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HomeMy WebLinkAboutNC0000272_2011 Dioxin Fish Tissue Report_20120208 n.M�I Canton Office evergree 175 Main Streer• Canton, NC 28716 packaging PSD-12-12 February 8, 2012 CERTIFIED MAU, RETURN RECEIPT RE UESTIED 02061 Chuck Cranford 7007 3 Regional Supervisor Division of Water Quality hh D D Asheville Regional Office ! North Carolina Department of Environment 3 and Natural Resources FEB 1 On 2090 US Highway 70 T Swannanoa,North Carolina 28778 WATER QUALITY SECTION ASHEVILLE REGIONAL OFFICE Subject: 2011 Dioxin in Fish Tissue Report NPDES NC 0000272 .: . . :;,...:.>.:.::.....ti: .,.,... Blue Ridge Paper Products Inc dba Evergreen Packaging Canton Mill Dear Mr. Cranford— Enclosed is the subject report with results of August 2011 dioxin in fish tissue for Waterville Lake as required by special condition I.A.(9.)of the May 2010 NPDES permit. Preparation of the report was delayed by time taken to obtain a second independent laboratory analysis of fish tissue fillet samples as a quality assurance check on the primary laboratory results. The second laboratory results are consistent with the primary laboratory and are included in the report appendix. In January 2007,the NC Department of Health and Human Services (DHHS) lifted the fish advisory for common carp in Waterville Lake and requested two additional years of fish tissue sampling and surveillance,which were completed in 2009. The May 2010 NPDES Permit for the Blue Ridge Canton Mill requires three (3) additional years of fish tissue sampling and surveillance in the summer of 2011,2013 and 2014. This report completes the 2011 surveillance. The concentrations of dioxin and furan congeners in channel catfish and common carp fillet samples collected from Waterville Lake in August 2011 remain below the 4 pin TEQ fish advisory level established by the NC DHHS. Very truly yours, BLUE RIDGE PAPER PRODUCTS INC. DOING BUSINESS AS EVERGREEN PACKAGING Paul Dickens Nick McCracken Manager,Environmental Affairs Water Compliance Coordinator 828-646-6141 828-646-2874 paul.dickens@eve[pack.com nick.mccracken@eve!pack.com Enclosure—2011 Dioxin in Fish Tissue Report fresh by design. — ,.,: t 4 _. fverg,aan Ik.vemEye Pocko9v:y 2)OJI -a � !"m D�ioxJnMdon110-r _ J I no F!s,h T !sS,mem y.3P4 I Now- 1 i Blue Ridge Paper Products Inc dba Evergreen Packaging Canton, NC :.......1 _,,. : .�:., _ .. . Can on evergreen,./ 175 N"^ °S`C8 packaging I " °;° Sheet- Canton, NC 28716 PSD-12-12 February 8,2012 CERTIFIED MAIL RETURN RE 1RFSTED 3 Chuck Cranford 7007 3020 611 T7691 Regional Supervisor Division of Water Quality Asheville Regional Office U 5 North Carolina Department of Environment DD el and Natural Resources FEB 1 0 2012 2090 US Highway 70 Swannanoa,North Carolina 28778 ➢' WATER QUALITY SECTION :I- ASHEVIlLE REGIONAL OFFICE ' 1 Subject: 2011 Dioxin in Fish Tissue Report "" t°�*" �+- 4 a:•.> . NPDES NC 0000272 Blue Ridge Paper Products Inc dba Evergreen Packaging Canton Mill Dear Mr. Cranford— Enclosed is the subject report with results of August 2011 dioxin in fish tissue for Waterville Lake as required by special condition I.A.(9.)of the May 2010 NPDES permit. Preparation of the report was delayed by time taken to obtain a second independent laboratory analysis of fish tissue fillet samples as a quality assurance check on the primary laboratory results. The second laboratory results are consistent with the primary laboratory and are included in the report appendix. In January 2007,the NC Department of Health and Human Services (DHHS) lifted the fish advisory for common carp in Waterville Lake and requested two additional years of fish tissue sampling and surveillance,which were completed in 2009. The May 2010 NPDES Permit for the Blue Ridge Canton Mill requires three (3) additional years of fish tissue sampling and surveillance in the summer of 2011,2013 and 2014. This report completes the 2011 surveillance. The concentrations of dioxin and furan congeners in channel catfish and common carp fillet samples collected from Waterville Lake in August 2011 remain below the 4 ppt TEQ fish advisory level established by the NC DHHS. Very truly yours, BLUE RIDGE PAPER PRODUCTS INC. DOING BUSINESS AS EVERGREEN PACKAGING r Paul Dickens Nick McCracken Manager, Environmental Affairs Water Compliance Coordinator 828-646-6141 828-646-2874 paul dickens(Weverpack.com nick mccracken(d)eveipack.com Enclosure—2011 Dioxin in Fish Tissue Report fresh by desV. Doing B :ofl . .,os Everaree,Be.emae Pockoaing 2011 Dioxin in Fish Tissue Report 8 Feb 2012, Page 2 cc w/enclosure: NC'DENR (2 copies) Division of Water Quality Water Quality Section ATTENTION—CENTRAL FILES 1617 Mail Service Center Raleigh,North Carolina 27699-1617 Sergei Chemikov, NC DWQ—Complex Permits Section(electronic) Rick Smith,Progress Energy(electronic) Larry Wilson, UTK(electronic) C-File(cover letter only) s RESULTS OF 2011 DIOXIN MONITORING IN FISH TISSUE Prepared for: Blue Ridge Paper Products Inc. dba Evergreen Packaging Canton Mill Canton,North Carolina Prepared by: Theodore B. Henry, Ph.D. Center for Environmental Biotechnology and Departments of Forestry,Wildlife and Fisheries University of Tennessee Knoxville,Tennessee J. Larry Wilson,Ph.D. Departments of Forestry,Wildlife and Fisheries ( University of Tennessee Knoxville,Tennessee January 2012 i TABLE OF CONTENTS Page List of Tables . . . . . . . . . . . . . . . . . ii List of Figures. . . . . . . . . . . . . . . . . iii EXECUTIVE SUMMARY . . . . . . . . . . . . . iv 1. INTRODUCTION . . . . . . . . . . . . . . . 1 2. SAMPLING LOCATIONS . . . . . . . . . . . . . 2 3. SAMPLING OBJECTIVES . . . . . . . . . . . . 6 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT . . . 7 5. SAMPLE PREPARATION . . . . . . .. . . . . . . 13 6. ANALYTICAL RESULTS . . . . . . . . . . . . 15 7. REFERENCES . . . . . . . . . . . . . . . 27 8. APPENDICES . . . . . . . . . . . . . . . . 30 APPENDIX A: CHAIN OF CUSTODY FORM APPENDIX B: ' COMPARISON OF TESTAMERCIA AND VISTA ANALYTICAL RESULTS FOR TISSUE FILLETS TESTAMERICA WEST SACRAMENTO ANALYTICAL REPORT VISTA ANALYTICAL EL DORADO HILLS ANALYTICAL REPORT APPENDIX C: BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS 1990-2004 APPENDIX D: 2006 REVISIONS TO DIOXIN MONITORING PLAN i LIST OF TABLES Number Title Page 2-1, Pigeon River Sampling Station Information . . . . . . . . . 3. 4-1 Fish Collection Techniques and Level of Effort . . . . . . . 8 4-2 Summary of Fish Composites Collected at Two Stations in Waterville Lake, August 2011 . . . . . . . . . . . . . . . . . 9 6-1 Summary of Pigeon River Fish Tissue Analysis Results—2011 . . . 17 6-2 Toxicity Equivalence Factors for CDD/F Isomers . . . . . . . 18 6-3 Summary of CDD/F Isomer Analyses, Toxicity Equivalent. Factors, and Toxicity Equivalent Values for the 2011 Waterville Lake Fish Tissue Composites . . . . . . . . . . . . . . . 