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HomeMy WebLinkAboutNC0000272_2007 Dioxin Monitoring Fish Tissue_20080415 200J M ox n M� Onjill Ourinn g I ne F I s, in TJ � s, uie � uY Blue Ridge Paper Products Inc Canton, NC BLUE RIDGE PAPER PRODUCTS INC. 15 April 2008 CERTIFIED MAIL Return Receipt Requested 7007 0710 0003 7311 3040 Roger C. Edwards Regional Supervisor North Carolina Department of Environment And Natural Resources Division of Water Quality Asheville Regional Office 2090 US Highway 70 Swannanoa, NC 28778 Subject: NPDES NC0000272 2007 Dioxin Monitoring in Fish Tissue Blue Ridge Paper Products hic. Canton, NC Dear Mr. Edwards: Enclosed is the 2007 Dioxin in Fish Tissue Report for Blue Ridge Paper Products Canton Mill. The 2007 report is the 18`s annual fish tissue study submitted by the mill. The study, required by our NPDES permit, consists of annual sampling of fish at specific sites in the Pigeon River and analysis of those fish for dioxin. Fish collection for the 2007 study took place between 14 and 21 Aug 2007. On 7 Feb 2008, we requested a 60-day extension for submission of the 2007 report. On 19 Feb 2008, the Division approved the due-date extension to 16 Apr 2008. The University of Tennessee Department of Forestry, Wildlife and Fisheries completed fish collection and the 2007 Dioxin in Fish Tissue Report. Fish collection followed the December 2001 monitoring plan approved the Division. The monitoring plan was modified in March 2006. The principal changes to the plan were the elimination of sampling in 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 (Station 4A or 4B). A copy of the approved monitoring plan is included as Appendix D to the report. Severn Trent Laboratories (STL,now TestAtnerica West Sacramento) completed the 2007 dioxin in fish tissue sample analysis. The 2007 dioxin in fish tissue results for the Waterville Lake catfish composite fillet samples and for the whole body carp sample were at non-detect levels and are consistent with previous year sampling results. Dioxin was detected in the common carp composite fillet sample from Station 4A. Dioxin in the Station 4B carp composite fillet sample was non-detect. There were analytical problems with the Station 4B sample that required dilution and resulted in an elevated non-detect level. Mr. Keith Haynes, NC DWQ Page 2, 4/15/2008 The carp collected at Stations 4A and 4B in Waterville Lake had higher mean weight in 2007 than in previous years and included individual carp that were significantly larger than fish collected in previous years. In addition, the lipid(fat) content of the composite carp samples from Stations 4A and 4B in 2007 was higher than in previous sampling years. Blue Ridge Paper will work with University of Tennessee fisheries scientists to collect common carp in 2008 with a size and weight distribution similar to fish collected in 2004, 2005 and 2006. We discussed our 2007 dioxin in fish tissue results with Progress Energy. Progress Energy collects similar dioxin in fish tissue samples from Waterville Lake(Walters Lake, Walters Hydroelectric Project) each year in the fall after our fish tissue sample collection in the summer. The results of 2007 Progress Energy dioxin in fish tissue sampling are similar to Blue Ridge Paper results for the period 2004 through 2006 with an average dioxin toxicity equivalent concentration(TEQ)below the North Carolina Department of Health and Human Services advisory level of 4 parts per trillion(ppt). A copy of the 2007 Progress Energy dioxin in fish tissue report is also enclosed for the Division's use and review. Please contact us if you have questions conceming the 2007 dioxin in fish tissue report. Sincerely. Paul Dickens Derric Brown Manager, Environmental Affairs Director,Environmental Health and Safety 828-646-6141 828-646-23181 dicker@blueridggpaper.com browndb@bluerideepaper.com Enclosures: 2007 Blue Ridge Paper Products Dioxin in Fish Tissue Report 2007 Progress Energy Dioxin in Fish Tissue Report C. File—Water Engr. File—River Studies Roger Edwards, NC DWQ, 2007 Dioxin in Fish Tissue Report 4/15/2008,Page 3 Distribution with enclosures: NC Division of Water Quality(two copies) Certified Mail Receipt: 7007 0710 0003 73113057 Central Files 1617 Mail Service Center Raleigh, NC 27699-1617 John Cruchfield Progress Energy 410 South Wilmington Street PEB 4A Raleigh, NC 27602-1551 Bryn Tracy Environmental Biologist North Carolina Department of Environment And Natural Resources Division of Water Quality 1617 Mail Service Center Raleigh, North Carolina 27699-1617 Jeff Engel Chief, Epidemiology Section NC Department of Health and Human Services 1912 Mail Service Center Raleigh, NC 27699-1912 Paul Davis TDEC—Water Pollution Control 401 Church Street 6u'Floor Annex Nashville, TN 37243 Jonathan Burr TDEC—Water Pollution Control Knoxville EAC 2700 Middlebrook Pike State Plaza Building,Suite 220 Knoxville,TN 37921 - Blue Ridge Paper Products Inc 175 Main Street • PO Box 4000 Canton, North Carolina 28716 • 828-646-2000 r RESULTS OF 2007 DIOXIN MONITORING IN FISH TISSUE Prepared for: Blue Ridge Paper Products,Inc. 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 April 2008 2007 Dioxin in Fish Tissue—April 2008 TABLE OF CONTENTS Page List of Tables . . . . . . . . . . . . . . . . . List of Figures. . . . . . . . . . . . . . . . . EXECUTIVE SUMMARY . . . . . . . . . . . . . . 1 L INTRODUCTION . . . . . . . . . . . . . . . 3 2. SAMPLING LOCATIONS . . . . . . . . . . . . . 4 3. SAMPLING OBJECTIVES . . . . . . . . . . . . . 8 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT . . . 9 5. SAMPLE PREPARATION . . . . . . . . . . . . .14 6. ANALYTICAL RESULTS . . . . . . . . . . . . 16 7. REFERENCES . . . . . . . . . . . . . . 27 8. APPENDICES . . . . . . . . . . . . . . . .30 APPENDIX A: CHAIN OF CUSTODY FORM APPENDIX B: SEVERN TRENT LABORATORY-SACRAMENTO ANALYTICAL REPORTS APPENDIX C: BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS 1990-2004 APPENDIX D: 2006 REVISIONS TO DIOXIN MONITORING PLAN APPENDIX E: NC DWQ AND DPH REVIEW OF 2006 FISH TISSUE ANALYSIS REPORT, LIFTING OF FISH ADVISORY FOR WALTERS LAKE. r Pagei 2007 Dioxin in Fish Tissue—April 2008 LIST OF TABLES Number Title Page 2-1 Pigeon River sampling station information . . . . . . . . . 5 4-1 Fish collection techniques and level of effort . . . . . . 10 4-2 Summary of fish composites collected in the Pigeon River, August 2007 . . . . . . . . . . . . . . . . 11 6-1 Summary of Pigeon River fish tissue analysis results—2007 . . . . 18 6-2 Toxicity equivalence factors for CDD/F isomers. . . . . . . . 19 6-3 Summary of CDD/F isomer analyses, toxicity equivalent factors, and toxicity equivalent values for the 2007 Pigeon River fish tissue composites . . . . . . . . . . . . . 20 6-4 Blue Ridge Paper Canton Mill fish fillet tissue analysis results 2005—2007 . . . . . . . . . . . . . . . 23 Page ii 2007 Dioxin in Fish Tissue—April 2008 LIST OF FIGURES Number Title Page ES-1 TCDD concentrations in carp fillets collected from the Pigeon River, 1990-2007. . . . . . . . . . . . . . . . . . 2 2-1 Historical Sampling Station locations on the Pigeon River . . . . . 6 2-2 Sampling Stations No. 4A and 4B on the Pigeon River . . . . . . 7 4-1 Lengths and Weights of Fish Collected from Waterville Lake for Tissue Analysis, 2004—2007 13 6-1 TCDD concentrations in carp fillets collected from the Pigeon River, 1990-2007 (Stations 4A and 4B) . . . . . . . . .24 6-2 TCDD concentrations in catfish fillets collected from the Pigeon River, 1997-2007 (Stations 4A and 413) . . . . . . . . . . .25 Page iii 2007 Dioxin in Fish Tissue—April 2008 EXECUTIVE SUMMARY The Blue Ridge Paper Products Inc., Canton Mill contracted the Department of Forestry, Wildlife and Fisheries of the University of Tennessee, Knoxville (UTK) to collect dioxin fish tissue samples from the Pigeon River during the summer of 2007 in accordance with NPDES permit conditions. UTK field personnel followed the March 2006 revision (Wilson 2006) to the December 2001 Fish Tissue Sampling Plan prepared by EA Engineering, Science and Technology, Inc., (EA Engineering 2001a) of Chicago, Illinois. UTK prepared this 2007 fish tissue sampling report using the template developed by EA Engineering for prior reporting years. 2007 is the 18`h year of monitoring dioxin in fish tissue samples from Waterville Lake. The 2007 concentrations of 2,3,7,8-TCDD and 2,3,7,8-TCDF in channel catfish fillet composites were below the level of detection at both Station 4A and Station 4B. TCDD and TCDF in the whole body common carp sample from Station 4A were also at or below detection limits. These results are consistent with previous years sampling data. In common carp composite fillets, 2,3,7,8-TCDD was detected (6.4 ppt) in the sample collected at Station 4A. Both the TCDD and dioxin toxicity equivalent (TEQ) result for the common carp composite at Station 4A were higher in 2007 compared to the previous 13 years of monitoring data at this location (since 1993, see Figure ES-1). TCDD was non- detect in the common carp composite fillet collected at Station 4B. The detection limit for TCDD is elevated for this sample because a 10-fold dilution was required to overcome sample matrix interference effects (high lipid concentration) during analysis. The concentration of 2,3,7,8-TCDF was 2.6 ppt in the common carp fillet composite at Station 4A and was 4.6 ppt in the common carp fillet composite from Station 4B. The carp collected at Stations 4A and 4B in Waterville Lake had higher mean weight in 2007 than in previous years and included individual fish specimens that were significantly larger than fish collected in previous years. In addition, the lipid (fat) content of the composite carp samples from Stations 4A and 4B in 2007 was higher than in previous sampling years. Sampling in 2008 targeted at a fish size distribution similar to that collected in 2004 through 2006 is necessary to determine any significant change or trend in dioxin in fish tissue concentrations. All catfish samples collected from Waterville Lake since 2002 have been at or below detection levels for TCDD, TCDF and related isomers. Page 1 2007 Dioxin in Fish Tissue—April 2008 Figure ES-1. TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990-2007 (Stations 4A and 4B). 70 \ 60 \ \ \ 50 A i \\ \\ 9 Station 4a Station 4b 40 1 — A -- a`r \ n \ 10 \ a 30 \� 0 0 v \ 20 \ \ \ \ �♦ 0 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 YEAR b) TCDD concentrations at Station 413 were not detected,therefore,the value plotted represents the detection limit for that sample. The detection limit for 2,3,7,8-TCDD is elevated in Station 4B because a 10 fold dilution of the sample 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 in 2007. Page 2 2007 Dioxin in Fish Tissue—April 2008 } 1. INTRODUCTION The Blue Ridge Paper Products Inc., Canton Mill contracted the Department of Forestry, Wildlife and Fisheries of the University of Tennessee, Knoxville (UTK) to collect dioxin fish tissue samples from the Pigeon River during the summer of 2007 in accordance with NPDES permit conditions. UTK field personnel followed the March 2006 revision(Wilson 2006) to the December 2001 Fish Tissue Sampling Plan prepared by EA Engineering, Science and Technology, Inc., (EA Engineering 2001a) of Chicago,Illinois. This report details the results of August 2007 sampling to determine the concentrations of 2,3,7,8-TCDD (dioxin) and 2,3,7,8-TCDF (furan) in bottom-feeding fish collected from Waterville Lake (Walters Lake) on the Pigeon River in North Carolina. The report follows the template developed by EA Engineering for prior reporting years. The 2007 fish tissue study is number 18 in a series of fish tissue surveys designed and conducted to be completely responsive to the requirements of A.(9.) Dioxin Monitoring Special Condition in Blue Ridge Paper's 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(EA 2001 a). 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, and Henry and Wilson 2007). However, selected project details were modified to be responsive to the suggestions/recommendations of the North Carolina Department of Environment and Natural Resources (NC DNR), the Tennessee Wildlife Resources Agency, U.S. EPA Region FJ, 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 sporttish 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., 2007). 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 2007 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 413) on the Pigeon River. The level in Waterville Lake during 2007 fish tissue sample collection was below normal pool due to drought conditions affecting Western North Carolina and the Pigeon River. Because of low water, the field crew had difficulty with boat access into the lake and difficulty collecting the target size distribution of fish. The total time spent on fish collection in 2007 was also less than in previous years. 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. Page 3 2007 Dioxin in Fish Tissue—April 2008 2. SAMPLING LOCATIONS In accordance with the study plan (Wilson 2006) that was implemented in 2006 (Henry and Wilson 2007), fish were collected from two sampling locations in Waterville Lake on the Pigeon River. During August 2007, two sites (Stations 4A and 4B) were sampled. Detailed sampling station information for both sites is provided in Table 2-1 and in Figures 2-1 &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 Canton Mill, 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 (Figure 2-2). Appropriate habitats were sampled within each study reach in an effort to collect the desired complement of fishes. Fish sampling was conducted in the vicinity of each location described above; however, the distance or effort at each station depended on how difficult it was to collect fish at that station. The Station 4B study area consisted of an approximate 1.0 RM reach of Waterville Lake located from the dam to the confluence of Wilkins Creek. Sampling at Stations 4A and 4B included gillnetting near the shore along both the left and right banks of Waterville Lake. Page 4 2007 Dioxin in Fish Tissue—April 2008 Table 2-1. Pigeon River Sampling Stations. 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 Relative abundance dominated by channel catfish. (21.8 RM downstream from habitat with bedrock covered by Bluegill,black crappie,flathead catfish,small the Canton Mill outfall) loose,unconsolidated bottom mouth bass,and largemouth bass are common. sediments. Maximum depth Common carp are present but not common. sam led a roximately 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,channel catfish, flathead catfish, with Wilkins Creek(24.3 sediments. Maximum depth smallmouth bass,and largemouth bass are common. RM downstream from the sampled approximately 12 in. Very Common carp are present but not common. Canton Mill outfall) steep banks with little cover. Page 5 2007 Dioxin in Fish Tissue—April 2008 Figure 2-1. Monitoring stations (1, 2, 3, 4A, 413,and 5, circled in blue text) on the Pigeon River. Fish tissues were collected from two sites (4A and 413) for dioxin analyses in 2007. More precise geographical locations of each site are presented in Figure 2-2 B41BpB.TN RalloN,TN Its. 5 xer BawLU enk" (ElR)Nm,aN, _..... N ROUN •� CAROIJNR or p NOTE: RNn mlys of ma Rat.sampling bcallon NyCio Plan) // t ibuG (M.0) 1 — rY mouth aM1Bwn in pYBntM1BSes. '>•' BNwc00 e Pear.and RBnu,oa sampbng Ftammr, 2 wham R.a J warenaa trace mwarnea 4B Creak NLpw.NC MI) 4A Mal cr..k 1�T1 caumacra<k N.Napco Sda" RiwLlb /Ky) Il qea Caga (aty (u.I) , crablrve FLOW (ez z) Jone0ivN 1a6.0) Balaw Clyea 15711 T�kD1, par,-on BrWya (555) k -Cl,& / FbeMlle (50.0) Fib—Ra B.Nw 2 WayrgLNIIO WWIP ..'i O.W.I Canton.NC W>yn—Rk RroNarM CI,d.,NC Canton Cmvr Isa.51 ISLPI (549) Page 6 2007 Dioxin in Fish Tissue—April 2008 Grassy KrwCilly Op wow, i / Q WATERVRIE LAKE ni 3568 2 „ / 26 poI !C) p5" ,r ❑ I M.,anieJ��o� ,y�V. 3567. Y I b 3599 �;/'.. ✓"—_{ __ .Moe+ VIGEON j "Mw!m Gn .1347 I Figure 2-2. Sampling Station 4A (indicated by A) and Station 4B (indicated by B) on the Pigeon River. Page 7 2007 Dioxin in Fish Tissue—April 2008 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. In 2007, each composite consisted of 4 to 5 similarly sized (shortest specimen within 75% of the length of the longest) adult individuals of the target species. Because of the difficulty in obtaining some species of bottom feeding fish at specific sites, target species varied among sites. Common carp and channel catfish (Ictalurus punctatzts) were the targeted species at sites 4A and 4B. In addition to fillet samples, one whole common carp was collected from Station 4A. In summary fish were collected as follows: • Bottom feeder fillet composite—one sample at both locations • Catfish fillet composite—one sample at both locations • Common carp whole body composite—one sample from Station 4A Every reasonable effort was made to collect the desired size, species and/or number of fish; however, the outcome of the sampling effort each year is dependent on physical river conditions and the natural diversity and abundance of target fishes at each sampling location. The 2007 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 percent rule was met \_ for all samples. Page 8 2007 Dioxin in Fish Tissue—April 2008 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT Sampling was conducted during 17—21 August 2007. Notes were recorded at each sampling station with regard to type of sampling gear, level of effort(time), and habitat(Table 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 2007, the mean total length of carp was 721 mm and fish ranged from 651-775 mm. In 