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HomeMy WebLinkAboutNC0000272_2013 Dioxin in Fish Tissue Report_20140331 75 evergreen,,, 1 a Office packaging 75 Main Street• Conlon, NC 28716 NMM#08-14 January 31, 2014 CERTIFIED MAIL RETURN RECEIPT REQUESTED Landon Davidson 7099 3220 0371 4392 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: 2013 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 2013 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 2013 surveillance. The concentrations of dioxin and furan congeners in channel catfish and common carp fillet samples collected from Waterville Lake in August 2013 remain below the 4 ppt TEQ fish advisory level established by the NC DHHS. Very truly y �ick McCracken EHS&S Water Supervisor 828-646-2874 RECEIVED nick.mccracken(a)eveMack.com Division of water Resources Enclosure—2013 Dioxin in Fish Tissue Report � _3 MU Water Ouatity Regtonat Ooeratlona Asheville Regional Office 1i h [)y desiaf) 2013 Dioxin in Fish Tissue Report 31 Jan 2014, Page 2 cc w/enclosure: NC DENR (2 copies) Division of Water Resources Water Resources Section ATTENTION—CENTRAL FILES 1617 Mail Service Center Raleigh,North Carolina 27699-1617 Sergei Chernikov, NC DWR—Complex Permits Section(electronic) Rick Smith,Duke Power(electronic) Larry Wilson, UfK(electronic) C-File(cover letter only) RESULTS OF 2013 DIOXIN MONITORING IN FISH TISSUE Prepared for: Blue Ridge Paper Products Inc., dba Evergreen Packaging Canton Mill Canton,North Carolina Prepared by: Theodore B. Henry,Ph.D. Center for Environmental Biotechnology and Departments of Forestry,Wildlife and Fisheries University of Tennessee Knoxville,Tennessee J. Larry Wilson,Ph.D. Departments of Forestry,Wildlife and Fisheries University of Tennessee Knoxville,Tennessee January 2014 TABLE OF CONTENTS Page List of Tables . . . . . . . . . . . . . . . . . List of Figures. . . . . . . . . . . . . . . . . EXECUTIVE SUMMARY . . . . . . . . . . . . . iv 1. INTRODUCTION . . . . . . . . . . . . . 1 2. SAMPLING LOCATIONS . . . . . . . . . . . . . 2 3. SAMPLING OBJECTIVES . . . . . . . . . . . . . 6 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT . . . 7 5. SAMPLE PREPARATION . . . . . . . . . . . . . 13 6. ANALYTICAL RESULTS . . . . . . . . . . . . . 15 7. REFERENCES . . . . . . . . . . . . . . . 27 8. APPENDICES . . . . . . . . . . . . . . 30 APPENDIX A: CHAIN OF CUSTODY FORM APPENDIX B: TESTAMERICA WEST SACRAMENTO ANALYTICAL REPORT APPENDIX C: BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS 1990-2004 APPENDIXD: 2006 REVISIONS TO DIOXIN MONITORING PLAN i 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 2013 . . . . . . . . . . . . . . . . . . 9 6-1 Summary of Pigeon River fish tissue analysis results—2013 . . . . 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 2013 Waterville Lake fish tissue composites . . . . . . . . . . . . . . . . 20 6-4 Blue Ridge Paper Canton Mill fish fillet tissue analysis results 2005—2013 . . . . . . . . . . . . . . . . 22 �fv n I LIST OF FIGURES Number Title Page ES-1 TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2013(Stations 4A and 413) . . . . . . . . . . . . . . . v ES-2 TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2013 (Stations 4A and 413) . . . . . . . . . . . . . . . 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, 2004-2013 . . . . . . . . . . . . . . . . . . 11 4-lb Weights of fish collected from Waterville Lake for tissue analyses,2004-2013 . . . . . . . . . . . . . . . . . . . 12 6-1 TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2013 (Stations 4A and 413) . . . . . . . . . . . . . . 25 6-2 TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2013 (Stations 4A and 413) . . . . . . . . . . . . . . . 26 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 2013 in accordance with NPDES permit conditions. This was the second sampling effort conducted by the university for the current permit. 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 2013 fish tissue sampling report using the revised protocol of 2006. Bottom feeding species (channel catfish and common carp) were collected in August 2013 from two locations (Stations 4A and 413) in the Pigeon River (Waterville Lake) and analyzed for 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD), 2,3,7,8-tetrachlorodibenzofilran(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 = 0.48 ppt for both 2,3,7,8-TCDD and 2,3,7,8-TCDF; 4B DL = 49 ppt for both 2,3,7,8-TCDD and 2,3,7,8-TCDF)... In common carp, 2,3,7,8-TCDD was 1.8 ppt in fillet composites collected at Station 4A and was 0.70 ppt (estimated) at Station 4B. For 2,3,7,8-TCDF the concentrations in common carp fillets were 2.0 ppt at Station 4A and 1.4 ppt at Station 4B. The concentration of 2,3,7,8-TCDF in the common carp whole body sample collected at Station 4B was 2.4 ppt and 5.8 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 (5.052 kg, Station 4A; 4.364 kg, Station B) 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 other previous years (2011, Station A, 4.144, Station B, 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 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 in 2013 were 4.2-8.7%. 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 requires three(3), additional years of fish tissue sampling and surveillance. All concentrations in fish tissue fillets remain below the NC DHHS 4 ppt TEQ action level for fish consumption advisory. i� iv Figure ES-1. TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2013 (Stations 4A and 413) 70 60 --- +Station 4A 50 i 12 -,t- Station 48 o M 40 30 O � 20 � C1 � 10 A b 0 -- 1990 1991 1992 1993 2994 1995 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 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 I0-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 r Figure ES-2. TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2013 (Stations 4A and 4B) 2.50 f Station 4A 2.00 --l- Station 4B 0 - c �A ro 1.50 a ; % i % A � a : ` 1.00 ` G a b — h ; �` FAr----,/-, b `. - a, b ,�A,_- a b a b A----A''' a a a 0.00 1 1 1 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 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 413, 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 hic., 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 2013 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 2001 a) of Chicago, Illinois. This report details the results of a study conducted during August 2013 to determine the concentrations of 2,3,7,8-TCDD (dioxin) and 2,3,7,8-TCDF (firan) 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 2013 fish tissue study is number 22 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). 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., 2013). 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 2013 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), 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 413 included electrofishing and setting of trot lines near the shore along both the left and right banks of Waterville Lake. Reservoir water level in 2013 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. �LJ 2 l 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 in. 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) I 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 413) for dioxin analyses in 2013. More precise geographical locations of each site are presented in Figure 2-2. Nwman..N pgfl �- Rav41x wr uo.n.*Ad, Nea.crou„enoy Wq •.�••�..,`TflYEEElE N 11911 ...I' WRrN ..�. •' GR01114 t NOTE: River mN[[el main[lurr[amplln8lxa11an or ��6 N�� Ir4ulary meuN Mewn in p9rinlheM[. Bry[[[tl x a Wxn BenlMn S mpLeg Slalan { 4 Ytllbn Oun WNerMnlYa 4B Grr N. NC wR 4A �:51 cm.• Nwn wNw Bray. amN.n na: RiwrpN IMJ) Nroen Ope— W.A ' NS.Q NwCrWln[ b ame s C� TNk4e Ni.q Mbwg�[ l�y IN.O�ry FVYu[m erlCY[ Rul JpOw tlYm FiOervlte ISB-01 IFWrvIN i f6p.01 RMew WgrM[NMIryIyIp MNIOWW C[nton,NC 151.67 IwJ) Mb� RM OIy0.NC � IW 9 4 aD. s,j Gmsy KMb illy op s� J Q IVATERVILLE LAR^f. �f Cwk u 44 2 e ti o '3567. nth e 0 44 40 —,� µexµ 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 (Cyprinus 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 4B. 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 4B 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 2013 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. u 6 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT Sampling was conducted during 5-6 August 2013. 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 2013, the mean total length of carp was 683 min and fish ranged from 630-722 mm. In 2011, the mean total length for carp was 685 min and fish ranged from 625-740 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 5.8 hours electrofishing and trot lines were used for 50.1 hours. 7 Table 4-1. Fish collection.techni ues and level of effort. Station Sampling Sampling Number RM Dates Techniques Level of Effort Comments 4A 41.5 5-6 Aug 2013 Boat An approximate 1.0 RM reach of river was sampled and the entire electrofishing 2.4 hours area was electrofished. No fish captured by trot lines. Trot lines(two) 5.3 hours total 4B 39.0 5-6 Aug 2013 Boat 3.4 hours An approximate 1.4 RM reach was sampled by electrofishing. Trot electrofishing lines were set throughout the area and yielded two channel catfish. Trot lines(two) 44.8 hours total 8 Table 4-2. Summary of fish composites collected at two stations in Waterville Lake,August 2013. 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 4B. Total Total Length whole body Date Station Species (mm) (g) Sample type Composite 5 Aug 13 4A Channel catfish 511 1270 Fillet R (RM 41.5)Channel catfish 489 925 Fillet R Channel catfish 460 935 Fillet R Channel catfish 485 1090 Fillet R Channel catfish 391 550 Fillet R MEAN 467 954 4A Common carp 690 4555 Fillet R (RM 41.5)Common carp 631 3525 Fillet R Common carp 722 5980 Fillet R Common carp 719 6300 Fillet R Common carp 680 4900 Fillet R MEAN 688 5052 5 Aug 13 4B Channel catfish 498 1140 Fillet R (RM 39.0)Channel catfish 445 920 Fillet R 6 Aug 13 Channel catfish 537 1200 Fillet R Channel catfish 525 1355 Fillet R Channel catfish 500 1050 Fillet R MEAN 501 1133 5 Aug 13 4B Common carp 685 4560 Fillet R 6 Aug 13 (RM 39.0)Common carp 695 4960 Fillet R Common carp 697 4700 Fillet R Common carp 677 4480 Fillet R Common carp 630 3120 Fillet R MEAN 677 4364 6 Aug 13 4B Common carp 724 5080 Whole body WB (RM 39.0) 9 t Target species were collected at both sampling stations in 2013. 