20 6-4 Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results 2005 —2011 . . . . . . . . . . . . . . 22 �J ii LIST OF FIGURES Number Title Page ES-1 TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2011(Stations 4A and 413) . . . . . . . . . . vi ES-2 TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2011 (Stations 4A and 413) . . . . . . . . . .. vii 2-1 Historical Sampling Station Locations on the Pigeon River . . 4 2-2 Sampling Stations 4A and 4B on the Pigeon River . . . . . . . 5 4-la Lengths of Fish Collected from Waterville Lake for Tissue Analysis, 2004-2011 . . . . . . . . . . 11 4-lb Weights of Fish Collected from.Waterville Lake for Tissue Analysis, 2004-2011 . . . . . . . . . . . . . . 12 6-1 TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2011 (Stations 4A and 413) . . . . . . . . . 25 1 6-2 TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2011 (Stations 4A and 413) . . . . . . . . . 26 iii EXECUTIVE SUMMARY The Blue Ridge Paper Products Inc. dba Evergreen Packaging, Canton Mill contracted the Department of Forestry, Wildlife and Fisheries of the University of Tennessee, Knoxville (UTK) to collect fish tissue samples for dioxin analysis from the Pigeon River during the summer of 2011 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 2011 fish tissue sampling report using the revised protocol of 2006. Bottom feeding species (channel catfish and common carp) were collected in August 2011 from two locations (Stations 4A and 413) in the Pigeon River (Waterville Lake) and analyzed for 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD),.2,3,7,8-tetrachlorodibenzofuran (TCDF), and other CDD and CDF isomers. Concentrations of 2,3,7,8-TCDD and 2,3,7,8-TCDF in channel catfish fillets (right-side) were below detection in Station 4A (DL = 0.24 ppt and 0.046 ppt respectively),and, for Station 4B; 2,3,7,8-TCDD was 1.7 ppt and 1.8 ppt for 2,3,7,8-TCDF. In common carp, 2,3,7,8-TCDD was 0.83 ppt (estimated) in fillet composites (right-side)collected at Station 4A and was 1.1 ppt at Station 4B. For 2,3,7,8-TCDF the concentrations in common carp fillets were 2.5 ppt at Station 4A and 2.6 ppt at Station 4B. The concentration of 2,3,7,8-TCDF in the common carp whole body sample collected at Station 4B was 2.3 ppt and 6.0 ppt for 2,3,7,8-TCDD and 2,3,7,8- TCDF respectively(Table 6-1). Composite samples of fish fillets (left-side) from each site were sent to a second laboratory for internal quality assurance of TCDD and -TCDF tissue concentrations. Results of these independent analyses were consistent with those reported above [for 2,3,7,8 TCDD and 2,3,7,8 TCDF respectively: Station A, channel catfish 0.300 ppt (estimated) and below detection (DL = 0.043), common carp 1.24 ppt and 2.21 ppt; and Station B, channel catfish 0.273 ppt (estimated) and below detection (DL = 0.049), common carp 2.63 ppt and 3.2 ppt]. The whole body carp sample was destroyed during the Test America analysis so an independent laboratory confirmation analysis could not be performed. The mean weights of common carp collected from Stations 4A and 4B (4.144 kg, Station 4A; 5.542 kg, Station B) were lower than those collected in 2007 (6.490 kg - Station 4A; 6.552 kg - Station 413), but consistent with weights of common carp collected in other previous years (2009, 4.303 kg - Station 4A; 4.848 kg - Station B; 2008, 4.727 kg - Station 4A, 4.067 kg - Station 413; 2006, 4.505 kg - Station 4A, 5.637 kg - Station 413; 2005, 3.857 kg - Station 4A, 4.695 kg - Station 413; 2004, 3.750 kg - Station 4A, 3.900 kg - Station 413; 1999-2003, 3.193 kg - Station 4A, 5.042 kg - Station 413). Lipid concentrations in common carp fillets in 2011 were 8.6 to 15%, within the range of past fish tissue collections. The lipid concentration for catfish fillets collected from Station 4B and for the whole body carp collected at station 4B both were higher than during the past 6 fish tissue collections (2004 thru 2009) at 12 and 27 percent, respectively. The 2011 dioxin in tissue analytical results for those samples are consistent with higher lipid concentration. IV In January 2007, the NC DHHS lifted the fish advisory for common carp in Waterville Lake and requested two additional years of fish tissue sampling and surveillance, which was completed in 2009. The May 2010 NPDES Permit for the Blue Ridge Canton Mill requires three (3) additional years of fish tissue sampling and surveillance.in the summer of 2011, 2013 and 2014. This report completes the 2011 surveillance. All concentrations in fish tissue fillets remain below the NC DHHS 4 ppt TEQ action level for fish consumption advisory. v Figure ES-1. TCDD Concentrations in Common Carp Fillets Collected from the Pigeon River, 1990-2011 (Stations 4A and 4B) 70 60 t i —+—Station4A 50 � --A--Station4B 0 40 O ` v v ' d 30 "t3 ` m ` 20 , 3 10 ' - �� D 1S90 1991 199Z 1993 1994 1.995 199E 1997 1998 1999 2000 Z001 200Z 2003 Z004 2005 Z006 2007 2008 2009 ZO10 Z011 TIME b) TCDD concentrations at Station 4B were not detected, therefore, the values plotted represent the detection limit for those samples. The detection limit for 2,3,7,8-TCDD was elevated in the 2007 carp fillet for Station 4B because of a 10-fold dilution of the sample which was required to overcome sample matrix effects (high lipid concentration) during analysis. Consequently, reporting the detection limit for this sample can give a misleading impression that the concentration of 2,3,7,8-TCDD increased that year. vi Figure ES-2. TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2011 (Stations 4A and 46) 2.50 0 Station4A -4 .00 --•--Station 4B v o m 1.50 N � L M r 1 rt o a b b b ` --A, a 0.50 `'�►--- �____ a a b It' a 0.00 1996 1997 1998 1999 2000 2001 20OZ 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 TIME a) TCDD concentrations were not detected at Station 4A, therefore the values plotted represent the detection limit for the sample. b) TCDD concentrations were not detected at Station 413, therefore the values plotted represent the detection limit for the sample. c) The 2011 TCDD result for catfish fillets in 2011 at Station 4B was above detection limit at 1.7 ppt . The TEQ for the 2011 Station 4B catfish fillets remained below the 4 ppt action level of the NC DHHS vii 1. INTRODUCTION The Blue Ridge Paper Products Inc., dba Evergreen Packaging, Canton Mill contracted the Department of Forestry, Wildlife and Fisheries of the University of Tennessee, Knoxville (UTK) to collect fish tissue samples for dioxin analysis from the Pigeon River during the summer of 2011 in accordance with NPDES permit conditions. UTK field personnel followed the March 2006 revision (Wilson 2006) to the December 2001 Fish Tissue Sampling Plan prepared by EA Engineering, Science and Technology, Inc. (EA Engineering 2001a) of Chicago, Illinois. This report details the results of a study conducted during August 2011 to determine the concentrations of 2;3,7,8-TCDD (dioxin) and 2,3,7,8-TCDF (furan) in bottom-feeding fish collected from the Pigeon River near Canton, North Carolina. -The report follows the template developed by EA Engineering for prior reporting years. The 2011 fish tissue study is number 21 in a series of fish tissue surveys designed and conducted to be responsive to the requirements of A.