2006, the mean total length for carp was 681 mm and fish ranged from 635-745 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). Electrofishing was used at all stations. At stations 4A and 4B (Waterville Lake), gill nets were also necessary because of water depth. A boat electrofishing unit (pulsed direct current) was used at all 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 hours electrofishing and 26 hours gill netting. Channel catfish and common carp - the target bottom feeder species at stations 4A, and 4B - were collected and prepared for fillet and/or whole body analysis at those stations. The physiography of the Waterville Lake Stations 4A and 4B necessitated the use of gill nets for the collection of bottom feeding species. All nets 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. The study plan (Wilson 2006) calls for composite fillet samples consisting of 3 to 5 similarly sized fish from each sampling station and a whole body common carp sample from either Station 4A or 4B. The bottom feeder fillet composites samples in 2007 consisted of 4 channel catfish and 4 common carp at Station 4A, and 4 channel catfish and 5 common carp at Station 4B. A single whole body common carp from Station 4A was also submitted for analysis (Table 4-2). All composite fillet samples submitted for analysis in 2007 met the US EPA Region IV recommendation (Cunningham 1990) that the smallest specimen in each composite be equal i to or greater than 75 percent of the total length of the largest specimen in that composite (Tables 4-2 and 6-4). Page 9 + _ 2007 Dioxin in Fish Tissue—April 2008 Table 4-1. Fish Collection Techniques and Level of Effort. Station Sampling Sampling Number RM Dates Techniques Level of Effort Comments 4A 41.5 14 Aug 07 Gill nets 1 net-hours An approximate 0.3 RM reach of river was sampled; lake level was below normal—visibility fair;station characterized by deep water Boat 1.75 hours lentic habitat with bedrock and soft,unconsolidated bottom electrofishing substrates. Sampling involved gill net sets just off the left and right shores; electrofished entire area. 4B 39.0 14,20, and 21 Gill nets 24.2 net-hours An approximate 1.0 RM reach was sampled; lake level was below Aug 07 normal—visibility fair; station characterized by deep-water lentic Boat 4.3 hours habitats with bedrock and soft bottom substrates. Sampling involved electrofishing gill nets and electrofishing throughout the forebay. Nets were set off banks as well as horizontal set at near surface,midwater and bottom sets. Page 10 2007 Dioxin in Fish Tissue—April 2008 Table 4-2. Summary of fish composites collected at two stations in the Pigeon River, August 2007. Total Total Length whole body Date Station Species (mm) (9) Sample type Composite 14 Aug 07 4A Channel catfish 535 3300 Fillet R' (RM 41.5) Channel catfish 560 1720 Fillet R Channel catfish 593 2060 Fillet R Channel catfish 490 1180 Fillet R MEAN 544 2065 4A Common carp 775 7860 Fillet R (RM 41.5)Common carp 755 6700 Fillet R Common carp 767 6920 Fillet R Common carp 680 4480 Fillet R MEAN 744 6490 14 Aug 07 4A Common carp 651 3860 Whole body WB" (RM 41.5) 20,21 Aug 07 4B Channel catfish 505 1340 Fillet Ra (RM 39.0)Channel catfish 670 2820 Fillet R Channel catfish 609 2240 Fillet R Channel catfish 630 2400 Fillet R Channel catfish 588 1760 Fillet R MEAN 600 2112 14,20 Aug 07 4B Common carp 728 8300 Fillet R (RM 39.0) Common carp 715 5780 Fillet R Common carp 706 5400 Fillet R Common carp 762 8840 Fillet R Common carp 672 4440 Fillet R MEAN 716 6552 Ra right fillet composite WBb whole body composite Page 11 2007 Dioxin in Fish Tissue—April 2008 For the target bottom feeder species in this study—catfish and carp- it is becoming increasing difficult to find small carp in Waterville Lake. The mean weights of carp collected from Stations 4A and 4B in 2007 were higher than in previous sampling years. Figure 4-1 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 2007. The size of the carp taken for whole body tissue analysis from Station 4A in 2007 was similar to size of whole body fish collected in previous years. The mean size of carp collected at Stations 4A and 4B was higher than in previous years. A statistical review of the fish weight data indicate that while some carp specimens collected in 2007 were similar in weight to previous years, the 2007 carp composite fillet samples for Stations 4A and 4B included individual carp whose weight was larger than any previously collected. The decision to keep and fillet several very large carp in 2007 was made at the time of sample collection because the field crew was not finding smaller carp that met the size distribution range of previous sampling years. Because of low water access problems, the sample collection hours on carp in 2007 were less than in previous years. l Page 12 2007 Dioxin in Fish Tissue—April 2008 Max, Min and Mean of Lengths taken from Fish Tissue Samples 2004-2007 800 750 � I E 700 E 650 •— w 600 550 I 500 1 450 400 m m E m m E� m m n d a n U m U m o U m U m o U m U `m o U m U `m o v I � Lv Lv < aLv m m a vam L 2004 2005 2006 2007 Max, Min and Mean of Weights taken from Fish Tissue Samples 2004-2007 9000 8000 7000 000 5 � 000 4000 3000 — 2000 1000 0 - n U m U m o U `m U `m o U m U `m o. U m` U `m o a U m ° L a L) m t a 0 m 0 r a 0 m L COv av v m � � a� a m � a a� a m p 2004 2005 2006 2007 Figure 4-1. Lengths and Weights of Fish Collected from Waterville Lake for Tissue Analysis, 2004—2007 Page 13 2007 Dioxin in Fish Tissue—April 2008 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 3 to 5 fish composite fillet samples at each station in Waterville Lake that met the species and size objectives discussed in Section 3. In addition, a whole body composite carp sample was collected from either station. 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. The fish not retained for analysis were returned to the lake. 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 dry ice. Right side fillets were sent to Sevem Trent Laboratory (STL, now TestAmerica West Sacramento) for analysis; left side fillets were retained by Blue Ridge Paper Products as back-up fillets. All individual specimens (fillets or whole bodies) composing a single composite sample were placed together in a water-tight plastic bag labeled with station name, sample number, and number of samples in that composite. All labels had the following information: • sample identification number, • sample location and station identification, • sampling team initials, • date of collection, • species name, • sample type (i.e., fillet or whole body) A chain-of-custody form was filled out for each cooler of samples submitted for analysis. Each form included composite specific information and instructions. Copies of the chain-of- custody records are provided in Appendix A. Page 14 2007 Dioxin in Fish Tissue—April 2008 All samples were frozen solid prior to shipment to the analytical laboratory. The frozen samples were packed on dry ice, shipped via overnight delivery and arrived on 8/27/07 at Severn Trent Laboratory— 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. The backup fillets were then destroyed. Page 15 2007 Dioxin in Fish Tissue—April 2008 6. ANALYTICAL RESULTS The fish tissue samples were received in one shipment(8/27/07) at Severn Trent Laboratory (STL) — Sacramento California 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 STL personnel, and equal aliquots of the homogenate from each fish were removed to constitute the composite. Dioxin and foran analyses were performed using high resolution Gas Chromatography/Mass Spectrometry (GC/MS) as required by the US 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 (US EPA 1994) as specified in the Fish Tissue Sampling Study Plan(EA 2001 a). The quality of the analytical results was assured through reproducible calibration and testing of the extractions and GC/MS systems. A laboratory method blank was prepared along with each batch of samples. The laboratory also used precision and recovery standards for determination of initial and ongoing precision and accuracy. Laboratory reports for all 2007 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 isomers. 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. 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 Curdle (1983)]. Concentrations of 2,3,7,8-TCDD and 2,3,7,8-TCDF in channel catfish fillet composites were below the level of detection at both Station 4A and Station 4B. TCDD and TCDF in the whole body common carp sample from Station 4A were also at or below detection limits. These results are consistent with previous years sampling data. In common carp, 2,3,7,8-TCDD was detected (6.4 ppt) in the fillet composite collected at Station 4A, but was not detected (6.9 ppt detection limit) at Station 4B. The detection limit for 2,3,7,8-TCDD is elevated for the common carp fillet composite from Station 4B because a 10-fold dilution of the sample was required to overcome sample matrix interference 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 in 2007 relative to recent previous years in which this contaminant was detected at lower concentrations. The concentration of 2,3,7,8-TCDF was 2.6 ppt in the common carp fillet composite at Station 4A and was 4.6 ppt in the common carp fillet composite from Station 4B. The percent lipids data for the 2007 common carp fillet composites in Table 6-1 are of note. Some of the carp collected were larger than in any of the previous 18 years of study, and percent lipids in the carp composite fillets were higher than in previous years. Page 16 2007 Dioxin in Fish Tissue—April 2008 The North Carolina Department of Health and Human Services (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 f iran (CDD/F) isomer is based on the toxicity equivalence factor (TEF) (WHO 1997, 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 farans and is expressed as an "equivalent amount of 2,3,7,8-TCDD" (NC DEHNR 1991). The measured concentration of each CDD/F isomer,when multiplied by its appropriate TEF, yields the TEQ of that isomer (the toxic concentration of that isomer relative to the toxicity of 2,3,7,8-TCDD). In cases where concentrations were below the level of detection, a value of 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. Table 6-3 is a TEQ calculation and summary following methods used by NC DHHS (NC (DEHNR 1991). Channel catfish TEQ values in Table 6-3 for 2007 are similar to those reported for 2004, 2005 and 2006 (Henry and Wilson 2006 and 2007). The 2007 channel catfish fillet TEQ values are well below the NC DHHS advisory limit of 4 ppt at both Waterville lake sampling stations. The 2007 TEQ value for the common carp composite at Station 4A was above the advisory limit (TEQ = 13.44 ppt). The TEQ value for the Station 4A whole body carp sample was below the advisory limit (TEQ =1.41 ppt). The 2007 TEQ ,1 for the common carp composite at Station 4B was 1.26 ppt. The TEQ values for common carp fillet composites collected from Stations 4A and 4B in 2004, 2005 and 2006 were all below 4 ppt. Table 6-4 illustrates 2,3,7,8 TCDD concentrations in common carp fillet samples collected in 2005, 2006, and 2007. Table results for previous years (1990-2004) are in Appendix C. Figures 6-1 and 6-2 illustrate long-term trends for TCDD in composite fillet fish samples collected from Waterville Lake. Between 1990 and 2006, 2,3,7,8-TCDD concentrations in carp fillets declined dramatically (94-99 percent) at all sampling stations (Table 6-4, Appendix C, Figure 6-1). In 2007 concentrations of 2,3,7,8-TCDD in common carp increased at Station 4A to 6.4 ppt. This is an anomalous result compared to the previous 13 years of monitoring data at this location (since 1993). Because detection level values are plotted in Figure 6-1 for non-detects, the 2007 TCDD data for common carp at Station 4B reflects an elevated detection level from sample dilution to overcome analytical inference effects and is not an actual increased concentration. Figure 6-2 shows that concentrations of 2,3,7,8-TCDD in channel catfish fillets have been below detection levels at all sites since 2002. Page 17 2007 Dioxin in Fish Tissue—April 2008 Table 6-1. Summary of the Pigeon River Fish Tissue Analysis Results 2007. Station Percent Number Sample ID Composite/Sample Tyne 2,3,7,8-TCDD(a) 2,3,7,8-TCDF(° Lipid 4A SITE 4A channel catfish 5 fillet samples 0.57("c) ND(DL=0.41) 8.7 SITE 4A common carp 4 fillet samples 6.4 2.6 26 SITE 4A common carp 1 whole body samples 0.75(b'`) 1.4(`) 11 4B SITE 4B channel catfish 5 fillet samples 0.67() ND(DL=0.34) 2.8 SITE 4B common carp 5 fillet samples ND (DL=6.9)(d) 4.6(`) 29 (a)Units=ppt(parts per trillion)or pg/g(picogram/gram), detection level reported for not detected(ND)values (b)Estimated results. Result is less than the reporting limit (c)Analyte was positively identified,but the quantitation is an estimate. (d)The detection limits for this sample are elevated because the sample was diluted 10-fold to overcome sample matrix effects (high lipid concentration) during the analysis. (e) The TCDF result for the common carp composite from Station 4B was confirmed on an undiluted QA sample analysis. (ND)Not detected, concentrations below the instrument detection limit. Page 18 2007 Dioxin in Fish Tissue—April 2008 Table 6-2. Toxicity Equivalence Factors for CDD/F Isomers (WHO 1997, 2005) DIOXIN DIBENZOFURAN Isomer(') TEFroI TEFroI 2,3,7,8-TCDD 1 2,3,7,8-TCDF 0.1 1,2,3,7,8-PeCDD 1 1,2,3,7,8-PeCDF 0.03 2,3,4,7,8-PeCDF 0.3 1,2,3,4,7,8-HxCDD 0.1 1,2,3,4,7,8-HxCDF 0.1 1,2,3,7,8,9-HxCDD 0.1 1,2,3,7,8,9-HxCDF 0.1 1,2,3,6,7,8-HxCDD 0.1 1,2,3,6,7,8-HxCDF 0.1 2,3,4,6,7,8-HxCDF 0.1 1,2,3,4,6,7,8-HpCDD 0.01 1,2,3,4,6,7,8-HpCDF 0.01 1,2,3,4,7,8,9-HpCDF 0.01 OCDD 0.0003 OCDF 0.0003 (a) In each homologous group, the relative toxicity factor for the isomers not listed is 1/100 of the value listed for the other isomers in that homologous group. (b)TEF=toxic equivalence factor=relative toxicity assigned. Page 19 i 2007 Dioxin in Fish Tissue-April 2008 Table 6-3. Summary of CDD/F Isomer Analyses, Toxicity Equivalent Factors and Toxicity Equivalent Values for the 2007 Waterville Lake Fish. STATION 4A Channel catfish-fillet Common carp fillet Common carp body whole bo CDD/F isomers TEF(`) Results(') TE tb) Results(a) TE ro) Resultst'� le bo Dibenzodioxin 2,3,7,8-TCDD 1.0 0.57(d) 0.57 6.4 6.4 0.75(d) 0.75 1,2,3,7,8-PeCDD 1.0 ND 0.000 3.3(d) 3.3 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 2.6(d) 0.260 11 1.1 3.9(d) 0.39 112,3,7,8,9-HxCDD 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDD 0.01 5.1 0.051 28 0.28 12 0.12 OCDD 0.0003 14(d) 0.0042 62 0.019 44 0.013 Dibenzofuran 2,3,7,8-TCDF 0.1 ND 0.000 2.6 0.26 1.4(d) 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 3.9(d) 1.17 ND 0.000 1,2,3,4,7,8-HxCDF 0.1 ND 0.000 3.0(d) 0.3 ND 0.000 1,2,3,6,7,8-HxCDF 0.1 ND 0.000 5.8 0.58 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 0.01 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDF 0.01 ND 0.000 2.9(d) 0.029 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 0.885 13.438 1.413 Page 20 I 2007 Dioxin in Fish Tissue-April 2008 Table 6-3 (continued). Summary of CDD/F Isomer Analyses,Toxicity Equivalent Factors and Toxicity Equivalent Values for the 2007 Waterville Lake Fish. STATION 4B Channel catfish-fillet Common carp fillet CDD/F isomers TEF(`) Resultsta) TE (') Results(a) TE ro) Dibenzodioxin 2,3,7,8-TCDD 1.0 0.67(d) 0.67 ND(e) 0.000 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 ND 0.000 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 71 0.710 OCDD 0.0003 5.1(d) 0.002 310 0.093 Dibenzofuran 2,3,7,8-TCDF 0.1 ND 0.000 4.6 (f) 0.46 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 0.01 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 0.672 1.263(e,f) (a) Units=ppt(parts per trillion)or pg/g(pictogram 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. (e)Diluted sample to overcome matrix interference effects,detection level elevated for all isomers except TCDF(see note f) (f)The TCDF result for the common carp composite from Station 4B was confirmed on an undiluted QA sample analysis. Page 21 2007 Dioxin in Fish Tissue—April 2008 Long-term monitoring of fish tissue as an indicator of change in environmental conditions requires that a similar size and age distribution of fish be collected each year. With improved water quality, it is becoming increasing difficult to find young carp of consistent size and weight for fish tissue sampling in Waterville Lake. The younger, smaller carp don't survive predation by the thriving, healthy population of game fish that now exists in Waterville Lake. The mean weights of common carp collected from Stations 4A and 4B in 2007 were higher (6.49 kg, Station 4A; 6.55 kg, Station B) than carp collected in 2006 (4.505 kg, Station 4A; 5.637 kg, Station 413)), and the mean weight in 2007 was greater than the mean weight of carp collected for the entire period of 1999-2003 (3.193 kg, Station 4A; 5.042 kg, Station 4B). As discussed in Section 4 of this report, several individual carp specimens collected for composite fillet samples from Stations 4A and 4B in 2007 were larger than in all previous sampling years. The larger size of common carp collected in 2007 may explain the anomalous elevation in the level of 2,3,7,8 TCDD observed in the fillet composite collected from Station 4A and the analytical problems with the composite sample from Station 4B that required dilution. Lipid concentrations in common carp fillets collected at Station 4A and 4B were higher than observed previously(2007 levels: 26%, Station A; 29% Station B; 2006 levels: 23%, Station A; 12% Station B), and these levels can relate to elevated concentrations of hydrophobic contaminants. In January 2007, the NC DHSS lifted the fish advisory for common carp in Waterville Lake t and requested two additional years of fish tissue sampling and surveillance (Appendix E). The anomalous increase in TEQ for the common carp fillet sample at Station 4A in August 2007 compared to samples collected in 2004, 2005 and 2006 is believed to be an artifact associated with the size of fish collected and does not reflect current conditions in Waterville Lake. Sampling in 2008 targeted at a fish size distribution similar to that collected in 2004 through 2006 — assuming the fish are available - is necessary to determine any significant change or trend. All catfish samples collected from Waterville Lake since 2002 have been at or below detection levels for TCDD,TCDF and related isomers. Page 22 r- - 2007 Dioxin in Fish Tissue—April 2008 Table 6-4. Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 2005—2007 2005 Results(d) 2006 Results(e) Number Length Range Number Length Range Station Species offish (mm) 2,3,7,8-TCDD('b) Station Species offish (mm) 2,3,7,8-TCDDt�b1 1 Black redhorse 5 359-384 ND(0.35) 4A Common carp 3 635-692 0.64(c) 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(c) RM 59.0 Channel catfish 3 443-460 ND(0.29) RM 39.0 Channel catfish 4 510-590 0.77(c) 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`) 5 Black redhorse 4 440-501 ND(0.41) RM 19.0 Total fish filleted= 33 Total fish filleted= 15 (a)Dioxin analyses conducted by Severn Trent Laboratories. (b)Units=ppt(parts per trillion)or pg/g(pictogram/gram),detection level reported for not detected(ND)values (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 - Page 23 C ! 2007 Dioxin in Fish Tissue—April 2008 Table 6-4 (continued). Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 2005-2007 2007 Results(e) Number Length Range Station Species offish (mm) 2,3,7,8-TCDD(a") 4A Common carp 4 601-665 6.4 RM 41.5 Channel catfish 5 464-508 0.571`I 4B Common carp 5 595-736 ND(6.9)t* RM 39.0 Channel catfish 5 513-603 0.67`I Total fish filleted= 19 (a)Dioxin analyses conducted by Severn Trent Laboratories. (b)Units=ppt(parts per trillion)or pg/g(pictogram/gram),detection level reported for not detected(ND)values (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August and September (e)Survey conducted in August (f)Dilution required to overcome sample matrix interference,reported detection level is elevated ND=Non-detectable at the detection limit in parentheses Page 24 2007 Dioxin in Fish Tissue—April 2008 Figure 6-1 (Cont.). TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990- 2006 (Stations 4A and 413). 70 60 \ \ \ 50 tStation 4a 0 1 / i— Station 4b 40 Y \ a \ W \ a 30 \ U \ U H \ 20 \ \ \ 10 \ • • ,• 1' 0 — 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 YEAR b) TCDD concentrations at Station 4B were not detected,therefore,the value plotted represents the detection limit for that sample. The detection limit for 2,3,7,8- TCDD is elevated in Station 4B because a 10 fold dilution of the sample was required to overcome sample matrix effects(high Iipld concentration)during analysis. Consequently,reporting the detection limit for this sample can give a misleading impression that concentration of TCDD increased in 2007. Page 25 2007 Dioxin in Fish Tissue-April 2008 Figure 6-2. TCDD Concentrations in Catfish Fillets Collected from the Pigeon River, 1997-2007 (Stations 4A and 411). 2.50 - - 2.00 - 0 Station 4A - W--Station 4B 0 Py 1.50 a se 5 1.00 - U % E a b b a 0.50 b �! -b a - a a a ' 0.00 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 YEAR a) TCDD coricentrations at Stations 4A and 4B were not deterred,therefore,the values plotted represent the detection limits for those samples. b) TCDD concentrations at Station 4B were not detected,therefore,the value plotted represents the detection limit for that sample. Page 26 2007 Dioxin in Fish Tissue—April 2008 7. REFERENCES Cordle, F. 1983. Use of epidemiology in the regulation of dioxins in the food supply, in Accidental Exposure to Dioxins: Human Health Aspects (F. Coulston and F. Pocchiara, eds.),pp 245-256. Academic Press,New York. Cunningham, W.R. 1990. Letter to Paul Wiegand. 30 January. EA Engineering, Science, and Technology Inc. 1990. Study Plan for the Monitoring of Dioxin in Fish Tissue. EA Report No. 11370.01, prepared for Champion International Corporation, Canton,North Carolina. EA Engineering, Science, and Technology Inc. 1991. Results of the 1990 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.02, prepared for Champion International Corporation, Canton,North Carolina. EA Engineering, Science, and Technology Inc. 1992. Results of the 1991 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.03, prepared for Champion International Corporation, Canton,North Carolina. EA Engineering, Science, and Technology Inc. 1993a. Results of the 1992 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.05, prepared for Champion International Corporation, Canton,North Carolina. April. EA Engineering, Science, and Technology Inc. 1993b. Results of the 1993 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.06, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1994. Results of the 1994 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.07, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1995. Results of the 1995 Dioxin Monitoring in Fish Tissue. EA Report No. 13043.01, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1996. Results of the 1996 Dioxin Monitoring in Fish Tissue. EA Report No. 13176.01, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 1997. Results of the 1997 Dioxin Monitoring in Fish Tissue. EA Report No. 13353.01, prepared for Champion International Corporation, Canton,North Carolina. November. Page 27 2007 Dioxin in Fish Tissue—April 2008 EA Engineering, Science, and Technology Inc. 1998. Results of the 1998 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2000. Results of the 1999 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01, prepared for Champion International Corporation, Canton,North Carolina. January. EA Engineering, Science, and Technology Inc. 2001a. Study Plan for Pigeon River Dioxin Monitoring in Fish tissue. Prepared for Blue Ridge Paper Products, Canton, North Carolina. November. 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. 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. February 2006. Henry, T.B. and J.L. Wilson. 2007. Results of 2006 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc. Canton Mill, Canton,North Carolina. January 2007. 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. Page 28 2007 Dioxin in Fish Tissue—April 2008 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 Dibenzofitrans (CDDs and CDFs) and 1989 Update Report No. EPA/625/3-89/016, U.S. EPA, Risk Assessment Forum, Washington, D.C. Versar, Inc. 1984. Sampling Guidance Manual for the National Dioxin Study. U.S. Environmental Protection Agency. EPA Contract 68-01-6160. Work Order Number 8.7. Office of Water Regulations and Standards, Monitoring and Data Support Division, Washington, D.C. Final Draft. July. Wilson, J.L. 2006. Study plan revision: dioxin monitoring in fish tissue, Waterville Lake. Prepared for Blue Ridge Paper Products, Inc. Canton Mill, Canton,North Carolina. March 2006. World Health Organization (WHO). 1997. Exposure and Human Health Reassessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) and Related Compounds: Part H Health Assessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin(TCDD) and Related Compounds. World Health Organization (WHO). 2005. The 2005 World Health Organization Re-evaluation U of Human and Mammalian Toxic Equivalency Factors for Dioxin and Dioxin-Like Compounds (Reported in Van den Berg et.al., Toxicological Sciences 93(2), 223-241 (2006). Page 29 2007 Dioxin in Fish Tissue—April 2008 8. APPENDICES APPENDIX A: CHAIN OF CUSTODY FORMS APPENDIX B: SEVERN TRENT LABORATORY-SACRAMENTO ANALYTICAL REPORTS APPENDIX C: BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS 1990-2004 APPENDIX D: 2006 REVISIONS TO DIOXIN MONITORING PLAN APPENDIX E: NC DWQ AND DPH REVIEW OF 2006 FISH TISSUE ANALYSIS REPORT, LIFTING OF FISH ADVISORY FOR WALTERS LAKE l Page 30 Chain ® STL Custody Record Severn Trent Laboratories, Inc. STLA124 (bebl) Clien �,, nn �, f" n Proje tManager Date W�- ''rA. Chain o7Cust tly Number a '�` s t, 1S9- Z1 '6) 7 3 1305 Address ,✓ C!-��J',+' p(L Te ephone Nu ber(Area Cade)/Fpax Number Lab Number L & .� "'� O74 Page of City ( State ZIP Code Site Conte t 1 Lab Ca tact Analysis(Attach list i/ Cj( t l TOW /�/L zZVO y more ace is needed Project me andlLocati' (St te) CamienWaybill umber b I It / 7 ��t S,Stn e Special Instructions/ P Conbact/Purchase OMer/Quote No. Matrix Containers$ 1 S ] c j Conditions of Receipt Preservatives Sample I.D.No.and Description v o '� z �x 0 c Date Time (Containers for each sample maybe combined on one line) l d'i Q l llvs X �(CIF C1�astne ' ,'u s . ' 2I f , Y no r; nr e (�bNt hOlt (2v htt 11 'ON -7 ) 5" q `rt (4 �' 9 '2 D 17t�SJ `1 o f ' 1d U t` ea y ✓ 60" I Possible Hazard Identification Sample Disposal (A lee may be assessed it samples are retained azartl ❑ Flammable ❑ Skin Irritant ❑ Poisons ❑ Unknown ❑0ReturnTo Client El Disposal By Lab ❑Archive For Months longer than 1 month) u Around Time Required OC Requirements(Specify) 1124 Hours ❑ 48 H urs ❑ 7 Days ❑ 14 Days ❑21 Days ❑ Other 1.Relinquished' r 4; Date Time 1.Receiv B 1 Y Date Time 2.Relinquis7 $yJ Oafe Time 2.Received By Dals I Time 3.RelinquihdBy Date Time 3.Received By Date Time Comments !'� J / i /%rye- - DISTRIBUTION: WHITE-Returned to Client with Report; CANARY.Stays with the Sample; PINK-Field Copy /TestAmedca -, THE LEADER IN ENVIRONMENTAL TESTING April 2, 2008 TestAmerica Project Number: G7H270143 Amendment PO/Contract: 7605001 Paul Dickens Blue Ridge Paper Products Inc 175 Main Street P.O. Box 4000 Canton, NC 28716 Dear Mr. Dickens, This report contains the analytical results for the samples received under chain of custody by TestAmerica on August 27, 2007. These samples are associated with your Waterville Lake- Fish Tissue project. This report has been amended to revise the 1,2,3,6,7,8-HxCDF result from a "J" qualified result to a non-detect. The test results in this report meet all NELAC requirements for parameters that accreditation is required or available. Any exceptions to NELAC requirements are noted in the case narrative. The case narrative is an integral part of this report. If you have any questions, please feel free to call me at (916) 374-4402. Sincerely, Jill Keilmann Project Manager 880 Riverside Parkway West Sacramento, CA 95605 tel 916.373.5600 fax 916.372.1059 www.testamericaino.com G7H270143 Amendment March 3,2008 TestAmerica West Sacramento(916)373-5600 Table of Contents TestAmerica West Sacramento Project Number G7H270143 Case Narrative Quality Assurance Program Sample Description Information Chain of Custody Documentation BIOLOGIC, 8290, Dioxins/Furans/ Lipids, Percent Samples: 1, 2, 3, 4, 5 Sample Data Sheets Method Blank Reports Laboratory QC Reports Full Raw Data Package t. � Case Narrative TestAmerica West Sacramento Project Number 1071-127O143 General Comments Please note the chain of custody (COC) indicates 4 fillets were sent by the client for sample ID SITE-4A Channel Cat R Fillet. The laboratory received 5 fillets for this sample. In addition, the COC indicated 5 fillets were sent by the client for sample ID SITE 4A Common Carp R Fillet. The laboratory received 4 fillets for this sample. All samples were logged in based on the number for fillets we received. BIOLOGIC, 8290, Dioxins/Furans / Lipids, Percent Sample(s): 1, 2, 3, 4, 5 The bracketing continuing calibration standard analyzed on September 25, 2007 at 0031 has internal standards 13C-1,2,3,4,6,7,8-HpCDF and 13C-OCDD with percent difference values that are above the method recommended criteria of 30% to 35% deviation from the initial calibration curve. Per method guidelines, all associated samples that have greater than 135% recovery for these compounds were reinjected. Otherwise, there is no impact on the data. The bracketing continuing calibration standard analyzed on September 25, 2007 at 0031 has internal standard 13C-1,2,3,4,6,7,8-HpCDD with a percent difference values that are between the method recommended criteria of 30% to 35% deviation from the initial calibration curve. Per method guidelines, an average relative response factor is calculated from bracketing continuing calibration standards and is used to quantitate any positive results in the associated samples for the affected analyte. There is no impact on the data as a result of this anomaly. The bracketing continuing calibration standard analyzed on September 25, 2007 at 0031 has analytes 1,2,3,4,7,MxCDD; 1,2,3,4,7,8,9-HpCDF and OCDF with percent difference values that are between the method recommended criteria of 20% to 25%. deviation from the initial calibration curve. Per method guidelines, an average relative response factor is calculated from bracketing continuing calibration standards and is used to quantitate any positive results in the associated samples for the affected analytes. There is no impact on the data as a result of this anomaly. samples for the affected analytes. There is no impact on the data as a result of this anomaly. Samples: 1, 5 The analyte 2,3,7,8-TCDD has been qualified with the "JA" flag as the ion abundance ratios is outside of criteria. The analyte has been reported as an "estimated maximum possible concentration" (EMPC) because the quantitation is based on the theoretical ion abundance ratio. G714270143 STL Sacramento(916).373-5660 1 of 707 Case Narrative TestAmerica West Sacramento Project Number 1371-1270143 Sample(s): 2, 4, 5 The results for 2,3;7,8-TCDF is reported from the confirmation analyses that occurred on September 24 and 25, 2007. Sample(s): 4 The above sample required a dilution that occurred on September 25, 2007. Several internal standard recoveries are lower than the method recommended goal of 40%. Generally, data quality is not considered affected if the internal standard signal-to-noise ratio is greater than 10:1, which is achieved for all internal standards in the sample. There is no adverse impact on data quality. This section has been amended on April 2,2008: The internal standards 13C-2,3,7,8-TCDF, 13C-1,2,3,4,7,8-HxCDF and 13C- 1,2,3,4,6,7,8-HpCDF have ion abundance ratios outside of acceptance criteria on the 1313-5 sequence analyzed on September 25, 2007 at 22:37 (note: the 130- 2,3,7,8-TCDF result was reported from the confirmation sequence analyzed on -� September 24, 2007 at 20:39 and met the ion abundance ratio criteria). This anomaly is directly related to the dilution and the associated lower sensitivity observed in the sample for these internal standards. The theoretical areas for the internal standards were used to.quantitate the recoveries and to quantitate related target analytes. The detection limits for affected native results have been raised to indicate the uncertainty of the reported results. There were no other anomalies associated with this project. •G7H270143 Amendment March 3,2008 TestAmerlcaWest Sacramento(916)373-5600 tp ACCO ,96 TestAmerica THE LEADER IN ENVIR6M1A'ENTAt'tESTING q a: � - TestAmerica Laboratories West Sacramento Certifications/Accreditations Certifying State Certificate Certifying State Certificate # Alaska UST-055 New York* 11666 Arkansas 04-067-0 Penns lvania 68-1272 California*') �`n� ' I ,�0111>2CA r .4-,.•"Soufh,CaiolL€ - .. Colorado NA Texas TX 270-2004A 7.'?