA 00144.. 1 mL 13C-2 3 7 S-TCDF 0.2 ug/mL' ..HRDXNIDA'00137 03/09/17' CIL, Lot ERD30907-02 (Purchased Reagent) 13C=1,:2,3,4,.6,-78eH CDD 50. ug/mL (Purchased Reagent) 13C-1,2,3,7,8-PeCDD 50 ug/mL ..HRDXNIDA:00138 0L/31/19 CIL, Lot ER030209-01 (Purchased Reagent) .13C-1;2,3,6,7.;8-HxCDD 50 U /mL ..HRDXNIDA-00139 01L01 21 'CIL; Lot ER01211-01 (Purchase d Rea ent) 13C-1,2,& 7:,8-PeCOF 50 u /mL' ..HRDXNIDA 00140 07/31/20 CIL,- Lot ER071610-01 (Purchased Rea ent) 13C-OCDD 10 Uq/mL ..HRDXNIDA U0142 11/30/21 CIL-, .-Lot ER102711-02 (Purchasetl Reagent) 13C-1;2,3,4;6,7,8-HpCDF 50 u mL ..HRDXNIDA-00143 06/30/17 CIL, Lot ERD60407-01 (Purchasetl Reagent) 13C-2,3,7,8=TCDD g HRDXNIDA 00144 09/25III CIL,.Lot ERO92507-01' S0 ug/mL' IPurchased Reagent) '13C-2 3;7,8-TCDF 50 ug/mL .HRDXNIDA_00156' 05/30/34 02l20/14r Iaoocta26 Lot -100 mL HRDXNIDA 00152. 0:8 hL: 13C-1 3,.3,4;7,B-HxCDF ;050 U /mL 0000026263. 9 ..HRDXNIDA 00152 07/31/20. CIL,.Lot ER072810-02 (Purchased Reagent) i3C-1,2,3,4,7,0-RxCDF 50 U /mL- :HRDXNIS_00053 .Ti/21l14"11121/13 C1'4y :Lot STEC7207V' .100 mL :HROXNIS_00052 2 mL 13C-1,2,3;7;8,9-X%CDD- g '0.1 uq/mL- ...HRDXNIS_00052. '11/21/14 11/21/13' isooctane; -I.ot 13C-1,2,3,9-TCDD' 0.1 u /mL 10 mL' HRDXNIS '00050 .2 ML :49CrI 2,3;7,6 9-HxCDD 0000026663 - � $,ug/mL. IHRDXNIS,00051 .1 ML .13C-1,2,3,4=TCDD 5 u /mL' .:HRDXNIS 00051 '02/2B/21. ' CIL Lot ER020111-02 (Purchasetl Reagent) .13C-1,2,3,7,8,9-HXCOD 5U a /mL .-..NADXNI5 00051 O6/O1/20 'CIL, Lot ER06071001 (Purchased Reagent) .13C-1,2,3,4-TCDD 50 u /m1, .HRDXN6U 00077 11/22714 [11/22/13 Isooctane, Lot 25 aw HRDXN5U.00076 .1 mL,,37C14-2,3,7;8-TCDD 0.2 ug/mL 0000026263 ..HRD%NSU_00076. OS'/31/20 11/22/13' Isooctane,:Lot 1Z mL-_1RDXNSU_00075 t1:2 mL.37C14�2;3,7;B-TCDD, 5.ug/mL 000002b263 ..HRDXNSU '00075 05731✓20 CIL„Lot.ERO52010'. pPurcAasetl Reagent) -37C14-2,3;7,:B=TCDD 50 ug/mL .HRDXNTA-00040 11/30/22 CIL, Lot, ER1111212-01 (Purchased Reagent) 1 2,.3,4y6,7,8-H COD 2 u ML 1;2,3yr4y 6;7,8-H COF 2'. 0 mL 1/2,3,4,1, 9-HPCDF 2 u 'mL T,2,3,9,7,8-HxCDD Zu /mL 1,2,3,4,7,B-HxCDF 2, ug/mL. 12,3,6,7,8-H%COD 2. ug mL. 'I;2,3,.6;7,:B,HXCDF. 2(u /mL 1,2;.3,7,8,.9-HxCDD g u /mL 1;2.3,7;8,.9-HxCDF 21'ug/mL, d'p2,3,7p8-PeCDD 2+U /mL 1.2,3,7,8-PeCDF 2'Uq/mL 2,'3,4,6,7,8-HxCDF 2, u /mL 2,:3;4,7p:8-PeCDF 2, u /mL. 2,3y 71,81ICDD O:A u /mL 2,3,7,8-TCDF 0:4 a /mL. GOOD 4 vg/m1 OCDF 4 ug/mL RPDXNL6_000OD 11/21/14 02/21L14 C14, Lot STHC2541v 0.Z Nd, HRDXNIDA 00146 U.1 mL 13C-ly2;J;4;6,7;5-HPCDD 100 ng/mL .13C.-1;2,3,7,.8-PeCDD IOU,n luL. 13C-1;2,'3,6„7;H-HxCDD 100'ng/ zi Page 3.9 of 934 10/0'6'/Z014 REAGENT TRACEABILITY SU104ARY Lab Name: TestAlnletica tSacramento Job No'.: '320-9127-1 SDG No.: 'Reagent Parent Reagent Ezp Prep Dilutant FSnal Volume Reagent ID Date Date Used Volume, Reagent ID Added Analyta Concentration 13C-1,2,3,7.,B-peCDF 100 ng/mt 13C-OCDD .200 ng/mL 13C-1,2,3,4,6,.7,8-H CDF 100•ng/mL 13C-2,.3,d.8-TCDD '100 ng/mL 13C=2,.3,7,8-TCDF 100 n /mL ;RRD%NIDA 01156. 0.05`mL 13C-1,2,.3,4,7,8-HxCDF 300 ng/mL. :XRDXNIS_00053 0.2'm0 13C-1,2,3,7,8,9-HxCDD. 100 n /mL 1I -L,2,3,4-TCDD '100 n /mL HRDXNSU 00077 0..1.mL 37C14-2,3.7,8-TCDD 100 n /mL RRDXHTA_00040 0.1 ML 1,2,3,4,6,7,8-H CDD 1000 ng/mL 1,2,3,4,60,8-H CDF 2000 ng/mL 8H CDF 1000 ng/mL B-H%CDD" 1,2,3,4r7,8-HxCDF 1000ing/mL _ 1,2,3,6)7,B-HxCDD: 1000,n /mL 1,2,3y.6,7,O-RXCDF 1000 ng/mL 1. 7,8,9-HxCDD 3000:ng/m1 1,.2,3,:7,By9-HxCDF 1000 n /mL 1,2;3>7;8-PeCDD. 1000 n /mL 1,2,3,7,B-PeCDF 1000 ,ng/mL 2,3,4sb,.7,;.8-HxCDF 1000 ng/mL 2,3,4vT,8-FOCDF 1000'n /mL 2,3,7,B-TCDD 200ng/mL 2,3,7,8-TCDF r200 :ng mL CCDD 2000 n /mL OCDF 2000:ng/niL.NRDXNLDA_00146 03/09/17 02/03/ld' Isooctane, Lot .250 ML ;HRDXNIDA_00136 1 mL 13C-1y 2,3;4�6),7";8-HpWD' Ott:ug/mL 0000026263; .HRD%NIDA 00137, 1.ML 13C-1,2,3,.7,8-PeCDD 0:2 ug/mL NRD%NIDA 00438 1 mL 13C-1,2,3,.6y7,B'-HxCDD' 0.7 v /mL HRDXNIDA 00239 1,mL 13C-1,2,3;7r8-PeCDF 0:2 m /mL HRDXNIDA 00240 lurm 13C-OCDD :0..4 mg/mL '.HRDXNIDA 00142 1 ME 13C-1,2,3,4,.6..758-HpCDF 0.2.ug/mL ,HRD%NIDA D0243 1 mL' T3C-2,3,.7r B-TCDD '0:2 ug/m1 '.NRDXNIDA 00344 lmti 13C-2' 3;7;8-TCDF OJ2 iug/niL..HRDXNIDA'00136 11/30/20 CIL, .DOt'ER111010F01 ..HRD%NIDA 00137 (Purchased.Reagent). _ 13C-L 2;3,4,-6,7,8-HpCDD 50 :u /mL 03/09/17 CIL, LOt.FRO30907-02 (Purchased:Reagent) 13C-1y.2,3;.7,8-PeCDD - 50 u /mL ..HRDXNIDA 00138 O1/31/1'9. CIL,.:Lot'ER010209-01' (Purchased Reagent) 13C-1;2,3,6,7;B-HxCDD -50 ug/mL' —HRDXNIDA 00139 01/01/21 CIL, Lot ER01211=01 (Puzchased Rea ent) 13C-1;2,3,R,B-peCDF SO:u /mL ..HRDXNIDA-00140 .07/31L20 CIL, Lot ER071610-01' (Purchased Rea gent) 13C-OCDD SO dug/mL .;HRD%NIDA 00142 11/30(21 CIL,. Lot ER102711-02 (Puzchased Reagent), 13C-1q 2;3;4p6,7;8-XpCOF 50 u mL ...HRDXNIDA 00143 'O6/30/17 CIL, Lot ER060407-01' (Purchased '.Reagent) 13C-2,3,7^8-TCDD SOu mL .;HRDXNIDA 0019d 09/25/17 CIL,. LOt 'ER092507=03 (Purchased Reagent) 13C-2,3,7,8-TCDF 50 u /mL .HRDXNIDA 00156; OS/301L7 02L20/14' Isooctane, hot '300 uW .HRDXNIDA 00152: O.B mti 13C-1,2,3,4,7,8-HxCDF' 0:4 ug/mL'0000026263 ..HRDXNIDA 00152 07/31/20. CIL, LOt�ERD72810-02 (Purchased Reagent) 13C-1,2,3,4,7;8-HxCDF SO ug/m0 .HRDXNIS_00053 11/21/14 11/21/13 C14, Lot STRC,7287V, 100 mL HRDXNIA00052 .2-mL 13C-.1,2,3,7.,8;9-H%COD O50 vq mL 13C-1;2,3,4-TCDD 0:1 uq/mE Page 40: 0E, 934 10/06/2014 REAGENT TRACEABILITY SUMMARY Lab Name: TestAmerica Sacramento Job No..: '320-9127-1 SDG No. : Reagent Parent Reagent Exp Prep Did'utarit Final Volume Reagent ID Date Date Used 'Volume Reagent ID Added .Anal, to Y :Concentration ..HRDXNIS_00052 11/21/14 11/21/33 Isooctane, Lot 30 mL HRDXNIS 00050 YmL 13C-1,2,3;7,8,9-HxCDD 5 Ug/mL 0000026663' - HRDXNIS 00051 _1:mli 13C-1,2,3,.4-TCDD 5 vgFmL ...HRDXNIS 00051 02128/21 CIL, .Lot:ER020111-02 (Purchase 'Reagent? 33C-L,2,3;7,.8,9-HxCDD• 50'.ug/mL ..,HRDXNIS 00051 O6lO1/20 'CIL EoC ER06071001 (Purchased Reagent) 13C-1,2,3,g-TCDD 50 u /mL JHRDXNSU_00077 11/22/14 11'1,22/13 :Isooctane, Lac 25 mL HRDXNSU 00076 SmL 37014-2,3,.7,,8-TCDD gig 'ug/mL 0000026263. ..HRDF.NSU_OOD76 OS/31/20 11/22/13 Isooctane, Lot, 12.mL HRDXNSU 00075 1:2 ML 37C14-2,3,7;8-TCDD S ug/mL'6000026263' - ...HRDXNSU 00075 OS/31/2U CIL, .Lot ERU52010 (Purchased Reagent) 37C14-2,3,7,8-TCDD ;HRDXNTA 00040 11/30/22 CIL, ;Lot.ER111212-OS (Purchas SO .0 /mL ed.Reagent) 1,2,3,4,6;7,8-NpCDD Z ,ug/mU 1,2;3,4,6,7,8-N CDF 2.ug/mL 1,2,3,4,3,819-HDCDF j2 ,ug/mL 1,2,:3;4,7,8-NXCDD 2 u /mL 1,2,3,4,7,8-H)jCDF 2 ug/mL 1,2,3,6;7,8-HxC1DD 2,ug/mL 1,2,•3,.6?,8-HxCDF .2.ug/mL 1,2,3y0y8,9-HxCDD '2 UV/mL 1,2,3,T,8;9-HxCDF 2 .0 /mL 1;2,3,7,0-PeCDD Zug/mL 1,2,3,7;8-PeCDF -- :2 .0 /mL 2,3;4,.6;7;8-HxCDF' .2 .0 /mL 8-2 eCD,F 2 1u /ME 2,3,78-TCDD 0.4 u0/mL' 2,3,7;8-TCDF u.4 a 1mL' OCDD" A a /mU HtuuD49v 00086 _ 11/22/14. 