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 five common carp at Station 4B. A single bottom feeder whole body common carp from Station 4B was submitted for analysis (Table 4-2). All 20 composite fillets submitted for analysis in 2013 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 2013. The size of the carp taken for whole body tissue analysis from Station 4B in 2013 was similar to size of whole body' fish collected in previous years. 10 Max, Min and Mean of Lengths taken from 80o Fish Tissue Samples 2004-2013 750 ^700 ' E 650 f --600 0 550 500 J 450 400 CO C CO "— fa a3 "— CO " ca — CU ca — M a3 "— M a., ca "— ca ca — aS CO - -) C-) asUcooUasUasoUmUmoUmUmoUmUasoUasUmoUasUcao ¢VooV-C¢Umy.¢Umv�¢�m��¢UmC�¢Om(),I-- ¢�m�� C Ca �r¢�m �r¢�rm v¢�m v¢�m v¢�m v v v v v d �t �t 4 c1 2004 2005 2006 2007 2008 2009 2011 2013 Figure 4-la. Lengths of fish collected from Waterville Lake for tissue analyses, years 2004-2013. 11 Max, Min and Mean of Weights taken from Fish Tissue Samples 2004-2013 9000 8000 7000 �6000 s 5000 24000 3000 2000 1000 } JL 0 •+ ++ �+ ++ r r 4 r-. .r+ N r a+ Q ++ •+ i+ .r+ .�.. .F. f0 � (D � — f0fti � f0 �— Ca ",Cc — M C13 Ca � f6 �— f6 � (0 �— f6 � f0 �— U f6U N OU c6U c0 OU (OU c6 OU c6() N OU c6U c0 OU c0U cl{ OU f6U c6 OU coU O �¢v m �¢�tm v¢vm v¢�m Ict �¢1rm �r �r . 2004 2005 2006 2007 2008 2009 2011 2013 Figure 4-lb. Weights of fish collected from Waterville Lake for tissue analyses, years 2004-2013. 12 I t ' ✓ 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 extensively with site water 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. 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 9/5/13 at 13 ' 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. t 14 6. ANALYTICAL RESULTS The fish tissue samples were received in one shipment (9/5/13) 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 2001a). 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 2013 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-p-dioxin (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= 0.48 ppt and 0.48 ppt respectively) and were also below DL at Station 4B (DL = 0.49 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 1.8 ppt at Station 4A and was detected (estimated 0.70 ppt, DL= 0.49) in fillet composites collected at Station 4B. For 2,3,7,8-TCDF, the concentrations in common carp fillets were 2.0 at Station 4A and 2.6 at Station 4B. The concentration of 2,3,7,8-TCDF in the common carp whole body sample collected at Station 4B was 2.4 and 5.8 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 relativd 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 TEFs 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 2013. Station Percent Number Sample ID Composite/Sample Type 2.3,7,8-TCDD(°l 2,3,7,8-TCDF'°) Livid 4A SITE 4A channel catfish 5 fillet samples ND(DL=0.48) ND(DL=0.48) 4.0 SITE 4A common carp 5 fillet samples 1.8 2.0 8.7 4B SITE 4B channel catfish 5 fillet sample ND(DL=0.49) ND(DL=0.49) 2.7 SITE 4B common carp 5 fillet samples 0.70'(DL=0.49) 1.4 4.2 SITE 4B common carp 1 whole body sample 2.4 5.8 15 (a)Units=ppt(parts per trillion)or pg/g(picogram/gram) (b)Estimated results. Result is less than the reporting limit (c)Analyte was positively identified,confirmation(CON)analysis used. (ND)Not detected,concentrations below the instrument detection limit(DL). 17 Table 6-2. Toxicity equivalence factors for CDD/F congeners. DIOXIN DIBENZOFURAN Isomer(a) 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,$-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. i (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 fish fillets analyzed had TEQ values below the NC DHHS advisory limit (3 ppt). For channel catfish, all TCDD and TCDF congeners analyzed were below detection resulting in a TEQ of 0.000. The TEQ for common carp was 2.455 at Station A and 0.893 at Station B. 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 (Station 4A, 13.44 ppt; Station 4B, 1.263 ppt) than observed in previous years (2005-2006), and results for 2008 and 2009 (2009, Station 4A, 1.560; Station 4B, 1.496 ppt) are further evidence that the 2007 results were anomalous. The 2013 whole body sample for common carp collected at Station 4B had a TEQ result of 3.196 ppt. Table 6-4 illustrates 2,3,7,8 TCDD concentrations in common carp fillet samples collected in 2005, 2006, 2007, 2008, 2009, 2011, 2013 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 mean weights of common carp collected from Stations 4A and 4B (5.052 kg, Station 4A; 4.364 kg, Station B) 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 in 2013 were 4.2-8.7%. 19 Table 6-3. Summary of CDD/F isomer analyses, toxicity equivalent factors, and toxicity equivalent values for the 2013 Waterville Lake fish tissue composites. STATION 4A Channel catfish fillet Common cart)fillet CDD/F congeners TEF(`) Results('! T Results") TEOro> Dibenzodioxin 2,3,7,8-TCDD 1.0 ND 0.000 1.8 1.8 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 3.2" 0.32 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 12 0.12 OCDD 0.0003 ND 0.000 50 0.015 Dibenzofuran 2,3,7,8-TCDF 0.1 ND 0.000 2.0 0.20 1,2,3,7,8-PeCDF 0.03 ND 0.000 ND 0.000 2,3,4,7,8-PeCDF 0.3 ND 0.000 ND 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 ND 0.000 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 2.455 (a)Units=ppt(parts per trillion)or pglg(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. 20 r Table 6-3 (cont). Summary of CDD/F isomer analyses,toxicity equivalent factors, and toxicity equivalent values for the 2013 Waterville Lake fish tissue composites. STATION 4E Channel catfish fillet Common cart)fillet Common carp whole body CDD/F congeners TEFt`) Results TEOtb� Results(') TEOc"� Resul[st°� TEOro> Dibenzodioxin 2,3,7,8-TCDD 1.0 ND 0.000 0.70 0.76d 2.4 2.4 1,2,3,7,8-PeCDD 1.0 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,7,8-HxCDD 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,6,7,8-HxCDD 0.1 ND 0.000 ND 0.000 4.9 0.49 1,2,3,7,8,9-HxCDD 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDD 0.01 ND 0.000 4.9 0.049 15 0.15 OCDD 0.0003 ND 0.000 14 0.0042 58 0.016 Dibenzofuran 2,3,7,8-TCDF 0.1 ND 0.000 1.4 0.14 1.4 0.14 1,2,3,7,8-PeCDF 0.03 ND 0.000 ND 0.000 ND 0.000 2,3,4,7,8-PeCDF 0.3 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,7,8-HxCDF 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,6,7,8-HxCDF 0.1 ND 0.000 ND 0.000 ND 0.000 2,3,4,6,7,8-HxCDF 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,7,8,9-HxCDF 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDF 0.01 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,7,8,9-HpCDF 0.01 ND 0.000 ND 0.000 ND 0.000 OCDF 0.0003 ND 0.000 ND 0.000 ND 0.000 Total TEQ 0.000 0.893 3.196 (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. 21 Table 6-4. Blue Ridge Paper Canton Mill fish fillet tissue analysis results,2005—2013 2005 Results(d) 2006 Results(e) Number Length Range Number Length Range Station Species of fish (mm) 2,3,7,8-TCDD(0." Station Species of fish (mm) 2,3,7,84CDDt4"1 1 Black redhorse 5 359-384 ND(0.35) 4A Common carp 3 635-692 0.64 t`I 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 t`I RM 59.0 Channel catfish 3 443460 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 0.76t`l 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 22 C; F C Table 6-4 (cont). Blue Ridge Paper Canton Mill fish fillet tissue analysis results, 2005—2013 2007 Results(d) 2008 Results(e) Number Length Range Number Length Range Station Species offish (mm) 2,3,7,8-TCDDjab1 Station Species offish (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 0.57t`t RM 41.5 Channel catfish 5 475-525 ND(0.29) 4B 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`I 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 (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 —2013 2009 Results(d) 2011 Results(e) Number Length Range Number Length Range Station Species of fish (mm) 2,3,7,8-TCDD'3,bi Station Species of fish (mm) 2,3,7,8-TCDDIN) 4A Common carp 5 620-698 1.1 4A Common carp 5 625-710 0.83` RM 41.5 Channel catfish 3 493-578 0.52t`l RM 41.5 Channel catfish 5 435-478 ND(0.24) 4B Common carp 5 647-696 0.93'`I 4B 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 Sevens 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 24 Table 6-4 (cont). Blue Ridge Paper Canton Mill fish fillet tissue analysis results,2005 —2013 2013 Results(d) Number Length Range Station Species offish (mm) 2,3,7,8-TCDD(ab) 4A Common carp 5 631-722 1.8 RM 41.5 Channel catfish 5 391-511 ND(0.48) 413 Common carp 5 630-697 0.701`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/gram) (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 25 Figure 6-1. TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990-2013 (Stations 4A and 413) 70 60 Station 4A 50 --or- Station 48 0 40 Z d a � W 30 m a 0 20 - O � F � 10 A� � A i 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 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 26 Figure 6-2. TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2013 (Stations 4A and 4B) 2.50 +Station 4A 2.00 -- - - - t- Station 4B o c Y d 1.50 \\ a ; ., Yl � M j `\ A � \ a 1.00 0 a b U �---�_, b I- A i �\ a `\ a \ 0.50 a I----�_, a a a --A a b ��__ b b a 0.00 _ _ - — 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 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 413, 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. 27 • 7. REFERENCES Curdle, 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 hie. 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 hie. 