(9.) Dioxin Monitoring Special Condition in Blue Ridge Paper's current NPDES permit for the Canton Mill (Permit No. NC0000272). Sampling locations, selection of target species, sampling methods, and sample preparation/preservation techniques are in accordance with the study plan. The approved study methods and scope detailed herein generally follow those used since 1990 (EA 1990, 1991, 1992, 1993a, 1993b, 1994, 1995, 1996, 1997, 1998, 2000, 2001b, 2001c, 2003, 2004, Wilson 2006, Henry and Wilson 2007, 2008, 2009, 2011)). However, selected project details were modified to be responsive to the suggestions/recommendations of the North Carolina Department of Environment and Natural Resources (NCDENR), the Tennessee Wildlife Resources Agency (TWRA), U.S. EPA Region IV, and the North Carolina Department of Health and Human Services (NC DHHS). The principal change in the program was that the collection and analysis of sportfrsh 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., 2011). 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 413). These changes are included in more detail in Appendix D. The 2011 study was conducted during August, during which time biologists from UTK collected and prepared fish tissue samples from the two Waterville Lake sampling locations (Stations 4A and 4B) on the Pigeon River. Details relevant to the location of Pigeon River sampling stations and fish tissue sampling objectives follow in Sections 2 and 3, respectively. Fish collection techniques and level of effort are detailed in Section 4; methods of sample preparation and shipment are presented in Section 5. Analytical results are summarized in Section 6 and references are provided in Section 7. 1 t_. 2. SAMPLING LOCATIONS In accordance with the study plan (Wilson 2006) that was implemented in 2006, 2007, and 2008 (Henry and Wilson 2007, 2008, 2009, 2011), fish were collected from two sampling locations on the Pigeon River. For this sampling period two sites (Stations 4A and 4B) were sampled. Detailed sampling station information for both sites is provided in Table 2-1 and Figure 2-2. Monitoring Stations 4A and 4B are located in Waterville Lake at RM 41.5 and 39.0, respectively (Figure 2-1). Station 4A is located approximately 21.8 RM downstream from the Mill outfall, near the Messer Branch-Pigeon River confluence (Figure 2-2). Monitoring Station 4B is in the vicinity of the Wilkins Creek-Pigeon River confluence, approximately 24.3 RM downstream from the Canton Mill outfall (Figure 2-2). Appropriate habitats were sampled within each study reach-in an effort to collect the desired complement of fishes. Fish sampling was conducted in the vicinity of each location described above; however, the distance or effort at each station depended on how difficult it was to collect fish at that station. The Station 4B study area consisted of an approximate 1.0 RM reach of Waterville Lake located from the dam to the confluence of Wilkins Creek. Sampling at Stations 4A and 4B included electrofishing and gillnetting near the shore along both the left and right banks of Waterville Lake. Reservoir water level in 2011 was approximately at full pool and was similar to water levels in 2006. Stations 4A and 4B sample areas covered approximately the same surface area as water levels in 2004-2006. 2 Table 2-1. Pi eon River Sampling Station Information Station Station Location and Site Description/Habitat Type Fish Community Number RM Distance from Outfall 4A 41.5 Upper Waterville Lake Characterized by deep-water lentic There are no dominant species. Bluegill,black (21.8 RM downstream from habitat with bedrock covered by crappie, flathead and channel catfish, small mouth the Canton Mill outfall) loose,unconsolidated bottom bass, and largemouth bass are common. Common sediments. Maximum depth carp are present but not common. sampled approximately 3 in. 4B 39.0 Lower Waterville Lake Characterized by deep-water lentic There are no dominant species. Bluegill,black from the dam to confluence 'habitat,bedrock, and soft crappie,flathead and channel catfish, small mouth with Wilkins Creek(24.3 sediments. Maximum depth bass, and largemouth bass are common. Common RM downstream from the sampled approximately 12 in. Very carp are present but not common. Canton Mill outfall) steep banks with little cover. 3 Figure 2-1. Historical Sampling Station Locations on the Pigeon River- fish tissue samples were collected from two sites (4A and 4B) for dioxin analysis in 2011. More precise geographical locations of each site are presented in Figure 2-2. TN Nanlwq Tl xea.emwu Ones WO) TENNESSEE PaA -...i NORTN� II • •• CAROLINA lnIP41 NOTE: ftWar miNa of malnztem sampling bcrtion or NY pP'prn // YYqqaa tnbuNry mouth shown In pareriheses. ``•J gPeacM1 A Fish art,Iterthos Sampli,SNlion 11 p a We1NR Uam NClervtia Laka cewooaree 4B Lr°ak Nepco,N(3 13s9 4A N201 cr:a. l43.rf cn000, eex Nw NaPco RMga Rj—x ft (bEl Nepco GNe—_ (1 3) (45.1) Nvr cn,tr (523) bnalhe s Creek cy(S Trickery (K.0) BNW CNEa (5).1).N (a1D Fe�9uson RMpe (5S'S) Apoy clYEa FlMrvilla BClow WaYnvWR-'S95)W P Me(63.3) Canfan.NC m Wg4,spy IGNIYd cFjde.NC can(On 15601 � I64,31 4 y ewa l \. C 4L f a x F� 1 4 Mom KMb LAW WA at 22 4 a a phew_ ._ f� ! 11 �• r 40, 1347 Figure 2-2. Sampling Stations 4A (indicated by A) and 4B (indicated by B) on the Pigeon River 5 3. SAMPLING OBJECTIVES In accordance with the study plan (Wilson 2006), the goal of the fish collection effort was to collect one composite bottom feeder fillet sample at both sampling stations 4A and 4B. Each composite consisted of 3 to 5 similarly-sized (shortest specimen within 75% of the length of the longest) adult individuals of the target species. Common carp (Cyprinus carpio) and channel catfish (Ictalurus punctatus) were the targeted species at sites 4A and 4B. In addition to fillet samples, one whole body common carp was collected from Station 4B. In summary fish were collected as follows: • Bottom feeder fillet composite—one sample at both locations • Catfish fillet composite—one sample at both locations • Common carp whole body composite--one sample from Station 4B Every reasonable effort was made'to collect the desired size, species and/or number of fish; however, the outcome of the sampling effort each year is dependent on physical river conditions and the natural diversity and abundance of target fishes at each sampling location. The 2011 Pigeon River collections yielded the desired species at each location. In addition, the number of specimens collected made it possible to composite individuals of similar weight and length (with larger/adult specimens preferred), and the 75%rule was met for all samples. r i 6 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT Sampling was conducted during 1-2 August 2011. Notes were recorded at each sampling station with regard to the type of sampling gear, level of effort(time), and habitat(Tables 2-1 and 4-1). All fish submitted for tissue analysis (including whole body specimen) were measured to the nearest millimeter (total length) and weighed to the nearest gram (wet weight). These data are summarized in Table 4-2. For 2011, the mean total length of carp was 685 mm and fish ranged from 625-740mm. In 2009, the mean total length for carp was 670mm and fish ranged from 620-698mm. 