08l05l14 Isooctane, Lot 500:mL 'NRDXN6U 00083 .2 mL 37 37C14-2,3,7;8-TCDD 0.0008 ug/mL' 00000537.99 .HRDXNSU_00083 'll/22/14 OE/11114 Isooe26263 Lot. 25 mL HRDXNSU 00076 1 ML 37C14-2;3,7,8-TCDD 0.2 ug/mL 0000026263, ..RRDXNSU_00076' OS/31/20 11/22/13 Isooctane; Lot 12 mL 'HRDXNSU 00075 :1.2 mL 37C14-2,3,7,0-TCDD 5 ug/mL' 0000026263 ..,HRDXNSU:00075 05/31/20 CIL,• Lot :ER052010' (Purchased Reagent) '37C14"2 9 7,8-TCDD 50 ug/mL,�1n:QtT1. 00042 .07/3B/15', 07/18/14' Acetone, •Lot 0000062748 25 mL :HRDXNTA.00040 07. 5 mL 1/2,3,4,6,7,8-HpCDD 20 n /niti 20 ng/mL. 1,2,3,4,7;8,9-HPCDF 20 nq/mL 3;4;7,8-NXCDD 20 ng/ML 4;1,B-HxCDF 20 n /ml 1;2,3,6,7,.8-NXCDD ;20 n /mL' 1,2,3,6,7.;B=HxCDF :20 n /mL 1/2,3,7,0,9-HxCDD 20' n /mL 7,8,.9-HxCDF '20 ng/mL '1,2,3r7{8-PeCDD .20 n /mL 420,74-POCDF 20 ng/mL 2,:3,.4;6,7„B-HxCDF .20. ng/mL 3,4,7,8-PeCDF 20n /mL: 2,i3,7,8-TCDD 4 ng/mL Page 41.'of .934• 10/06/2014 REAGENT TRACEABILITY SUMMARY Lab Name: TestAmerica Sacramento Job, No.,: 320-9127-1. SDG No. : Parent .Reagent Reagent; RXp 'Prep DSlutant, Final Volume Reagent ID Date Date Used Volume Reagent iD Added: Analyte' Concentration 2,3,1,8-TCDF 4 n /mL OCDD 40. ng/mL ' . .HRDXNTA_00040 1L/30/22 CIL OCDP .40'ng/mL ', Lot ER111212-01. )Purchased Reagent), i1,2,3,4,:6,7;,B-H COD 2 /mL. 1•;2,3,4,6,7;8-HzCDF 2. 0 /mL 1,2 3,'4,7..,,a;9-N CDF 2 u /mL '1,4:3,4,7,$-HXCDD 2lug/mL r1,2,3;4,7,-9-HXCDF _ 2'u /mL 1y2,3,:6;7,B-HxCDD 2 u mL 1,2,:3/6,7!8-HzCDF 2 ug/mL :1,2,3,7,18,PLED 21 ug/mL 1,2i3,7,8,9-H%CDF 2 u /mL 1 2;3;7,8-PeCDD 2.ug/mL .1;2,3,7;8-Pe CDF 2.uq/mL' 72,3,4.,6;7;.8-HzCDF 2'uq/mL '2;3,:4,Tj8ePeCDF' 2'u /mL �2p3,7,8-1'CDD 0:.4- u /mL .2,3,7y.8-TCDF 0,4,1 /mL 'OCDD 4, u /mL. OCOF' 4 u /mL 'Page 42 .of 934 '10r06/2014 APPENDIX C BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS, 1990-2004 36 Table 6-4. Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 1990-2004(a). 1990 Restdts� 1991 Resole) No=of Length Station Species Plsh Runge(rm) 2.3.7.8-TCDDm Station - Number of Length 1 Rock bass Species Fish Rattle(mm) 2.3,7,8-TCDD�r 5 151-197 ND(0.15) 1 Rock bass 10 151.190 ND(0.40) RM 64.5 Rock bass 2 8a31133 N D(0.15) RM 64.5 Redbreast sawfish Black redhorse N� 30 358-471 ND(0.33) Black redhorse 5 358-071 ND(0.35) 2 Redbreast sunfish 5 2 Redbreast sunft RM 59.0 Redbreast sunfish 5 148-20 3.4 s 154 202 0.87 Common carp 1 517 19.7 AM 59.0 Redbreast sunfish 8 91-570 0.93 Common carp 10 491-570 9.7 I88203 0. 3 Redbreast sunfish 5 79 RM 52.3 Redbreast sunfish 5 188-198 .6 3 Redbreast sunfish 10 176-209 ND(0.89) Common RM 52.3 B1uc&M 6 164-197 �P 2 489-55S 4.2 Common ND(0.63) �rP 10 408463 2.4 RM 41.5 Blueglu ill S 178-192 ND(1.2) 4A Lac emouth bass 313-468 e6 5 153-174 ND(0.63) RM 41.5 Black crappie 10 3.0 ND Common carp 1 574 27 102-688 23 (0,p) Common carp ID SD2fi88 23 . 4B Blueg0l 5 183.196 0.76 43 Bluegill S RM 39.0 Largemouth boas 2 2794M ND(1.8) RM 39.0 BluegID 5 166212 ND(0.34) Common carp 4 551-08 66 19D.208 ND Common Cary 10 532.605 40 (0.fit) . 5 Redbreast sunfish 10 143 223 0.98 RM 16.5 Spotted hiss 2 266-368 ND Common 2 511.539 1.7 (0.35) . TOW Fish Filleted 57 138 E a Oe� Q[C� OO OO OO 000 apapDDB8O b +0 O��O o 00 �n o�oO NN� V N��[YorV NN r��f Nov] toN N tV vbi Rb�+ m G OHO O 220 a7 W S; z W w� za�u aau' wc3 ��u' ahm ^ c v3 o mm vi �jo 0 � a m n oop QO 0_ Qgoq qqC qe popqg qqo q0 M N Z2 -�'� o�a Z�a �Z T.cai ZiZ v� 7Zo a CC m� a�a n 3 °� v� OO�p 000 OOO y0o QyQ ONy� ymj ids( 9q W a z H 17 u u m qq m aI Ila a u 9 �y b awyw aa8 aau' r'ar�au M96 H W . � vd o m vi o 0 F ratan N� p oo pop pop(p� [oqff(q0� (opff(pe a ppe (ep pv][poff vi xZX z7..% .ZZ.: Cizvi eizo �2zX m� O�e� Tmm 1° Oppppe. egnQ�-. [OJ.ti� (�qGO O � �� OOh 000 000 vfo� eTmy e>•hh h � z o e^ n o v •e ..5$ Nvai ms�i a�v' mym+ er d p F gee Sff Fi oo go ff 68 dos, (o/�0(� o 0 ^00�++0^�+ /po/pi�g o'�•/qo�/e QR! �i.40 F�he�l F�7n0 l�f�.4 Opp ��ptNNN q(Vn tV�r N�b Nq� � o •� .00m o00 000 000 000 ,aa°, g � fL n 9 5 0 ENO od Eon g� = e aw � 8 ww'c4 wmmS Aw w •a N h en Q vv men. v� Table 6-4 (coat.). 1996 Reultsw . 1997 Itmultsm . Number of Length Number of Len Station Species Fish Range(rm,J 2,3,7,8•TCDDt4 Scotian Species Fish Range(mm) 2,3,7,8-TCDDo) 1 Redbreast sunfish 5 154.185 ND(0.13) 1 Redbreast stutftsh RM 64.5 Rock bass 5 I60-208 ND(0.085) RM 64.5 Rock bass 5 162-194 ND(0.13) . Black redhorse 5 401440 ND(O.DM Black redhorse 5 91-424 ND(0.23) 4 291.424 ND(0.22) . 2 Redbreast sunfish 5 179-187 ND(0.10) 2 Redbreastsunfuh 5 RM 59.0 Redbreast sunfish 5 183-191 ND(0.12) RM 59.0 Redbreast sunfish t63-200 ND(p,� Common carp 5 543-580 15 Common carp 5 506.615 1.4 160-181 ND 3 Redbreast sunfish 5 1WI90 ND(0.13) 3 Redbreast sunfish 5 187.202 RM 52.3 Redbreast sunfish 5 165.185 ND(0.13) RM 52.3 Redbreast sunfish 5 ND(0.18) Common arp 5 516.630 0.87 Common carp 5 450.505 ND ND(0.18) 3 ro. ) 4A Black crappie 5 216-233 ND(0.15) 4A Black mapppie 5 235 231 ND(0.27) RM 41.5 Black crappie 5 215-229 ND(0.18) RM 41.5 Black maPPu S Common carp 5 562-632 42 Commol carp 5 57�0.665555 2.ND 310) Channe5 418-482 2.0 4H Black cmpple 5 223.258 ND(0.11) 4B Blade crappie 5 226-241 ND(0.17) RM 39.D Largemouth bass 5 278-310 ND(0.13) RM 39.0 largemouth bass Common5 270-360 ND(021) . eery 5 470-b13 4.0 Common carp 5 605-690 11.0 Flathead catfish 5 430-540 0.62 5 Rock bass 4 169.186 ND a(m) 5 Rock bass 5 143-214 ND(0.15) RM 19.0 3maDmonth bass 5 315454 ND(0.12) RM 19.0 Smailmouth bass 5 276.367 Smallmouthbuffdo 5 451-555 ND 0.12 SmaOmouth buffalo 5 ND(0'� 406.525 ND .22 Total Fish Filleted 89 Total Fish FIDeted 99 Table 6-4 (cont.). 1998 RestdhsQJ 1999 Resultsm Number of Length Station Specks Fish Range(nun) 2,3,7,8-TCDD(4 Number of Length Station des Fish Range(om) 2,3,7,8-TCDW-) I Redbreast suatish 5 145-176 ND(0,19) 1 Redbreast sualislt RM 64.5 Rock bass 5 158-179 ND(0.29) RM 64.5 Rock bass 5 14-180 ND(0.21) 5 164d Black redlmrse 5 340-396 ND(0.18) Buck redhorse ND(0.37) 5 352A27 ND(0,33) 2 Redbreast sunfish 5 164-M ND(0.20) 2 Redbreast sunfish RM 59.0 Redbreast sunfish 5 166.193 ND(0.28) RM 59.0 Redbreast sunfish 5 167-190 ND(0.37) Common carp 5 SSIfi61 1.3 5 158-178 ND(0.29) Ca�unnon carp 5 544.615 ND(0.27) 3 Redbreast sunMh 5 167-193 ND(0.34) 3 Redbreast sunfish 5 162-176 ND(0.36) RM 52,3 Redbreast sunfish 5 167-200 �(00.22) RM 52,3 Redbreast sunfish ro.3 Coumon carp 5 449550 5 162.171 ND 7) ( � Common carp 5 500-591 0,57 4A Black cra m RM 41.5 Largemouth bass 5 227-330 ND(0.15) RM 41.5 Black crapmaple le 5 2�7A4 ND(0.18) Common carp 5 585-621 1.6 Common p 5 (0.08) Charnel catfish 5 416458 ND(0.28) Chancel catfish arp 5 574.645 0.58 5 425-482 0.83 4B Blank cmpple 5 233-252 ND 0. RM 39.0 Largemouth bass 5 259330 ND(0.17) RM 39.0 Hlaekmauthplhass 5 233-244 ND(0.27) Common carp 5 Sti3fi86 9.1 IXF 5 276305 ND(0.32) Flathead catfish 5 414.523 ND(0.20) Commona kh 5 621-680 4.7 372-513 ND(0.46) 5 Rock bass 4 155-190 ND(0.11) 5 Rock bass 5 170-203 ND(029) RM 19.0 Smallmouth bags 5 295-365 ND(0.21) RM 19.0 Smallmouth bass 5 297-430 Smallmouth buffalo 5 464.537 ND 0.31 Smallmouth buffalo 5 ND(0.39) 476-565 ND .31 Total Fish Filleted 99 Tool Fish FHleted 100 (r Y Q N N � O O G Q. O .p N Z e o O is b Q ld Q 95 6 aq a q n add Qo QQe o gas Q ❑0p QQ0 2 ad QE add d N ZiZ2 QZZ QZZ ZZ.