„v ,s"�P,F1-�69.1r �„xm xs:.wta}IMb. Florida* E87570 Virginia 00178 V/as)tm ton r PUN- 087 ','Kk vF Hawaii NA West Vir 'nia 9930C,334 - 13j037,5 t t sedn In Louisiana* 01944 NFESC NA A L AS rcE S d ZYr 6 !b NA L` Nevada CA44 USDA Foreign Plant 37-82605 New7eise 'TISDA3Fo`iei"'x$a[1rx A S 4ftb TF A *NELAP accredited. A more detailed parameter list is available upon request.Updated 9/21/07 QC Parameter Definitions QC Batch: The QC batch consists of a set of up to 20 field samples that behave similarly(i.e.,same matrix) and are processed using the same procedures,reagents,and standards at the same time. Method Blank: An analytical control consisting of all reagents,which may include internal standards and surrogates,and is carried through the entire analytical procedure. The method blank is used to define the level of laboratory background contamination. Laboratory Control Sample and Laboratory Control Sample Duplicate(LCS/LCSD): An aliquot of blank matrix spiked with known amounts of representative target analytes. The LCS(and LCSD as required)is carried through the entire analytical process and is used to monitor the accuracy of the analytical process independent of potential matrix effects. If an LCSD is performed,it may also be used to evaluate the precision of the process. Duplicate Sample (DU): Different aliquots of the same sample are analyzed to evaluate the precision of an analysis. Surrogates: Organic compounds not expected to be detected in field samples,which behave similarly to target analytes. These are added to every sample within a batch at a known concentration to determine the efficiency of the sample preparation and analytical process. Matrix Spike and Matrix Spike Duplicate (MS/MSD): An MS is an aliquot of a matrix fortified with known quantities of specific compounds and subjected to an entire analytical procedure in order to indicate the appropriateness of the method for a particular matrix. The percent recovery for the respective compound(s)is then calculated. The MSD is a second aliquot of the same matrix as the matrix spike,also spiked,in order to determine the precision of the method. Isotope Dilution: For isotope dilution methods,isotopically labeled analogs(internal standards)of the native target analytes are spiked into the sample at time of extraction. These internal standards are used for quantitation,and monitor and correct for matrix effects. Since matrix effects on method performance can be judged by the recovery of these analogs,there is little added benefit of performing MS/MSD for these methods. MS/MSD are only performed for client or QAPP requirements. Control Limits: The reported control limits are either based on laboratory historical data,method requirements,or project data.quality objectives. The control limits represent the estimated uncertainty of the test results. G7H270143 STL Sacramento(916)373-5600 3 of 707 Sample Summary TestAmerica West Sacramento Project Number G71i270143 WON Sample N Client Sample ID Semolina Date Received Date JSNLJ 1 SITE 4A CHANNEL CAT R FILLET B/14/2007 04:40 PM 8/27/2007 09:25 AM JSNLL 2 SITE 4A COMMON CARP R FILLET 8/14/2007 05:36 PM 8/27/2007 09:25 AM JSNLP 3 SITE 4B CHANNEL CAT R FILLET 8/21/2007 11:05 AM 8/27/2007 09:25 AM (0/20/07-0/21/07) J5NL0 4 SITE 48 COMMON CARP R FILLET 8/20/2007 03:45 PM 8/27/2007 09:25 AM (8/14/07.8/20/07) J5NL2 6 SITE 4A COMMON CARP WHOLE BODY 8/14/2007 04:50 PM 8/27/2007 09:25 AM Notes(s): The analytical results of the samples listed above are presented on the following pages. - All calculations are performed before rounding to avoid round-off errors in calculated results. - Resuits noted as"ND"were,not detected at or above the stated limit. - This report must not be reproduced,except in full,without the written approval of the laboratory. Results for the following parameters are never reported on a dry weight basis:color,corrosivity,density,fiashpoint, Ignitability,layers,odor,paint filter test,pH,porosity,pressure,reactivity,redox potential,specific gravity,spot tests, solids,solubility,temperature,viscosity,and weight G71-1270143 STL Sacramento(916)373.5600 4 of 707 STLChain o Custody Record Severn Trent Laboratories, Inc. STL-4124 (0e01) Clien Projoct Manager Oa(e Chain of Custody Number kt i rob �.c , �1Y Z- c7 344305 Address C�{���/y7�" Telephone N ber(Area Code/Faax Number Lab Nu ber / lqr 'M ✓'�Y LV 'gZg � "�2D ! Page of 6 uny r State Zip Code Site Conta t Lab Co tact Analysis(Attach list if 00j t',.7BD4 ive 7$ q NI tj� e ke I mores ace is needed Pro%ect N��QQm�e antl Locafio (St feJ y{�� I /� Carder/Waybill Number 1 C Special Instructional Contrad/Purchese Order/Quote No Matrixh Containers& .+ N p? Conditions of Receipt Preservatives ,,n Sample LD.No.and Description note Time f 3 c°, o �¢o q © Iv , (Containers for each sample maybe combined on one line) t(J"(" -TI T Hoot -( 4 gai � (q P a. X �, ?C dsi�e 'a Ith col -S R i, -�s 8 i o f I-v4 X Cr ast�V-: l e a �Sk46 CWh .fie 1 21 "7 rigs aw k l c� d�R C L w 0 S�E � �e,•.�Ae-fi, L'c,.r � f ' ? ! ,S?� X � t fie ed el 1r, Possible Hazard identification sample Disposal 10— (A fee may be assessed if samples are retained - Non-Hazard [I Flammable ❑ Skin Irritant ❑ Poison B ❑ Unknown ❑Return To Client ❑ Disposal By Lab ❑Archive For_ Months longer than I month) Turn Around Time Required - OC Requirements(Specify) ❑ 24 Hou ❑48 Hpum ❑ 7Days ❑ 14 Days ❑ 21 Oays ❑ Other 1.Relinqui y D Time. I,Rec By Date iime 7( 7 rr4-f z.� 2� �fy 2.Refinqu I Data iime ived By D f Tim c . 3.Refinquisift4d By Date Time J.R eived By Date Time J�c o Comments le I J DISTRIBUTION. WHITE"Returned to Client with Report. CANARY-Stays with the Sample. PINK-Field Copy met w.�4�Le V.1 i ire..:( 4 P1Ilets C,-,,- Lid CCc et� S"�` -�,�0L(L Test erica LOT RECEIPT CHECKLIST TestAmerica West Sacramento THE LEADER IN ENVIRONMENTAL TESTING 2 CLIENT '.—e ��� PMJJZ _ LOG#t�-� LOT#(QUANTIMS ID) UOTE P i LOCATIOf —I Initials Date DATE RECEIVED ` TIME RECEIVED 09a5 DELIVERED BY 'El FEDEX ❑CA OVERNIGHT ❑ CLIENT ❑AIRBORNE ❑ GOLDENSTATE KDHL ❑ UPS ❑ BAX GLOBAL GO-GETTERS ❑TAIL COURIER ❑VALLEY LOGISTICS ❑ MORGAN HILL COURIE ❑OTH R CUSTODY SEAL STATUS }INTACT ❑BROKEN ❑ N/A CUSTODY SEAL#(S) r)l/!ni SHIPPPING CONTAINER(S) ❑TAL CLIENT ❑ N/A TEMPERTURE RECORD (IN °C) IR 4)] 5 ❑ ❑ OTHER COG#(S) 3L)4`�QS TEMPERATURE BLANK Observed: n/Jq Corrected: cAMPLE TEMPERATURE aserved J Average: _3 Corrected Average:-3 COLLECTOR'S NAME: ❑Verified from COG 'Not on COG pH MEASURED ❑YES ❑ANOMALY --&fN/A LABELEDBY.......................................................................................... LABELS CHECKED BY......................................,j.,�..,. . ............................. PEER REVIEW I.KNA SHORT HOLD TEST NOTIFICATION SAMPLE RECEIVING WETCHEM N/A VOA-ENCORES N/A ❑ METALS NOTIFIED OF FILTER/PRESERVE VIA VERBAL 6 EMAIL ] N/A COMPLETE SHIPMENT RECEIVED IN GOOD CONDITION WITH ❑ N/A [APPROPRIATE TEMPERATURES;CONTAINERS, PRESERVATIVES LI(I CLOUSEAU ❑ TEMPERATURE EXCEEDED (2°C—6°C) J❑WET ICE El BLUE ICE ❑I GEL PACK ❑ NO COOLING AGENTS USED t �PM NOTI)FIED/ Notes: 1'I.Jz.G�� 5 Fti, tt 11-4-1 TOY Sic w'-P6 Ill} S)lie 11A CI IG nr) el N4 P-C'1 4PZY- 5A 4 1 l-34 'F yfLC 41101 G rQ W IFS, `1 Acceptable temperature range for State of Wisconsin samples is<4°C. . LEAVE NO SPACES BLANK. USE"NIA"IF NOT APPLICABLE. CA-185 5/05 EM, Page 1 G7H270143 STL Sacramento(916)373-5600 6 of 707 TestAmerica West Sacramento Bottle Lot InventoryTestAmedca Lot ('+T/ IF �^(�7/ THE LEADEN IN EMMONP.IENTAL TESTING _ ID: `1 1 1 �✓` ! Lt3 1 2 3 4 1 5 6 1 7 1 8 1 9 10 11 12 13 14 15 16 17 18 19. 20 VOA' VOAh' AGB AGBs 250AGB 250AGBs 250AGBn 500AGB _AGJ 500AGJ 250AGJ 125AGJ _CGJ 500CGJ 250CGJ 125CGJ Pi I Pi 500PJn 500PJna 500PJzn/na 250PJ 250PJn 250PJna 250PJzn/na Acetate Tube - _"CT Encore Folder/filter PUF Petri/Filter XAD Trap Ziploc 11\e S 5 f 1 2 3 1 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 h=hydrochloric acid s =sulfuric acid na=sodium hydroxide In nitric acid zn=zinc acetate erI of VOAs with air bubbles present 1 total number of VORs QA-185 5105 EM )OC Page 3 LEAVE NO SPACES BLANK. USE; A°IF NOT APPLICABLE. C�rnrn��L��. L 1371-1270143 ��a--1 I asacramento(916)373-5600 7 of 707 BIOLOGIC , 8290 , Dioxins/Furans / Lipids , Percent G7H270143 STL Sacramento(916)373-5600 8 of 707 Blue Ridge Paper.Products Inc Client Sample ID: SITE 4A CHANNEL CAT R FILM _ Trace Level Organic Compounds Lot-Sample #.. . : G7H270143-001 Work order it...: JSNLJIAC Matrix.... ..... : BIOLOGIC Date Sampled. .. : 08/14/07 Date Received. .: 08/27/07 Prep Date.. . . .. : 09/14/07 Analysis Date. -: 09/24/07 Prep Batch #. . . : 7260401 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD 0.57 J,JA pg/g SW846 8290 Total TCDD 0.57 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 0.81 pg/g SW846 8290 Total PeCDD ND 1.2 pg/g SW846 8290 1,2,3,4,7,8-HXCDD ND 0.81 pg/g SW846 8290 1,2,3,6,7,8-HxCDD 2.6 J pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 0.64 pg/g SW846 8290 Total HxCDD 2.6 pg/g SW846 8290 .1,2,3,4,6,7,8-HpCDD 5.1 pg/g SW846 8290 Total HpCDD 5.1 pg/g SW846 8290 OCDD 14 pg/g SW846 8290 2,3,7,8-TCDF NO 0.41 pg/g SW846 8290 Total TCDF 0.51 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.52 pg/g SW846 8290 ,2,3,4,7,8-PeCDF NO 0.71 pg/g SW846 8290 Total PeCDF ND 2.6 pg/g SW846 8290 1,2,3,4, 7,8-HXCDF ND 0.56 pg/g SW846 8290 1,2,3,6,7,8-HxCDF ND 0.49 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.56 pg/g SW846 8290 1,2,3,7,8,9-HxCDF NO 0.56 pg/g SW846 8290 Total HxCDF NO 2.8 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 0.78 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.57 pg/g SW846 8290 Total HpCDF ND 0.78 pg/g SW846 8290 OCDF ND 0.68 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 86 (40 - 135) 13C-1,2,3,7,8-PeCDD 80 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 95 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 87 (40 - 135) .13C-OCDD 106 (40 - 135) 13C-2,3,7,8-TCDF 91 (40 - 135) 13C-1,2,3,7,8-PeCDF 88 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 124 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 113 (40 - 135) NOTE(S) : I Estimated eesulL Resuh is less Own the repotting limit. IA The analyte was positively identified,but the quantitation is an estimate. G7H270143 STL Sacramento(916)373-5600 9 o1707 Blue Ridge Paper Products Inc Client Sample ID: SITE 4A COMMON CARP R FILLET - Trace Level Organic Compounds Lot-Sample #__.: G7H270143-002 Work order 4. ..: JSNLLIAC Matrix.. .. .. .. . : BIOLOGIC Date Sampled...: 08/14/07 Date Received. .: 08/27/07 Prep Date......: 09/14/07 Analysis Date..: 09/24/07 Prep Batch #...: 7260401 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD 6.4 pg/g SW846 8290 Total TCDD 6.4 pg/g SW846 8290 1,2,3,7,8-PeCDD 3.3 J pg/g SW846 8290 Total PeCDD 3.3 pg/g SW846 8290 1,2,3,4,7,8-HxCDD NO 0.77 pg/g SW846 8290 1,2,3,6,7,8-HxCDD 11 pg/g SW846 8290 1,2,3,7,8,9-HXCDD ND 2.0 pg/g SW846 8290 Total HxCDD 11 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD 28 pg/g SW846 8290 Total HpCDD 31 pg/g SW846 8290 OCDD 62 pg/g SW846 8290 2,3,7,8-TCDF 2.6 CON pg/g SW846 8290 Total TCDF 5.1 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 2.4 pg/g SW846 8290 2,3,4,7,8-PeCDF 3.9 J pg/g SW846 8290 Total PeCDF 3.9 pg/g SW846 8290 1,2,3,4,7,8-HxCDF 3.0 J pg/g SW846 8290 1,2,3,6,7,8-HXCDF 5.8 pg/g SW846 8290 2,3,4,6,7,8-HXCDF ND 1.1 pg/g SW846 8290 1,2,3,7,8,9-HxCDF NO 0.71 pg/g SW846 8290 Total HxCDF 8.9 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF 2.9 J pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.76 pg/g SW846 8290 Total HpCDF 2.9 pg/g SW846 8290 OCDF NO 0.68 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 76 (40 - 135) 13C-1,2,3,7,8-PeCDD 72 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 68 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 76 (40 - 135) 13C-OCDD 96 (40 - 135) 13C-2,3, 7,8-TCDF 80 (40 - 135) 13C-1,2,3,7,8-PeCDF 83 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 85 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 80 (40 - 135) NOTE(S) - Estimated result.Result is less than the reporting limit. :ON Confirmation analysis. G7H270143 STL Sacramento(916)373-5600 10 of 707 Blue Ridge Paper Products Inc Client Sample ID: SITE 4B CHANNEL CAT R FILLET (8/20/07-8/21/07) - Trace Level Organic Compounds Lot-Sample #.. .: G7H270143-003 Work Order #. ..: J5NLPIAC Matrix. . .. ..... : BIOLOGIC Date Sampled...: 08/21/07 Date Received..: 08/27/07 Prep Date... ...: 09/14/07 Analysis Date..: 09/24/07 Prep Batch (). . .: 7260401 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD 0.67 J Pg/g SW846 8290 Total TCDD 0.67 Pg/g SW846 8290 1,2,3, 7,8-PeCDD ND 0.57 pg/g SW846 8290 Total PeCDD ND 0.65 pg/g SW846 8290 1,2,3,4,7,8-HxCDD ND 0.48 pg/g SW846 8290 1,2,3,6, 7,8-HxCDD NO 1.3 pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 0.38 pg/g SW846 8290 Total HxCDD ND 1.3 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD ND 1.8 pg/g SW846 8290 Total HPCDD ND 1.8 pg/g SW846 0290 OCDD 5.1 J pg/g SW846 8290 2,3,7,8-TCDF ND 0.34 pg/g SW846 8290 Total TCDF ND 1.1 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.36 pg/g SW846 8290 2,3,4,7,8-PeCDF .ND 0.56 pg/g SW846 8290 Total PeCDF ND 1.4 pg/g SW846 8290 1,2,3,4,7,8-HxCDF NO 0.34 pg/g SW846 8290 1,2,3,6,7,8-HXCDF NO 0.30 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.34 pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 0.34 pg/g SW846 8290 Total HxCDF NO 1.6 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF NO 0.37 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.45 pg/g SW846 8290 Total HpCDF ND 0.45 pg/g SW846 8290 OCDF NO 0.52 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 89 (40 - 135) 13C-1,2,3,7,8-PeCDD 84 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 97 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 99 (40 - 135) 13C-OCDD 122 (40 - 135) 13C-2,3,7,8-TCDF 98 (40 - 135) 13C-1,2,3,7,8-PeCDF 100 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 126 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 132 (40 - 135) NOTE(S) : t Euim led remit.Reach is I=than the reporting limit. G7H270143 STL Sacramento(916)373-5600 11 of 707 Blue Ridge Paper Products Inc Client Sample ID: SITE 4B COMMON CARP R FILLET (8/14/07-8/20/07) Trace Level Organic Compounds Lot-Sample #...: G7H270143-004 Work Order #...: J5NL0lAC Matrix.........: BIOLOGIC Date Sampled...: 08/20/07 Date Received..: 08/27/07 Prep Date......: 09/14/07 Analysis Date..: 09/25/07 Prep Batch #.... 7260401 Dilution Factor: 10 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD ND 6.9 pg/g SW846 8290 Total TCDD ND 6.9 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 30 pg/g SW846 8290 Total PeCDD ND 30 pg/g SW846 8290 1,2,3,4,7,8-HxCDD ND 46 pg/g SW846 8290 1,2,3,6,7,8-HxCDD ND 49 pg/g SW846 8290 1,2,3,7,8,9-HxCDD NO 38 pg/g SW846 8290 Total RxCDD ND 49 pg/g SW846 8290 1,2,3,4,6,7,8-HPCDD 71 pg/g SW846 8290 Total HxCDD 71 pg/g SW846 8290 OCDD 310 pg/g SW846 8290 2,3,7,8-TCDF 4.6 CON,H pg/g SW846 8290 Total TCDF 7.2 pg/g SW846 8290 1,2,3,7,8-PeCDF NO 14 pq/g SW846 8290 2,3,4,7,8-PeCDF ND 15 pg/g SW846 8290 } Total PeCDF ND 46 pg/g SW846 8290 1,2,3,4,7,8-HxCDF ND 35 pg/g SW846 8290 1,2,3,6,7,8-HxCDF ND 38 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 36 pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 36 pg/g SW846 8290 Total HxCDF ND 38 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 29 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 29 pg/g SW846 8290 Total HpCDF ND 29 pg/g SW846 8290 OCDF ND 24 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 86 (40 - 135) 13C-1,2,3,7,8-PeCDD 34 * (40 - 135) 13C-1,2,3,6,7,8-HxCDD 18 * (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 34 * (40 - 135) 13C-OCDD 50 (40 - 135) 13C-2,3,7,8-TCDF 54 (40 - 135) 13C-1,2,3,7,8-PeCDF 44 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 17 * (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 23 * (40 - 135) NOTE(S) : CON Conrmwtim amlysi€ Sorrogete recovery b outside sated mntrol limos. H: The conremation for 2,3.7,8-TCDF we run m the tmdikeed ealrsa on 24SE077D2 at 20:39. G7H270143 Amendment March 3,2008 TestAmerica West Sacramento(916)373-5600 Blue Ridge Paper Products Inc Client Sample ID: SITE 4A COMMON CARP WHOLE BODY - Trace Level Organic Compounds Lot-Sample #...: G7H270143-005 Work order #. .. : J5NL21AC Matrix.. .. .. .. .: BIOLOGIC Date Sampled...: 08/14/07 Date Received. .: 08/27/07 Prep Date...... : 09/14/07 Analysis Date. .: 09/25/07 Prep Batch #. ..: 7260401 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD 0.75 J,JA pg/g SW846 8290 Total TCDD 0.75 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 1.9 pg/g SW846 8290 Total PeCDD NO 1.9 pg/g SW846 8290 1,2,3,4,7,8-HXCDD ND 0.75 pg/g SW846 8290 1,2,3,6,7,8-HXCDD 3.9 J pg/g SW846 8290 1,2,3,7,8,9-HXCDD NO 0.59 pg/g SW846 8290 Total HxCDD 3.9 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD 12 pg/g SW846 8290 Total HpCDD 17 pg/g SW846 8290 OCDD 44 pg/g SW846 8290 2,3,7,8-TCDF 1.4 CON,JA pg/g SW846 8290 Total TCDF 3.4 pg/g SW846 8290 1,2,3,7,8-PeCDF NO 0.77 pg/g SW846 8290 2,3,4,7,8-PeCDF NO 1.1 pg/g SW846 8290 Total PeCDF ND 4.9 pg/g SW846 8290 1,2,3,4,7,8-HxCDF _ ND 1.0 pg/g SW846 B290 1,2,3,6,7,8-HXCDF NO 1.2 pg/g SW846 8290 2,3,4,6,7,8-HxCDF NO 0.38 pg/g SW846 8290 1,2,3,7,8,9-HxCDF NO 0.34 pg/g SW846 8290 Total HxCDF NO 6.0 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF NO 1.3 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF NO 0.44 pg/g SW846 8290 Total HpCDF ND 1.3 pg/g SW846 8290 OCDF ND 0.53 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 92 (40 - 135) 13C-1,2,3,7,8-PeCDD 87 (40 - 135) 13C-1,2,3,6,7,8-HXCDD 107 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 100 (40 - 135) 13C-OCDD 91 (40 - 135) 13C-2,3,7,8-TCDF 89 (40 - 135) 13C-1,2,3,7,8-PeCDF 87 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 112 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 101 (40 - 135) NOTE(S) : 1 Eaimated result.Result is less than the reporting limit. IA The amslyte was positively identified,but the quantitation is an estimate. CON Confirmation analysis. G71­1270143 STL Sacramento(916)373-5600 13 of 707 QC DATA ASSOCIATION SUNMMRY G7B270143 - Sample Preparation and Analysis Control Numbers ANALYTICAL LEACH PREP SAMPLE# MATRIX METHOD BATCH # BATCH # MS RUN# 001 BIOLOGIC SW846 8290 7260401 BIOLOGIC SW846 8290. 7260403 002 BIOLOGIC SW846 8290 7260401 BIOLOGIC SW846 8290 7260403 003 BIOLOGIC SW846 8290 7260401 BIOLOGIC SW846 8290 7260403 004 BIOLOGIC SW846 8290 7260401 BIOLOGIC SW846 6290 7260403 005 BIOLOGIC SW846 8290 7260401 BIOLOGIC. SW846 8290 - 7260403 G7H270143 STL Sacmmento(916)373-5600 14 of 707 METHOD BLANK REPORT - Trace Level Organic Compounds Client Lot #. . . : G7H270143 Work Order II. ..: J61651AA Matrix. . ..- - ... : BIOLOGIC MB Lot-Sample #: G71170000-401 Prep Date. .... .: 09/14/07 Analysis Date. .: 09/24/07 Prep Batch #. . . : 7260401 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD ND 0.43 pg/g SW846. 