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). Gill nets were also necessary because of water depth. A boat electrofishing unit (pulsed direct current) was used at both stations. The boat electrofisher was equipped with a Smith Root Type VIA electrofisher, and powered by a 240-volt, 5000-watt generator. Electrofishing techniques followed those described in the National Dioxin Study(Versar 1984). Fish collection techniques and level of effort (time) expended at both stations are summarized in Table 4-1. Total study effort for collection offish at Stations 4A/413 was 167 min electrofishing and 14.1 h gill netting. 7 Table 4-1. Fish Collection Techni ues and Level of Effort Station Sampling Sampling Number RM Dates Techniques Level of Effort Comments 4A 41.5 1 Aug I 1 Boat An approximate 1.0 RM reach of river was sampled and the entire electrofishing 82 min area was electrofished. 4B 39.0 2 Aug 11 Gill nets 14.1 h An approximate 1.4 RM reach was sampled; sampling involved gill nets at selected locations throughout the entire area. Nets were set off Boat 85 min the shoreline areas. Electrofishing was not utilized since sufficient electrofishing numbers of fish were collected in gill nets. 8 Table 4-2. Summary of Fish Composites Collected at Two Stations in Waterville Lake, August 2011. A composite sample was generated for each site and each composite consisted of the right-side fillet(R)from all five fish collected from the site. A whole body(WB) composite from a single common carp was obtained from site 4B. Total Total Length whole body Date Station Species (mm) (g) Sample type Composite I Aug 11 4A Channel catfish 478 885 Fillet R (RM 41.5) Channel catfish 435 636 Fillet R Channel catfish 450 681 Fillet R Channel catfish 461 799 Fillet R Channel catfish 469 763 Fillet R MEAN 459 753 4A Common carp 625 3160 Fillet R (RM 41.5) Common carp 660 3680 Fillet R Common carp 675 4300 Fillet R Common carp 685 4660 Fillet R Common carp 710 4920 Fillet R MEAN 671 4144 2 Aug 11 4B Channel catfish 550 1390 Fillet R (RM 39.0) Channel catfish 466 880 Fillet R Channel catfish 475 925 Fillet R Channel catfish 482 1010 Fillet R Channel catfish 547 1480 Fillet R MEAN 504 1137 2 Aug 11 4B Common carp 625 3490 Fillet R (RM 39.0) Common carp 680 4620 Fillet R Common carp 725 6280 Fillet. R Common carp 727 7040 Fillet R Common carp 740 6280 Fillet R MEAN 699 5542 1 Aug 11 4B Common carp 693 5020 Whole body WB (RM 39.0) 9 Target species were collected at both sampling stations in 2011. Common carp, the target bottom feeder at Stations 4A, and 4B, were collected (and prepared for fillet and/or whole body analysis) at those stations. Because of the physiography of the Waterville Lake Stations 4A and 4B, gill nets were used (Station 4B) in addition to the electrofishing gear 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. Bottom feeder fillet composites samples consisted of five channel catfish and five common carp at Station 4A, and five channel catfish and five common carp at Station 4B. A single bottom feeder whole body common carp from Station 4B was submitted for analysis (Table 4-2). All 20 composite fillets submitted for analysis in 2011 met the US EPA Region IV recommendation (Cunningham 1990) that the smallest specimen in each composite be equal to or greater than 75% of the total length of the largest specimen in that composite (Tables 4-2 and 6-4). Figure 4-la-b illustrates the length and weight distribution of fish collected for tissue analysis from Waterville Lake since 2004. The size distribution of catfish remained similar between 2004 and 2011. The size of the carp taken for whole body tissue analysis from Station 4B in 2011 was similar to size of whole body fish collected in previous years. Analysis of lipids in the 2011 fish tissue samples did show a difference from past year fish tissue collections. The lipid concentration for catfish fillets collected from Station 4B and for the whole body carp collected at station 4B both were higher than during the past 6 fish tissue collections (2004 thru 2009) at 12 and 27 percent,respectively. 10 , Length (mm) 0 0 0 0 0 0 0 0 0 4A Cat N 4A Carp x 0 4B Cat 4B Carp ° Whole 4A Cat 4A Carp o No 0 4B Cat N Q :51i 4B Carp N F= WholeCD C 4A Cat r N 4A Carp 3 0 4B Cat 4B Carp y Whole • r r'} 4A Cat N N 4A Carp 0 4B Cat N 4B Carp 0 3 Whole 4Phh y CD 4A Cat IV 4A Carp O 7r w 4B Cat j 0 4B Carp -fi Whole • C 4A Cat N 4A Carp 0 4B Cat '11 4B Carp N' Whole • 4A Cat N 4A Carp 0 4B Cat 4B Carp Whole CD Weight (g) 41. N W U1 d� -4 M CO O O O O O O O O O C O O O O O O O O O O 0 4A Cat -11 4A Carp X 0 4B Cat f o 4B Carp CD Whole a 4A Catfu o N 4A Carp- O S 0 4B Cat N Q 4B Carp CD Whole 4A Cat r 4A Carp CD0 4B Cat O o °' 4B Carp ~' N � -1 Whole 4A Cat yCD 4A Carp w 0 4B Cat G N 4B Carp Q N Whole CD 4A Cat N O 4A Carp � 0 4B Cat j O o °D 4B Carp Whole ■ 4A Cat 4A Carp 0 46 Cat TI Co 4B Carp N Whole S 4A Cat ■ 4A Carp 4B Cat 4B Car Whole 5. SAMPLE PREPARATION All fish tissue samples were prepared in accordance with U.S. EPA Region IV recommendations (Cunningham 1990) as described in EA (2001a). To prevent cross-contamination between sampling stations, all sampling equipment likely to come into contact with the fish was rinsed extensively with site water between stations. Specimens collected at each station were sorted by size and species, and target species were identified. The objective was to obtain a 3= to 5-fish composite sample for channel catfish and. common carp at both 4A and 4B sample locations, as well as a common carp whole body sample from either station in Waterville Lake which met the species and size objectives discussed in Section 3. From the target fishes collected, specimens of similar length and weight were selected for each composite sample. All specimens retained were immediately placed on ice for later processing. For each fish retained, length and weight data were recorded on the appropriate fisheries data sheet. Following identification of target organisms, selection of composite samples, and collection of length/weight data, each specimen was prepared for shipment and analysis. Bottom feeder fillet samples consisted