-:Z Q2oQ GQQ g s m w m str a Y o ES 9� �hwt utMh hhh hv.a vt wtmaN w,hN 0 z' N p C eg x �e ' &' a new aad 'm"'wutl `wm6� C N O {n bt O O Table 6-4 (cont.). z662 Results 2003 Resdfs6e Number of Length Station Species Fish Range(men) 2.3,7.8-TCDDt°t Number of Length S � Station Range(mn0 2,3,7,8.TCDDtQ I Black redhorse 5 372-431 ND(0,14) 1 Black redhome RM 64.5 5 343-420 ND(0,70) RM 64.5 2 Common cam s 517-548 ND(o.zrs) RM 59.0 RM 59.0 Common carp 5 512-584 ND(0.18) 3 Common carp 5 575-632 ND(022) RM 52.3 52.9 Common cerP 5 545-605 ND(0.3I) RM 4A Common carp 5 523-649 2.2 4A Common PM 41.5 Channel catfish 5 425-475 ND(0.3Q cup 5 655 717 3.4 RM 41.5 Flathead catfish 5 521.575 ND(DL-0.35) 4H Common carp 5 647-670 6.6 0 Common carp 5 602-745 RM 39.0 Flathead catfish 5 41SM5 ND(0.22) RM 39.0 Flathead catfish 12.0 5 511-533 ND(DLm020) 5 Black redhorse 5 430-089 ND(0,14) RM I9.0 RM 5 19.0 Black redhorse 5 445-524 ND(DL=0.19) Total Fish Filleted 40 Total Fish Fileted 40 ' Table 6-4 (cont.). 2004 Resultste . Stadoa Number of Length ��es Fish Ra46e(MM) 2,3,7,8-TCDDm RM I 64.5 Black redhorse 5 352-440 ND(0.11) 2 Common cup 5 545-69 ND(0.19) . RM 59.0 Channel catfish 5 369-453 MD A 17) 3 Common carp 5 RM 52.3 587.609 ND(0.27) 4A Common carp 5 59"55 1.7 ' RM 41.5 Flathead catfsb 5 508-565 ND(0.30) 4B Common P 5 570-M 1.6 RM 39.0 Channel catfish 5 485-542 ND(0,31) RM 5 I9.0 Black redhorse 5 420490 ND(0,13) Total Plsh Filleted 40 (a) Survey conducted by&A F.nginxring,Science,and Technology. Analyses conducted by HNSECO Laboramries 1990.1994,Qmnterra Laboratories 1995-1999,Severn Trem Laboratories bommries In 200D- 003. @) Survey conducted in August. (c) Survey conducted in August and September. (d) Survey conducted in September. (e) Units=PPt(Parts Per trillion)or pg/g(picop m 1w gam) ND=Non-detectable at the detection limit In parentheses. f APPENDIX D 2006 REVISIONS TO DIOXIN MONITORING PLAN 37 �DF VA Michael F.Easley,Governor William G.Ross Jr.,Secretary `0 (� North Carolina Department of Environment and Natural Resources rAlen W.(Uirnek,P.E Director _( Division of WatcrQuality C C Coleco H.Ca � Sullins,Depaty Director nn E . . . ality June 6,2006 JUN 12 Mr. Paul S.Dickens Manager,Environmental Affairs MM IIDGE PApEFt Pfl00 MS 1116 Blue Ridge Paper Products eHs o P.O.Box 4000 Canton,North Carolina 28716 Subject: Revisions to Dioxin Monitoring Plan Blue Ridge Paper Products NPDES No.NC0000272 Dear Mr.Dickens: The Water Quality Section has reviewed your request for modifications to the subject study plan originally approved by the Division of Water Quality in February 1990. The 2001 dioxin fish tissue monitoring plan is approved with the following changes: • Elimination of main stem river sampling stations-beginning in 2006 fish tissue samples will be collected only from Waterville Lake. • Collect a least one whole body bottom feeder sample from Waterville Lake(stations 4A or 4B)to monitor ecological impacts of dioxin contamination in bottom species. • Continue with the collection of bottom feeder fillet samples in Waterville Lake as approved in the 1990 study plan. After reviewing your request to eliminate whole body dioxin analyses from Waterville Lake, our staff recommends that this analysis be continued. Although the Waterville Lake data submitted in your 2005 report shows low levels of dioxin,data submitted by Progress Energy in 2005 showed a mean dioxin TEQ value of 6.7 pg/g for common carp. The value was above the 4.0 pg/g TEQ value used by NCDHHS to post fish advisories for dioxin. As this time the dioxin advisory for Waterville Lake remains in effect,and in our view,warrants continued monitoring. If you have any further questions or comments please feel free to contact Mark Hale at 919/733- 6946. ce�ely, immie erton nmental Sciences Section cc: Roger Edwards-ARO Dr.Luanne Williams—NCDHHS Susan Wilson -DWQ Permits John Crutchfield—Progress Energy WWI tJ flENR N.C.Division of Water Quality 1617 Mail Service Center Raleigh,North Caroline 27699-1617 (919)733-7015 Customer Service I-87 -M 6748 BLUE RIDGE �O [Ply PAPER PRODUCTS INC. Certified Mail Return Receipt Requested 7099 3220 0007 03716235 30 March 2006 Mr. Mark Hale Environmental Biologist Environmental Services Section Division of Water Quality North Carolina Department of Environment and Natural Resources 1621 Mail Service Center Raleigh,North Carolina 27699-1621 Subject: Study Plan Revision Dioxin Monitoring in Fish Tissue—Waterville Lake March 2006 NPDES No.NC0000272 Blue Ridge Paper Products Inc. Canton Mill Dear Mr.Hale— The subject study plan revision is enclosed for Division of Water Quality(DWQ)review and approval. Background The Blue Ridge Paper Products Inc.mill in Canton,North Carolina has completed biological monitoring for dioxin in fish in the Pigeon River for the past 16 years. This annual biological monitoring is a requirement of the Canton Mill's NPDES permit. The permit requires that we follow a study plan approved by the DWQ for this work. Dioxin in fish sample collection and reporting for 2002 through 2005 was conducted under the December 2001 Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue prepared by EA Engineering,Science and Technology. EA Engineering completed the dioxin in fish sampling and reporting for years 2002 thru 2004. In 2005,Blue Ridge Paper contracted with the University of Tennessee, Knoxville(UTK)Department of Forestry,Wildlife and Fisheries for the dioxin in fish tissue work. UTK followed the 2001 Study Plan for the 2005 dioxin in fish sampling and report. The 2005 report was submitted to the DWQ on 20 Feb 2006. 175 Main Street • PO Box 4000 Canton, North Carolina 28716. 