8290 Total TCDD ND 0.43 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 0.57 pg/g SW846 8290 Total PeCDD ND 0.72 pg/g SW846 8290 1,2,3,4,7,8-HXCDD ND 0.65 pg/g SW846 8290 1,2,3,6,7,8-HxCDD ND 0.61 pg/g SW846 8290 1,2,3,7,8,9-HXCDD ND 0.52 pg/g SW846 8290 Total HxCDD ND 0.65 pg/g SW846 8290 1,2,3,4,6,7,E-HpCDD ND 0.65 pg/g SW846 8290 Total HpCDD ND 0.70 pg/g SW846 8290 OCDD ND 4.1 pg/g SW846 8290 2,3,7,8-TCDF ND 0.38 pg/g SW846 8290 -otal TCDF ND 0.38 pg/g SW846 8290 2,3,7,8-PeCDF ND 0.39 Pg/g SW846 8290 _,3,4,7,8-PeCDF ND 0.41 pg/g SW846 8290 Total PeCDF ND 0.52 pg/g SW846 8290 1,2,3,4,7,8-HxCDF ND 0.35 pg/g SW846 8290 1,2,3,6,7,8-HxCDF ND _ 0.31 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.35 pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 0.35 pg/g SW846 8290 Total HxCDF ND 0.35 Pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 0.35 Pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.43 pg/g SW846 8290 Total HpCDF ND 0.43 Pg/g SW846 8290 OCDF ND 0.49 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 91 (40 - 135) 13C-1,2,3,7,8-PeCDD 86 - (40 - 135) 13C-1,2,3,6,7,8-HxCDD 104 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 105 (40 - 135) 13C-OCDD 108 (40 - 135) 13C-2,3,7,8-TCDF 96 (40 - 135) 13C-1,2,3,7,8-PeCDF 94 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 131 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 116 (40 - 135) NOTE(S) : Wadations arc performed before rounding to avoid round off errors in alculatcd results. G7H270143 STL Sacramento(916)373-5600 15 of 707 LABORATORY CONTROL SAMPLE DATA REPORT Trace Level Organic Compounds Client Lot #...: G7H270143 Work Order #. ..: J61651AC Matrix.. ... ... .: BIOLOGIC LCS Lot-Sample#: G7I170000-401 Prep Date... ... : 09/14/07 Analysis Date.. : 09/25/07 Prep Batch #.. .: 7260401 Dilution Factor: 1 SPIRE MEASURED PERCENT PARAMETER AMOUNT AMOUNT UNITS RECOVERY METHOD 2,3,7,8-TCDD 20.0 22.0 pg/g 110 SW846 8290 1,2,3,7,8-PeCDD 100 112 Pg/g 112 SW846 8290 1,2,3,4,7,8-Hx= 100 107 pg/g 107 SW846 8290 1,2,3,6,7,8-HxCDD 100 113 pg/g 113 SW846 8290 1,2,3,7,8,9-HxCDD 100 99.4 pg/g 99 SW846 9290 1,2,3,4,6,7,8-HpCDD 100 113 pg/g 113 SW846 8290 OCDD 200 227 pg/g 114 SW846 8290 2,3,7,8-TCDF 20.0 23.2 pg/g 116 SW846 8290 1,2,3,7,8-PeCDF 100 114 pg/g 114 SW846 8290 2,3,4,7,8-PeCDF 100 110 pg/g 110 SW846 8290 1,2,3,4,7,8-HxCDF 100 110 pg/g 110 SW846 8290 1,2,3,6,7,8-HxCDF 100 116 pg/g 116 SW846 8290 2,3,4,6,7,8-HxCDF 100 112 pg/g 112 SW846 8290 1,2,3,7,8,9-HxCDF 100 103 pg/g 103 SW846 8290 1,2,3,4,6,7,8-HpCDF 100 116 pg/g 116 SW846 8290 1,2,3,4,7,8,9-HpMF 100 112 Pg/g 112 SW846 8290 OCDF 200 236 pg/g 118 SW846 8290 PERCENT RECOVERY INTERNAL STANDARD RECOVERY LIMITS 13C-2,3,7,8-TCDD 83 (40 - 135) 13C-1,2,3,7,8-PeCDD 76 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 100 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 92 (40 - 135) 13C-OCDD 84 (40 - 135) 13C-2,3,7,8-TCDF 81 (40 - 135) 13C-1,2,3,7,8-PeCDF B1 (40 - 135) 13C-1,2,3,4,7,8-HXCDF _ 102 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 95 (40 - 135) NOTE(S) - Calcalatlerla am performed before rounding to avoid round-off errors in ulculated results. Bold print denotes coot parameters G7H270143 STL Sacramento(916)373-5600 16 of 707 LABORATORY CONTROL SAMPLE EVALUATION REPORT Trace Level Organic Compounds Client Lot #.. . : G7H270143 Work Order #--.: JG1651AC Matrix-. -. .. .. . : BIOLOGIC LCS Lot-Sample#: G71170000-401 Prep Date. . . . . .: 09/14/07 Analysis Date.. : 09/25/07 Prep Batch #.. . : 7260401 Dilution Factor: 1 PERCENT RECOVERY PARAMETER RECOVERY LIMITS METHOD 2,3,7,8-TCDD 110 (50 - 150) SW846 0290 1,2,3,7,8-PeCDD 112 (50 - 150) SW846 8290 1,2,3,4,7,8-HxCDD 107 (50 - 150) SW846 8290 1,2,3,6,7,8-HxCDD 113 (50 - 150) SW846 8290 1,2,3,7,8,9-HXMD 99 (50 - 150) SW846 8290 1,2,3,4,6,7,8-HPCDD 113 (50 - 150) SW846 8290 OCDD 114 (50 - 150) SW846 8290 2,3,7,8-TCDF 116 (50 - 150) SW846 8290 1,2,3,7,8-PeCDF 114 (50 - 150) SW846 8290 2,3,4,7,8-PeCDF 110 (50 - 150) SW846 8290 1,2,3,4,7,8-HXCDF 110 (50 - 150) SW846 8290 1,2,3,6,7,8-HxCDF 116 (50 - 150) SW846 8290 2,3,4,6,7,8-HxCDF 112 (50 - 150) SW846 8290 1,2,3,7,8,9-HXCDF 103 (50 - 150) SW846 8290 1,2,3,4,6,7,8-HpCDF 116 (50 - 150) SW846 8290 1,2,3,4,7,8,9-HpCDF 112 (50 - 150) SW846 8290 OCDF 118 (50 - 150) SW846 8290 PERCENT RECOVERY INTERNAL STANDARD RECOVERY LIMITS 13C-2,3,7,8-TCDD 83 (40 - 135) 13C-1,2,3,7,8-PeCDD 76 (40 - 135) 13C-1,2,3,.6,7,8-HXCDD 100 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 92 (40 - 235) 13C-OCDD 84 (40 - 135) 13C-2,3,7,8-TCDF 81 (40 - 135) 13C-1,2,3,7,8-PeCDF 81 (40 - 135) 13C-1,2,3,4,7,8-HXCDF 102 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 95 (40 - 135) NOTE(S) : Calculations are perfumed before rounding to avoid round-off errors in calculated results. Bald print denotes control parameters G71­1270143 STL Sacramento(916)373-560D 1701707 Percent Lipids 07H270143 STL Sacramento(916)373-5600 1801707 Blue Ridge Paper Products Inc Client Sample ID: SITE 4A CHANNEL CAT R FILLET Trace Level Organic Compounds Lot-Sample #. _. : G7H270143-001 Work Order #. .. : TSNLTIAA Matrix.. .. .... . : BIOLOGIC Date Sampled. ..: 08/14/07 Date Received. . : 08/27/07 Prep Date.. .. ..: 09/17/07 Analysis Date.. : 09/25/07 Prep Batch #... : 7260403 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS- METHOD Percent Lipids 8.7 g SW846 8290 G7H270143 STL Sacramento(916)373-5600 19 of 707 Slue Ridge Paper Products Inc Client Sample ID_ SITE 4A COMMON CARP R FILLET Trace Level Organic Compounds Lot-Sample #...: G7H270143-002 Work Order #... : JSNLLIAA Matrix. ...... ..: BIOLOGIC Date Sampled. .. : 08/14/07 Date Received..: 08/27/07 Prep Date. . .. . . : 09/17/07 Analysis Date. . : 09/25/07 Prep Batch #. ..: 7260403 Dilution Factor: I DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 26 & SW846 8290 G7H270143 STL Sacramento(916)373.5600 20 of 707 Blue Ridge Paper Products Inc Client Sample ID: SITE 4B CHANMM CAT R FILLET (8/20/07-8/21/07) Trace Level Organic Compounds Lot-Sample #.. .: G7H270143-003 Work Order #. . .: J5NLPIAA Matrix. . .. ... . .: BIOLOGIC Date Sampled.. . : 08/21/07 Date Received. .: 08/27/07 Prep Date.. . .. .: 09/17/07 Analysis Date.. : 09/25/07 Prep Batch #. . . : 7260403 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 2.8 & SW846 8290 G7H270143 . STL Sacramento(916)373-5600 21 of 707 Blue Ridge Paper Products Inc Client Sample TD: SITE 4B COMMON CARP FILLET (8/14/07-8/20/07) Trace Level Organic Compounds Lot-Sample #. . . : G7H270143-004 Work Order #. . .: J5NL01AA Matrix. .. . . . . .. BIOLOGIC Date Sampled. ..: 08/20/07 Date Received..: 08/27/07 Prep Date. .. .. . : 09/17/07 Analysis Date. . : 09/25/07 Prep Batch #...: 7260403 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD - Percent Lipids 29 & SW846 8290 G7H270143 STL Sacramento(916)373-5600 22 of 707 Blue Ridge Paper Products Inc Client Sample ID: SITE 4A COMMON CARP WHOLE BODY Trace Level Organic Compounds Lot-Sample #.. .: G7H270143-005 Work Order #. • .: JSNL21AA Matrix.. . . . . . . . : BIOLOGIC Date Sampled...: 08/14/07 Date Received..: 08/27/07 Prep Date.... ..: 09/17/07 Analysis Date_.: 09/25/07 Prep Batch #.. . : 7260403 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 11 t SW846 8290 G7H270143 STL Sacramento(916)373-5600 23 o1707 N A � " o m amm o�z omx mOe CSC w CD C. � ff O �Yj "• R f+. ro ro u M z n ANM' + uN Nuu ..0 In NNu �� uN" Arr urr W i+r yy ��.vvAp tmif Aim b rm JmE,'i O W r b wOU AN �bt�i �a w W V O �v &z O Nggzz ANO W�+ nj "Oa ECG Nae �'> p Odd G y . cy� cyy Ry1 c��f 2y `G� yWy Nyy lIl O u W O lA G N W o,e S e w w C]01 od t O a W" F+ to Q � b W N N O O u V' 0 0� 0 0'O O m m u 0 0 C•° J C QQ .may H WO Mat t r b W tag tOnmN mT W W V� G�sWJW CCG w O 0 0 O O O O O O J n 0 e 1992 Results(b) 1993 ResuRs(s( Number of Length Number of Length Station Species Fish Range(ram) 2,3,7,8-TCDD(`) Station Species Fish Range(ram) 2,3,7,5-TCDDt°t 1 Rack bass 10 147-194 ND(0.085) I Rock bass 10 185-208 ND(0.10) RM 64.5 Redbreast sunfish 10 147-182 ND(0.075 RM 64.5 Redbreast sunfish 5 148-203 ND(0.12) Black redharse 6 365-441 1.4 Black redhorse 10 365410 ND(0.80) 2 Redbreast sunfish 10 180-220 0.72 2 Redbreast sunfish 10 168.206 ND(0.27) RM 59.0 Redbreast sunfish 10 178-220 ND(0.38) RM 59.0 Redbreast sunfish 10 140.191 ND(0.15) 'I Common carp 10 486-581 9.3 Common carp 10 462-620 3.1 3 Redbreast sunfish 10 175-200 ND(0.34) 3 Redbreast sunfish - 10 155-210 ND(0.27) " RM 52.3 Redbreast sunfish 30 183-200 ND(0.29) RM 52.3 Redbreast sunfish 7 180-213 ND(0.36) Common carp 10 43B-600 4 Common carp 10 440.576 3.4 4A Black crappie 10 153-232 ND(0.094) 4A Black crappie 10 178-201 ND(0.15) RM 41.5 Black crappie 10 177-224 ND(0.10) RM 41.5 Black crappie 10 182-204 ND(0.089) Common crap 10 492-622 29 Common carp 10 525.611 19 4B BluegiR 10 182-212 ND(0.23) 4B Largemouth bass 10 190-310 ND(0.12) RM 39.0 Largemouth bass 5 215332 ND(0.19) RM 39.0 BluegiR 10 185-210 ND(0.20) Common carp 10 558-640 51 Common carp 10 530.644 28 5 Redbreast sunfish 10 175,245 ND(0.38) 5 Redbreast sunfish 6 180-231 ND(0.17) RM 19.0 Spotted bass 2 256-355 ND(0.30) RM 19.0 Smallmouth bass 9 212-281 ND(0.13) Smalhnouth buffalo 5 428-510 0.61 Smalhnouth buffalo 5 450.550 ND .41 Total Fish Filleted 158 162 5 l 1994 Results() 1995 Results(c) Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDDt'1 Station Species Fish Range(mm) 2,3,7,8-TCDDt°I 1 Rock bass 6 156-185 ND(0.063) 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 I50-220 ND(0.26) Black redhorse 3 367-435 ND(0.096) Black redhorse 7 375A64 ND(0.21) 2 Redbreast sunfish 10 176-206 ND(0.073) 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 10 490-590 0.99 Comon carp 10 435-664 1.7 3 Redbreast sunfish 10 149.196 ND(0.15) 3 Redbreast sunfish 10 170-206 ND(0.18) RM 52.3 Redbreast sun 10 158-210 ND(0.074) RM 52.3 Redbreast sunfish 10 154-202 ND(0.20) Cotnnton carp l0 456-565 0.74 Common carp 10 391-571 1.2 4A Black cripple 10 203-231 ND(0.085) 4A Largemouth bass 5 281-439 2.0 RM 41.5 Bluegill 10 185-205 ND(0.084) RM 41.5 Bluegill 10 167-199 ND(0.26) Common cazp 10 465-591 3.4 Common tarp 10 520.615 5.8 4B Black crappie 10 200-215 ND(0.084) 4B Largemouth bass 9 248-391• 0.68 RM 39.0 Black crappie 10 195-220 ND(0.062) RM 39.0 Bluegill 8 158-216 ND(0.34) Common cup 10 520-635 6.6 Common tarp 4 532-626 11.0 5 Redbreast sun0sb 6 129489 ND(0.075) 5 Smallmouth bass 9 280-423 ND(0.1]) RM 19.0 Smallmouth bass 9 234-442 ND(0.11) RM 19.0 Redbreast sunfish 7 163-192 ND(0.15) Smallmouth buffalo 9 440-520 ND 0.089 Black redhorse 7 440481 N➢(0.45) Total Fish Filleted 163 156 l 1996 Results(b) 1997 Resultsv i Number of Length Number of Length Species Fish Range(ram) 2,3,7,8-TCDDt°t StationSpecies Fish Range(mm) 2,3,7,8-TCDD(°) 1 Redbreast sunfish 5 154-I85 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 redlimse 4 291.424 ND(0.22) 2 Redbreast sunfish 5 179-187 ND(0.10) 2 Redbreast sunfish 5 183-200 ND(0.26) RM 59.0 Redbreast sunfish 5 193-191 ND(0.12) RM 59.0 Redbreast sunfish 5 160.181 ND(0.12) Common carp 5 543-580 1.5 Common carp 5 506-615 1.4 3 Redbreast sunfish 5 184-190 ND(0.13) 3 Redbreast sunfish 5 187-202 ND(0.18) RM 52.3 Redbreast sunfish 5 165-185 ND(0.13) RM 52.3 Redbreast sunfish 5 164-195 ND(0.18) f1 Common carp 5 516-630 0.87 Common carp 5 450.505 ND(0.33) 4A Black crappie 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 4.2 Common carp 5 570.655 2.3 Charnel catfish 5 418-482 2.0 4B Black crappie 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(0.17) ' Common carp 5 470-623 4.0 Common carp 5 605-690 11.0 Flathead catfish 5 430540 0.62 1 5 Rock bass 4 169-186 ND(0.077) 5 Rock bass 5 143-214 ND CO.15) RM 19.0 Smallmouth bass 5 315.454 ND(0.12) RM 19.0 Smallmouth bass 5 Smallmouth ND(0.27) nouth buffalo 5 451-555 ND 0.12) Smalimcuth buffalo 5 278-367 ND(0.22 Total Fish Filleted 89 Total Fish Filleted 99 1 1998 ResultsP) 1999 Resultso'l Number of Length Station Species Fish Range(ram) 2,3,7,8-TCDDt't Station Species Number of age(�) 2,3,7,8-TCDD(0 1 Redbreast sunfish 5 145-176 ND(0.19) 1 Redbreast sunfish 5 141-177 ND(0.21) RM 60..5 Rock bass 5 158-179 ND(0.29) RM 64.5 Rock bass 5 164-180 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(p.29) Common carp 5 551-661 1.3 Common carp 5 544-615 ND(0.27) 3 Redbreast sunfish 5 168.193 ND(0.34) 3 Redbreast sunfish 5 169-169 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 5 220-2fi8 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 585fi21 1.6 Common carp 5 574-645 0.58 Channel catfish 5 416-058 ND(0.28) Chanel catfish 5 475-482 0.83 4B Black crappie 5 233.252 ND(0.15) 4B Black crappie 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 5 563-696 9.1 Common carp 5 621.680 4.7 Flathead catfish 5 414-523 ND(0.20) Flathead catfish 5 372-513 ND(0.46) 5 Rock bass 4 155-190 ND(0.11) 5 Rockbass 5 170-203 ND(029) RM 19.0 Smallmouth bass 5 295-365 ND(0.21) RM 19.0 Smallmouth bass 5 297-430 ND(0.19) Smallmouth buffalo 5 464-537 ND 0.31 Smallmouth buffalo 5 476.565 ND 0.31 Total Fish Filleted 99 Total Fish Filleted 100 bN b� rAY NW bN �r o O O W1 (�(]lA 41 FAO N � o T!O m W `Jb m m pO VdA pO t� II10.'c7 �Sl aCJ �yq w�b'o � Nq �j g M � ti C. N Z e b N N U N A U U N A N U NUN U U N U N N S W n a ANi+ AU�N AN �JN Mr Nr W rr NOJ W U W O Q UO�W N J WHO Nr W W W.PuAA �Db� N�Q QT W 000 O�WW oNor � zz zz '�z zz zz zz '�z zz t7�C C>CO C�-OO 3G O 000 CYC z C'�' w Wvv to to �yS iyy yy 2y1 � O O N W O U y si 9�m n n � 91 � �r n g 0 7i e pez 8 C� O �^ JA O�oa N p jQU' A W_ [pores tAA VI W A V, F Oa O J lJ Gt W N U tUll O YO zz ZZ O yO O O O �t H n 0 c 2002 Resultsto 21103 Resultst"t . Number of Length Number of Length Station Species Fish Range(ow) 2,3,7,8-TCDDt4 station Species Fish Remge(mm) 2,3,7,8-TCDDW I Black redhorm 5 372-431 ND(0.14) 1 Black redhorse 5 343-420 ND(0.20) RM 64.5 .RM 64.5 RM 59.0 Common carp 5 517-548 ND(0.28) 2 Common carp 5 512-584 ND(0.18), RM 59.0 3 Common carp 5 575-632 ND(022) 3 Common carp 5 545.605 ND(0.31). RM 52.3 RM 52.3 4A Common carp 5 523548 2.2 4A Common carp 5 655-717 3.4 RM 41.5 Channel catfish 5 425475 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 5 418-505 ND(0.22) RM 39.0 Flathead catfish 5 511-533 ND(DL-0.20) 5 Black redhorse 5 430-489 ND(0.14) 5 Black redhorse 5 445-524 ND(DL=0.19) RM 19.0 RM 19.0 i Total Fish Filleted 40 Total Fish Filleted 40 2004 Resultsw Number of Length Station Species Fish Range(mm) 2,3,7,8 TCDDM 1 Black redhorse 5 352-440 ND(0.11) RM 64.5 2 Common carp 5 545-668 ND(0.19) RM 59.0 Channel catfish 5 369-453 ND(0.17) 3 Common carp 5 587-609 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 5 570-660 1.6 RM 39.0 Channel catfish 5 485-542 ND(0.31) RM 5 19.0 Black redhorse 5 420480 ND(0.13) Total Fish Filleted 40 (a) Survey conducted by EA Engineering,Science,and Technology. Analyses conducted by ENSECO Laboratories 1990-1994,Quanterre Laboratories 1995-1999,Severn Trent Laboratories in 2 2003. (b) Survey conducted in August. (c) Survey conducted in August and September. (d) Survey conducted in September. (e) Units=Plu(parts per trillion)or P818(Picogrem Per gram) ND=Non-detectable at the detection limit in paremheses. 1i 1 r aoF IA rE9P Michael F.Easley,Governor William G.Ross Jr.,Secretary \0 G North Carolina Department of Environment and Natural Resources y r Alan W.Klimek,P.E.Director —{ Division of Water Quality (7 'C Coleen H.Sullins,Deputy Director _v utility - June 6,2006 AN 1 Mr. Paul S. Dickens Manager,Environmental Affairs BLUE RIDGE PAPER PRODUCTS RIC Blue Ridge Paper Products BHS OEPARTMENT P.O. Box 4000 Canton,North Carolina 28716 Subject: Revisions to Dioxin Monitoring Plan Blue Ridge Paper Products NPDES No.NC0000272 Dear Mr.Dickens: The Water Quality Section has reviewed your request for modifications to the subject study plan originally approved by the Division of Water Quality in February 1990. The 2001 dioxin fish tissue monitoring plan is approved with the following changes: o Elimination of main stem river sampling stations -beginning in 2006 fish tissue samples will be collected only from Waterville Lake. o 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. o 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 John Crutchfield—Progress Energy ��� VC-100 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 MIDGE "V 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 hic. 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 f6llowed the 2001 Study Plan for the 2005 dioxin in fish sampling and report. The 2005 report was submitted to the DWQ on 20 Feb 2006. 