of epaxial muscle tissue and skin from one side of the fish. Bottom feeder whole body samples consisted of the entire fish. Fillet samples were prepared by removing scales (or removing the skin from catfishes) and then making an incision behind the opercula(on both sides of the fish) from the base of the spine (behind the skull) to just below the pectoral fin. Care was taken to cut through the epaxial muscle without puncturing the rib cage or gut lining. A second incision was made along,the length of the spine to the caudal fin on both sides of the fish. The epaxial muscle was then gently cut away from the rib cage to obtain a fillet. In this fashion, all flesh and skin was obtained from head to tail on both sides of the fish. Fillet knives were solvent rinsed (hexane and acetone)between fish from different stations. Each composite sample was wrapped in aluminum foil (dull side toward sample), labeled, and placed on ice in the field. All individual specimens (fillets) composing a single composite sample were placed in a water- tight plastic bag labeled with the station name, sample number, and species identification. A chain-of-custody form was filled out for each cooler of samples submitted for analysis. Each form included composite specific information and instructions. All chain-of-custody forms had the following information: • sample location and station identification, • sampling team initials, • date of collection, • species name, • sample type (i.e., fillet or whole body) A copy of the chain-of-custody record is provided in Appendix A. All samples were frozen solid prior to shipment to the analytical laboratory. The frozen samples were packed on dry ice and shipped via overnight delivery, where they arrived on August 23, 13 2011 at TestAmerica West Sacramento, CA, USA. 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. After evaluation of the results from TestAmerica, back-up fillet samples (left-side fillets) from each site were sent to Vista Analytical Laboratory (El Dorado Hills, CA, USA). The purpose was independent laboratory confirmation of the TestAmercia results for the 2011 fish tissue fillets. The whole body carp sample was destroyed in analysis, so an independent laboratory confirmation analysis could not be performed. The chain of custody forms and shipping procedure were identical to those described for the samples sent to TestAmerica. Samples arrived at Vista Analytical Laboratory on November 2, 2011. 14 6. ANALYTICAL RESULTS The fish tissue samples were received in one shipment (8/23/11) at TestAmerica under chain-of- custody protocol. Once received at the laboratory, samples were compared to the chain-of- custody record to verify the content of each shipping container. Each individual fish or fillet within a composite was homogenized separately by TestAmerica personnel, and equal aliquots of the homogenate from each fish were removed to constitute the composite. Dioxin and furan analyses were performed using high resolution Gas Chromatography/Mass Spectrometry (GC/MS) as required by the U.S. EPA. Laboratory documentation of all chemical extractions and analyses are provided in Appendix B. All chemical analyses of the samples were conducted using EPA Method 8290 (U.S. EPA 1994) as specified in the Fish Tissue Sampling Study Plan (EA 2001a). Methodology for analysis of samples sent to Vista Analytical Laboratory for confirmation were consistent(i.e., EPA Method 8290)with those used by TestAmerica. 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 2011 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. Only fillet results are discussed below because North Carolina Department of Health and Human Services (NC DHHS) considers only fillet results when issuing health advisories. Concentrations of 2,3,7,8-TCDD and 2,3,7,8-TCDF in channel catfish fillets were below detection in Station 4A (DL = 0.24 ppt and 0.046 ppt respectively) and for Station 4B 2,3,7,8- TCDD was 1.7 ppt and 1.8 ppt for 2,3,7,8-TCDF (Table 6-1). In common carp, 2,3,7,8-TCDD was detected (estimated 0.83 ppt) in fillet composites collected at Station 4A and was 1.1 ppt at Station 4B. For 2,3,7,8-TCDF the concentrations in common carp fillets were 2.5 ppt at Station 4A and 2.6 ppt at Station 413. The concentration of 2,3,7,8-TCDF in the common carp whole body sample collected at Station 4B was 2.3 ppt and 6.0 ppt for 2,3,7,8-TCDD and 2,3,7,8- TCDF respectively (Table 6-1). Examination of the data in Table 6-1 indicates that all fish collected during this study had body burdens well below the FDA dioxin health advisory level (25 ppt) for fish tissue [as established and presented in FDA (1981, 1983) and Cordle (1983)]. The NC DHHS recommends an average dioxin toxicity equivalent(TEQ) level of 3 ppt or less in fish tissue fillets. The NC DHHS issues dioxin fish tissue advisories at an average toxicity equivalent of 4 ppt or greater (e-mail correspondence with Dr. Luanne Williams 18 January 2005). The TEQ of each chlorodibenzodioxin and furan (CDD/F) isomer is based on the toxicity equivalence factor(TEF) (WHO 2005 and Table 6-2) as described in the 2001 Study Plan (EA 2001b). The TEQ value is calculated assuming additivity of effects for the individual congeners of dioxin and furans and is expressed as an"equivalent amount of 2,3,7,8-TCDD" (NC DEHNR 1991). The measured concentration of each CDD/F isomer, when multiplied by its appropriate f' TEF,yields the TEQ of that isomer(the toxic concentration of that isomer relative to the toxicity 15 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. 16 Table 6-1. Summary of the Pigeon River Fish Tissue Analysis Results 2011 Station Percent Number Sample ID Composite/Sample Tyne 2,3,7,8-TCDD(') 2,3,7,8-TCDFt') Livid 4A SITE 4A channel catfish 5 fillet samples ND (DL=0.24) ND (DL=0.046) 3.0 SITE 4A common carp 5 fillet samples 0.83° 2.5` 8.6 4B SITE 4B channel catfish 5 fillet sample 1.7 1.8` 12 SITE 4B common carp 5 fillet samples 1.1 2.6` 15 SITE 4B common carp 1 whole body sample 2.3 6.0` 27 (a)Units=ppt(parts per trillion)or pg/g(picogram/gram) (b)Estimated results. Result is less than the reporting limit (c)Analyte was positively identified, confirmation(CON) analysis used. (ND)Not detected, concentrations below the instrument detection limit(DL). 17 Table 6-2. Toxicity Equivalence Factors for CDD/F Isomers. DIOXIN DIBENZOFURAN Isomerta? TEF(b) TEF(b) 2,3,7,8-TCDD 1 2,3,7,8-TCDF 0.1 1,2,3,7,8-PeCDD 1 1,2,3;7,8-PeCDF 0.03 2,3,4,7,8-PeCDF 0.3 1,2,3,4,7,8-HxCDD 0.1 1,2,3,4,7,8-HxCDF Al 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. 