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 hie. 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 hie. 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 hie. 1997. Results of the 1997 Dioxin Monitoring in Fish Tissue. EA Report No. 13353.01, prepared for Champion International Corporation, Canton,North Carolina. November. t..J 28 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. 29 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- 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. i 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. 30 APPENDIX A: CHAIN OF CUSTODY FORM APPENDIX B: TESTAMERICA WEST SACRAMENTO ANALYTICAL REPORT APPENDIX C: BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS 1990-2004 APPENDIX D: 2006 REVISIONS TO DIOXIN MONITORING PLAN Appendices to the 2013 dioxin in fish tissue report are in separate PDF file document 31 APPENDIX A CHAIN OF CUSTODY FORM l.� 32 TestAmer)ca Sacramento Chain of Cui tody Record Te$t encq 88D Riverside Parkway IlIe1,1a'111'm,,IltI1IIm1111It ; �� 'D91111 'NE LFAam IN NwRONMEMAL TEBTINa West Sacramento.CA 95605 I NIII1tID111It'Lllmly111 ' phone 9116.3744378 fax 916.372 tosa Regulatory Program;.. ❑DW ❑+ ❑NPOF3 Rau ❑Olh I 'estArrieric tLaboratorles,Inc. $ Client contact Project Manager. Nick McCracken _ Site COM :Dr.Le. 113203948 Chant of Cus o�fy •- )C No' 0 2013 Evergreen Packaging. - - Tdffax:(S28)8462874 - lab Contact 1 of • 1 coca 175 Main Street - AnaWn Turnaround Time ampler.Univ rally of Tennessee Carton,NC 28716 ❑ CALENDAR DAYS ❑WORMG DAYS For Lab Use I Mr. 828 646-6700 Phone TAT 0 ddaantevm Below x alkm Client(628)646-6892 FAX ❑ 2 weeo = y �b Sampling. Project Name,Fish Tissue Sampling ❑ 1 week Site.Waterville Lake ❑ 2da/s •q M g1 I oe No. PO# _. _ ❑ Ida/ - E m it LTk s Semple Sample l F our $ f Sample Identification Date Time s.rAeq Mstrix corn. Sample pedfle Notes; e C ,1 I L L9rr 5 i I N L 'f yl - - ° t z sk its n « r y Y5 ✓< LS i _ I COMMaI4 6/ 1310 i I Poe a e Narmd Identification: - Sample Disposal(A fee may M essased H mpl a ne longer then moot Are any samples from a Listed EPA Hazardous Waste? Please List any EPA Waste�Codes for the Sample In the _ Comments Section itthe lab Is to dispose of the sample i .+❑Nm-Nazmd- ❑naemebk U SO Dnimt LJ Powe 0 - LJ URbeml E]RermtDChfflt ❑Dap id by Lab AVNmNs Special Inst ruction=Requirements 6 Comments: - i i I • Custody Seals In4V, Ye No Custody Seal No.. er Temp. erm Relin she Coal /3 Redefv n Im 6 �a k''1 Re Da li h - Company. D 6. WCOM Com � ldT;S I8 (i / a tin Co T ate /3 Reee in Laboralo Cpm D -. - W 1. by Y• m ,, ill 19A/M omt C -NWI-00g2,�Rev. dated O4e212013 77 4L 1 APPENDIX B TESTAMERICA WEST.SACRAMENTO ANALYTICAL REPORT 33 TestAmenca THE LEADER IN ENVIRONMENTAL TESTING ANALYTICAL REPORT TestAmerica Laboratories, Inc. TestAmerica Sacramento 880 Riverside Parkway West Sacramento, CA 95605 Tel: (916)373-5600 TestAmerica Job ID: 320-3948-1 Client Project/Site: Tissue For: Evergreen Packageing FKABlue Ridge Paper PO BOX 1549 Canton, North Carolina 28716 Attn: Nick McCracken Authorized for release by: 113012014 2:56:57 PM Jill Kellmann, Senior Project Manager (916)374-4402 jill.kellmann@testamericainc.com LINKS Review your project results through TotalAcce% Have a Question? Ask /The This report has been electronically signed and authorized by the signatory. Electronic signature is intended to be the legally binding equivalent of a traditionally handwritten signature. Ex ert Results relate only to the items tested and the sample(s)as received by the laboratory. Visit us at: www.testamericai ncDOM Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 Project/Site:Tissue Table of Contents �� CoverPage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Table of Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 F1 Definitions/Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Case Narrative . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 ❑ Detection Summary ° Client Sample Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Isotope Dilution Summary . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . 12 QC Sample Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 ° QC Association Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 d Lab Chronicle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 410 Certification Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 Method Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19 Sample Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 Chain of Custody . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 Receipt Checklists . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 i TestAmedca Sacramento Page 2 of 22 1/30/2014 Definitions/Glossary Client: Evergreen Packageing FKABlue Ridge Paper TestAmenca Job ID: 320-3948-1 Project/Site:Tissue Qualifiers Dioxin Qualifier Qualifier Description H Sample was prepped or analyzed beyond the specified holding time J Result is less than the RL but greater than or equal to the MDL and the concentration is an approximate value. q The isomer is qualified as positively identified,but at an estimated quantity because the quantitation is based on the theoretical ratio for these samples. Glossary Abbraviatlat Thesis commonly used abbreviations may or may not be pnasint In Oft report o Listed under the"D"column to designate that the result is reported on a dry weight basis %R Percent Recovery CNF Contains no Free Liquid DER Duplicate error ratio(normalized absolute dMerence) Di Fac Dilution Factor DL,RA,RE,IN Indicates a Dilution,Re-analysis,Re-exlmction,or additional Initial metals/amon analysis of the sample DLC Decision level concentration MDA Minimum detectable activity EDL Estimated Detection Limit MDC Minimum detectable concentration MDL Method Detection Limit MIL Minimum Level(Dioxin) NC Not Calculated ND Not detected at the reporting limit(or MDL or EDL ff shown) PQL Practical Quantitabon Limit QC Quality Control RER Relative eror ratio RL Reporting Limit or Requested Limit(Radiochemistry) RPD Relative Percent Difference,a measure of the relative difference between two points TEF Toxicity Equivalent Factor(Dioxin) TEQ Toxicity Equivalent Quotient(Dioxin) TestAmerica Sacramento Page 3 of 22 1/30/2014 Case Narrative Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID: 320-3948-1 Project/Site:Tissue Job ID: 3203948-1 Laboratory:TestAmerica Sacramento Na aft CASE NARRATIVE , 320-3948-1 Receipt The samples were received on 9/5/2013 8:15 AM;the samples arrived in good condition,properly preserved and where required.on ice. Except: Received fish samples frozen solid from dry ice. The laboratory IR thermomenter could not read at that low of a range. Dioxin-Method 8290 The Ion abundance ratios are outside criteria for one or more analytes in the following sample:SITE 4A COMMON CARP R-FILLETS (320-3948-2). Ouanfitation is based on the theoretical ion abundance ratio;therefore,these analytes have been reported as an estimated maximum possible concentration(EMPC). The affected analytes have been flagged. No other analytical or quality issues were noted. Dioxin Prep The following samples were prepared outside of preparation holding time:COMPOSITE OF 4B CHANNEL CAT#3,5(320-3948-8), COMPOSITE OF 4B COMMON CARP #4,6(320-3948-9).SITE 4A CHANNEL CAT R-FILLETS(320-3948-1),SITE 4A COMMON CARP R-FILLETS(320-3948-2),SITE 4B COMMON CARP WB(320-3948-7). Samples were received at the laboratory on 9/5/13. The method 8290 preparation holding fines expired 914113 and 9/5113, Sample extraction was initiated 9/12/13. No other analytical or quality issues were noted. TestAmerica Sacramento Page 4 of 22 1/30/2014 Detection Summary C Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 Project/Site:Tissue Client SampleSample ID: SITE 4A CHANNEL CAT R-FILLETS Lab Sample ID: 320-3948-1 1 1; L FAnalyte Result Qualifier NONE NONE Unit Dil Fac D Method Prep Type Percent Lipids 4.0 % 1 Lipids Total/NA �47 Client Sample ID: SITE 4A COMMON CARP R-FILLETS Lab Sample ID: 320-3948-2 (© Analyte Result Qualifier NONE NONE Unit DII Fac D Method Prep Type L"9 Percent Lipids 8.7 % 1 Lipids Total/NA Analyte Result Qualifier RL TDL Unit DII Fac D Method Prep Type IY OCDD 50 H 9.8 4.9 pg/g 1 8290 TotaIMA r Total TCDF 3.0 H 0.98 0.49 pg/g 1 8290 Total/NA iLLr�}=_ 1,2,3,6,7,8-HxCDD 3.2 J H 4.9 2.4 pg/g 1 8290 Total/NA Total TCDD 1.8 H 0.98 0.49 pg/g 1 8290 Total/NA I9 Total PeCDF 2.8 J H q 4.9 2.4 pg/g 1 8290 Total/NA Total HpCDD 15 H 4.9 2.4 pg/g 1 8290 TotaVNA 7tJa Total HpCDD 3.2 J H 4.9 2.4 pg/g 1 8290 Total/NA --- 1,2,3,4,6,7,8-HpCDD 12 H 4.9 2.4 pg/g 1 8290 Total/NA 2,3,7,8-TCDD 1.8 H 0.98 0.49 pg/g 1 8290 TotaIMA 2,3,7,8-TCDF 2.0 H 0.98 0.49 pg/g 1 8290 Total/NA Client Sample ID: SITE 4B COMMON CARP WB Lab Sample ID: 320-3948-7 4 Analyte Result Qualifier NONE NONE Unit DII Fee D Method Prep Type I i. '„ Percent Lipids 15 % 1 Lipids Total/NA 1J Analyte Result Qualifier RL TOL Unit DII Fee D Method Prep Type lid, OCDD 58 H 9.7 4.8 p9/9 1 8290 Total/NA - TotaITCDF 7.1 H 0.97 0.48 pg/g 1 8290 ToteVNA 1,2,3,6,7,8-HxCDD 4.9 H 4.8 2.4 pg/g 1 8290 TotaIMA Total TCDD 2.4 H 0.97 0.48 pg/g 1 8290 Total/NA Total PeCDF 3.8 J H 4.8 2.4 pg/g 1 8290 Total/NA Total HpCDD 15 H 4.8 2.4 pg/g 1 8290 Total/NA Total HpCDD 4.9 H 4.8 2.4 pg/g 1 8290 TotaIMA 1,2,3,4,6,7,8-HpCDD 15 H 4.8 2.4 pg/g 1 8290 TotaIMA 2,3,7,8-TCDD 2.4 H 0.97 0.48 pg/g 1 8290 TDtaIMA 2,3,7,8-TCDF 5.8 H 0.97 0.48 pg/g 1 8290 TotaIMA Client Sample ID: COMPOSITE OF 4B CHANNEL CAT#3,5 Lab Sample ID: 320.3948-8 rAnalyte Result Qualifier NONE NONE Unit Dil Fac D Method Prep Type Percent Lipids 2.7 % 1 Lipids Total/NA Client Sample ID: COMPOSITE OF 4B COMMON CARP #4,6 Lab Sample ID: 320-3948-9 Analyte Result Qualifier NONE NONE Unit DII Fee D Method Prep Type Percent Lipids 4.2 % 1 Lipids Total/NA Analyte Result Qualifier RL TDL Unit DII Fee D Method Prep Type OCDD 14 H 9.8 4.9 p9/9 1 8290 TotalMA Total TCDF 1.7 H 0.98 0.49 pg/g 1 8290 TotaVNA Total TWO 0.70 J H 0.98 0.49 pg/g 1 8290 7otalMA Total HpCDD 4.9 H 4.9 2.5 pg/g 