828-646-2000 Raising Your Expectations Mark Hale, NC DENR DWQ,ESS- 3/30/06, Page 2 Biological Monitorine Review The first annual dioxin fish tissue sampling study of the Pigeon River was in 1990. At that time, public health fish consumption advisories related to dioxin were in place for the Pigeon River downstream of the Canton Mill for both North Carolina and Tennessee reaches of the river. Dioxin fish tissue concentrations determined from annual sampling declined sharply following completion of the Canton Mill modernization in 1993. Dioxin fish tissue sample concentrations in bottom feeding species at main stem river sample locations became non-detect in 2000 and have remained below analytical detection levels since that time. Dioxin fish tissue sample concentrations in sport fish species from all sampling locations in the Pigeon River became non- detect in the mid-1990s. Based on annual fish tissue sampling,the State of North Carolina lifted the dioxin in fish advisory for the Pigeon River upstream of Waterville Lake in August 2001. The State of Tennessee lifted the dioxin in fish advisory for the Tennessee portion of the Pigeon River in January 2003. The only fish advisory remaining is for carp in Waterville Lake. Dioxin levels in carp collected from Waterville Lake since 2000 continue to be at or near analytical detection levels and are below the North Carolina Department of Health and Human Services (NC DHHS) dioxin toxicity equivalent(TEQ)fish advisory action level of 4 parts per trillion(ppt). The NC DHHS has indicated that two consecutive years of TCDD TEQ levels in carp of 3 ppt or less would provide basis for lifting the public health advisory for consumption of carp from Waterville Lake(e-mail correspondence from Dr.Luanne Williams,DHHS to Blue Ridge Paper dated 9 Mar 2006). The TCDD TEQs for carp fillet composite samples from Stations 4A&4B in Waterville Lake for the last two years are as follows: Year Station 4A Station 4B 2004 2.5 ppt 2.2 ppt 2005 2.1 ppt 3.6 ppt Study Plan Revision Blue Ridge Paper proposes the following changes to the 2001 biological monitoring Study Plan: • elimination of main stem river sampling stations--fish tissue samples beginning in 2006 will be collected only from Waterville Lake Blue Ridge Paper Products Inc 175 Main Street • PO Box 4000 Canton, North Carolina 28716. 828-646-2000 Raising Your Expectations Mark Hale, NC DENR DWQ,ESS- 3/30/06, Page 3 • elimination of whole body fish composite samples from the lake--only composite fillet samples of target bottom feeding fish species will be collected for laboratory analysis of dioxin. The 2006 study plan revision is enclosed for your review and approval. A copy of the 2001 study plan is also enclosed for your reference. Summary The 2006 dioxin in fish sampling work is planned for the mid-summer period of August and early September. We request DWQ approval of the 2006 study plan revision no later than the end of May 2006. Please contact us if you have questions. Paul S.Dickens J. Glenn Rogers Manager,Environmental Affairs Water Compliance Coordinator 828-646-6141 828-646-2874 dickep@blueridgepaper.com rogerg@blueridggpaoer.com Enclosures: Study Plan Revision,Dioxin Monitoring in Fish Tissue— Waterville Lake March 2006 Prepared by University of Tennessee for Blue Ridge Paper Products Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue December 2001 Prepared by EA Engineering for Blue Ridge Paper Products cc(w/enclosures): Bryn Tracy- NC DENR DWQ,ESS Susan Wilson—NC DENR DWQ,Permits Sergei Cherinkov—NC DENR DWQ, Permits Roger Edwards—NC DENR DWQ,ARO Keith Haynes -NC DENR DWQ, ARO Dr. Louanne Williams—NC DHHS Larry Wilson—UTK Billy Clarke—Roberts &Stevens John Crutchfield—Progress Energy Blue Ridge Paper Products Inc 175 Main Street • PO Box 4000 Canton, North Carolina 28716. 828-646-2000 Raising Your Expectations BLUE RIDGE DOPY PAPER PRODUCTS INC. STUDY PLAN REVISION DIOXIN MONITORING IN FISH TISSUE Waterville Lake Prepared for: Blue Ridge Paper Products,Inc. Canton Mill Canton,North Carolina NPDES No.NC 0000272 Prepared by: J.Larry Wilson,Ph.D. Departments of Forestry,Wildlife and Fisheries University of Tennessee Knoxville,Tennessee March 2006 Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville bake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 1 INTRODUCTION The Blue Ridge Paper Products Inc. Canton Mill conducts annual biological monitoring of dioxin in fish in the Pigeon River under conditions of the NPDES permit for the mill. This monitoring for years 2002 thru 2005 was in accordance with the December 2001 Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue prepared by EA Engineering, Science and Technology(EA 2001a). This document details changes for dioxin in fish monitoring beginning in 2006. The 2001 study plan is incorporated by reference. The specific changes to the 2001 study plan include: • elimination of main stem river sampling stations —fish tissue samples in 2006 will be collected only from Waterville Lake • elimination of whole body fish composite samples from the lake-- only composite fillet samples of target bottom feeding fish species will be collected for laboratory analysis of dioxin. The 2006 dioxin in fish tissue sampling from Waterville Lake will be conducted by personnel from the University of Tennessee, Knoxville(UTK),Department of Forestry,Wildlife and Fisheries. SAMPLE LOCATIONS The schedule for fish tissue collection will be consistent with prior years targeting dry weather periods in late August and early September. UTK will collect and prepare fish tissue samples from two locations in Waterville Lake on the Pigeon River(PRM 39.0-41.5). In previous studies,the fish collection sites in Waterville Lake have been designated 4A(PRM 41.5)and 4B (PRM 39.0). Site 4A is located approximately 21.8 RM downstream from the Canton Mill outfall,near the Messer Branch-Pigeon River confluence. Site 4B is in the vicinity of the Wilkins Creek-Pigeon River confluence, approximately 24.3 RM downstream from the Canton Mill outfall. Fish sampling will be conducted in the vicinity of each location described above; however,the distance or effort at each station will depend on how difficult it is to collect target fish species at that location. In 2005,common carp in the lower portion of the Waterville Lake were extremely difficult to collect. FISH COLLECTION TECHNIQUES AND TARGET SPECIES The goal of the 2006 fish collection effort is one composite bottom feeder fillet sample at each Waterville Lake sampling station 4A and 4B. Each composite consists of 3 to 5 similarly sized (shortest specimen within 75% of the length of the longest) adult individuals of the target species. Common carp (Cyprinus carpio)and channel catfish(Ictalunts punctatus) are the targeted bottom feeder species at sites 4A and 4B. Every reasonable effort will be made to collect the desired size, species, and number of fish.However,the outcome of sampling effort Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 2 each year is dependent on physical river conditions and the natural diversity and abundance of target fishes at each location. The field investigators will be equipped with an array of collecting gear, which will enable sampling of all habitats regardless of river conditions. The US EPA recommends active methods of fish collection in the Sampling Guidance Manual(Versar 1984), such as electrofishing, trawling, angling, or seining. These are preferred over passive methods (e.g., gill nets,trap nets, trot lines)because samples are collected from more defineable areas(Versar 1984). Electro- fishing may be used at both locations (4A and 4B); gill nets may also be used in areas where water depth will limit the electro-fishing gear. A boat electrofishing unit(pulsed direct current, Smith Root Type VIA electro-fisher powered by a 240-volt, 5000-Watt generator) will be provided. Electro-fishing techniques will follow those described in the National Dioxin Study (Versar 1984). All gill nets will be pulled and examined on a regular basis to reduce specimen stress or mortality,and specimens submitted for analysis will be selected for good health and condition. Fish collection techniques and level of effort(time)expended at both locations (4A and 4B)will be recorded. Total study effort for the 4A/4B collections in 2005 took 460 gill-net hours and approximately six hours of electro-fishing over a four-day period to obtain the necessary specimens.Channel catfish were easily caught,but common carp were extremely difficult to collect,particularly in the lower portion of the lake(4B). In summary,fish tissue samples will be collected as follows: • bottom-feeder composite—one composite bottom feeder fillet sample at each location 4A and 4B • catfish composite—one composite catfish fillet sample at each location 4A and 4B SAMPLE PREPARATION All fish tissue samples will be prepared in accordance with U.S.EPA Region IV recommendations (Cummingham 1990 as described in EA 2001a). To prevent cross- contamination between sampling stations,all sampling equipment likely to come into contact with the fish will be rinsed extensively with site water between stations. Specimens collected at each location will be sorted by size and species, and target species identified. UTK will obtain a 3 to 5-fish composite sample at each location(4A and 4B)which meet the species/size objectives discussed earlier.All specimens retained will be immediately placed on ice for later processing.All fish submitted for tissue analysis will be measured to the nearest millimeter(TL) and weighed to the nearest gram(wet weight). Following collection of channel catfish and common carp, each specimen will be prepared for shipment and analysis. Samples will consist of epaxial muscle tissue and skin from one side of the fish. Fillet samples will be prepared by removing scales (or removing the skin from Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 3 catfishes) and then making an incision behind the opercula(on both sides of the fish)from the base of the spine(behind the skull)to just below the pectoral fin. Care will be taken to cut through the epaxial muscle without puncturing the rib cage or gut lining. A second incision will be made along the length of the spine to the caudal fin on both sides of the fish. The muscle will be cut away from the rib cage to obtain a fillet. Fillet knives will be solvent rinsed(hexane and acetone)between fish from different locations. Each composite sample will be wrapped in aluminum foil(dull side toward sample), labeled, and placed on dry ice. One side fillets will be sent to Sevem Trent Laboratory for analysis; the opposite side fillets will be retained by Blue Ridge Paper as back-up fillets. All individual specimens (fillets)composing a single composite sample will placed together in a water-tight plastic bag labeled with the station name,sample number, and the number of samples in that composite. All labels will contain following information: sample identification number, sample location and station identification, sampling team initials, date of collection, species name,and sample type(i.e.,fillet). A chain-of-custody form will be filled out for each cooler of samples submitted for analysis, and each form will include composite specific information and instructions. All samples will be frozen solid prior to shipment to the analytical laboratory.The frozen samples will be packed on dry ice and shipped via overnight delivery to Severn Trent Laboratory (STL)—Sacramento for analysis.The back-up fillets will be retained in a freezer at the Canton Mill until laboratory analytical results for the composite fillet samples are received and verified; the back-up fillet samples will then be destroyed. SAMPLE ANALYSIS The composite fillet fish tissue samples received by STL will be analyzed for dioxin(2,3,7,8- TCDD),furan(2,3,7,8-TCDF) and related isomers using EPA Method 8290(US EPA 1994). Percent lipids will also be determined for each composite sample. STL will provide laboratory analytical reports including QA/QC summaries and completed chain-of-custody forms documenting receipt by the lab. REPORTING Results of 2006 dioxin in fish tissue sampling from Waterville Lake will be submitted to the NC DENR within 180 days of the completion of field work as required by the Blue Ridge Paper NPDES permit. The fish tissue sampling and analytical report will follow the general format of prior year reports. Dioxin toxicity equivalent(TEQ)levels will be calculated for all 17 chlorodibenzo dioxin and furan(CDD/F) isomers included in EPA Method 8290. The TEQ of each detectable isomer will be calculated based on the toxicity equivalent factor(TEF)for the isomer provided by the World Health Organization(WHO 1997). The measured concentration of each CDD/F isomer will be multiplied by its appropriate TEF to obtain a concentration of the isomer equivalent to the toxicity of 2,3,7,8-TCDD, the most toxic of the CDD/F isomers. Non- detectable concentrations will be treated as zero values for TEQ calculation. As requested by the Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 