18 The TEQ calculation and summarization schemes presented in Table 6-3 followed methods used by NC DHHS (NC DEHNR 1991). All fish tissue fillets analyzed had TEQ values below the NC DHHS advisory limit (4 ppt) and ranged from 0.3 ppt for channel catfish fillets collected at Station 4A to 2.8 ppt for common carp collected from Station 4B. The values reported in years 2005-2009 for channel catfish are consistent with the results for 2011. Common carp TEQ results in 2007 were higher(Station 4A, 13.44 ppt; Station 4B, 5.35 ppt) than observed in previous years (2005-2006), and results for 2008 and 2009 (2009, Station 4A, 1.562 ppt; Station 4B, 1.496 ppt) are further evidence that the 2007 results were anomalous. The whole body sample for common carp collected at Station 4B had a TEQ result of 9.82 ppt. This TEQ result includes several estimated congener concentrations below the method level of quantification. The TEQ calculated from 2,3,7,8 TCDD and 2,3,7,8 TCDF concentrations in the whole body sample is 2.9 ppt. Table 6-4 illustrates 2,3,7,8 TCDD concentrations in common carp fillet samples collected in 2005, 2006, 2007, 2008, 2009, 2011 and results for previous years (1990-2004) are in Appendix C. Between 1990 and 2006, 2,3,7,8-TCDD concentrations in carp fillets declined dramatically (94-99 %) at all sampling stations (Table 6-4, Appendix C, Figure 6-1). The mean weights of common carp collected from Stations 4A and 4B (4.144 kg, Station 4A; 5.455 kg, Station B) were lower than those collected in 2007 (6.490 kg - Station 4A; 6.552 kg -, Station 4B), but consistent with weights of common carp collected in previous years (2008, 4.727 kg - Station 4A, 4.067 kg - Station 4B; 2006, 4.505 kg - Station 4A, 5.637 kg - Station 4B; 2005, 3.857 kg - Station 4A, 4.695 kg - Station 4B; 2004, 3.750 kg - Station 4A, 3.900 kg - Station 4B; 1999-2003, 3.193 kg - Station 4A, 5.042 kg - Station 4B). Lipid concentrations in common carp fillets in 2009 were 8.6-15%, within the range of past fish tissue collections. The lipid concentration for catfish fillets collected in 2011 from Station 4B and for the whole body carp collected at station 4B both were higher than during the past 6 fish tissue collections (2004 thru 2009) at 12 and 27 percent, respectively. The 2011 dioxin in tissue analytical results for those samples are consistent with higher lipid concentration. F 19 Table 6-3. Summary of CDD/F Isomer Analyses,Toxicity Equivalent Factors, and Toxicity Equivalent Values for the 2011 Waterville Lake Fish Tissue Composites STATION 4A Channel catfish fillet Common carp fillet CDD/F isomers TEF(`) Results(') TE f Results(a) TE N) Dibenzodioxin 2,3,7,8-TCDD 1.0 ND 0.000 0.83" 0.83 1,2,3,7,8-PeCDD 1.0 ND 0.000 ND 0.000 1,2,3,4,7,8-HxCDD 0.1 ND 0.000 ND 0.000 1,2,3,6,7,8-HxCDD 0.1 ND 0.000 3.2° 0.32 1,2,3,7,8,9-HxCDD 0.1 ND 0.000 ND 0,000 1,2,3,4,6,7,8-HpCDD 0.01 ND 0.000 21 0.21 OCDD 0.0003 7.6 0.0023 73 0.0219 Dibenzofuran 2,3,7,8-TCDF 0.1 ND 0.000 2.5 0.25 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 3.7d 0.37 10 1.0 2,3,4,6,7,8-HxCDF 0.1 ND 0.000 ND 0.000 1,2,3,7,8,9-HxCDF 0.1 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDF 0.01 ND 0.000 4.3" 0.043 1,2,3,4,7,8,9-HpCDF 0.01 ND 0.000 ND 0.000 OCDF 0.0003 ND 0.000 8.1d 0.0024 Total TEQ 0.3723 2.6773 (a)Units=ppt(parts per trillion) or pg/g(picogramper gram) (b)Dioxin Equivalent Concentration using methodology from U.S. EPA(1989) (c)Toxicity Equivalent Factors from World Health Organization(WHO 2005) (d)Estimated result. Result is less than reporting limit. 20 1 Table 6-3 (cont). Summary of CDD/F Isomer Analyses, Toxicity Equivalent Factors, and Toxicity Equivalent Values for the 2011 Waterville Lake Fish Tissue Composites STATION 4B Channel catfish fillet Common carp fillet Common carp whole body CDD/F isomers TEF(`) Resultsla) T O Results(a) TE ro) Results(a) TE ! Dibenzodioxin 2,3,7,8-TCDD 1.0 1.7 1.7 1.1 1.1 2.3 2.3 1,2,3,7,8-PeCDD 1.0 ND 0.000 ND 0.000 2.5d 2.5 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 3.7d 0.37 3.9d 0.39 7.0 0.70 1,2,3,7,8,9-HxCDD 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDD 0.01 13 0.13 19 0.19 35 0.35 OCDD 0.0003 37 0.0111 52 0.0156 200 0.06 Dibenzofuran 2,3,7,8-TCDF 0.1 1.8 0.18 2.6 0.26 6.0 0.6 1,2,3,7,8-PeCDF 0.03 ND 0.000 ND 0.000 3.6d 0.108 2,3,4,7,8-PeCDF 0.3 ND 0.000 ND 0.000 3.0' 0.9 1,2,3,4,7,8-HxCDF 0.1 ND 0.000 ND 0.000 2.7d 0.27 1,2,3,6,7,8-HxCDF 0.1 3.ld 0.31 8.4 0.84 20 2.0 2,3,4,6,7,8-HxCDF 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,7,8,9-HxCDF 0.1 ND 0.000 ND 0.000 ND 0.000 1,2,3,4,6,7,8-HpCDF 0.01 ND 0.000 ND 0.000 3.1d 0.031 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 2.701 2.796 9.819 (a)Units=ppt(parts per trillion) or pg/g(picogram per gram) (b)Dioxin Equivalent Concentration using methodology from U.S. EPA(1989) (c) Toxicity Equivalent Factors from World Health Organization(WHO 2005) (d)Estimated result. Result is less than reporting limit. 21 Table 6-4. Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 2005 —2011 2005 Results (d) 2006 Results(e) Number Length Range Number Length Range Station Species of fish (mm) 2,3,7,8-TCDDt°,"1 Station Species of fish (mm) 2,3,7,8-TCDD(°b) -- — - 1 Black redhorse 5 359-384 ND(0.35) 4A Common carp 3 635-692 0.64(_) RM 64.5 RM 41.5 Channel catfish 5 430-500 ND(0.37) 2 Common carp 4 595-650 ND(0.45) 4B Common carp 3 650-745 0.73(`) RM 59.6 Channel catfish 3 443-460 ND(0.29) RM 39.0 Channel catfish 4 510-590 0.77(<) 3 Common carp 4 605-630 ND(0.46) RM 52.3 4A Common carp 3 601-665 1.3 RM 41.5 Channel catfish 5 464-508 ND(0.36) 4B Common carp 4 595-736 2.8 RM 39.0 Channel catfish 5 513-603 0.76(`) 5 Black redhorse 4 440-501 ND(0.41) RM 19.0 Total fish filleted= 37 Total fish filleted= 15 (a)Dioxin analyses conducted by TestAmerica(formerly Severn Trent Laboratories). (b)Units=ppb(parts per trillion)or pg/g(picogram/gram) (c)Estimated result. Result is less than the reporting limit. (d) Survey conducted in August and September (e)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 22 Table 6-4 (cont). Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 2005 —2011 2007 Results (d) 2008 Results(e) Number Length Range Number Length Range Station Species offish (mm) 2,3,7,8-TCDD Station Species offish (mm) 2,3,7,8-TCDDf'st 4A Common carp 4 680-775 6.4 4A Common carp 3 653-686 1.2 RM 41.5 Channel catfish 4 490-593 0.57t`I RM 41.5 Channel catfish 5 475-525 ND(0.29) 4E Common carp 5 672-762 ND(6.9) 413 Common carp 3 630-665 ND(0.36) RM 39.0 Channel catfish 5 505-670 0.67° RM 39.0 Channel catfish 5 459-595 ND(0.34) Total fish filleted= 18 Total fish filleted= 16 (a)Dioxin analyses conducted by TestAmerica(formerly Sevem Trent Laboratories). (b)Units=ppt(parts per trillion)or pg/g(picogram/gram) (c)Estimated result. Result is less than the reporting limit. (d)Survey conducted in August and September (e)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 23 Table 6-4 (cont). Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 2005—2011 2009 Results(d) 2011 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-TCDD(�b1 4A Common carp 5 620-698 1.1 4A Common carp 5 625-710 0.830 RM 41.5 Channel catfish 3 493-578 0.52t`I RM 41.5 Channel catfish 5 435-478 ND(0.24) 4B Common carp 5 647-696 0.93(`) 4B Common carp 5 625-740 1.1 RM 39.0 Channel catfish 5 467-574 ND(0.43) RM 39.0 Channel catfish 5 466-550 1.7 Total fish filleted= 18 Total fish filleted= 20 (a)Dioxin analyses conducted by TestAmerica(formerly Severn Trent Laboratories). (b)Units=,ppt(parts per trillion)or pg/g(picogram/gram) (c)Estimated result. Result is less than the reporting limit. (d) Survey conducted in August and September (e)Survey conducted in August ND=Non-detectable at the detection limit in parentheses 24 Figure 6-1. TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990-2011 (Stations 4A and 413) 70 - -- --.. - - - - 60 0 Station4A • -a--Station4B 80 v v ; 'MG - - tn o 510 1990 1991 1992 1993 1994 1995 1906 1997 1998 1999 2000 ZOO1 ZOOZ Z003 2004 ZOOS 2006 2007 Z008 2009 2010 2011 TIME b)TCDD concentrations at Station 4B were not detected, therefore,the values plotted represent the detection limit for those samples. The detection limit for 2,3,7,8-TCDD was elevated in the 2007 carp fillet for Station 4B because of a 10-fold dilution of the sample which was required to overcome sample matrix effects (high lipid concentration) during analysis. Consequently, reporting the detection limit for this sample can give a misleading impression that the concentration of 2,3,7,8-TCDD increased that year 25 Figure 6-2. TCDD Concentrations in Channel Catfish Fillets Collected from the Pigeon River, 1997-2011 (Stations 4A and 413) 2.50 *—Station 4A .. .--.-..---.._ z.o0 --A--Sladon4B - n v r v , , d.50 a ' m ::�.00 b a b _�, b ' o ♦--- ; a ' b ♦--- a a 0.00 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 TIME a) TCDD concentrations were not detected at Station 4A, therefore the values plotted represent the detection limit for the sample. b) b) TCDD concentrations were not detected at Station 413, therefore the values plotted represent the detection limit for the sample. c) The 2011 TCDD result for catfish fillets in 2011 at Station 4B was above detection limit at 1.7 ppt . The TEQ for the 2011 Station 4B catfish fillets remained below the 4 ppt action level of the NC DHHS 26 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. r 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. 27 EA Engineering, Science, and Technology Inc. 1998. Results of the 1998 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01, prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2000. Results of the 1999 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01, prepared for Champion International Corporation, Canton, North Carolina. January. EA Engineering, Science, and Technology Inc. 2001a. Study Plan for Pigeon River Dioxin Monitoring in Fish tissue. Prepared for Blue Ridge Paper Products Inc., Canton, North Carolina. November. EA Engineering, Science, and Technology Inc. 2001b. Results of the 2000 Dioxin Monitoring in Fish Tissue. EA Report No. 13745.01, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2001c. Results of the 2001 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.01, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2003. Results of the 2002 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.02, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. December. EA Engineering, Science, and Technology Inc. 2004. Results of the 2003 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.03, prepared for Blue Ridge Paper Products Inc., Canton,North Carolina. January. Food and Drug Administration. 1981. FDA advises Great Lakes States to monitor dioxin- contaminated fish. FDA Talk Paper dated 28 August, in Food Drug Cosmetic Law Reports, paragraph 41, 321. Commerce Clearing House, Inc. 8 September. Food and Drug Administration. 1983. Statement by Stanford A. Miller, Director, Bureau of Foods, FDA before the Subcommittee on Natural Resources, Agriculture Research and Environment, U.S. House of Representatives. 30 June. Henry, T.B., and J.L. Wilson. 2006. Results of 2005 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc., Canton Mill, Canton,North Carolina. January 2006. Henry, T.B., and J.L. Wilson. 2006. Results of 2006 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc., Canton Mill, Canton,North Carolina. December 2006. Henry, T.B., and J. L. Wilson. 2008. Results of 2007 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products,Inc., Canton Mill, Canton,North Carolina. April 2008. 28 Henry, T.B., and J. L. Wilson. 2008. Results of 2008 dioxin monitoring in fish tissue. Prepared for Blue Ridge Paper Products, Inc., Canton Mill, Canton,North Carolina. November 2008. Henry, T.B., and J. L. Wilson. 2009. Results of 2009 Dioxin Monitoring in Fish Tissue. Final Report to Blue Ridge Paper Products, Inc., dba Evergreen Packaging. December 2009. 29 pp. North Carolina Department of Environment, Health, and Natural Resources. 1991. Fish Tissue Dioxin levels in North Carolina: 1990 update. Division of Environmental Management, Water Quality Section. U.S. Environmental Protection Agency (U.S. EPA). 1994. Analytical procedures and Quality Assurance for Multimedia Analysis of Polychlorinated Dibenzo-para-dioxins and Polychlorinated Dibenzofurans by High-Resolution Gas Chromatography/High-Resolution Mass Spectrometry (Method 8290). U.S. Environmental Protection Agency (U.S. EPA). 1989. Interim Procedures for Estimating Risk Associated with Exposures to Mixtures of Chlorinated Dibenzo-p-dioxins and Dibenzofurans (CDDs and CDFs) and 1989 Update Report No. EPA/625/3-89/016, U.S. EPA, Risk Assessment Forum, Washington, D.C. Versar, Inc. 1984. Sampling Guidance Manual for the National Dioxin Study. U.S. Environmental Protection Agency. EPA Contract 68-01-6160. Work Order Number 8.7. Office of Water Regulations and Standards, Monitoring and Data Support Division, Washington, D.C.Final Draft. July. Wilson, J.L. 2006. Study plan revision: Dioxin monitoring in fish tissue, Waterville Lake. Prepared for Blue Ridge Paper Products, Inc. Canton Mill, Canton,North Carolina. March 2006. World Health Organization (WHO). 1997. Exposure and Human Health Reassessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) and Related Compounds: Part II: Health Assessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin(TCDD) and Related Compounds. 29 APPENDIX A: CHAIN OF CUSTODY FORM APPENDIX B: COMPARISON OF TESTAMERCIA AND VISTA ANALYTICAL RESULTS FOR TISSUE FILLETS TESTAMERICA WEST SACRAMENTO ANALYTICAL REPORT VISTA ANALYTICAL EL DORADO HILLS ANALYTICAL REPORT APPENDD:C: BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS 1990-2004 APPENDIX D: 2006 REVISIONS TO DIOXIN MONITORING PLAN tf t 30 2 OJ 111 �JJ IN al "APPENDICES" Blue Ridge Paper Products Inc dba Evergreen Packaging Canton, NC APPENDIX A CHAIN OF CUSTODY FORM 31 Chaln Of Temperature on Receipt_ 1 es 1 Am ed ca Custody Record DrinldngWatel? Yes❑ Nov THE LEADER IN ENVIRONMENTAL TESTING TAL4124(1007) ClientLY Ira, � `�'��f �� Project Manager ��� /�r� r p$�O L' 1 t Chain o(Cusl Number Address ( Telephone Nuh�gk er(Area CodeyFarNumb/Number 073907 1 '�jy!T2i7j Lan Number .