1 8290 Total/NA 1,2,3,4,6,7,8-HpCDD 4.9 H 4.9 2.5 p9/9 1 8290 Total/NA 2,3,7,8-TCDD 0.70 J H 0.98 0.49 pg/g 1 8290 Total/NA This Detection Summary does not include radiochemical test results. TestAmerica Sacramento Page 5 of 22 1/30/2014 Detection Summary Client Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 I - - Project/Site:Tissue ` Client Sample ID: COMPOSITE OF 4B COMMON CARP #4,6 Lab Sample ID: 320-3948-9 [J (Continued) t Analyte Result Qualifier RL TDL Unit DII Fac D Method Prep Type 2,3,7,8-TCDF 1.4 H 0.98 0.49 pg/g 1 8290 Total/NA 1-61 T/ 0 1-� RAI This Detection Summary does not include radiochemical test results. TestAmerica Sacramento Page 6 of 22 1/30/2014 Client Sample Results Client: Evergreen Packageing FKABlue Ridge Paper TestAmenca Job ID: 320-3948-1 Project/Site:Tissue Client Sample ID: SITE 4A CHANNEL CAT R-FILLETS Lab Sample ID: 320-3948-1 Date Collected:08/05/13 14:00 Matrix:Tissue Date Received:09/06/13 08:15 _ Method:8290-Dioxins and Furans(HRGC/HRMS) ArWyu Result Qualifier RL TDL Una D Prepared Analyzed Dil Fac OCDD ND H 9.6 4.8 pg/g 09/12/1312:21 09/1811320:41 7 Total PeCDD NO H 48 2.4 P9/9 09/12/13 12:21 09/18/13 20:41 1 1,2,3,7,8,9-HxCDD NO H 4.8 2.4 P9/9 09/1211312:21 09/1811320:41 1 1,2,3,4,7,8,9-HpCDF ND H 4.8 2.4 pg/g 09/1211312:21 09/18/1320:41 1 1,2,3,4,6,7,8-HpCDF NO H 4.8 2.4 P9/9 09/1211312:21 09118/1320:41 1 TOW TCDF NO H 0.96 048 P9/9 09/12/1312:21 09/18M320:41 1 TOW HpCDF NO H 48 2.4 pWg 09/12/13 12:21 09/18/13 20:41 1 1,2,3,7,8-PeCOD NO H 4.8 2.4 P9/9 0911211312:21 09/18/1320:41 1 1,2,3,7,8-PeCDF NO H 4.8 2A p9/9 09112/1312:21 09/1811320:41 1 1,2,3,6,7,8-HxCDD NO H 48 2A P9/9 09/12/1312:21 09/1811320:41 1 1,2,3,6,7,8-HpCDF NO H 4.8 2.4 P9/9 09/1211312:21 09/18/1320:41 1 Total TWO NO H 0.96 0.48 P9/9 09/12/1312:21 09/1 aft 320:41 1 1,2,3,7,8,9-HxCDF NO H 4.8 2A pg/9 0911211312:21 09118/1320:41 1 OCDF NO H 9.6 4.8 P919 09/12/1312:21 09/1811320:41 1 Total PeCDF NO H 4.8 2A pg/g 0911211312:21 09/1811320:41 1 TON HpCDD NO H 4.8 2A P9/9 09/171131221 0911811320:41 1 - - 1,2,3,4,7,8-HxCDD NO H 4.8 2.4 pg/9 09117J1312:21 09118/1320:41 t TON HxCDD NO H 4.8 2.4 pWg 09/12J1312:21 09/1811320:41 1 Total HpCDF NO H 4.8 2.4 pg/g 09112/1312:21 09/1W1320:41 1 1,2,3,4,7,8-HxCDF NO H 4s 2A pyg 09/12/13 12:21 09/18/13 20:41 1 1,2,3,4,6,7,8-HpCDD NO H 4s 2.4 pW9 09/12/1312:21 09118/1320:41 1 2.3,4,6.7,8-HxCDF NO H 4.8 2A pg/g M12/1312:21 09/18/1320:41 1 2,3,7,8-TCDD NO H 0.96 0.48 p9/g 09112/1312:21 091181132041 1 2,3,7,84CDF NO H 0.96 0.48 P9/9 09/12/1312:21 0911811320:41 1 2,3,4,7,8-PeCDF ND H 4.8 2.4 pg/g 09/12/1312*21 0911811320:41 1 ko"Dilution %Recovery Qual/1Nr Lbrdtr Prepared Ansyzed Da Fac 13C-1,2,3,4,7,8-HpCDF 62 40- 335 09/12/1312:21 09118H32041 1 13G1,2,3,6,7,8-HxCDD 68 40-135 0911211312.21 09/1W320.41 1 13C-2.3,7,8-TCDD 66 40-135 09/12/1312:21 0911811320.41 1 13C-1,2,3,7,8-PeCDO 69 40-135 09/1211312.21 09/110320.41 1 13C.1,2,3,4,6,7,8-HpCDF 66 40-136 0911211312.21 0911W320:41 1 1 /3C-1,2,3,7,8-PeCDF 63 40-135 09//2/1312:21 0911W320.41 1 13C-2,3,7,8-TCDF 64 40-135 0911211312:21 OW18/1320.41 1 13C-1,$3,4,6,7,8-HpCDD 68 40-135 0911211312.21 0911W320.41 / 13C-OCDD 72 40-135 M211312.21 09/1811320.41 1 General Chemistry Anayte Result Qualifier NONE NONE Una D Prepared Analyzed Oil Fac Percent Lipids 4.0 % OW1211312:21 OW13/1311:07 i Client Sample ID: SITE 4A COMMON CARP R-FILLETS Lab Sample ID: 320-3948-2 Date Collected:08105/13 16:20 Matrix:Tissue Date Received:09/05/13 08:15 Method:8290-Dioxins and Furans(HRGC/HRMS) Am" Result Qualifier RL TDL Una D Prepared Analyzed oil Fac OCDD 50 H 9.8 4.9 pg/p 09/1211312:21 09/18/1321:24 1 Total PeCDD ND H 4.9 2.4 pg/g 09112113 1211 09/18/13 21:24 1 1,2,3.7,8,9-HxCDD NO H 4.9 2.4 pyp OW12JI312:21 09/18/1321:24 1 TestAmenca Sacramento Page 7 of 22 1/30/2014 Client Sample Results Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID: 320-3948-1 Project/Site:Tissue Client Sample ID: SITE 4A COMMON CARP R-FILLETS Lab Sample ID: 320-3948-2 Date Collected: 08/05/13 16:20 Matrix: Tissue Date Received:09/05/13 08:16 Method:8290-Dioxins and Furans(HRGC/HRMS)(Continued) Arlalyre Result Ouallfler RL TDL UnR D Prepared Analyzed Dil Fac 1,2,3,4,7,s9-HpCDF ND H 4.9 2.4 pg/g 09/12/1312:21 09/18/1321:24 1 1,2,3,4,6,7,8-HeCDF ND H 4.9 2.4 p9/9 09/1211312:21 09/18/1321:24 1 r Total TCDF 3.0 H 0.98 0.49 pg/g 09/12/13 12:21 09/18/13 21:24 1 Total HxCDF ND H 4.9 2.4 P9/9 09/12/13 12:21 09118/13 21:24 1 1,2,3,7,8-PeCDD ND H C9 2.4 pg/g 09/12/13 12:21 09/18113 21:24 1 1,2,3,7,8-PeCDF ND H 49 2.4 P9/9 09/12/1312:21 OW18/1321:24 1 1,2,3,6,1,8-1xCDD 3.2 JH 4.9 2.4 pg/g 09/1211312:21 09118/13 21:24 1 1,2,3,s7,8-HxCDF ND H 4.9 2.4 P9/9 09/12/1312:21 09/18/1321:24 1 Total TCDD 1.8 H 0.98 0.49 p9/9 09/1211312:21 09/18/1321:24 1 1,2,3,7.8,9.HxCDF ND H 4.9 2.4 p9/9 09/1211312:21 0911811321:24 1 OCDF ND H 9.8 4.9 P9/9 09/1211312:21 09/18/1321:24 1 Total PeCDF 2.8 J H q 4.9 2.4 p91g 09/12/13 12:21 09118/13 21:24 1 Total HpCDD 15 H 4.9 2.4 1>9/9 0911211312:21 09/18/1321:24 1 1,2,3,4,7,8-HxCDO ND H 4.9 2.4 P9/9 0911211312:21 09/1811321:24 1 Total HpCDD 3.2 J H 4.9 2.4 P9/9 0911211312:21 09/18/13 21:24 1 Total HpCDF ND H 4.9 2.4 p9/9 091121131221 09/18/1321:24 1 - 1,2,3,4,7,8-HxCDF ND H 4.9 2.4 pg/g 0911211312:21 0911811321:24 1 ` 1,2,3,4,6,7,8-HpCDD 12 H 4.9 2.4 P919 09/12/1312:21 09118/13 21:24 1 2,3,4,6,7,8-HxCDF ND H 4.9 2.4 pg/9 09/1211312:21 09/1811321:24 1 2,3,7,8-TCDD 1.8 H 0,98 0.49 Py9 09/12/1312:21 09/18/1321:24 1 2,3,7,8-TCDF 2.0 H 0.98 0.49 P9/9 0911211312:21 0912011302:30 1 2.3,4,7,8-PeCDF ND H 4.9 2.4 p9/9 09/1211312:21 09/18/1321:24 1 AlooM DOwdon %Recovey Qual1Mr LANb Pipared Analyzed Da rac 13C-1,$3,4,7,8.HxCDF 55 40-135 09/121i312:21 09/18�1321:24 1 13C-1,2,3,6,7,8-HxCDD 60 40-135 0911211312:21 09/la/1321:24 1 13C-2,3,7,8-TCDD 60 40-135 09/1V1312.21 091IN1321:24 1 13C-1,2,3,7,8-PeCDD 62 40-135 091121131221 09118/13 21:24 1 13C-1,23,4,6,7,8-HpCDF 62 40-135 0911211312:21 09//811321:24 1 13C-1,2,3,7,8-PeCDF 58 40-135 0911211312.21 0911&1321:24 / 13C-2,3,7,8-TCDF 57 40-135 09/12/1312:21 0911811321:24 1 13C-2,3,7,8-TCDF 62 40-135 09/12/13 ffi21 0920//302.30 1 13C-1,23,4,6,7,8-HpCDD 64 40-135 09/12/1311-21 09H8/1321:24 1 13C-WDD 67 40-135 0911V1312.21 0911W321:24 / General Chemistry Am" Result QuallRer NONE NONE Unit D Prepared Analyzed Dil Fac Pemern Lipids 8.7 % M12113 12:21 09/13/13 11:07 1 Client Sample ID: SITE 48 COMMON CARP WEI Lab Sample ID: 320-3948-7 Date Collected:08/06/13 13:10 Matrix:Tissue Date Received:09/06113 08:15 Method:8290-Dioxins and Furans(HRGC/HRMS) Am" Rewa Qualltbr RL TOL unk D Prepared Anai Oil Fac OCDO 58 H 9.7 4.8 py9 09/12/13 12:21 OW18113 22:07 1 Total POWD ND H 4.8 2.4 P9/9 09/12/1312:21 09/18/1322:07 1 1,2,3,7,8,9-HxCDD ND H 4.8 2.4 p9/9 09/12/1312:21 09/1811322:07 1 1,2,3A,7,8,9-HpCDF ND H 4.8 2.4 p9/9 09/12/1312:21 09/18/1322:07 1 1,2,3,4,6,7,8-HpCDF ND H 4.8 2.4 p9/9 09/1211312:21 09/18/1322:07 1 Total TCDF 7.1 H 0.97 0.48 pale 09/12/1312.21 09/1811322:07 1 TestAmerica Sacramento Page 8 of 22 1/30/2014 Client Sample Results Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID 320-3948-1 ProjectlSite:Tissue Client Sample ID: SITE 4B COMMON CARP WB Lab Sample ID: 320-3948-7 Date Collected:08/06/13 13:10 Matrix: Tissue Date Received:09/05/13 08:15 Method:8290-Dioxins and Furans(HRGC/HRMS)(Continued) Analyte Result Oualxier ILL TDL Unit D Prepared Analyzed Dil Fac Total HxCDF NO H 4.8 2.4 p9/9 M1211312:21 09/18/1322.07 1 1,2,3.7,8-PeCDD NO H 4.8 2.4 p9/9 09/1211312:21 0911811322:07 1 1,2,3,7,8-PeCDF ND H 4.8 2.4 pg/g 09112/131221 09118/1322:07 1 1,2,3,6,7,8-HxCDD 4.9 H 4.8 2.4 p9/9 09/12/13 12:21 09/18/13 22:07 1 1,2,3,6,7,8-HxCDF ND H 4.8 2.4 p9/9 09112/1312:21 09/1811322:07 1 Total TCDD 2.4 H 0.97 OA8 p9/9 09/12/13 12:21 09/18/13 22:07 1 1,2,3,7,8,9-HxCOF ND H 4.8 2A pg/9 09/1211312:21 09/1811322:07 1 OCDF NO H 9.7 4.8 p9/9 09/1211312*21 09118/1322:07 1 Total PeCDF 3.8 J H 4.8 2.4 p9/9 09/12/13 12:21 09/18/13 22:07 1 Total HpCDD 15 H 4.8 2.4 P9/9 09112/1312:21 0911811322:07 1 1,2,3,4,7,8-HxCDD ND H 4.8 2.4 p9/9 0911211312:21 09/1a/1322:07 1 Total HxCDD 4.9 H 4.8 2.4 Pyg 09/12/13 12:21 09/18/13 22:07 1 Total HPCDF ND H 4.8 2.4 p9/9 09112J1312:21 09/18/13 22:07 1 1,2,3,4,7,8-HXCDF ND H 4.8 2.4 p910 09/12/13 12:21 09/18/13 22:07 1 1,2,3,4,6,7,8-HpCDD 15 H 4.8 2A pole 09/1211312:21 0911811322:07 1 2,3,4,6,7,5.HxCDF NO H 4.8 2.4 polo 09/1211312:21 09/1811322:07 1 2,3,7,8-TCDD 2.4 H 0,97 0.48 p9l9 09/12/13 12:21 09/18/13 22:07 1 2,3,7,8-TCDF 5.8 H Os7 0.48 polo 09/12/13 12:21 09/20/13 03:08 1 2,3,4,7,8-PeCDF ND H 4.8 2.4 py9 09/12/13'12:21 0911811322:07 1 /aotope D1ludon %RaCowry Ow118er Limas Prepared Analyzed Dd Fac 13C-1,2,3,4,7,8-HxCDF 58 40-135 0911211312.21 09N8/1322,07 1 /3C-1,2,3,8,7,8-HxCDD 60 40-135 0911211312.21 09/1811322:07 1 13C-23,7,8-TCDD 59 40-135 OM211312.21 09/1W322.07 / 13C-1,23,7,8-PeCOD 62 40-135 0911211312.21 09/la'1322:07 1 13C-1,2,3,4,6,7.8-HpCDF 63 40-135 0911211312.21 09/18/1322.07 1 13C-1,23,7,8-PeCDF 57 40-135 0911211312:21 09/18n322:07 1 13C-2,3,7,8-TCDF 56 40-135 091121131t21 09//a/1322:07 1 13C-2,3,78-TCDF 60 40-135 09/1211312:21 0920/1303.as 1 13C-1,2,3,4,6,78-HxCDD 65 40-135 08/12(1312:21 09/18132207 / L 13C-OCDD 71 40-135 09/12/13 12:21 09//a/13 22:07 1 General Chemistry And" Resun Oualifier NONE NONE Unit D Prepared An@WW Dil Fac Percent Lipids 15 % OW12/13 12.21 O9/13/13 11:07 1 Client Sample ID: COMPOSITE OF 4B CHANNEL CAT#3,5 Lab Sample ID: 320-3948-8 Date Collected:08/06/13 00:00 Matrix:Tissue Data Received:09/05113 08:15 Method:8290-Dioxins and Furans(HRGC/HRMS) Ana" Result OualBfer RL TDL Unx D Prepared Analyzed Dil Fac OCDD NO H 9.9 4.9 p9/9 09M2/1312:21 09/18/1322:51 1 Total PeCDD NO H 4.9 2.5 p9/9 0911211312:21 09/1811322:51 1 1,2.3,7,8,9-HxCDD ND H 4s 25 p9/9 09/1211312:21 OW18/1322:51 1 1,2,3,4,7,8,9-HpCDF ND H 4.9 2.5 pgig 09/1211312:21 09/18/1322:51 1 1,2,3,4,6,7,8-HpCDF ND H 4.9 2.5 pg/g 09/12/13 1221 09/18/1322:51 1 Total TCDF ND H 0.99 0.49 pg/g 09/12/13 12:21 09/18/1322:51 1 Total HxCDF ND H 4.9 2.5 pg/g 09/12/13 12:21 09/18/13 