175 Main Street o PO Box 4000 Canton, North Carolina 28716 o 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 in2000 and have remained below analytical detection levels since that time. Dioxin fish tissue sample concentrations in sport fish species from all sampling locations in the Pigeon River became non- detect in the mid-1990s. Based on annual fish tissue sampling, the State of North Carolina lifted the dioxin in fish advisory for the Pigeon River upstream of Waterville Lake in August 2001. The State of Tennessee lifted the dioxin in fish advisory for the Tennessee portion of the Pigeon River in January 2003. The only fish advisory remaining is for carp in Waterville Lake. Dioxin levels in carp collected from Waterville Lake since 2000 continue to be at or near analytical detection levels and are below the North Carolina Department of Health and Human Services (NC DHHS) dioxin toxicity equivalent(TEQ)fish advisory action level of 4 parts per trillion(ppt). The NC DHHS has indicated that two consecutive years of TCDD TEQ levels in carp of 3 ppt or less would provide basis for lifting the public health advisory for consumption of carp from Waterville Lake(e-mail correspondence from Dr. Luanne Williams, DHHS to Blue Ridge Paper dated 9 Mar 2006). The TCDD TEQs for carp fillet composite samples from Stations 4A &4B in Waterville Lake for the last two years are as follows: Year Station 4A Station 4B 2004 2.5 ppt 2.2 ppt 2005 2.1 ppt 3.6 ppt Study Plan Revision Blue Ridge Paper proposes the following changes to the 2001 biological monitoring Study Plan: o 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 o PO Box 4000 Canton, North Carolina 28716 o 828-646-2000 Raising Your Expectations Mark Hale, NC DENR DWQ, ESS- 3/30106, Page 3 o 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 dickers@blueridgeoauer.com roeere@blueridgepaaper.com Enclosures: Study Plan Revision,Dioxin Monitoring in Fish Tissue— Waterville Lake March 2006 Prepared by University of Tennessee for Blue Ridge Paper Products Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue December 2001 Prepared by EA Engineering for Blue Ridge Paper Products cc(w/enclosures): Bryn Tracy- NC DENR DWQ, ESS Susan Wilson—NC DENR DWQ,Permits Sergei Cherinkov—NC DENR DWQ Permits Roger Edwards—NC DENR DWQ ARO I{eith 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 o PO Box 4000 Canton, North Carolina 28716 o 828-646-2000 Raising Your Expectations BLUE RIDGE COPY PAPER PRODUCTS RD UCTS INC. STUDY PLAN REVISION DIOXIN MONITORING V1 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 I{noxville,Tennessee March 2006 Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake 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 under conditions of the NPDES permit for the mill. This monitoring for years 2002 thru 2005 was in accordance with the December 2001 Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue prepared by EA Engineering, Science and Technology(EA 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: o 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(Ictalurus 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 Papei Products Inc.Canton Mill Page 2 each year is dependent on physical river conditions and the natural diversity and abundance of target fishes at each location. The field investigators will be equipped with an array of collecting gear, which will enable sampling of all habitats regardless of river conditions. The US EPA recommends active methods of fish collection in the Sampling Guidance Manual (Versar 1984), such as electrofishing, trawling, angling, or seining. These are preferred over passive methods (e.g., gill nets,trap nets, trot lines) because samples are collected from more defineable areas (Versar 1984). Electro- fishing may be used at both locations (4A and 413); 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 413) 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(413). In summary, fish tissue samples will be collected as follows: o bottom-feeder composite—one composite bottom feeder fillet sample at each location 4A and 413 © 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 413) which meet the species/size objectives discussed earlier. All specimens retained will be immediately placed on ice for later processing. All fish submitted for tissue analysis will be measured to the nearest millimeter(TL) and weighed to the nearest gram(wet weight). Following collection of channel catfish and common carp, each specimen will be prepared for shipment and analysis. Samples will consist of epaxial muscle tissue and skin from one side of the fish. Fillet samples will be prepared by removing scales (or removing the skin from Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 3 catfishes) and then malting 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 Severn 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 chlotodibenzo dioxin and furan (CDD/F) isomers included in EPA Method 8290. The TEQ of each detectable isomer will be calculated based on the toxicity equivalent factor(TEF) for the isomer provided by the World Health Organization(WHO 1997). The measured concentration of each CDD/F isomer will be multiplied by its appropriate TEF to obtain a concentration of the isomer equivalent to the toxicity of 2,3,7,8-TCDD, the most toxic of the CDD/F isomers. Non- detectable concentrations will be treated as zero values for TEQ calculation. As requested by the Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 4 NC DHHS (Williams 2006), the TEQ results for the last two years will be presented in a columnar, side-by-side format to allow easy comparison against health advisory action levels. References EA Engineering,Science,and Technology Inc. 1990. Study Plan for the Monitoring of Dioxin in Fish Tissue. EA Report No. 11370.01,prepared for Champion International Corporation, Canton, North Carolina. EA Engineering,Science,and Technology Inc. 1991. Results of the 1990 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.02,prepared for Champion International Corporation,Canton,North Carolina. EA Engineering,Science,and Technology Inc. 1992. Results of the 1991 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.03,prepared for Champion International Corporation, Canton,North Carolina. EA Engineering,Science,and Technology Inc. 1993a. Results of the 1992 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.05,prepared for Champion International Corporation,Canton,North Carolina. April. EA Engineering,Science,and Technology Inc. 1993b. Results of the 1993 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.06,prepared for Champion International Corporation, Canton, North Carolina. December. EA Engineering,Science,and Technology Inc. 1994. Results of the 1994 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.07,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 1995. Results of the 1995 Dioxin Monitoring in Fish Tissue. EA Report No. 13043.01,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 1996. Results of the 1996 Dioxin Monitoring in Fish Tissue. EA Report No. 13176.01,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 1997. Results of the 1997 Dioxin Monitoring in Fish Tissue. EA Report No. 13353.01,prepared for Champion International Corporation,Canton,North Carolina. November. EA Engineering,Science,and Technology Inc. 1998. Results of the 1998 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2000. Results of the 1999 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01,prepared for Champion International Corporation,Canton,North Carolina. January. ! EA Engineering,Science,and Technology Inc. 2001a. Study Plan for Pigeon River Dioxin Monitoring in Fish tissue. Prepared for Blue Ridge Paper Products,Canton,North Carolina. November. Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 5 EA Engineering,Science,and Technology Inc. 2001b. Results of the 2000 Dioxin Monitoring in Fish Tissue. EA Report No. 13745.01,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2001c. Results of the 2001 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.01,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2003. Results of the 2002 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.02,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2004. Results of the 2003 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.03,prepared for Blue Ridge Paper Products, Canton,North Carolina. January. Henry,A.G. and J.L.Wilson. 2006. Results of2005 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). Versar,Inc. 1984. Sampling Guidance Manual for the National Dioxin Study. U.S.Environmental Protection Agency. EPA Contract 68-01-6160. Work Order Number 8.7. Office of Water Regulations and Standards,Monitoring and Data Support Division,Washington,D.C. Final Draft. July. Williams, L. 2006. E-mail correspondence from North Carolina Department of Health and Human Services to Blue Ridge Paper Products concerning review of 2005 Dioxin Monitoring in Fish Report, March 9. World Health Organization(WHO). 1997. Exposure and Human Health Reassessment of 2,3,7,8- Tetrachlorodibenzo-p-dioxin(TCDD) and Related Compounds: Part II Health Assessment of 2,3,7,8-Tetrachlorodibenzo-P-dioxin(TCDD and Related Compounds. copy y EA Project 13900.01 STUDY PLAN FOR PIGEON RIVER DIOXIN MONITORING IN MSH 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 Oecember2001 TABLE OF CONTENTS Page 1..........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-- (19.3j ,,Hartford,TN TENNESSEE N NORTH CAROLINA N �t0 Hydro Plant i( (26.0) Ile °f �x gnyG Walters Dam— B Station 46 Station 4A RM 39.0 RM 41.5 4 Waterville Lake Fines Greek New Hepro Bridge FLOW Jonathans 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 Outfall a RM 50.4 f`r�GtaaF Clyde Station 1 1 RM 64.5 (Control) Figure 2-1. Fish tissue sampling station locations on the Pigeon River. TABLE2-1 PIGEON RIVER SAMPLING STATIONS Station River Station Location and Number Mile Distance from Ontfall Site De c' ti n/Nab'ml Tyne Fish Community 1 64.5 Pigeon Riverupstream from Canton, Characterized by rifle,ran,and pool habitats. Maximum Relative abundance dominated by minnows and darters. River ' NC,adjacent to Canton Recreational depth approximately 6 ft. Substrate primarily cobble and chub,greenfin darter and rock bass arc dominant. Nonhem hog Pak(1.2 RM upstream from Canton boulders interspersed with gravel and sand. sucker,black redhorse,mimar shiner,redbreast sunfish,central Mill outfal0. stoneroller,greenside darter,and mottled sculpin are common. 2 59.0 Pigeon River upstream from Clyde,NC Characterized by riffle,run,and pool habitats with canopy Relative abundance dominated by redbreast sunfish,central (43 RM downstream from the Canton rover. Maximum depth approximately 5 R. Substrate stoneroller,and northern hog sucker. Mill outfall). primarily cobble/gravelisand with some boulders and bedrock. 3 52.3 Pigeon River in the vicinity of the Rt. Characterized by riffle,ran,and pool habitats with some Redbreast sunfish,northern hog sucker,and common carp arc 209 bridge(11.0 RM downsmaum canopy cover. Maximum depth approximately 5 ft dominant. Central stoncroller is common. from the Canton Mill ourfall) Substrate primarily bedrock and boulders with some cobble and sand(gravelffmcs deposited in pool areas. 4A 41.5 Upper Waterville Lake(21.8 RM Characterized by deep•water]mile habitat,bedrock, Relative abundance dominated by black cmpphe Bluegill, downsneam from the Canton Mill and soft bottom sediments. Maximum depth sampled flathead catfish,channel catfish,largemouth bass,and common outfail) approximately 14 ft. carp are common. 4B 39.0 Lower Waterville Lake(24.3 RM Characterized by deep-water lentie habitat,bedrock, Relative abundance of catch dominated by black crappie. downstream from the Canton Mill and soft botrom sediments. Maximum depth sampled Bluegill,channel catfish,flathead catfish,and carp are common. outfalp approximately 40 ft Very steep banks with little cover. 5 19.0 Pigeon River near Bluffton,TN,just Characterized by deep pools and runs with some shallow Central stoneroller and northern ling sucker am dominant. upstmam of 140(443 RM downstream rifles. Maximum depth approximately 6 to 8 ft. Substrate Smzlimouth bass,whitetail shiner,telescope shiner,grecaside from the Canton Mill outfall) primarily bedrock,boulder,and cobble. darter,and banded sculpin are common. Except for smallmouth bass and rock bass,centrachids are uncommoon. I 3. FISH COLLECTION TECHNIQUES AND TARGET SPECIES A listing of the Pigeon River fish collection techniques is provided below: Station Number River Mile Sampling Technique 1 64.5 Electrofishing 2 59.0 Electrofishing 3 52.3 Electrofishing 4A 41.5 Gill nets 4B 39.0 Gill nets 5 19.0 Electrofishing Except in Waterville Lake,the principal sampling gear will be electrofishing. Depending on depth,either a pram or boat electrofisher will be used. Gillnetting is the most effective technique for the collection of bottom-feeder species from the Waterville Lake monitoring stations. Gill nets will be checked at least once a day,usually within 12 hours of being deployed. Other appropriate sampling techniques may be used if necessary. Field notes will be recorded at each sampling station including the type of sampling gear,level of effort(time),flow and clarity conditions, and selected physiochemical data(e.g., dissolved oxygen,water temperature,and conductivity [electrofishing 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 413, with northern hog sucker and black redhorse as alternative species in the riverine portion of the river below the mill(i.e., Stations 2 and 3). Common carp are absent at Stations 1 and 5. At these stations, black redhorse will be the target bottom feeder, with northern hog sucker and smallmouth buffalo being alternative species. Alternative representative bottom feeder species may be collected in the rare event that these target species are not collected. In Waterville Lake, one additional fillet composite sample using either channel catfish or flathead catfish will be collected at Stations 4A and 4B. Catfish are rare in the river between the mill and Waterville Lake. However,in the event that three or more catfish of a similar size are encountered at either Stations 2 or 3, a catfish fillet composite will be prepared for either or both of these stations. In addition to the fillet composites, a whole body composite consisting of 3-5 similarly sized common carp will be collected at either Station 4A or 4B in Waterville Lake. 5 Table 3-1 Fish Collection Techniques Station Number Station Location Sampling Technique 1 Pigeon River Mile 64.5 Electrofishing 2 Pigeon River Mile 59.0 Electrofishing 3 Pigeon River Mile 52.3 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: o 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 Station 4A or 4B o Catfish fillet composite—one sample at Stations 2 and at 3, if specimens are encountered 7 4. SAMPLE PREPARATION Fillet samples will consist of the epaxial muscle tissue from one side of the fish. The fillet from the other side will be retained as a backup until laboratory results are obtained. Bottom feeder whole-body samples will consist of the entire fish. Specimens collected will be rinsed in site water, stunned with a sharp blow to the head and placed on wet ice until processing.Each fish selected for analysis will be weighed and measured. Fillet samples will be prepared by removing all scales (or removing skin from catfishes)and subsequently making an incision behind the opercula(on both sides of the fish)from the base of the spine(behind the skull)to just below the pectoral fin. Care will be taken to not puncture the gut lining. A second incision will be made along the length of the spine to the caudal fin on both sides of the fish. The epaxial muscle will then be gently cut away from the rib cage to obtain a fillet. In this fashion, all flesh and skin(except catfishes)will be obtained from head to tail. The fillets from specimens comprising a particular composite will be combined, then the sample will be wrapped in aluminum foil(dull side toward sample),placed in a water-tight plastic bag,labeled (see Section 6), and placed on wet ice. Within 24 hours of processing, the samples will be frozen. 8 5. ANALYSIS OF FISH TISSUE SAMPLES Samples will be analyzed for dioxin using EPA Method 8290 (U.S. EPA 1994). Percent lipids will also be determined for each sample. The laboratory will measure the concentration of 17 isomers of chlorodibenzo dioxins and furans (CDD/F). The toxic equivalent(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. 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_ o Sample identification number, o Station identification, o Sampling team initials, o Date of sample collection, c Species name, o Sample type(i.e.,fillet or whole body) o A unique composite number Chain-of-Custody(COC) sheets will be completed following sample preparation and compositing. The composite identification number and corresponding number and type of fish comprising that composite sample will be recorded on the COC. Copies of all COCs will be retained. Following completion of sampling,samples will be shipped on dry ice to the analytical laboratory via an overnight courier. Upon receipt,the laboratory will compare the contents with that noted on the COC sheets and will note the condition of the samples. . 10 7. PROJECT SCHEDULE To be consistent with past collections, all samples will be collected in August or September. A final report will be provided to NCDEQ within 180 days of sampling. 11 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 Dibenzofarans 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-Tetrachlorodibenzo-p-dioxin(TCDD) and Related Compounds: Part II Health Assessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin(TCDD)and Related Compounds. 13 �oF WArF9Q Michael F.Easley,Governor William U.Ross Jr.,Secretary rNorth Carolina Depaumont of Environment and Natural Resources � 1 O Y Alan W.Klimek P.E.Director Division of Water Quality March 8, 2007 Mr. J. Glen Rogers Water Compliance Coordinator Blue Ridge Paper Products P.O. Box 4000 Canton, North Carolina 28716 Subject: Review of 2006 Monitoring Report for Dioxin in Fish Tissue. Blue Ridge Paper Products NPDES No. NC0000272 Dear Mr. Rogers: The Division's Environmental Sciences Section has reviewed the Blue Ridge Paper Products 2006 dioxin fish tissue monitoring results for Waterville Lake, resulting in the removal of the fish advisory for carp along the Pigeon River. The declining trend of TCDD concentrations in reservoir fish is certainly good news for water quality in the Pigeon River. The 2006 results highlight this trend in Waterville Lake, and justify the removal of carp from the Pigeon River fish advisory. However, in order to maintain accordance with the existing DHHS protocol,we agree that sampling and dioxin contamination analysis of carp from Waterville Lake(at station 4A or 4B)should continue through 2007 and 2008. Please feel free to contact Jeff DeBerardinis at 919-733-6946 with any questions or comments. Sin ely, q I . Chief, Environmental Sciences Section cc: Mark Hale—ESS Roger Edwards—ARO Dr. Luanne Williams—NCDHHS Susan Wilson—DWQ Permits John Crutchfield—Progress Energy NorrthCarolina Ivl1t' r-711rf North Carolina Division of Water Quality 1621 Mail Service Center Raleigh,NC 27699-1621 Phone(919)733-6946 Internet h2o.emstate.nc.us 4401 Reedy Creek Rd, Raleigh,NC 27607 FAX (919)733-9959 An Equal OpportunitylAfhrmative Action Employer—0%RecydedflO%Post Consumer Paper d YST�e - North Carolina Department of Health and Human Services Division of Public Health •Epidemiology Section 1912 Mail Service Center•Raleigh,North Carolina 27699-1912 Tel 919-707-5900•Fax 919-870-4810 \lichael P.liasley,Governor Cnonen Ilooker Odom,Secretary June 14, 2007 Mr- Cecil Gurganus, Manager D Hydro Operations D Progress Energy Carolinas, Inc. Tillery Hydroelectric Plant JUN 2 2 2007 179 Tillery Dam Road Mt. Gilead,NC 27306 BLUE RIDGE PAPER PRODUCTS INC OHS DEPARTME14T Dear Mr. Gurganus: SUBJECT: Walters Hydroelectric Project No. 432—Walters Lake 2006 Annual Dioxin Monitoring Report The North Carolina Department of Health and Human Services (NC DHHS) has reviewed the Walters Lake 2006 Annual Dioxin Monitoring Report and has no comments on the submitted report. In January 2007, the NC DHHS totally rescinded the existing dioxin fish consumption advisory for colunion carp at Walters Lake based on dioxin fish data submitted by Blue Ridge Paper Products, Inc. and Progress Energy. This rescission is the last step in removal of the dioxin fish consumption advisory that was enacted by the NC DHSS for the Pigeon River, North Carolina, including Walters Lake, in 1988. Based on discussions with Mr. John Crutchfield, Progress Energy, the following sampling protocol will be needed following the rescission of the dioxin fish advisory. These recommendations are based on the NCDHHS protocol for issuing dioxin fish consumption advisories in North Carolina: 1. Conduct two additional years of monitoring (2007 and 2008) to determine if dioxin levels in coimnon carp muscle tissue remain below the consumption advisory threshold of 4 parts per trillion Toxic Equivalent Value (TEQ). 