4 NC DHHS (Williams 2006),the TEQ results for the last two years will be presented in a columnar, side-by-side format to allow easy comparison against health advisory action levels. References EA Engineering,Science,and Technology Inc. 1990. Study Plan for the Monitoring of Dioxin in Fish Tissue. EA Report No. 11370.01,prepared for Champion International Corporation,Canton, North Carolina. EA Engineering,Science,and Technology Inc 1991. Results of the 1990 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.02,prepared for Champion International Corporation,Canton,North Carolina. EA Engineering,Science,and Technology Inc 1992. Results of the 1991 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.03,prepared for Champion International Corporation,Canton,North Carolina. EA Engineering,Science,and Technology Inc. 1993a. Results of the 1992 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.05,prepared for Champion International Corporation,Canton,North Carolina. April. EA Engineering,Science,and Technology Inc. 1993b. Results of the 1993 Dioxin Monitoring in Fish Tissue EA Report No. 11370.06,prepared for Champion International Corporation,Canton, North Carolina. December. EA Engineering,Science,and Technology Inc 1994. Results of the 1994 Dioxin Monitoring in Fish Tissue EA Report No. 11370.07,prepared for Champion International Corporation,Canton,North Carolina December. EA Engineering,Science,and Technology Inc 1995. Results of the 1995 Dioxin Monitoring in Fish Tissue- EA Report No. 13043.01,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc 1996. Results of the 1996 Dioxin Monitoring in Fish Tissue. EA Report No. 13176.01,prepared for Champion International Corporation,Canton,North Carolina December. EA Engineering,Science,and Technology Inc 1997. Results of the 1997 Dioxin Monitoring in Fish Tissue. EA Report No. 13353.01,prepared for Champion International Corporation,Canton,North Carolina November. EA Engineering,Science,and Technology Inc. 1998. Results of the 1998 Dioxin Monitoring in Fish Tissue EA Report No. 13478.01,prepared for Champion International Corporation,Canton,North Carolina December. EA Engineering,Science,and Technology Inc 2000. Results of the 1999 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01,prepared for Champion International Corporation,Canton,North Carolina January. EA Engineering,Science,and Technology Inc 2001a. Study Plan for Pigeon River Dioxin Monitoring in Fish tissue. Prepared for Blue Ridge Paper Products,Canton,North Carolina November. Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 5 EA Engineering,Science,and Technology Inc. 2001b. Results of the 2000 Dioxin Monitoring in Fish Tissue. EA Report No. 13745.01,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2001c. Results of the 2001 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.01,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc 2003. Results of the 2002 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.02,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2004. Results of the 2003 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.03,prepared for Blue Ridge Paper Products,Canton,North Carolina. January. Henry,A.G.and J.L.Wilson. 2006. Results of 2005 Dioxin Monitoring in Fish Tissue. Center for Environmental Biotechnology and Department of Forestry,Wildlife and Fisheries, University of Tennessee,Knoxville,Tennessee. U.S.Environmental Protection Agency(US EPA). 1994. Analytical Procedures and Quality Assurance for Multimedia Analysis of Polychlorinated Dibenzo-para-dioxins and Polychlotnated Dibenzofutans by High Resolution Gas Chromatography/High Resolution Mass Spectrometry(Method 8290). Versar,Inc 1984. Sampling Guidance Manual for the National Dioxin Study. U.S.Environmental Protection Agency. EPA Contract 68-01-6160. Work Order Number 8.7. Office of Water Regulations and Standards,Monitoring and Data Support Division,Washington,D.C.Final Draft July. Williams, L 2006. E-mail correspondence from North Carolina Department of Health and Human Services to Blue Ridge Paper Products concerning review of 2005 Dioxin Monitoring in Fish Report, March 9. World Health Organization(WHO). 1997. Exposure and Human Health Reassessment of 2,3,7,8- Tetrachlorodibenzo-p-dioxin(TCDD)and Related Compounds: Part II Health Assessment of 2,3,7,8-Tetmchlorodibenzo-P-dioxin(rCDD and Related Compounds. COPY EA Project 13900.01 STUDY PLAN FOR PIGEON RIVER DIOXIN MONITORING IN FISH TISSUE Prepared for. Blue Ridge Paper Products Canton, NC Prepared by.• I EA Englneering, Science, and Technology 444 Lake Cook Road, Suite 18 Deerfield, IL60015 December2001 TABLE OF CONTENTS Page I..........Introduction .................................................................................... 1-1 2. Station Locations .............................................................................. 2-1 3. Fish Collection Techniques and Target Species .......................................... 3-1 4. Sample Preparation........................................................................... 4-1 5. Analysis of Fish Tissue Samples ............................................................ 5-1 6. Quality Assurance ............................................................................. 6-1 7. Project Schedule............................................................................... 7-1 8. Monitoring Report............................................................................. 8-1 9. References ...................................................................................... 9-1 i 1. INTRODUCTION This study plan details the materials and methods that will be used to annually assess the levels of dioxins and flamns in fish tissues from the Pigeon River downstream of the discharge from the Blue Ridge paperm ll in Canton,North Carolina. This study plan was developed in response to requirements in the mill's current NPDES permit(Permit No.NC0000272). Changes to original permit conditions as detailed in letters from North Carolina Division of Water Quality(NCDWQ)and North Carolina Department of Health and Human Services (NCDHHS)dated 22 August 2001 and 31 August 2001,respectively have been incorporated into this study plan. Section 2 of this study plan provides information regarding the locations of the sampling stations. Section 3 details the techniques that will be used to collect fish at each station and the target species. Section 4 describes the procedures that will be used to prepare the collected fishes for tissue analysis. Section 5 specifies the analytical technique that will be used to determine the concentrations of the different dioxin and fnran isomers in each tissue sample. The Quality Assurance plan is presented in Section 6,and the project schedule, monitoring report,and references are found in Sections 7, 8,and 9,respectively. 