22:51 1 1.2,3,7,E-PeCDD ND H 4.9 2.5 p9/g 0911211312:21 09/1811322:51 1 1,2,3,7,8-PeCDF ND H 49 2.5 p9/9 09/12/13 12:21 09/18/13 22:51 1 TestAmerica Sacramento Page 9 of 22 1/30/2014 Client Sample Results Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID: 320-3948-1 Project/Site:Tissue Client Sample ID: COMPOSITE OF 4B CHANNEL CAT #3,5 Lab Sample ID: 320-3948-8 Date Collected: 08106113 00:00 Matrix:Tissue Date Received:09/05/13 08:15 Method:8290-Dioxins and Furans(HRGC/HRMS)(Continued) AR*W Reaua Qualifier RL TDL Unit D Prepared Analyzed Oil Fac 1,2,3,6,7,&HxCDD NO H 4.9 2.5 pg/9 09/1211312:21 0911611322:51 1 1,2,3,6,7,8-HxCDF NO H 4.9 2.5 P9/9 09/1211312:21 09/la/1322:51 1 Total TCDD NO H 0.99 0.49 pg/g 09/12/1312:21 09/18/1322:51 1 1,2,3,7,8s-HxCDF NO H 4.9 2.5 pg/g 09/12/1312:21 09118/1322:51 1 OCDF ND H 9.9 4.9 pg/g 09/12/1312:21 09/18/1322:51 1 Total PeCDF NO H 4.9 2.5 pg/g 09/12/1312:21 09118/1322:51 1 Total HPCDD ND H 4.9 2.5 pg/g 09/1211312:21 09118/1322:51 1 1,2.3,4,7,&HxCDD NO H 4.9 2.5 pg/9 09/12/1312:21 09/18/1322:51 1 Total HxCDD NO H 4.9 2.5 pg/g 09/12/1312:21 09/18/1322:51 1 Total HpCDF NO H 4.9 2.5 pg/g 0911211312:21 09/18/1322:51 1 1,2,3,4,7,8-HxCDF NO H 4.9 2.5 p9/9 09112J1312:21 09/18/1322:51 1 1,2,3,4,6,7,8-HPCDD NO H 4.9 2.5 P9/9 09/1211312:21 09fi8/1322:51 1 2,3,4,6,7,8-HxCDF NO H 4A 2.5 p9/9 09/12/1312:21 09/18/1322:51 1 2,3.7,8-TCDD NO H 0-99 0A9 p9/9 09/12/1312:21 09/1811322:51 1 2,3,7,8-TCDF NO H 0.99 049 p9/9 09/12/1312:21 09118/1322:51 1 2,3,4,7,8-PeCOF NO H 4.9 2.5 pg/9 09/12/1312:21 0911811322:51 1 bo/ope Davison %Recovery Owllnar L6N# Prpwed Analyzed Da Fat 13C-1,2,3,4,7,&HxCDF 62 40-135 09/1Yf312:21 69H8H322:61 1 /3C-1,2,3,6,7,8-HXCDO 64 40-135 0911211312:21 Mas,1322:51 1 13C-2.3,7,8-TCDD 66 40-135 0911211312:21 09H811322:51 1 13C-1,2,3,7,8-PeCDD 69 40-135 0911211312.21 09/18n1322:51 1 13G7,23,4,6,7,8a1pCDF 72 40-135 091121'1312:21 OWlIV1322:51 1 13C-1,2,3,7,8-PeCDF 64 40-135 0911211312.21 0911W322:51 1 13C-2,3,7,8-TCDF 62 40-135 09/12/13/2.21 09/18/1322:51 1 13C-1,2,3,4,Q7,8HPCDD 75 40-135 091121131221 0911&1322.51 1 13C-OCDO 80 40-135 09112113 12.21 COMM 22.51 1 CGeneral Chemistry An*W Result Qualifier NONE NONE Unit D Prepared Analyzed Oil Fa: Parted Llpids 2.7 i 09/12/1312:21 09/13/1311:07 1 Client Sample ID: COMPOSITE OF 4B COMMON CARP #4,6 Lab Sample ID: 320-3948-9 Date Collected:08106/13 00:00 Matrix: Tissue Date Received:09/05/13 08:15 Method:8290-Dioxins and Furarts(HRGCIHRMS) Analyte Result Qualifier RL TDL Una D Prepared Analyzed oil Fac OCDD 14 H 9.8 4.9 Pg/g 09/1211312:21 OW1811323:34 1 Total PeCDD NO H 4.9 2.6 p91g 09/12/1312:21 09/18/1323:34 1 1,2.3,7,8,9-HxCDD NO H 4.9 2.6 pg/9 09/1211312:21 09118/1323:34 1 /,2,3,4,7,8,9.HpCDF NO H 4.9 2.5 119/9 0911211312:21 0911811323:34 1 1,2,3,4,6,7,8-HpCDF ND H 4.9 2.6 P9/9 09/12/1312:21 09/1811323:34 1 Total TCDF 1.7 H 0,98 0.49 pg/p 09/1211312:21 0911811323:34 1 TOW HxCDF NO H 4.9 2.6 pg/9 09/12/1312:21 0911811323:34 1 1,2,3,7,&PeCDD NO H 4.9 2.6 pg/g 09/1211312:21 09/18/1323:34 1 1,2,3,7.8-PeCDF NO H 4s 2.5 PW9 09/12/1312:21 09118/1323:34 1 1,2.3,6,7,8-HxCDD ND H 4.9 2.5 Pg/9 09/1211312:21 09/18/1323:34 1 1,2,3,6,7,8-HxCDF NO H 4.9 2.5 pg/g 09/12/13 12:21 09/18/13 23:34 1 Total TCDD 0.70 J H 0.98 0.49 pg/g 09/12/1312:21 09/18/13 23:34 1 1,2,3,7,8,9-HxCDF NO H 4.9 2.5 p9/9 09/12/'1312:21 09118/1323:34 1 TestAmerica Sacramento Page 10 of 22 1/30/2014 Client Sample Results Client: Evergreen Packageing FKABlue Ridge Paper TestAmenca Job ID. 320-3948-1 Project/Site:Tissue Client Sample ID: COMPOSITE OF 4B COMMON CARP #4,6 Lab Sample ID: 320-3948-9 Date Collected: 08/06/13 00:00 Matrix:Tissue Date Received:09106113 08:15 Method:8290•Dioxins and Furans(HRGCIHRMS)(Continued) Am" Resuit QualMer RL TDL unit D Preparod Analyzed Oil Fad OCDF ND H 9.8 4.9 pg/g 09/12/1312:21 09/18/1323:34 1 Total PeCDF ND H 4.9 2.5 pg/g D9/1 211 3 12:21 09118/1323:34 1 Total HpCDD 4.9 H 4.9 2.5 Pg/g 09/12/1312:21 09118/1323:34 1 1,2,3.4,7.8-HxCDD ND H 4.9 2.5 139/9 OW1211312:21 09118/1323:34 1 Total HxCDD NO H 4.9 2.5 Pg/g OW1211312:21 09118/1323:34 1 Toted HpCDF ND H 4.9 2.6 pg/g 09/12/1312:21 09118/1323:34 1 1,2,3,4,7,8-HxCDF NO H 4.9 2.5 p9/9 09/1211312:21 09118/1323:34 1 1,2,3,4,6,7,8-HpCDD 4.9 H 4.9 2.5 p9/9 09/1211312:21 09/1811323:34 1 2,3,4,6,7,8-HxCDF NO H 4.9 2.5 pg/g 09/1211312:21 09118/1323:34 1 2,3,7,8-TCDD 0.70 JH 0.98 0,49 pg/g 09/1211312:21 0911811323:34 1 2,3,7,8-TCDF 1.4 H 0.98 0.49 P9/9 09/1211312:21 09/20/1303:47 1 2,3,4,7,8-PeCDF NO H 4.9 2.5 p9/9 09/1211312:21 0911811323:34 1 1ao11 Dfiutlml %Recovery Que189er LerdO Prepaved Andynd DN Fad 13C-1,23,4,7,8-HxCDF 58 40-135 0911211312:21 091IM323.34 1 13C-1,2,3,6,7,8-HxCDD 60 40-135 09nW1312.21 OWIW1323.34 1 13C-2,3,7,8-TCDD 64 40-135 09/1271312:21 09/1a/1323.34 1 13C-1,2,3,7,8-PeCDO 67 40-135 08/1211312:2i 09118//323.34 1 13C-1,2,3,4,6,7,8-HpCDF 63 40-135 0911211312.21 0,M&1323.34 / 13C-1,$3,7,8-PeCOF 63 40-135 091120312.21 09118N323.34 / 13C-2,3,7,8-TCDF 61 40-135 09112113 12:21 09118113 23.34 1 1302,3,7.8-TCDF 65 40-135 0911211312:21 0912W303.47 / 13C-1,2,3,4,6,7,8-HpCDD 67 40-135 0911211312.21 09/1ar1323.34 / 13C-OCDD 72 40-135 OWIV1312.21 0911ar1323.34 1 General Chemistry Analrb Result Qualifier NONE NONE unit D Pregnd Analyzed oil Fac Percent uplds 4.2 % 09/12/1312:21 09/1311311:07 1 TestAmerica Sacramento Page 11 of 22 1/30/2014 Isotope Dilution Summary ❑ Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 1 ProjectlSite:Tissue 12 L. — I Method: 8290-Dioxins and Furans (HRGC/HRMS) Matrix:Tissue Prep Type:Total/NA Percent Isotope Dilution Recovery(Acceptance Limits) L HxCDF1 HxCDD2 TCDD PeCDD HpCDF1 PeC0F1 TCDF HpCDD Lab Sample ID Client Sample ID (40.135) (40435) (40435) (40.135) (40435) (40435) (40-135) (40.135) 320-3948-1 SITE 4A CHANNEL CAT R-FILLET: 62 68 66 69 66 63 64 68 320-3948-2 SITE 4A COMMON CARP 55 60 60 62 62 58 57 64 ° R-FILLETS 320.3948-2 SITE 4A COMMON CARP 62 R-FILLETS ❑ 320J946-7 SITE 46 COMMON CARP NB 56 60 59 62 63 57 56 65 32D3948-7 SITE 4B COMMON CARP WB 60 3203948-8 COMPOSITE OF 4B CHANNEL 62 64 66 69 72 64 62 75 (1 CAT#3,5 C'1 3203948-9 COMPOSITE OF 4B COMMON 58 60 64 67 63 63 61 67 CARP 94,6 i 3203948-9 COMPOSITE OF 4B COMMON 65 _ CARP #4,6 I LCS 320.25010/2-A Lab ConWl Sample 69 68 87 68 72 64 65 72 MB 320-2501011-A Method Blank 58 58 59 60 62 56 57 64 Percent Isotope Dilution Recovery(Acceptance Limits) OCDD !t Lab Sample ID Client Sample ID (40.135) 320-3948-1 SITE 4A CHANNEL CAT R-FILLET: 72 3203948-2 SITE 4A COMMON CARP 67 R-FILLETS I _� 320-3948-2 SITE 4A COMMON CARP R-FILLETS 320.3948-7 SITE 4B COMMON CARP WB 71 3203948-7 SITE 4B COMMON CARP WB 3203948-8 COMPOSITE OF 4B CHANNEL 80 CAT#3,5 3203948-9 COMPOSITE OF 48 COMMON 72 CARP #4,6 32D3948-9 COMPOSITE OF 4B COMMON CARP #4,6 LCS 320-25010/2-A Lab Control Sample 74 MB 320-25010/1-A Method Blank 69 Surrogate Legend HxCDF1=13C-1,2,3,4,7,8-HxCDF HxCDD2=13C-1,2,3,6,7,8-HpCDD TCDD=13C-2,3,7,8-TCOD PeCDD=13C-1,2,3,7,8-PeCDD HpCDF1=13G7,2,3,4,6,7,8-HpCDF PeCDF1=13C-1,2,3,7,8-PeCDF TCDF=13C-2,3,7,8-TCDF HpCDD=13C-1,2,3,4,6,7,8-HpCDD OCDD=13C-OCDD TestAmerica Sacramento Page 12 of 22 1/30/2014 QC Sample Results Client Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 Project/Site:Tissue Method: 8290-Dioxins and Furans(HRGC/HRMS) F Lab Sample ID: MB 320-2501011-A Client Sample ID: Method Blank Matrix: Tissue Prep Type:TotaUNA Analysis Batch: 25486 Prep Batch: 25010 MB Me Analyte Result Owlkir RL TDL Unit D prepared Analyzed Dil Fac OCDD ND 10 5.0 pwg 09/1211312:21 09/18/1319:15 1 Total PeCDD ND 5.0 2.5 P9/9 09/12/1312:21 09/18/1319:16 1 1,2,3,7,8,9-HxCDD ND 5.0 2.5 p9/9 09/12/13 12:21 09/1 all 19:15 1 1,2,3,4,7,8,9-HpCDF ND 5.0 2.5 p9/9 09/12/13 12:21 09/18/13 19:15 1 1,2,3,4,6,7,8-HpCDF ND 5.0 2.5 P9/9 09/12/13 12:21 09/18/13 19:15 1 Total TCDF ND 1.0 0.50 p9/9 09/12/13 12:21 09/18/13 19:15 1 Total H%CDF ND 5.0 2.5 P9/9 0911211312:21 09/18/1319:15 1 1,2,3,7,8-PeCDO ND 5.0 2.5 p9/9 0911211312:21 09/18/1319:15 1 1,2,3,7,8-PeCDF ND 5.0 2.5 P9/9 0911211312:21 09/18/13 19:15 1 1,2,3,6,7,8-HxCDD ND 5.0 Is pyg 09/12/13 12:21 09/1 all 19:15 1 1,2,3,6,7,8-HxCDF ND 5.0 2.5 pg/g 0911211312:21 09/18/13 19:15 1 Total TCDD ND 1.0 0.50 pg/g 09/12/1312:21 09/18/13 19:15 1 1,2,3,7,8,9-HxCDF ND 5.0 2.5 pyg 0911211312:21 09118/1319:15 1 OCDF ND 10 5.0 p9/g 0911211312:21 09/18/1319:15 1 Total PeCDF ND &0 2.5 Pg/g 0911211312:21 09/18/13 19:15 1 Total HpCDD ND 5.0 2.5 P9/9 09/12/1312:21 09/18/1319:15 1 1,2,3,4,7,8-HxCDD ND 5.0 2.5 p9/9 09/12/13 12:21 09/18/13 19:15 1 Total HxCDD ND 5.0 2.5 P9/9 09/1211312:21 09/18/13 19:15 1 Total HPCDF ND 5.0 2.5 p9/9 09/1211312:21 09/18/13 19:15 1 1,2,3,4,7,8-HxCDF ND 5.0 25 Pg/g 09/12/13 12:21 09/18/13 19:15 1 1,2,3,4,6,7,8-HpCDD ND 5.0 2.5 pg/g 09/12/13 12:21 09/11IM3 19:15 1 2,3,4,6,7,8-HxCDF ND 5.0 2.5 P9/9 09/12/13 12:21 09/18/13 19:15 1 2,3,7,8-TCDD ND 1.0 0.50 pg/g 09/12/13 12:21 09/18/13 19:15 1 2,3,7,8-TCDF ND 1.0 0.60 pg/g 09112/1312:21 0911811319:15 1 2,3,4,7,8-PeCDF ND 5.0 2.5 p9/9 09/12/13 12:21 09/18/13 19:15 1 MB Me bo"DiiUdon %Recovery OwIMr Limns Frepawd Ana/yxd DB Fac 13C-1,2,3,4,7,&HxCDF 58 40-135 08/fYi912:21 09/i&1319:15 1 13C-1,2,3,8,7,8-HxCDD 58 40-135 0911211312.21 09M8/1319:15 1 13C-2,3,7,8-TCDD 59 40-135 09112/1312.21 0911410319.15 1 13C-1,2,3,7,8-PeCDD 60 40-135 0911211312.21 091180319.15 1 13C-1,2,346,7,8-HpCDF 62 40-135 09112J1312.21 0911S/1319:15 1 13C-1,237,8-PeCDF 56 40-135 0911211312.21 09118H319:16 1 13C-2,3,7,8-TCDF 57 40-135 0911211312.21 09/18/1319:15 1 13C-1,$34,6,7,8-HPCDD 64 40-135 09/12/1312.21 0911811319:/5 1 13C-OCDD 69 40-135 09/12/13 12.21 09/18/13 19.15 1 Lab Sample ID: LCS 320-2501012-A Client Sample ID:Lab Control Sample Matrix:Tissue Prep Type:Total/NA Analysis Batch:25486 Prep Batch:25010 Spike LCS LCS %Rec. Analyte Added Result Qualifier Unit D %Rec Lknits OCDD 200 208 Pg/g 104 50-160 1,2,3,7,8,9-HxCDD 100 105 pg/g 105 50-150 1,2,3,4,7,8,9-HpCDF 100 98.0 p9/9 98 50-150 1,2,3.4,6,7,8-1-lpCDF 100 106 P9/9 106 50-150 1,2,3,7,8-PeCDD 100 98.8 P9/9 99 50-150 1,2,3,7,&PeCDF 100 105 pg/g 105 