2. Continue to sample common carp at Transects D (Pigeon River Mile 39.0) and G (Pigeon River Mile 41.5) in Walters Lake during November of each year(see Figure 1). 3. Collect 4 composites comprised of 5 fish per composite with preferably 2 composites from Transect D and 2 composites from Transect G. However, if there is an insufficient number of fish collected at either transect to complete a composite, a composite can be mixed with fish from either transect to complete the 5 fish per composite. 'Protocol for Issuing Fish Consumption Advisories due to .,Chlorinated Dibenzo-p-dioxins (CDDS) and Clilorinated Dibenzo-p-furans (CDFs) Found in Fish. Prepared by Luanne K. Williams, Pharm.D., Toxicologist Occupational and Environmental Epidemiology Branch, North Carolina Department of Health and Human Services September 20,2006. ® Ltru 60W 5505 Six Pork's Road.2 t Moor,Ronm DI • Rnlcigh.N.C.217609 An liyual Opportunity Finploycr ..........-I........ . ........ .......................... 4. Perform laboratory analysis of all 17 congeners of dioxins and furans including the calculated TEQ values. Use the revised World Health Organization(WHO)Toxic Equivalent Factors (TEF) for determination of TEQ ValUeS.2 5. Arithmetic mean TEQ of less than 4 pg/g must be achieved in each year sampled with the arithmetic mean TEQ calculated from the Progress Energy and Blue Ridge data sets. 6. If the arithmetic mean TEQ is equal to or exceeds 4 pg1g during each year, then further monitoring may be required based on input and recommendations from NC DHHS and N.C. Division of Water Quality (NC DWQ). 7. All other sampling procedures will follow that outlined in the revised dioxin sampling protocol submitted by Progress Energy to NC DHHS and NC DWQ dining October 20013. If the post advisory monitoring requirements are satisfied(i.e., two consecutive annual data sets with arithmetic mean value of less than 4 ppt TEQ, then the NC DHHS will consider that no additional monitoring of fish from Walters Lake will be necessary for the dioxin consumption advisory requirement. If you have any questions regarding this post advisory monitoring protocol, please call me at (919)707-5912. ShIperely, Dr.Luanne K. Williams,Toxicologist NC Department of Health and Human Sei vices LICW/bc cc: Mr. John Crutchfield-Progress Energy Mr. Paul Dickens-Blue Ridge Paper Products,Inc. Mr. Patricia MacPherson-NC DWQ Mr. Jimmie Overton-NC DWQ '-World Health Organization (WHO) 2005. The 2005 World Health Organization Re-evaluation of Human and Mammalian Toxic Equivalency Factors for Dioxins and Dioxin-like Compounds. lkfl055Toxicological Sciences,doi:10.1093/toxsci. -'CP&L—A Progress Energy Company. 2001. Revised protocol for determining the concentration of dioxins and furans in fish tissues from Walters Hydroelectric Project, FERC Project No. 432, Article 409 of the Walters Hydroelectric Project License. Tunnel Pigeon River Intake 4;; River Mile 38.0 a#,Matters Hydroeleclnc ., -%, Plant, r } Dam _s NORTH CAROLINA «' Cataloochee Creek River Mile 39.0 D Wilkins Creek i N River Mile 40.0 T� Fl.ow River Mile 41.25 New Hepco G Bridge River Mile 41.5� 0 400 800 MI—ete� 0 1200 2400 Pigeon River Feet Figure 1. Location of Progress Energy dioxin monitoring stations on Walters Lake, North Carolina. Michael F. Easley Carmen Hooker Odom way Governor " ! Secretary y" North Carolina Department of Health and Human Services For Release: IMMEDIATE Contact: Debbie Crane Date: January 9, 2007 State Removes Last Fish Consumption Advisory Below Canton Paper Mill RALEIGH—State Health Director Leah Devlin today announced the removal of the last remaining fish consumption advisory below the Blue Ridge paper mill in Haywood County. Today's announcement is the final chapter in a situation that first came to light in the late 1980s, when byproducts of the paper production process led to fish consumption advisories in the Pigeon River and the Walters Lake Reservoir. "This is both a public health and an environmental success story," said Devlin. "It is a good example of an industry addressing a potential public health problem by changing its processes. I'm pleased we can close the book on this one." The original advisory was issued by the State Health director in 1988. It warned against consumption of any fish from below the then Champion International paper mill. In 1994, that advisory was reduced to cover only carp and catfish. hi 2001, it was reduced still further to just a limited advisory on carp in Walters Lake, which is also known as the Waterville reservoir. The advisory was originally issued because of high levels of dioxin found in fish taken below the paper mill. Dioxin is a byproduct of chlorine bleaching. Studies have shown that exposure to dioxin increases the risk of several types of cancer in animals and humans. The most common health effect in people exposed to large amounts of dioxins is chloracne, which is a severe skin disease, fr- characterized by large, deep acne-like lesions. Some other effects include liver damage and changes l in hormonal levels. Improved pollution controls at the Canton paper mill were enacted during the late 1980s. The �_- Canton mill, formerly owned by Champion International, was purchased by mill employees and renamed Blue Ridge Paper Products Inc. in 1999. More information on fish consumption advisories in North Carolina can be found at http://www.epi.state.ne.us/et)i/fish/. 1f1� Public Affairs Office Debbie Crane 101 Blair Drive, Raleigh, NC 27603 Director (919)733-9190 FAX(919)733-7447 r Walters Hydroelectric Plant Federal Energy Regulatory Commission Project No. 432 Dioxin and Furan Concentrations in the Axial Muscle Tissue of Fish from Walters Lake,November 2007 i Environmental,Health and Safety Services Section Progress Energy Carolinas,Inc. Raleigh, North Carolina March 2008 Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report r' Preface This copy of the report is not a controlled document as detailed in the Environmental, Health and Safety Services Section Biology Program Procedures Manual and Quality Assurance Manual. Any changes made to the original of this report subsequent to the date of issuance can be obtained from: Director Environmental,Health and Safety Services Section(EH&SS) P.O. Box 1551 Raleigh,North Carolina 27602-1551 r' Progress Energy Carolinas, Inc. 1 EHBSS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report 2007 Walters Project Dioxin Monitoring in Fish Tissue Introduction Progress Energy, previously known as Carolina Power and Light Company (CP&L), conducted the annual dioxin and furan monitoring program in 2007 for fish tissue at the Walters Hydroelectric Project as required by the Federal Energy Regulatory Commission's (FERC) license for the Project (Article 409). The monitoring program was initiated in 1991 during relicensing of the Project and was incorporated into the operating license issued by the FERC in November 1994. The monitoring program has been conducted to provide the environmental regulatory agencies of the State of North Carolina with sufficient data on which to maintain, modify, or rescind the fish consumption advisory, which became effective in June 1988. The North Carolina Department of Health and Human Services (NCDHHS) modified the original advisory in September 1994 to allow consumption of all species of fish except common carp and catfish species. In August 2001, the advisory was totally rescinded for common carp and catfish species in the Pigeon River. In Walters Lake, the advisory was partially rescinded to include only common carp. Catfish species were dropped from the monitoring program in 2004 based on dioxin concentrations below the NCDHHS threshold for Toxicity Equivalent (TEQ) values of 4 picograms per gram (pg/g) for two consecutive monitoring years (Williams 2004). These changes to the dioxin monitoring protocol were approved by the NCDHHS, North Carolina Division of Water Quality (NCDWQ), and the FERC (CP&L 2001). In January 2007, the NCDHHS removed the common carp consumption advisory from Walters Lake (Appendix 12). The advisory was lifted based on an overall TEQ below 4.0 pg/g calculated from a combined weighted arithmetic average TEQ using Progress Energy and Blue Ridge Paper Products, Inc. (BRPP) from the 2005 and 2006 data sets. Progress Energy and BRPP will continue their respective monitoring programs for two years after the removal of the advisory per guidance from NCDHSS and NCDWQ. If the monitoring data meet the consumption threshold criteria after the second year of post-advisory monitoring, the State of North Carolina will no longer require tissue monitoring for dioxin and furans. The data presented in this report represents the first year of the post-advisory monitoring. l Progress Energy Carolinas, Inc. 2 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report Objectives The objective of this report is to summarize dioxin and furan data from common carp collected in November 2007, as required by Article 409 of the FERC operating license for the Walters Hydroelectric Project. As also required by the license, results from Blue Ridge Paper Products, Inc.'s (BRPP, formerly owned by Champion International Corporation) sampling during August-September 2007 are included in this report (Henry and Wilson 2008). This report also presents dioxin and furan data for common carp that have been previously collected and . reported to date by the U.S. Environmental Protection Agency (EPA), Champion International Corporation/Blue Ridge Paper Products, Inc., and Progress Energy during the period from July 1991 to November 2007. Methods Transects sampled by Progress Energy in 2007 were the same as those sampled since monitoring began in 1991 (i.e., Transects D and G) (Appendix 1). Methods used during 2007 were also the same as those used in 2006 (TestAmerica Labs 2007; Progress Energy Carolinas, Inc. 2007). In September 2006,NCDHHS requested that Progress Energy use the revised World Health Organization (WHO) Toxic Equivalent Factors (TEF) for determination of TEQ values (personal communication, Dr. Luanne Williams NCDHHS; WHO 2005). These revised TEF were used in the determination of the TEQ values in this report. The laboratory analyses were conducted using standardized EPA 8290 dioxin and furan methodologies by TestAmerica Laboratories, formerly Severn Trent Laboratories, West Sacramento California. (880 Riverside Parkway,West Sacramento, California 95605). Results and Discussion On November 5-7, 2007, Progress Energy collected 18 common carp from Walters Lake during its annual dioxin and furan monitoring sampling. These fish were combined into four composites. Two of the composites consisted of five fish each and the other two consisted of four fish each (Appendix 2). The desired length range goal for fish in a composite sample (i.e., the smallest fish should not be less than 75% of the total length of the largest fish in a composite sample) was achieved for all four composites (Appendix 3). The mean length for common carp collected in 2007 was the greatest since collection began in 1991 (Appendix 4). Mean weight Progress Energy Carolinas, Inc. 3 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report was not as high as in 2006, but was the second greatest ever collected. The common carp mean lengths and weights collected by Progress Energy were lower than the mean values for common carp collected by BRPP during this same period (Appendices 4 and 5). The mean estimated age of all fish combined (17 years) collected by Progress Energy in 2007 was three years lower than the mean in 2006 but was similar to mean ages reported in previous years (Appendix 4). The mean length, mean weight and mean age of common carp collected by Progress Energy have increased since monitoring began in 1991. Larger, older common fish would be expected to have the greatest dioxin and furan concentrations, and this segment of the common carp population has been analyzed for dioxin and furan in recent years. External deformities and anomalies were noted in 12 of the 18 (67%) common carp retained for dioxin and furan analyses (Appendix 2). The overall prevalence of deformities and anomalies considering all fish species collected during sampling was 11.3% (n= 12), based on a total sample size of 106 fish. Deformities were only noted in common carp and consisted mostly of deformed opercular flaps. Composite samples of common carp collected in 2007 had dioxin (2,3,7,8-TCDD) i concentrations ranging from 0.83 to 3.4 pg/g with an overall mean concentration of 1.7 pg/g (Appendices 6-8). The mean dioxin concentration in common carp in 2007 continued the general downward trend in dioxin levels and represents the lowest mean concentration observed since Progress Energy began sampling in 1991 (Appendix 8). Furan (2,3,7,8-TCDF) concentrations in the common carp composites ranged from 2.0 to 3.4 pg/g with an overall mean concentration of 2.5 pg/g (Appendices 6-8). The mean furan concentration in 2007 was lower than the mean concentration observed in 2006 (3.7 pg/g) and was similar to mean concentrations seen within the last few years. Dioxin and furan data (2,3,7,8-TCDD and 2,3,7,8-TCDF) were also normalized on a per gram lipid basis because of the affinity of these contaminants for lipids (Appendix 9). Normalizing these data served to: (1) account for differences in lipid content of the fillets among composites and (2) adjust for seasonal changes in the contaminant concentrations (Stober 1991). The mean lipid normalized dioxin concentration of 12.5 pg/g was slightly higher than in 2006, but again demonstrated the general downward trend of the dioxin concentrations observed since sampling began in 1991. L . Progress Energy Carolinas, Inc. 4 EHBSS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report The TEQ values calculated for common carp composites collected by Progress Energy in 2007 ranged from 1.86 to 5.42 pg/g with a mean of 2.7 pg/g (Appendices 6 and 11). The mean TEQ value of 2.7 pg/g reported by Progress Energy in 2007 was lower than the mean TEQ values from 2006 (4.1 pg/g) and 2005 (6.7 pg/g) and the lowest TEQ value reported by Progress Energy since 2001. Generally, mean TEQ values have decreased since 2001 (Appendix 11). The TEQ value for the common carp composite collected by BRPP in August 2007 at River Mile 41.5 was 13.4 pg/gt. This TEQ value was the greatest value observed in 13 years of monitoring by BRPP and was attributed to very large carp with high lipid content in the composite (26% lipid). Blue Ridge intends to target fish during the 2008 sampling collection that will be comparable in size distribution to those collected from 2004 to 2006. This information will determine if there has been any significant change or trend in dioxin concentrations. It should be noted that the BRPP common carp whole body composite sample had a nondetectable level of dioxin(2,3,7,8 TCDD, estimated result of 0.75 pg/g). Summary The mean TEQ value for common carp of 2.7 pg/g collected in November 2007 was the lowest reported since TEQ values were initially reported in 2001. The mean TEQ value in 2007 was below the 4.0 pg/g TEQ value used by the NCDHHS to enact fish consumption advisories for dioxin. All dioxin(2,3,7,8-TCDD) and furan (2,3,7,8-TCDF) concentrations in common carp have decreased substantially in Walters Lake since monitoring began in 1991. The entire Pigeon River, including Walters Lake in North Carolina and Tennessee is no longer posted for any dioxin fish consumption advisories (Appendix 12). The data collected by Progress Energy in 2007 supports the rescission of the advisory and further demonstrates the favorable environmental improvements observed in the Pigeon River and Walters Lake since the early 1990s. 