1 2. STATION LOCATIONS Six stations have been established for the collection of fishes(Figure 2-1 and Table 2-1). Station 1,the background site,is located at Pigeon River Mile(RM)64.5 adjacent to the Canton Recreational Park, approximately 1.2 RM upstream from the Canton Mill outfall. Except at very high flows, the Canton Mill dam blocks the movement of fishes thereby preventing the interaction of control and monitoring station fishes. Station 2 is located at RM 59.0,upstream from Clyde,NC and approximately 4.3 RM downstream from the Canton Mill outfall. Station 3 is located at RM 52.3 just upstream of the old Rt.209 bridge,approximately 11.0 RM downstream from the Canton Mill outfall. Stations 4A and 4B are located in Waterville Lake at RM 41.5 and 39.0,respectively. Station 4A is located approximately 21.8 RM downstream from the Canton Mill outfall,near the Messer Branch-Pigeon River confluence. Station 4B is in the vicinity of the Wilkins Creek-Pigeon River confluence, approximately 24.3 RM downstream from the Canton Mill outfall. Stations 4A and 4B correspond to the upper and lower ends,respectively,of Waterville Lake. Station 5 is at RM 19 near Bluffton,TN,44.3 miles downstream of the mill outfall. Fish sampling will be conducted in the immediate vicinity of each location described above,however, the sample reach may be extended somewhat, if necessary,to facilitate collection of the required number Of fish. 2 1a0 Station 5 RM 19.0 5 Bluffton,TN-- (19.3) artford,TN TENNESSEE N NORTH CAROLINA �K �19 Hydro Plant (26.0) 0 m f Waiters Dam B Station 46 Statio41 4 RM 39.0 RM 4 Waterville Lake Flnes ONE New Hepeo Bridge FLOW Jonathan Crook O)dRL209 3 Station 3 Station 2 n��l RM 52.3 RM 50.0 Waynesville ay Ouf�ll STP d 2 Canton,NC RM 50A \Q 1 GN Clyde S 1" RMM 84.64.5 (Control) Figure 24. Fish tissue sampling station locations on the Pigeon River. TABl.E2-1 PIGEON RIVER SAMPIQIG STATIONS Station River Station Location and Numbs Mile Distance Item OmPall Site llescrintionfFfobi it Toe Fsh Community 1 64.5 Pigean River upstream from Canton, Characterized by riffle,me,and pool habitats Maximum NC, Abundance dominated by minnow and dusters. River NC,adjata:ntmOmton Rcereatlmnl depth approximately 6 ft nd Substrate primarily cobble and chub,greenfin darter and rock boss arodominont, Northemhog Ptak(1.2 RM upstream from Canton boulders interspersed with gravel and sand. sucker,black outhouse,ml=shiner,redbreast sunfish,central Mill outfall). stoncrolleti gmenside darter,and nmtticd sculpin are common. 2 59.0 Pigmy River upstream from Clyde,NC Characterized by riffle,any and pool habitats with canopy Relative abundance dominated by redbreast sunfish,central (43 RM downstream from the Canton cove. Maximum depth approximately 5 ft. Substrate smneroller,and nonhem hog sucker. Mill culfalU• primarily cobbldgmvellsand with some boulders and bedrock 3 52.3 Pigeon River in the vicinity of the Rt. Cluawlerized by riffle.mn,and pool habitats with some Redbrmsr Worth,northern hog sucker,and common carp am 209 bridge(11.0 RM dowastremn canopy cove Maximum depth approzimately5 fL dominant. Central storrerolla is common. from the Croton M0l outfol0 Subsume primarily bedrock and boulders with soma I cobble and sandfgmvelffnes deposited In pod meal l i 4A 41.5 Upper Waterville lake(21.8 RM Characterized by deep-wutalemtle habitat,bedrock, Relative abundance dominated by black crappie. Bluegill,downstream fiom the Canton Mill and soft bottom sediments. Maximum depth sampled fiaWead catfish,channel catfish,largemouth boss,and common 4 outfalt) approximately 14 ft cary ore common. 411 39.0 Lov or Waterville lake(243 RM Characterized by deep-water lemle habitat,bedrock, Relative abundance of catch dominated by block crappih,downstream fmm the Canton Mill and softbotmm sediments. Maximum depth sampled BNegill,channel catfish,flathead catfish,and carp am common. outfalp approximately 40 ft. Very aterp banks with little coma. 5 19.0 Pigeon River near BlufRoo,TN,Just Chomctirized by deep ponds and now mith some,shallow Central stonerollerand northern hog sucker we dominant. Dom the Canton MiB omfalowmm riffles trea Maximum depth approximately 6 to 8 ft. Substrate Smalbnmah bass,whitemll shiner,telescope shiner,greeasido 9 primarily bedrock boulder,and cobble, darter,and banded sculpin are common. Except for smallmouth bass and took bass,cenuamhids arc uneommaon, , { j `r: 3. FISH COLLECTION TECHNIQUES AND TARGET SPECIES A listing of the Pigeon River fish collection techniques is provided below: Station Number River Mile Sampling Technique 1 64.5 Electrofishing 2 59.0 Electrofishing 3 52.3 Electrofishing 4A 41.5 Gill nets 4B 39.0 Gill nets 5 19.0 Electrofishing Except in Waterville Lake,the principal sampling gear will be electrofishing. Depending on depth,either a pram or boat electrofisher will be used. Gillnetting is the most effective technique for the collection of bottom-feeder species from the Waterville Lake monitoring stations. Gill nets will be checked at least once a day,usually within 12 hours of being deployed. Other appropriate sampling techniques may be used if necessary. Field notes will be recorded at each sampling station including the type of sampling gear,level of effort(time),flow and clarity conditions,and selected physiochemical data(e.g.,dissolved oxygen,water temperature,and conductivity[electrofrshing locations only])using accepted proceedures and equipment. All fishes submitted for tissue analysis will be measured(total length),weighed(wet weight),examined for anomalies,and recorded on a standard Fisheries Data Sheet(Figure 3-1). The goal of the fish collection effort is to collect one composite bottom feeder fillet sample at each of the six sampling stations. Each composite will consist of 3 to 5 similarly sized(shortest specimen within 75%of the length of the longest)adult individuals of the target species. Common carp will be the target species at Stations 2,3,4A,and 4B,with northern hog sucker and black redhorse as alternative species in the riverine portion of the river below the mill(i.e., Stations 2 and 3). Common carp are absent at Stations 1 and 5. At these stations,black