50-150 TestAmerica Sacramento Page 13 of 22 1/30/2014 QC Sample Results Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID: 320-3948-1 Project/Site:Tissue Method: 8290-Dioxins and Furans(HRGC/HRMS)(Continued) Lab Sample ID: LCS 320-25010/2-A Client Sample ID: Lab Control Sample Matrix: Tissue Prep Type: Total/NA Analysis Batch: 25486 Prep Batch: 25010 Spike LCS LCS %Rec. Analyre Added Reeuit Qualifier Unit D %Rec Limits 1,2,3,6,7,8-HxCDD 100 106 pg/9 106 50-150 1,2,3,6,7,8-HxCDF 100 118 p9/9 118 50-150 1,2,3,7,8,9-HxCDF 100 108 pg/g 108 50-150 OCDF 200 197 pg/g 99 50-150 1,2.3,4,7,8-HXCDD 100 110 pg/g 110 50-150 e 1,2.3.4,7,8-HxCDF 100 111 pg/g 111 50-150 1.2.3,4,8,7,8-HpCDD 100 106 pg/g 106 50-150 2,3,4,6,7,8-HxCDF 100 114 pg/g 114 50-150 2,3,7,8-TCDD 20.0 20.4 p9/9 102 50-150 2,3,7,8-TCDF 20.0 230 pg/g 115 50.150 2,3,4,7,8-PeCDF 100 102 pg/g 102 50-150 LCS LCS ktohipe Dilution %Recovery Qualifier Lhnits 13C-1,2,3,4,7,8-HxCDF 69 40-135 13C-1,2,3,8,7,8-HxCDD 68 40.135 = 13C-2,3.7,8-TCDD 67 40-135 " f" 13C-1,2,3,7,8-PeCDD 68 40-135 13C-1.2,3,4,6,7,8-HxCDF 72 40-135 13C-1,2,3,7,8-PeCDF 64 40.135 13C-2,3,7,8-TCOF 65 40.135 13C-1,2,3,4,8,7,6-HpCDD 72 40-135 13C-OCDD 74 40-135 TestAmerica Sacramento Page 14 of 22 1/30/2014 QC Association Summary Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID 320-3948-1 Project/Site:Tissue Specialty Organics Prep Batch:26010 Lab Sample ID C 1wit Sample ID Prep Type Matrix Method Prep Batch 320-3948-1 SITE 4A CHANNEL CAT R-FILLETS Total/NA Tissue 8290 320-3948-2 SITE 4A COMMON CARP R-FILLETS Total/NA Tissue 8290 320-3948-7 SITE 4B COMMON CARP WS Total/NA Tissue 8290 320-3948-8 COMPOSITE OF 48 CHANNEL CAT#3,5 Total/NA Tissue 8290 320-3948-9 COMPOSITE OF 4B COMMON CARP 94,6 Total/NA Tissue B290 LCS 320-2501012-A Lab Control Sample Total/NA Tissue 8290 MB 320-25010/1-A Method Blank Total/NA Tissue 8290 Analysis Batch:25486 Lab Sample ID Client Sample to Prep Type Matrix Method Prep Bach 3203948-1 SITE 4A CHANNEL CAT R-FILLETS TOlel/NA Tissue 8290 25010 320-3948-2 SITE 4A COMMON CARP R-FILLETS Total/NA Tissue 8290 25010 320-3948-7 SITE 4B COMMON CARP We Total/NA Tissue 8290 25010 320-394" COMPOSITE OF 4B CHANNEL CAT#3,5 Total/NA Tissue 8290 25010 320-3948-9 COMPOSITE OF 4B COMMON CARP #4,6 Total/NA Tissue 8290 26010 LCS 32 0-2 6 01 0/2-A Lab Control Sample Total/NA Tissue 8290 25010 MB 320-25010/1-A Method Blank Total/NA Tissue 8290 25010 Analysis Batch:25602 Lab Sample ID CINm Sample ID Prep Type Matrix Method Prop Bach 320-3948-2 SITE 4A COMMON CARP R-FILLETS Total/NA Tissue 8290 25010 320-3948-7 SITE 48 COMMON CARP WB Total/NA Tissue B290 25010 320-3948-9 COMPOSITE OF 413 COMMON CARP $4.6 Total/NA Timm 8290 25010 General Chemistry Prep Batch:25092 Lab Sasipla ID CBatt Sample ID Prep Type Ma di, Method Pnp Batch 320-3948-1 SITE 4A CHANNEL CAT R-FILLETS Total/NA Tissue HRMS-Sox 320-3948-2 SITE 4A COMMON CARP R-FILLETS Total/NA Tissue HRMS-Sox 320-3948.7 SITE 4B COMMON CARP WS Total/NA Tissue HRMS-Sox 320-3948-8 COMPOSITE OF 48 CHANNEL CAT#3,5 Total/NA Tissue HRMS-Sox 320-3948-9 COMPOSITE OF 4B COMMON CARP #4,6 Total/NA Tissue HRMS-Sox Analysis Batch:25097 Lab Sample 10 Clan Sample ID Prep Type Mob Method Prep Balch 3203948-1 SITE 4A CHANNEL CAT R-FILLETS TOtal/NA Tissue Lipids 25092 320-3948-2 SITE 4A COMMON CARP R-FILLETS Total/NA Tissue Lipids 25092 320-3948-7 SITE 4B COMMON CARP WS Total/NA Tissue Lipids 25092 320-3948-8 COMPOSITE OF 4B CHANNEL CAT#3,5 Total/NA Tissue Lipids 25092 320-3948-9 COMPOSITE OF 48 COMMON CARP #4,6 Total/NA Tissue Lipids 25092 TestAmerica Sacramento Page 15 of 22 1/30/2014 Lab Chronicle Client Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 -i Projectl5ite:Tissue L? r 7 Client Sample ID: SITE 4A CHANNEL CAT R-FILLETS Lab Sample ID: 320-3948-1 Date Collected:0 810 6113 14:00 Matrix:Tissue Date Received:09/05/13 08:16 Batch Batch oil Initial Final Batch Prepared Prep Type , Type Method Run Factor Amount Amount Number or Analyzed Analyst Lab TOtallNA Prep 8290 10.44 g 20 uL 25010 09/12/13 12:21 GOB TAL SAC e TOtat1NA Analysis 8290 1 10.44 g 20 uL 25486 09/18l13 20:41 ALM TAL SAC TotaVNA Prep HRMSSox 10.44g 10.44g 25092 09112/1312:21 AVM TALSAC TotallNA Analysis Lipids 1 10.44g 10.44g 25097 0911311311:07 GOB TALSAC Client Sample ID: SITE 4A COMMON CARP R-FILLETS Lab Sample ID: 320-3948-2 ❑ Date Collected:0 810511 3 1 6:20 Matrix:Tissue o Date Received:09105113 08:16 m Batch Batch Oil Initial Final Batch Prepared Prep T Type Method Run Factor Amount Amount. Number or Analyzed Analyst Lab r t Total/NA a Prep 8290 10.22 g 20 uL 25010 09/12/13 12 21 GOB TALSAC I Total/NA Analysis 8290 1 10.22 g 20 uL 25486 09/18/13 21:24 ALM TAL SAC Total/NA Prep 8290 10.22 g 20 uL 25010 09/1211312:21 GOB TAL SAC �— Total/NA Analysis 8290 1 10.22 g 20 uL 25602 09/20/13 02:30 LLH TALSAC Total/NA Prep HRMS-Sox 10.22 g 10.22 g 25092 09/12/1312:21 AVM TALSAC TotagNA Analysis Lipids 1 10.22 g 10.22 g 25097 09/13/13 11:07 GOB TALSAC i I I' Client Sample ID: SITE 413 COMMON CARP WB Lab Sample ID: 320-3948-7 Date Collected:0 810 611 3 13:10 Matrix:Tissue Date Received:09/06113 08:15 Batch Batch oil Initial Final Batch Prepared Prep Type Type Method Run Factor Amount Amount Number or Analyzed Analyst Lab Total/NA Prep 8290 10.36 g 20 uL 25010 09/12/13 12:21 GOB TALSAC TOta1/NA Analysis 8290 1 10.36g 20 uL 25486 0911811322:07 ALM TALSAC Total/NA Prep 8290 10.36 g 20 uL 25010 09/12/13 12:21 GOB TALSAC TOtel/NA Analysis 8290 1 10.36 g 20 uL 25602 09/20/13 03:08 LLH TAL SAC TotagNA Prep HRMS-Sox 10.36g 10.36g 25092 09/1211312:21 AVM TALSAC Total/NA Analysis Lipids 1 10.36 g 10.36 g 25097 09/13/13 11:07 GOB TALSAC Client Sample ID: COMPOSITE OF 4B CHANNEL CAT#3,5 Lab Sample ID: 320-3948-8 Date Collected:08106/13 00:00 Matrix:Tissue Date Received:09/05/13 08:16 Batch Batch DII Initial Final Batch Prepared Prep Type Type Method Run Factor Amount Amount Number or Analyzed Analyst Lab TotaVNA Prep 8290 10.15 g 20 uL 25D10 09/1211312:21 GOB TALSAC Total/NA Analysis 8290 1 10.15 g 20 uL 25486 09/18/13 22:51 ALM TALSAC TotaVNA Prep HRMS-Sox 10.15 g 10.15 g 25092 09/12/13 12:21 AVM TAL SAC TotagNA Analysis Lipids 1 10.15 g 10.15 g 25097 09/13/13 11:07 GOB TAL SAC TestAmerica Sacramento Page 16 of 22 V30I2014 Lab Chronicle M Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 Project/Site:Tissue [ Client Sample ID: COMPOSITE OF 4B COMMON CARP #4,6 Lab Sample lb: 320-3948-9 C1 Date Collected:0810 6113 0 0:00 Matrix:Tissue Date Received:09/05/13 08:16 1-61 Batch Batch DII Initial Final Batch Prepared Prep Type Type Method Run Factor Amount Amount Number or Analyzed Analyst Lab TotalfNA Prep 8290 10.16 g 20 uL 25010 09/12/13 12:21 GDB TAL SAC TotaUNA Analysis 8290 1 10.16 g 20 uL 25486 09/18/13 23:34 ALM TAL SAC Total/NA Prep 8290 10.16 g 20 uL 25010 09/12/13 12:21 GDB TAL SAC Tmal/NA Analysis 8290 1 10.16 g 20 uL 25602 09/20/13 03:47 LLH TAL SAC TotaUNA Prep HRMS-Sox 10.16 g 10.16 g 25092 0911211312:21 AVM TAL SAC Total/NA Analysis Lipids 1 10.16 g 10.16 g 25097 09/13/13 11:07 GDB TAL SAC Laboratory References: 0 TAL SAC=TestAmerica Sacramento,B80 Riverside Parkway,West Sacramento,CA 95605,TEL(916)373-5600 m f d, 0 0 TestAmerica Sacramento Page 17 of 22 1/30/2014 Certification Summary �] Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 Project/Site:Tissue Laboratory: TestAmerica Sacramento J� All certifications held by this laboratory are listed. Not all certifications are applicable to this report /I Authority Program EPA Region Certification ID Expiration Date 7 A21-A A21-A NE-OS-22-13 01-31-14 A21-A DoD ELAP 2928-01 03-31-14 Alaska(UST) State Program 10 UST-055 02-03-14' ❑ Arizona State Program 9 AZ0708 08-11-14 Arkansas DEQ State Program 6 88-0691 06-17-14 California NELAP 9 1119CA 01-31-14 Colorado State 8 N/A 08-31-14 FV Connecticut State Program 1 PH-0691 06-30-15 Florida NELAP 4 E87570 06-30-14 101 Guam State Program 9 N/A 08-31-14 (1 Hawaii Stale Program 9 N/A 01-31-14' �' Illinois NELAP 5 200060 03-17-15 1 Kansas NELAP 7 - E-10375 10-31-14 Louisiana NELAP 6 30612 06-30-14 m Michigan State Program 5 9947 01-31-14 Nebraska State Program 7 NE-OS-22-13 01-31-14 [ Nevada State Program 9 CA44 07-31-14 L�_ New Jersey NELAP 2 CA0g5 06-30-14 New York NELAP 2 11666 03-31-14 Northern Mariana Islands State Program 9 MP0007 02-01-14 Pennsylvania NELAP 3 68-01272 03-31-14 1I�� South Carolina State Program 4 87014 06-30-14 Texas NELAP 6 T104704399-08-TX 05-31-14 1�4 US Fish&Wildlife Federal LE148388-0 12-31-14 USDA Federal P330-11-00436 12-30-14 USEPA UCMR Federal 1 CA00044 11-06-14 Utah NELAP 8 QUAN1 01-31-14 Washington State Program 10 C581 05-05-14 West Virginia DHHR State Program 3 9930C 02-03-14' Wyoming State Program 8 8TMS-0 01-31-14 •Expired certification is currently pending renewal and is considered valid. TestAmerica Sacramento Page 18 of 22 1/30/2014 Method Summary Client Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3,948-1 r Project/Site:Tissue .Method Method Description _ Protocol Laboratory 8290 Dioxins and Furans(HRGC/HRMS) SW846 TALSAC Lipids Percent Lipids TestAmerica SOP TAL SAC -" Protocol References: SW846="Test Methods For Evaluating Solid Waste,Physical/Chemical Methods',Third Edition,November 1986 And Its Updates. TestAmedca SOP=TestAmerica,Inc., Standard Operating Procedure r Laboratory References: TAL SAC=TestAmerica Sacramento,880 Riverside Parkway,West Sacramento,CA 95605,TEL(916)373-5600 0 �o i . .t c H� 1 Li] A TestAmerica Sacramento Page 19 of 22 1/30/2014 Sample Summary Client: Evergreen Packageing FKABlue Ridge Paper TestAmerica Job ID:320-3948-1 Project/Site:Tissue Lab Sample ID Client Sample ID Matrix Collected Received 320-3948-1 SITE 4A CHANNEL CAT R-FILLETS Tissue 6810511 114:00 09/05/1 008:15 �1 320-3948-2 SITE 4A COMMON CARP R-FILLETS Tissue 0 810 5113 16:20 09/05/13 08:15 320-3948-7 SITE 48 COMMON CARP WB Tissue 0 8/0 6113 13:10 09/05/13 08:15 ,320-3948-8 COMPOSITE OF 4B CHANNEL CAT#3,5 Tissue 08/0611300:00 09/0511308:15 320-3948-9 COMPOSITE OF 4B COMMON CARP #4,6 Tissue 08/06/13 00:00 09/05/13 