'Please note that the Blue Ridge laboratory results indicated the dioxin analysis for one composite sample for common carp(Station,4B,River Mile 39.0)was misleading due to a 10 fold dilution of the sample to overcome sample matrix interference effects(high lipid concentration) . The common carp composite sample results from River Mile 41.5 (Station 4A) were within acceptable laboratory reporting parameters. Therefore, only this composite sample data are presented in this report data. Progress Energy Carolinas, Inc. 5 EHBSS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report J References CP&L. 1997. Dioxin and furan concentrations in the axial muscle tissue of fish from Walters Lake,November 1996. April 1997. Carolina Power&Light Company,New Hill,NC. 2001. Revised protocol for determining the concentrations of dioxins and furans in fish tissues from the Walters Hydroelectric Project. FERC Project No. 432, Article 409 of the Walters Hydroelectric Project. CP&L—A Progress Energy Company, New Hill,NC. TestAmerica Laboratories West Sacramento. 2007. Case narrative. TestAmerica West Sacramento Project Number G6K28028. BIOLOGIC, 8290, Dioxin Furans. TestAmerica Laboratories West Sacramento, Sacramento, CA. Henry, T. B., and J. L. Wilson. 2008. Results of 2007 dioxin monitoring in fish tissue. January 2007. Center for Environmental Biotechnology, Departments of Forestry, Wildlife and Fisheries, University of Tennessee, Knoxville, Tennessee. Prepared for Blue Ridge Paper Products, Canton Mill, Canton,NC. April 2008. Progress Energy Service Company. 2006. Walters Hydroelectric Plant. Federal Energy Regulatory Commission Project No. 432. Dioxin and furan concentrations in the axial muscle tissue of fish from Walters Lake, November 2005. Progress Energy Service Company, Raleigh,NC. Stober, Q. J. 1991. Guidelines for fish sampling and tissue preparation for bioaccumulative contaminants. Draft document. Region IV, Toxics Evaluation Section, Ecological Support Branch,Environmental Services Division,U.S. EPA,Athens, GA. U.S. EPA. 1995. Guidance for assessing chemical contaminant data for use in fish advisories. Volume 1. Fish sampling and analysis. Second edition. EPA 823-R-95-007. U.S. Environmental Protection Agency, Office of Science and Technology, Office of Water, Washington, DC. Williams, L. K. 2004. Protocol for issuing fish consumption advisories due to chlorinated dibenzo-p-dioxins (CDDS) and chlorinated dibenzo-p-furans (CDFs) found in fish.North Carolina Department of Environment, Health, and Human Services, Occupational and Environmental Epidemiology Branch,Raleigh,NC. World Health Organization (WHO) 2005. The 2005 World Health Organization Re-evaluation of Human and Mammalian Toxic Equivalency Factors for Dioxins and Dioxin-like Compounds./kfl055Toxicological Sciences, doi:10.1093/toxsci. r Progress Energy Carolinas, Inc. 6 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report Tunnel,, Pigeon River Intake ;; River Mile 38.0 Walters Hydroelectric Plant Dam NORTH CAROLINA Catalooclee Creek ,River Mile 39.0 D Wilkins Creek N River Mile 40.0 Flow New Hepco G Bridge River Mile 41.5 0 400 800 MF�� 0 1200 2400 Pigeon River FIB-I Appendix 1. Sampling locations for common carp analyzed for dioxin and furan from Walters Lake,November 5-7,2007. Progress Energy Carolinas, Inc. A-1 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report j Appendix 2. Location and measurement data for common carp collected for dioxin and furan analyses from Walters Lake,November 5-7,2007. Location Composite Fish ID Collection Length Weight (river mile) number number date mm ( ) Deformity e Caudal,Left Pectoral Wavy&Fleshy 41.5 1 1921 11/5/07 608 3250 Growth on Lower Li 41.5 1 1922 11/5/07 641 3600 Wavy pectoral and pelvic fins 41.5 1 1923 11/5/07 704 5050 Cranial anomaly and opercular 41.5 1 1924 11/5/07 745 6600 depression Cranial anomaly and opercular 41.5 1 1925 11/5/07 570 2250 de ression Left Opercular Depression 41.5 2 1926 11/5/07 716 5450 41.5 2 1927 11/5/07 780 7400 Depressed Right Operculum 41.5 2 1928 11/6/07 642 3650 Depressed Right and Left Operculum 41.5 2 1929 11/6/07 588 2700 Depressed Left&Right Operculum 39.0 3 1931 11/5/07 670 4800 Asymmetrical Cranium 39.0 3 1932 11/5/07 780 8300 39.0 3 1933 11/5/07 666 4150 Depressed Right Operculum,Wavy 39.0 3 1934 11/6/07 725 6350 Left Pectoral 39.0 3 1935 11/7/07 710 5700 39.0 4 1930 11/7/07 695 4600 Wavy Left&Right Pectoral,Wavy 39.0 4 1936 10107 670 4500 Left&Right Pelvic Fins 41.5 4 1937 11/7/07 680 4700 Depressed Cranium 39.0 1 4 1938 11/7/07 705 5050 Appendix 3. Composite means and ranges (in parentheses) of the total length, weight, and estimated age of common carp collected for dioxin and furan analyses from Walters Lake,November 5-7, 2007. Composite Sample Length Desired Weight Age number size (mm) length(%)+ (9) (years) 1 5 654(570-745) 76.5 4150(2250-6600) 20(14-24) 2 4 682(588-780) 75.4 4800(2700-7400) 20(20-21) 3 5 710(666-790) 85.4 5860(4150-8300) 19(17-21) 4 4 688(670-705) 95.0 4712(4500-5050) 21 (19-23) Desired length=the minimum fish length divided by the maximum fish length x 100. Progress Energy Carolinas, Inc. A-2 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report Appendix 4. Mean total length (mm), mean weight (g), and mean estimated age (years) of common carp collected for dioxin and furans analyses from Walters Lake by CP&L/Progress Energy, 1991-2007. Year Mean length (mm) Mean weight(g) Mean age,(years) Jul 1991 511 1782 9 Dec 1991 554 2368 10 Dec 1992 545 2473 9 Nov 1993 592 2747 10 Nov 1994 557 2542 10 Nov 1995 593 3175 12 Nov 1996" 621 3633 11 Nov 1997' 618 3581 11 Nov 1998 630 3794 13 Nov 1999 599 3141 11 Nov 2000 638 3947 15 Nov 2001 634 3775 15 Nov 2002 616 3458 14 ( Nov 2003 642 3762 12 Nov 2004 626 3539 16 Nov 2005 651 4204 16 Nov 2006 665 4994 20 Nov 2007 683 4881 17 +Composite number 12 (one fish composite) from November 1996 was not included in calculations of mean values due to the stressed condition of the fish when collected. 'The mean length and weight values reported in CP&L (1997) for common carp collected in 1996-1997 were calculated from all individual lengths and weights. Mean length and weight values for all other years reported are mean values for composite mean values. Progress Energy Carolinas, Inc. A-3 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report Appendix 5. Mean total length (mm) and mean weight (g) of common carp collected for dioxin and furan analyses from Walters Lake by Champion International Corporation and Blue Ridge Paper Products, Inc. during August-September, 1991-2007.+ Year Mean length (mm) Mean weight (g) 1991 579 2808 1992 572 2725 1993 574 2759 1994 548 2593 1995 573 2487 1996 574 2554 1997 636 3711 1998 618 3781 1999 626 3403 2000 632 3796 2001 644 4246 2002 622 3882 2003 626 3414 2004 631 3825 2005 655 4276 2006 684 5071 2007 730 6521 +These data include only fish used for composite fillet analyses. Progress Energy Carolinas, Inc. A-4 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report Appendix 6. Summary of dioxin and furan isomer analyses, Toxic Equivalent Factors (TEF), and Toxicity Equivalent (TEQ) values for common carp collected from Walters Lake,November 5-7,2007. Common carp Composite 1 Composite 2 Composite 3 Composite 4 CCD/CDF Isomers TEF pg/g TEQ pg/g TEQ pg/g TEQ pg/g TEQ Dibenzodioxins 2,3,7,8-TCDD 1.0 1.2 1.2 1.3 1.3 3.4 3.4 0.83§ 0.83§ 1,2,3,7,8-PeCDD 1.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1,2,3,4,7,8-HxCDD 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1,2,3,6,7,8-HxCDD 0.1 3.3§ 0.33§ 3.3§ 0.33§ 6.4 0.64 3.7§ 0.37§ 1,2,3,7,8,9-HxCDD 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1,2,3,4,6,7,8-HpCDD 0.01 11.0 0.11 13.0 0.13 21.0 0.21 14.0 0.14 OCDD 0.0003 54.0 0.0162 46.0 0.0138 56.0 0.0168 21.0 0.0063 Dibenzofurans 2,3,7,8-TCDF 0.1 2.0 0.2 2.1 0.21 3.4 0.34 2.5 0.25 1,2,3,7,8-PeCDF 0.03 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 2,3,4,7,8-PeCDF 0.3 0.0 0.0 0.0 0.0 2.7§ 0.81§ 0.0 0.0 1,2,3,4,7,8-HxCDF 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1,2,3,6,7,8-HxCDF 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 2,3,4,6,7,8-HxCDF 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1,2,3,7,8,9-HxCDF 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1,2,3,4,6,7,8-HpCDF 0.01 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1,2,3,4,7,8,9-HpCDF 0.01 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 OCDF 0.0003 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Total TEQ" 1.86 1.98 5.42 1.60 §Estimated Maximum Possible Concentration (EMPC). The analytes abundance was lower than the reporting limit. The analytes have been reported as an "estimated maximum possible concentration"because the quantitation is based on theoretical ion abundance ratios. ¥Calculation of toxic equivalent values follows methodology from U.S. EPA(1995) and the World Health Organization(2005). Progress Energy Carolinas, Inc. A-5 EHBSS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report j Appendix 7. Concentrations of dioxin (2,3,7,8-TCDD pg/g wet weight) and furan (2,3,7,8- TCDF pg/g wet weight), percent recovery of internal standards, and percent lipids in muscle fillets of common carp collected from Walters Lake, November 5-7,2007. Composite Dioxin TCDD Furan TCDF% Lipids Species No. (pg/g) %Recovery (pg/g) Recovery (%) Common carp 1 1.2 91 2.0 87 9.2 2 1.3 93 2.1 89 11.0 3 3.4 90 3.4 85 20.0 4 0.83§ 90 2.5 86 10.0 Laboratory standards Blank 0.12+ 81 0.30+ 79 N/Al Control spike 20.0 87 20.0 83 N/A §Estimated Maximum Possible Concentration (EMPC). The analytes abundance was lower than the reporting limit. The analytes have been reported as an "estimated maximum possible concentration"because the quantitation is based on theoretical ion abundance ratios. +Not Detected. 9N/A=Not Applicable. 1 Progress Energy Carolinas, Inc. A-6 EHBSS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report `t Appendix 8. Mean concentrations of dioxin (2,3,7,8-TCDD pg/g wet weight) and furan (2,3,7,8-TCDF pg/g wet weight), in muscle fillets of common carp collected on various sampling dates from Walters Lake, 1991-2007.+ Composite sample size is given in parentheses. Collection date` Dioxin Fortin Jul 1991 9.0 (1) 1.1 (1) Aug 1991 31.5 (2) 2.4(2) Dec 1991 14.4(2) 1.5 (2) Aug 1992 40 (2) 3.1 (2) Dec 1992 12.8 (4) 1.1 (4) Aug 1993 23.5 (2) 1.9(2)- Nov 1993 11.8 (3) 2.0(3) Aug 1994 5.0 (2) 0.9(2) Nov 1994 12.2(4) 1.8 (4) Aug 1995 8.4(2) 2.0(2) Nov 1995 9.2(1) 1.7(1) Aug 1996 4.1 (2) 1.8 (2) Nov 1996 12.0(3)' 1.9 (3)' Aug 1997 6.7 (2) 2.1 (2) Nov 1997 2.7 (5) 2.0(5) Aug 1998 5.4 (2) 2.6(2) Nov 1998 5.2 (5) 2.3 (5) Aug 1999 2.6 (2) 2.2(2) Nov 1999 2.3 (3) 1.3 (3) Aug 2000 2.8 (2) 2.8 (2) Nov 2000 3.5 (5) 2.2(5) Sep 2001 3.4 (2) 2.6(2) Nov 2001 4.4(4) 3.3 (4) Sep 2002 4.4(2) 2.6(2) Nov 2002 2.5 (4) 1.4(4) Aug 2003 7.7 (2) 3.4(2) Nov 2003 2.5 (4) 2.0(4) Aug 2004 1.6 (2) 2.0(2) Nov 2004 1.9 (4) 1.2(4) Aug 2005 2.0 (2) 1.4(2) Nov 2005 2.4(4) 2.2(4) Aug 2006 0.7(2) 2.4(2) Nov 2006 2.0(4) 3.7(4) Aug 2007 0.0(1) 0.5 (1) Nov 2007 1.7(4) 2.5(4) *The arithmetic mean for each species was calculated from all data available disregarding the collection location within Walters Lake. Concentrations less than the detection limit were assumed to be at the detection limit for the calculation of the mean. `The U.S. EPA collected samples during April 1988. CP&L/Progress Energy collected samples during July 1991,December of 1991 and 1992,April 1993,and November of 1993-2007. Champion International Corporation collected samples during August of 1991-1998. Blue Ridge Paper Products, Inc. collected samples in August of 1999,2000,2003,2004, September of 2001, 2002,and August-September of 2007. 'Composite number 12 (one fish composite) in November 1996 (CP&L 1997) was not included in this mean value because of the stressed condition of the fish when collected. 'Only one composite was reported by Blue Ridge Paper Products,Inc.at the time of this report. Progress Energy Carolinas, Inc. A-7 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report Appendix 9. Lipid-normalized concentrations of dioxin (2,3,7,8-TCDD reported in pg/g lipid) and furan (2,3,7,8-TCDF reported in pg/g lipid) in muscle fillets of common carp collected from Walters Lake,November 5-7,2007.+ Composite Dioxin (2,3,7,8-TCDD) Furan (2,3,7,8-TCDF) Number (lipid-normalized) (lipid-normalized) 1 13.0 21.7 2 11.8 19.1 3 17.0 13.5 4 8.3+ 25.0 Mean of.composites 12.5 19.8 +Estimated maximum possible concentration values were used in calculation of the normalized values in those cases where only estimated values or estimated maximum possible values were given. r' r L Progress Energy Carolinas, Inc. A-8 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report-' Appendix 10. Mean lipid-normalized concentrations of dioxin (2,3,7,8-TCDD reported in pg/g lipid) and furan (2,3,7,8-TCDF reported in pg/g lipid) in muscle fillets of common carp collected on various sampling dates from Walters Lake, 1991-2007.+ Collection date` Dioxin Furan Jul 1991 204.5 25.0 Aug 1991 387.0 28.5 Dec 1991 190.6 20.3 Aug 1992 292.3 19.7 Dec 1992 336.2 23.4 Aug 1993 203.4 15.4 Nov 1993 223.7 44.9 Aug 1994 40.6 7.0 Nov 1994 143.4 23.5 Aug 1995 52.8 12.3 Nov 1995 117.9 21.8 Aug 1996 23.6 10.0 Nov 1996 109.7° 17.9* Aug 1997 41.2 14.0 Nov 1997 29.0 23.9 Aug 1998 28.5 14.7 Nov 1998 38.1 16.7 Aug 1999 17.7 17.3 Nov 1999 26.8 18.6 Aug 2000 13.7 14.2 Nov 2000 40.7 26.9 Sep 2001 21.9 17.7 Nov 2001 36.0 29.2 Sep 2002 30.4 19.3 Nov 2002 27.1 20.1 Aug 2003 37.8 19.6 Nov 2003 25.8 21.4 Aug 2004 13.7 17.0 Nov 2004 22.4 19.4 Aug 2005 21.2 14.6 Nov 2005 23.3 21.8 Aug 2006 9.8 30.3 Nov 2006 10.3 19.9 Aug 2007 e f Nov 2007 12.5 19.8 'The arithmetic mean for each species was calculated from all data available disregarding the collection location within Walters Lake. Concentrations less than the detection limit were assumed to be at the detection limit for the calculation of the mean. The number of composite samples for each species can be found listed in parentheses in Appendix 8. `The U.S. EPA collected samples during April 1988. CP&UProgress Energy collected samples during July 1991, December of 1991 and 1992, April 1993, and November of 1993-2007. Champion International Corporation collected samples during August of 1991-1998.Blue Ridge Paper Products, Inc,collected samples in August of 1999,2000,2003,2004,September of 2001,2002,and August-September of 2007. 'Composite number 12(one fish composite)in November 1996(CP&L 1997)was not included in this mean value because of the stressed condition of the fish when collected. 'These data were not available from Blue ridge Paper Products,Inc.at the time of this report. Progress Energy Carolinas, Inc. A-9 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report f ,= Appendix 11. Composite means and ranges (in parentheses) of the Toxicity Equivalent Values (TEQ) of common carp collected by Progress Energy and Blue Ridge Paper Products,Inc, for dioxin and furan analyses from Walters Lake, 2001- 2007. Number of Collection date composites TEQ (pg/g) Sep 2001 2 5.4 (2.1-8.7) Nov 2001 4 9.3 (6.1-15.4) Sept 2002 2 6.1 (2.9-9.3) Nov 2002 4 5.2 (0.7-10.0) Aug 2003 2 14.3 (8.6-20.0) Nov 2003 4 5.4(3.4-7.2) Aug 2004 2 2.4 (2.2-2.5) Nov 2004 4 4.0 (0.7-8.0) Aug 2005 2 2.8 (2.1-3.6) Nov 2005 4 6.7 (3.6-9.5) Aug 2006 2 1.2 (0.9-1.6) Nov 2006 4 4.1 (1.5-8.2) Aug 2007£ 1 13.4 Nov 2007 4 2.7 (1.6-5.4) £Only one composite was reported by Blue Ridge Paper Products, Inc. Progress Energy Carolinas, Inc. A-10 EH&SS Walters Hydroelectric Project No.432 2007 Dioxin Monitoring Report Appendix 12. NCDHSS press release,January 9, 2007. NC DHHS'release:State Removes Last Fish Consumption Advisory Below Canton Paper... Page 1 of 2 Michael F:Easley 'Carmen Hooker Odom Governor a� Secretary North Carolina Department of Health and Human Services For Release:IMMEDIATE Contact:Debbie Crane Date:January 9,2007 State Removes; Last Fish Consumption Advisory Below Canton Paper Mill RALEIGH—State Health Director Leah•.Devlin today'am dmced'the remogal'of the last remaining fish,consumption advisory below the Blue Ridge paper mill;in Haywood County.Today's announcement is the-final'chapter in a'situation-that first came to light in the late 1980s,when tiyproducisofthe paper production process led to fish consumption.advisoriesin the Pigeon,River and the Walters Lake Reservoir. "This is both a.public health and-.an environmental success story, said Devlin."It is a good example i of an industry addressing apotential public health problem by changing its:processes.I'm pleased we can close the book on this one." The original advisory was issued by the State Health director in 1988.It warned against consumption of any fish from below the then Champion International paper mill.In 1994,that advisory was reduced to cover only carp and catfish.In 2001,it was reduced still further to just a limited advisory on carp.in Walters Lake,which is also,known as the Waterville reservoir. The advisory was originally issucd.because of high levels of dioxin found in fish taken below the paper mill.Dioxin is a byproduct of chlorine bleaching.Studics:have shown that exposure'to dioxin increases the risk.of several types of cancer in animals and humans.The most co min onhealth effect in people exposed to.large amounts of dioxins is chlorame,which is a severe skin disease, characterized by large,deep acne-like lesions.Some other effects include liver damage and changes in hormonal levels. Improved pollution controls at the Canton paper mill were enacted during the late 1980s.The Canton mill,formerly owned by Champion International,was purchased by mill employees and renamed Blue-Ridge Paper Pmducts:Ine.:in 1999. More'information on fishconsumption advisories in North Carolina can be found at http;/hv_tyay.ePisutte nc ps/epi/f sW HN# http://w%vw.nedhbs.gov/presstclVI-9-07a:htm 3/22/2007 Progress Energy Carolinas, Inc. A-11 EH&SS