redhorse will be the target bottom feeder,with northern hog sucker and smallmouth buffalo being alternative species. Alternative representative bottom feeder species may be collected in the rare event that these target species are not collected In Waterville Lake,one additional fillet composite sample using either channel catfish or flathead catfish will be collected at Stations 4A and 4B. Catfish are rare in the river between the mill and Waterville Lake. However,in the event that three or more catfish of a similar size are encountered at either Stations 2 or 3, a catfish fillet composite will be prepared for either or both of these stations. In addition to the fillet composites, a whole body composite consisting of 3-5 similarly sized common carp will be collected at either Station 4A or 4B in Waterville lake. 5 Table 3-1 Fish Collection Techniques Station Number Station Location Sampling Technique 1 Pigeon River Mile 64.5 Electrofishing 2 Pigeon River Mile 59.0 Electrofishing 3 Pigeon River Mile 52.3 Mectrofishing 4A Pigeon River Mile 41.5 Gill nets 4B Pigeon River Mile 39.0 Gill nets 5 Pigeon River Mile 19.0 Electrofishing In summary,fish will be collected as follows: c Bottom feeder fillet composite—one sample at all six stations • Catfish fillet composite—one sample at Stations 4A and at 4B • Common carp whole body composite--one sample from either Station 4A or 4B • Catfish fillet composite—one sample at Stations 2 and at 3,if specimens are encountered 7 4. SAMPLE PREPARATION Fillet samples will consist of the epaxial muscle tissue from one side of the fish. The fillet from the other side will be retained as a backup until laboratory results are obtained. Bottom feeder whole-body samples will consist of the entire fish. Specimens collected will be rinsed in site water,stunned with a sharp blow to the head and placed on wet ice until processing.Each fish selected for analysis will be weighed and measured. Fillet samples will be prepared by removing all scales (or removing skin from catfishes)and subsequently making an incision behind the opercula(on both sides of the fish)from the base of the spine(behind the skull)to just below the pectoral fin. Care will be taken to not puncture the gut lining. A second incision will be made along the length of the spine to the caudal fin on both sides of the fish. The epaxial muscle will then be gently cut away from the rib cage to obtain a fillet. In this fashion, all flesh and skin(except catfishes)will be obtained from head to tail. The fillets from specimens comprising a particular composite will be combined,then the sample will be wrapped in aluminum foil(dull side toward sample),placed in a water-tight plastic bag,labeled (see Section 6),and placed on wet ice. Within 24 hours of processing,the samples will be frozen. 8 5. ANALYSIS OF FISH TISSUE SAMPLES Samples will be analyzed for dioxin using EPA Method 8290(U.S.EPA 1994). Percent lipids will also be determined for each sample. The laboratory will measure the concentration of 17 isomers of chlorodibenzo dioxins and furans(CDD/F). The toxic equivalent CMQ)of each detectable isomer will be calculated based on toxicity equivalent factors(TT3F)provided by the World Health Organization(WHO 1997). The measured concentration of each CDD/F isomer will be multiplied by its appropriate TEF to obtain a concentration of that isomer equivalent to the toxicity of 2,3,7,8-TCDD,the most toxic of the many CDD/F isomers. As per the directive of NCDHHS,non-detectable concentrations will be treated as zero values for TEQ calculations. 9 6. QUALITY ASSURANCE The following procedures will be followed to prevent contamination of samples collected at different stations or between composites collected at the same station. Dip nets,fish scalers, and holding containers will be rinsed with site water prior to use at each station. All fish will be rinsed in site water to remove any debris(e.g.,sediment)prior to processing. During processing,the measuring board will be wrapped with clear plastic wrap and this wrap will be changed among stations. Fillet knives will be solvent rinsed(hexane and acetone)between fish from different stations. Each composite sample will be wrapped in aluminum foil(dull side toward sample),labeled,and placed on dry ice within 24 hours of processing. All fillets or whole bodies composing a single composite sample will be foil-wrapped, then placed in a water-tight plastic bag labeled with the station name,sample number,and the species in that composite. All labels will contain the following information: • Sample identification number, • Station identification, • Sampling team initials, • Date of sample collection, • Species name, • Sample type(ie.,fillet or whole body) • A unique composite number Chain-of-Custody(COC)sheets will be completed following sample preparation and compositing. The composite identification number and corresponding number and type of fish comprising that composite sample will be recorded on the COC. Copies of all COCs will be retained. Following completion of sampling,samples will be shipped on dry ice to the analytical laboratory via an overnight courier. Upon receipt,the laboratory will compare the contents with that noted on the COC sheets and will note the condition of the samples. 10 7. PROJECT SCHEDULE To be consistent with past collections,all samples will be collected in August or September. A final report will be provided to NCDEQ within 180 days of sampling. 11 S. MONITORING REPORT Each annual monitoring report will include the sampling methods and procedures employed, a description of the sampling locations,descriptions of each fish collected(e.g.,species,length, and weight),as well as the results of the chemical analysis(reported as individual TCDD/F isomers and 2,3,7,8-TCDD Toxic Equivalent Values). Also included in appropriate appendices will be field notes,copies of all chain-of-custody sheets,and any pertinent memorandum or communication record forms. 12 9. REFERENCES U.S.Environmental Protection Agency(U.S.EPA) 1994. Analytical Procedures and Quality Assurance for Multimedia Analysis of Polychlorinated Dibenzo-para-dioxins and Polychlorinated Dibenzofurans by High-Resolution Gas Chromatography/High- Resolution Mass Spectrometry(Method 8290). World Health Organization(WHO). 1997. Exposure and Human Health Reassessment of 2,3,7,8-Tetmchlorodibenzo-p-dioxin(TCDD)and Related Compounds: Part II Health Assessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin(TCDD)and Related Compounds. 13