08:15 e a 0 � a I TestAmerica Sacramento Page 20 of 22 1/30/2014 TestAmerlca Sacramento Chain of Custody Record n �pp1 Test erica 88D Riverside Pad:Way 1I1p1Ip1t1 II1IIIIf1 11p11 I11,II1II11�I�I II 1111►Y,1 )j111pVIIIW'111{1 1 iqu1 'NE LFAUEe 1N NVINONMENTAL iEBnNe West SaCraIllEelO,CA 9$605 1111,WIIIV III1IVIIl`IIHI I I phone 916.3744378 fax 916.3721059 Regulatory Program: ❑DW QNPDES ❑RCM ❑ota 11 'estAmeric ILaboratorles,Ina ? Client Contact Project Manager. Nlek McCmcllen Sib Came Dr.La 320-3948 Chain of-Cars oNy X; No, 0 2013 1. Evergreen Packaging ToWax:(US)646.2674 tab Conine 1 of Coca: _ 175 Main Street Analysis Turnaround Time iampler.Univ roily of Tennessee Canton.NC 2B716 ❑ CALENDAR DAYS El WOPMG DAYS -or Lab Use C nly: 828 646-67DO Phone TATdddremntnem Below Malk-m Client (828)648-6892 FAX ❑ 2weft AbSampling. Project Name,Fish Tissue Semplkig ❑ 1 weds Site.Waterville Lake ❑ 2 days Job/SDO No. POR ❑ Iday E S 2 oarnple Semple Sample (T yp,, •or g - ' Sample Identification Dam Time Ga A) Maw Coat S SamPle a6e Notes: S e C — 9 nva Yi (: 1( 1f a is ayfw CD i o we. z Ate. S;k 0 n « rffmgy 5-&a 13qs 4 ilylow 6-I 1310 y i l �. Possible Hazard Identification: - Sample Ohposal(A fee rosy be msnsed N1 Impinalenee longer than I month Are any samples from a listed EPA Hazardous Waste? Please List any EPA Waste Codes for the sample In the Comments Section tithe lab is to dispose of the sample I, ❑+ Nm Hamrd ❑Flammable LJ So ontmt - person a Unbmrm ❑Re um to dart ❑Dspmal W Lab Ar t, to1 Hands Special InstructlonslOC Requirements&Commerce: i i I ' Custody Seals IntiV, 0 Ye No Custody See No.. ® er amp. en/n lu Relinq she _ V r O /•j Recehr ` n O m .. f.P CD Re0 q h Company. Cam wry, '7 `I elinqu tl Co sterrime: Revs In Lebomto by Com 04 903 IF omi klajc CLWI-0112,Rev.L2.dated 04I02120113 e._.�r X ® _c7 LUG LJ !�J L J L s I I LJ L'_J 0 Login Sample Receipt Checklist FJ Client:Evergreen Packageing FKABlue Ridge Paper Job Number:320-3948-1 Login Number:3948 List Source:TestAmerica Sacramento List Number:1 Creator.Hytrek,Cheryl Question Answer Comment Radioactivity wasn't checked or is</=background as measured by a survey True meter. 7 The coolers custody seal,if present,is intact. True Sample custody seals,if present,are intact. NIA F3 The cooler or samples do not appear to have been compromised or True ❑ tampered with. Samples were received on ice. True ri Cooler Temperature is acceptable. True U I Cooler Temperature is recorded. True COG is present. True COG is filled out In ink and legible. True i COG is filled out with all pertinent information. True Is the Feld Samplers name present on COC? N/A G1 lt There are no discrepancies between the containers received and the COG. True U7 Samples are received within Holding Time. True Sample containers have legible labels. True f Containers are not broken or leaking. True Sample collection date/times are provided. True Appropriate sample containers are used. True Sample bottles are completely filled. True Sample Preservation Verified. NIA There is sufficient vol.for all requested analyses,incl.any requested True MS/MSDs Containers requiring zero headspace have no headspace or bubble is True <6mm(1/4'). Multiphasic samples are not present. True Samples do not require splitting or compositing. True Residual Chlorine Checked. N/A TestAmerica Sacramento Page 22 of 22 1/30/2014 APPENDIX C BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS, 1990-2004 33 APPENDIX C Table 64. Blue Ridge Paper Canton Mill Fish Fillet Tissue Results. 1990-2004 From: EA Engineering, Science, and Technology, Inc. December 2004 36 A Gci v! am g � m V.M M m m l�N 2 q20 C0 e0R0 eO e02 0 4 2O Om� gepVO C, M m�pm ^pm In {(y�mq pip .q-�.�- her m(V h ��Vim' qNm NH� NMN .a Cd. 11 tL �}spj O 3 y m OO V1 cows 2b2 1�22 V1v1p ON N ti a z W R o -to o q o q o CD mq A Ly o �� v� � lm ��� sad aam A a awu awu wcw8 am tl H O M V� O h •p �� N v�q'i M� Qv W m h$�$'' QGq m H H n oG qo qc gLq"gEq q�q N `" zZR aa�'+a oaeia ZZc�i oZ� w �� �Nm wry Nqh �n MOm . cow 1� a O U w z , m � m b _N lit III a � o �• �a� e � E' ee 'g _tee`e ego O ut 9fi CM v'Aq G pF FQ Fk'NC.PICU f707U QiU W k N MN Q� Ntq�l C < F a �% AO Oo 00 00 s s s N Z Z Z Z P � op08� OO�N �mn pO'• �.Or may{ �1m vOi eY0 N N•a tV ti� N N�l N N E r1 N�+ N N Vf ,g, hp]N MON Vf00 Cl N'!j ONO dNd Y y �� o„�0 000 0�0 000 000 _ p� bam b @w m Z a A � o cn m d F C L' Y I Y Q - Y Uy n Sad a q azU axu �qU 6 Y Y NYaf mvNl Qi 5a qn h.Q•. <r � s � o � [off�a (o_�� o ee0 0(1 e0(1 0 e0q e0❑0 N Z Ti •+ O Ti P Z f•V' N N N Z Z v 1 f..Z O pryO + SSGpGp �Nn N �N RRNNO 3 •v OOb 2o2 Zoo o22 limo Pdii w a z 0 v � y � EI 4a � � pppo N V u p W W p I P' p = YG' Y V Y p '!Z tl P a Lry PiCq cvq� �x w'd qq u q..l u Crhm h. F Table 6-4 (cont.). 1994 R.ecultsv* 199S Itesultsm Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDD(-) Station Species Fish Range(mm) 2,3,7,8-TCDDt t 1 Rockbass 6 156-185 ND(0,083) 1 Rock bass 10 162-205 ND(0.10) RM 64.5 Redbreast sunfish 10 155-197 ND(0.10) RM 64.5 Rock bass 10 150-220 ND(0.26) Black redhorse 3 367.435 ND(D.096) Black redhorse 7 375.464 ND(0.21) 2 Redbreast sunfish 10 176-206 ND(0.(Y73) 2 Redbreast sunfish 10 152-194 ND(0.20) RM 59.0 Redbreast sunfish 10 160-210 ND(0.092) RM 59.0 Redbreast sunfish 10 161-188 ND(0.16) Common carp 10 490.59D 0.99 Comon carp 10 435-664 1.7 3 Redbreast sunfish 10 148-196 ND(0.15) 3 Redbreast sunfish 10 170-206 ND(0.18) RM 52.3 Redbreast sunfish 10 158 210 ND(0.074) RM 52.3 Redbreast sunfish 10 154 202 ND(0.20) Common carp 10 456-565 0.74 Common carp 10 391-571 1.2 4A Black crappie 30 203-231 ND(0,085) 4A Largemouth bass 5 281-439 2.0 RM 41.5 Bluegill 10 185-205 ND(0.084) RM 41.5 Bloeg0l 10 167.199 ND(0.26) Common carp 10 465.591 3.4 Common carp 10 520-615 5.8 4B Black crapple 10' 20D-215 ND(0.084) 4B Largemouth bass 9 248-391 0.68 RM 39.0 Black Grapple 10 195.220 ND(0.062) RM 39.0 Bluegill 8 158-216 ND(0.34) Common carp 10 520.635 6.6 Common carp 4 532.626 11.0 5 Redbreast sunfish 6 129.239 ND(0.075) 5 Smallmouth bass 9 280.423 ND(0.11) RM 19.0 Smallmouth bass 9 234442 ND(0.11) RM 19.0 Redbreast sunfish 7 163-192 ND(0.15) Smallmouth buffalo 9 440-520 ND 0.06 Black redhorse, 7 44G481 ND f0.45) Total Fish Filleted 163 156 Table 6-4 (cont.). 1996 Rusultf 1997 Results%) Number of Length Number of Length ' Station Species Fish Range(mm) 2,3,7,8-TCDDo) Station Species Fish Range(man) 2,3,7,8-TCDD(-) I Redbreast sunfish 5 154.185 ND(0.13) 1 Redbreast sunfish 5 144-161 ND(0.11) RM 64.5 Rock bass 5 160-208 ND(0.085) RM 64.5 Rock bass 5 162-194 ND(0.23) Black redhorse 5 401.440 ND(0,089) Black redhorse 4 291-424 ND(0.22) 2 Redbreast sunfish 5 179-197 ND(0.10) 2 Redbreast sunfish 5 183-200 ND(0.26) RM 59.0 Redbreast sunfish 5 183-191 ND(0.12) RM 59.0 Redbreast sunfish 5 160-I81 DID(0.12) Common carp 5 543-580 1.5 Common carp 5 506-615 1.4 3 Redbreast sunfish 5 184-19D ND(0.13) 3 Redbreast sunfish 5 187.202 ND(0.18) ' RM 52.3 Redbreast sunfish5 165-185 ND(0.13) RM 52.3 Redbreast sunfish 5 164-195 ND A lg) ' Common carp 5 516-630 0.87 Common carp 5 450-505 ND(0.33) 4A Black cmppie 5 216.233 ND(0.15) 4A Black crapppie 5 215 231 ND(0.27) RM 41.5 Black crappie 5 215-229 ND(0.18) RM 41.5 Black crappie 5 220.230 ND(0.10) Common carp 5 562.632 42 Common carp 5 220-230 20. Channel catfish 5 419-482 2.0 413 Black cmpple 5 223.258 ND(0.11) 4B Black crappie 5 226.241 ND(0.17) RM 39.0 Largemouth bass 5 278.310 ND(0.13) RM 39.0 Largemouth bass 5 270-360 ND(0.21) Common carp 5 470.623 4.0 Common carp 5 605.690 11.0 Flathead catfish 5 430-540 0.62 5 Rock bass 4 169.186 ND(0.077) 5 Rock bass 5 143-214 ND A 15) . RM 19.0 Small-oath bass 5 315454 ND(0.12) RM 19.0 -Smallmouth bass 5 278.367 ND(0.27) Smallmouth buffalo 5 451-555 ND 0.12 Smallmouth buffalo 5 406.525 ND 0 22 Total Fish Filleted 89 Total Fish Filleted 99 i Table 6-4 (cont.). 1998 Resultsra 1999 Results(b) Number of Length Number of Length Station Species Fish Range(min) 2,3,7,8-TCDDt't Station Species Fish Range(min) 2,3,7,8-TCDDt t 1 Redbreast sunfish 5 145-176 ND(0.19) 1 Redbreast sunfish 5 141-177 ND(0.21) RM 64.5 Rock bass 5 158-179 ND(0.29) RM 64.5 Rock bass 5 164.190 ND(0.37) Black redhorse 5 340-396 ND(0.18) Black redhorse 5 352-427 ND(0.33) 2 Redbreast sunfish 5 164-177 ND(0.20) 2 Redbreast sunfish 5. 167-190 ND(0'.37) RM 59.0 Redbreast sunfish 5 166.193 ND(0.28) RM 59.0 Redbreast sunfish 5 158-178 ND(0.29) Common carp 5 551661 1.3 Common carp 5 544.615 ND(0.27) 3 Redbreast sunfish 5 169-193 ND(034) 3 Redbreast sunfish 5 169-189 - ND(0.36) RM 52.3 Redbreast sunfish 5 167-200 ND(0,22) RM 52.3 Redbreast sunfish 5 162-176 ND(0.37) Common carp 5 449-550 ND(0.38) Common carp 5 500-591 0.57 4A Black crappie 5 220.240 ND(0.49) 4A Black crappie 5 220-268 ND(0.18) RM 41.5 Largemouth bass 5 227-330 ND(0.15) RM 41.5 Black crappie 5 219-244 ND(0.08) Common carp 5 585621 1.6 Common carp 5 574-645 0.58 Channel catfish 5 416458 ND(0.28) Channel catfish 5 425.482 0.83 4B Black crappie 5 233-252 ND(0.15) 4B Black erspple 5 233-244 ND(0.27) RM 39.0 Largemouth bass 5 259.330 ND(0.17) RM 39.0' Largemouth bass 5 276-305 ND(0.32) Common carp 5 563686 9.1 Common carp 5 621680 4.7 Flathead catfish 5 414.523 ND(0.20) Flathead catfish 5 372-513 ND(0.46) 5 Rock bass 4 155-M ND(0.11) 5 Rock bass 5 170.203 _ ND(029) RM 19.0 Sroallmoudn bass 5 295-365 ND(0.21) RM 19.0 Smallsamah bass 5 297-430 ND(0.19) Smalbnouth buffalo 5 464.537 ND 0.31 Smallmouthbuffalo 5 476-565 ND .31 Total Fish Filleted 99 Total Fish Filleted 100 I Table 6-4 (cunt.). 2000 Results 2001 Resultst'o Number of Length Number of Len Station Species Fish Range(tom) 2,3,7,8-TCDDt'> 901 Station Species Fish Range(mm) 2,3,7,8-TCDD(O 1 Redbreast sunfish 5 137-148 ND(0.48) I Black redhorse 5 312.4D7 ND(0.25) RM 64.5 Rock bass 5 162-186 ND(0.45) RM 64.5 Black redhorse 5 357-396 ND(0.38) 2 Redbreast sunfish 5 169-176 ND(0.31) 2 Common carp 5 456-555 ND(0,27) RM 59.0 Redbreast sunfish 5 164-181 ND(0.43) RM 59.0 Common carp 5 505-582 ND(0.42) 3 Redbreast sunfish 5 169-181 ND(0.43) 3 Common carp 5 5D4.615 ND(0.35) RM 52.3 Redbreast sunfish 5 186-199 ND(0.32) RM 52.3 Common carp . 5 514-569 ND(0.53) 4A Black crappie 5 212-241 ND(0.29) 4A Channel catfish 5 476-612 1.2 RM 41.5 Black crappie 5 220-241 ND(0.24) RM 415 Common carp 5 528-668 1.3 Common carp 4 559-604 1.1 Charnel catfish 5 435-487 ND(0.70) 4B Black crappie 5 213.231 ND(0.41) 0 Flathead catfish 5 405.463 ND(0.29) RM 39.0 Black crappie 5 220-230 ND(0.37) RM 39.0 Common carp 5 654-723 5.6 Common carp 4 593-712 4.4 Flathead catfish 5 407-45D ND(0,42) 5 Rock bass 5 171-198 ND(0.45) 5 Black redhorse 5 437-497 ND(0.26) RM 19.0 Smaldmouth bass 5 209.238 ND(0.31) RM 19.0 Black reborse 5 427-476 ND 0.3 Total Fish Filleted 98 Toml Fish Filleted 40 Table 64 (cont.). 2002 Results(O 2003 Resultsro) Number of Length Number of Station Species Fish Range(cam) 2,3,7,8-TCDDm Station Species Fish Length Range(mm) 2,3,7,8-TCDDat 1 Black redhorse 5 372-431 ND(0.14) 1 Black redhorse 5 343-420 RM 64.5 RM 64.5 ND(0.20) 2 Common carp 5 517.548 ND(0.28) RM 59.0 RM 59.0 Common cup 5 512-584 ND(0.18) 3 Common carp 5 575-632 ND(0,22) 3 Common cupRM 52.3 RM 52.3 P 5 545-605 ND(0.31) ' 4A Common carp 5 523-648 2.2 4A Common tarp 5 655-017 3.4 RM 41.5 Channel catfish 5 425A75 ND(0.31) RM 41.5 Flathead catfish 5 521.575 ND(DL=0.35) 4B Common carp 5 647-670 6.6 4B Common carp 5 602-745 12.0 RM 39.0 Flathead catfish 5 41M5 ND(0.22) RM 39.0 Flathead catfish 5 511-533 ND(DL-0.20) RM 5 19.0 Black redhorse 5 430-089 ND(0.14) 5 Black redhorse 5 445-524 ND(DL-0.19) RM 19.0 Total Fish Filleted 40 Total Fish Filleted 40 i Table 6-4 (cont.). 2004 Resultsw Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDDtn RM 1 64.5 Black redhorse 5 352440 ND(0.11) 2 Common carp 5 545-668 ND(0.19) RM 59.0 Channel catfish 5 369-453 ND(0.17) 3 Common carp 5 587-M ND(0.27) RM 52.3 4A Common carp 5 598-655 1.7 RM 41.5 Flathead catfish 5 508-565 ND(0.30) . 4B Common carp 5 570.66D 1.6 RM 39.0 Channel catfish 5 485-542 ND(0,31) RM 5 I9.0 Black redhorse 5 _ 420-480 ND(0.13) ' Total Fish Filleted 40 . (a) Survey conducted by EA Engineering,Science,and Technology. Analyses conducted by ENSECO Laboratories 1990-1994,.Quanterra Laboratories 1995-1999,Severs Trem Labommries in 2Q00. 2003. (b) Survey conducted in August. (c) Survey conducted in August and September. . (d) Survey conducted is September. (a) Units=ppt(parts per trillion)or pgfg(picogman pa gram) ND=Non-detectable at the detection limit In parentheses. i APPENDIX D 2006 REVISIONS TO DIOXIN MONITORING PLAN i 34 V A Michael F.Easley,Governor \O�� 9QG William G.Ross Jr.,Secretary North Carolina Department of Environment and Natural Resources CO r Alan W.Klimek,P.E.Director Division of Water Quality Y LS(� Coleen H.Sullins,Deputy Director nn C E 0 . . . ality June 6,2006 JUN 12 Mr. Paul S.Dickens Manager,Environmental Affairs BLUE USE PAPER PRODUCTS INC Blue Ridge Paper Products BHS DEPARTMENt P.O. Box 4000 Canton,North Carolina 28716 Subject: Revisions to Dioxin Monitoring Plan Blue Ridge Paper Products NPDES No.NCO000272 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. 'ncerely,�� immie verton ironmental Sciences Section cc: Roger Edwards-ARO Dr.Luanne Williams—NCDHHS Susan Wilson -DWQ Permits IJohn Crutchfield—Progress Energy MAT, ENR N.C.Division of Water Quality 1617 Mail Service Center Raleigh,North Carolina 27699.1617 (919)733-7015 Customer Service 1-877-623-6748 BLUE RIDGE COPY PAPER PRODUCTS INC. Certified Mail Return Receipt Requested 7099 3220 0007 0371 6235 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. J % 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 Monitoring 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 f' 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: v 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 a PO Box 4000 Canton, North Carolina 28716 a 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@bluerideepaper.com roeere@blueridgepaper.com I ' U 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 7Yssue 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 R.IDGE COPY PRODUCTS RQDUCTs 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 Iake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page I INTRODUCTION The Blue Ridge Paper Products Inc. Canton Mill conducts annual biological monitoring of dioxin in fish in the Pigeon River trader 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 2001 a). 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(Ictalums 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 I 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 Shen 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. I 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 1, / 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 Polychlorinated Dibenzofurans by High Resolution Gas Chromotography/High Resolution Mass Spectrometry(Method 8290). I - 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 lI Health Assessment of 2,3,7,8-Tetrachlorodibenzo-P-dioxin(TCDD 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. EA Engineering, Science, and Technology 444 Lake Cook Road, Suite 18 Deerfield, IL 60015 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 furans in fish tissues from the Pigeon River downstream of the discharge from the Blue Ridge papermill 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 furan 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 1.40 Station 5 .. RM 19.0 5 Bluffton TN-- (19.35 Hertford,TN TENNESSEE N NORTH ... — CAROLINA Bi0 Hydro Plant I a (26.0) ` o' r e `m n �I gP 5 4� Walters Dam— B Station 46 Station 4A RM 39.0 RM 41.5 4 Waterville Lake Fines Creek Now Hepeo Bridge FLOW ✓onathans Creek Old Rt.209 3 Station 3 Station 2 Mill Outfall RM 52.3 RM 50.0 RM 63.3 Waynesville STP— 2 Canton,NC Ouffall D RM SOA �Q�� Q?oGtee Clyde Station 1 1 RM 64.5 (Control) Figure 2-1. Fish tissue sampling station locations on the Pigeon River. i TABIE 2-1 PIGEON RIVER SAMPLING STAT1ON5 Station River Station Location and Numb er Ile Distance from Outfall Site DescrintioNHabital Type Fish Common*ro 1 64.5 Pigeon Riverupstream from Canton, Characterized by riffle,ion,and pool habitats. Maximum Relative abundance dominated by minnows and darters. River NC,adjacent to Canton Recreational depth approximately 6 tL Substrate primarily cobble and chub,greenfin darter and rock bass am dominant. Nortbem hog Park(1.2 RM upstream from Canton boulders interspersed with gravel and sand. sucker,black redhorse,mirror shiner,redbreast sunfish,central Mill outfall). stoneroller,gri enside darter,and mottled scullim am common. 2 59.0 Pigeon River upstream ftom Clyde,NC Characterized by riffle,rim,and pool habitats with canopy Relative abundance dominated by redbreast sunfish,central (4.3 RM downstmam from the Contort cover. Maximum depth approximately 5 ft. Substrate stommoller,and northern hog sucker. Mill outfall). primarily cobble/gravebsand with someboulders and bedrock. 3 52.3 Pigeon River in the vicinity of the Rt. Characterized by rif ce ran,and pool habitats with some Redbreast suofisb,northern hog sucker,and common carp am 209 bridge(11.0 RM downsumm canopy cover. Maximum depth approximately 5 R. dominant. Central stoneroller is common. from the Canton Mill outfall) Substrate primarily bedrock and bouldets with some i cobble and sand/gravelffines deposited in pool areas. i 4A 41.5 UpperWmerville Like(21.8 RM Characterized by deep-water fertile habitat,bedrock, Relative abundance dominated by black crappie. Bluegill, downstream from the Canton Mill and soft bottom sediments. Maximum depth sampled flathead catfish,channel catfish,largemouth bass,and common outfall) approximately 14 ft. coup are common. i i 4B 39.0 Lower Waterville lake(243 RM Characterized by deep-water lentic habitat.bedrock, Relative abundonmofcatch dominated by black crappie. downstream from the Canton MITI and softbottam sediments. Maximum depth sampled Bluegill,channel catfish,Flathead catfish,and carp am common. outfall) approximately 40 ft. Very steep banks with little cover. 5 19.0 Pigeon Rivernear BlufRoa,TN,just Characterized by deep pools and runs with some shallow Central stoneroller and nurthem hog sucker are dominant. I upstream of 140(443 RM downstream ilium Maximum depth approximately 6 to 8 FL Substrate Smallmouth bass,whitetail shiner,telescope shiner,greensick I from the Canton Mill omfal0 primarily bedrock boulder,and cobble, darter,and banded sculpin are common, Except for smalim pith bass and rock bass,centramhids am uncommoon. fF: 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. Gilinetting 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[eectrofishing 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 riverinc 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 raze 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 C 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 Electrofishing 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 o Catfish fillet composite—one sample at Stations 4A and at 4B o Common carp whole body composite--one sample from either Station4A or 4B o Catfish fillet composite—one sample at Stations 2 and at 3,if specimens are encountered 7 r' 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 cutaway 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/n. The toxic equivalent(TEQ)of each detectable isomer will be calculated based on toxicity equivalent factors (TEF)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. r. i 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 c Sample identification number, • Station identification, o Sampling team initials, • Date of sample collection, • Species name, • Sample type(i.e.,fillet or whole body) q 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. I. � 10 C �1 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 , 8. 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-Tetrachlomdibenzo-p-dioxin(TCDD) and Related Compounds: Part 11 Health Assessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin(TCDD)and Related Compounds. 1 ' 13