� AI e �'" Page of ciry �.q State jZpColde Stte ontact Lab Contact Analysis(Attach list if more space Is needed) Project N me imd 9 y l 0 Special lnstructionsl Con7ract/Purchase OrdedOuote No. �., !f .ZZ Matdx Containers& Conditions of Receipt Preservatives , Sample I.D.No.and Description Date Time e < $ o SSo (Containers for each sample may be combined on one line) a w w :Me. IIA NA ., l cid (2-Frl( 1452 x X �x� or,� ri l! i NIM U++ c IQ-{i tk+s S—1-l) 1(m b x )( )( X �c>~ sf � l ) 4 A 1- -a-,I 11 a o x x Cb,� stye s /Qt � `` -It CotNl+�or.0 {z"I� 8-�li 1rf60 S;6U �,, w6 z-1 1c.5 x x l 11�4e �m Possible Hazard Identification H Disposal ❑ Non-Hazard ❑ Flammable ❑ Skin lnitant ❑ Pa(5ons ❑ Unknownm To Client ❑ Dis (A tee maybe assessed if samples are retained posal By Lab ❑Archive For Months longarthan 1 month) Turn Around Time Required .00 Requirements(Specify) ❑xHours ❑43Hours ❑ 7Days ❑ 14Days ❑21 Days ❑ Other 1. quiche By Data Tlme 1.R g (9 eceiv y m Date Time D' 2 ►1 d.�0 flgoz I 5t� 2.Ael q ed Data • Time 2.Recetvsd By Dalb ITime evvIll 130t) 3.Relinquished By Date Time 3.Received By pate Tune Comments�/f DISTRIBUnur WHITE Returned to C7Jen1 w71h Report UAW Y-stays Mur° ppw r ye Mind Uapy APPENDIX B COMPARISION OF TESTAMERCIA AND VISTA ANALYTICAL RESULTS FOR TISSUE FILLETS TESTAMERICA WEST SACRAMENTO ANALYTICAL REPORT VISTA ANALYTICAL EL DORADO HILLS ANALYTICAL REPORT 32 Comparision of Trace Dioxin Analyses of Right and Left Tissue Fillet Samples from August 2011 Waterville Lake Sampling EPA Method 8290 for tetra-through-octa chlorinated dioxins and furans on biological samples composited in the laboratory from field tissue fillets Test America (primary laboratory)did composite analysis of the right fillets Vista Analytical (confirmation laboratory)did composite analysis of the left fillets 4A Channel 4A Carp 4B Channel 4B Carp Test America Vista Analytical Test America Vista Analytical Test America Vista Analytical Test America Vista Analytical Lipids 3 2.95 8.6 11.7 12 5.79 15 17.8 2,3,7,8-TCDD ND .3 J 0.83 J 1.24 1.7 0.273 J 1.1 2.63 1,2,3,7,8-PeCDD NO ND NO 1.52 J NO 0.363 J NO 1.88 J 1,2,3,4,7,8-HxCDD ND .169 J ND 1.05 J ND 0.149 J NO 1.57 J 1,2,3,6,7,8-HxCDD NO .768 J 3.2 J 4.09 J 3.7 J 0.715 J 3.9 J 5.63 1,2,3,7,8,9-HxCDD ND ND NO 0.664 J NO ND NO 0.989 J 1,2,3,4,6,7,8-HpCDD ND .727 J 21 11 13 0.589 J 19 13.7 OCDD 7.6 J 1.34 J,B 73 29.4 B 37 1.31 J,B ND 34.1 B 2,3,7,8-TCDF NO NO 2.5 CON 2.21 1.8 CON ND 2.6 CON 3.2 1,2,3,7,8-PeCDF ND NO ND 0.843 J ND ND NO 1.26 J 2,3,4,7,8-PeCDF NO 256 J ND 1.51 J ND NO ND 2.23 J 1,2,3,4,7,8-HxCDF ND .0839 J NO .987 J NO ND ND 1.38 J 1,2,3,6,7,8-HxCDF 3.7 J .0638 J 10 .854 J 3.1 J 0.0764 J 8.4 1.16 J 2,3,4,6,7,8-HxCDF NO .0742 J ND .416 J ND NO ND ND 1,2,3,7,8,9-HxCDF ND ND NO ND NO ND ND ND 1,2,3,4,6,7,8-HpCDF ND NO 4.3 J 2 J ND 0.170 J NO 2.12 J 1,2,3,4,7,8,9-HpCDF NO ND ND ND ND ND ND ND OCDF ND ND 8.1J NO NO ND ND NO J - Estimated value, below level of method quantification B - Compound was also detected in method blank CON - Required confirmation TestAmedca THE LEADER IN ENVIRONMENTAL TESTING pECEIVE D September 23, 2011 BLUE RIDGE PAPER PRODUCTS INC TestAmerica Project Number: G1 H230506 BNS DEPARTMENT PO/Contract: 420224 Nick McCracken Evergreen Packaging PO Box 4000 Canton, NC 28716 _ Dear Mr. McCracken, ' This report contains the analytical results for the samples received under chain of custody by TestAme6ca on August 23, 2011. These samples are associated with your Tissue project. 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 Kellmann Project Manager �i 880 Riverside Parkway West Sacramento,CA 95605 teI916.373.5600 fax 916.372.1059 www.testamericainc.com GIH23ONS TestAmedca West Sacramento(910)373.5600 1.of 831 -" Table of Contents TestAmerica West Sacramento Project Number G1 H230506 Case Narrative Sacramento Quality Assurance Program Sample Summary Sample Data Sheets BIOLOGIC, Percent Lipids, Samples: 1, 2, 3, 4, 5 BIOLOGIC, 8290, Dioxins/Furans Samples: 1, 2, 3, 4, 5 QC Data Association Summary Laboratory QC Reports Raw Data Package Shipping and Receiving Documents GIH230506 TestAmertca West Sacramento(916)373-5600 2 of 831 Case Narrative TestAmerica West Sacramento Project Number G1 H230506 BIOLOGIC, 8290, Dioxins/Furans Sample(s): 2, 3, 4, 5 The above samples required a confirmation (CON) analysis for 2,3,7,8-TCDF which occurred on September 19, 2011. There were no other anomalies associated with this project. i- � GIH230506 TestAmerica West Sacramento(916)373-5600 3 of 831 `�0 mN ACCogO N TestAmerica THE LEADER IN ENVIRONMENTAL TESTING TestAmerica Laboratories West Sacramento Certifications/Accreditations A2LA(DoD-ELAP) 2928-01 New Mexico NA `aJi�^`r'i-..a^- 6<2 .a�,%�-:U_ .1166 ,we- _._ .. Arizona AZ0708 Oregon* CA 200005 'fir':"''=4 1�ffi&aS=.-E� .. .t . . r.88=069.1'''�+`.+f'�!,r � ir!"�w..?riY,9" �va'niati.`:r"X�`;9, 4.It.-f 6$.1272�i"�sr."ter.:= California* 01119CA South Carolina 87014 Colorado . texas. ...., ', TsI:04304399 08,T7C _- Connecticut PII-0691 UCMR CA00044 �n r .FI M Oridaa*ZY IN , ? 7 Georgia 960 USDA Foreign Plant 37-82605 5s_-rt.Guatti��__.".r. Ip-009r s��l; _�USD`ArEorei ":Soil<'�x. <-.-Q330,09 00 55+ Hawaii c NA Utah* QUANI f's 002701 'c..f`. , 4�Uu ntakr u5; "M �c. Kansas* E-10375 Washington C581 0.1944 West Uu nia'; +.9930C 334 Michigan 9947 Wisconsin 998204680 r,.,mW omm 8TMS=:,' New Jersey* I CA005 *NCLAP'accredited. A more detailed parameter list is available upon request. Updated 512512011 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 infield 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. G1 H230506 TestAmerim West Sacramento(916)373-5600 4 of 831 Sample Summary TestAmerica West Sacramento Project Number G1 H230506 WO# Sample# Client Sample ID Sampling Date Received Date MLX8E 1 SITE 4A CHANNEL CAT 6/1/2011,02:52 PM 8/23/2011 09:00 AM MLX8F 2 SITE 4A COMMON CARP 8/1/2011 04:02 PM 8/23/2011 09:00 AM MLXBG 3 SITE 4B CHANNEL CAT 8/2/2011 11:00 AM 8/23/2011 09:00 AM MLXSH 4 S1TE 4B COMMON CARP 8/2/2011 02:00 PM 8/23/2011 09:00 AM MLX8J 5 SITE 4B COMMON CARP WB B/2/2011 11:15 AM 8/23/2011 09:00 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. Results noted as'ND'were not detected at or above the staled IImtL 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,cormsivity,density,9ashpoint, ignitability,layers,odor,paint filler test,pH,porosity,pressure,reactivity,redox potential,specific gravity,spot tests, solids,solubility,temperature,viscosity,and weight. G1 H230506 TestAmerica West Sacramento(916)373-5600 5 of 831 Evergreen Packaging Sample ID: SITE 4A CHANNRL CAT Trace Level Organic Compounds SW8468290 1. Lot-Sample a...: G[11230506-001 Work OrderN_..: IvILX8HIAA Matsu._: BIOLOGICAL F Date Sampled....: 08/01/11 Date Received....: 08/23/11 Dilution Faetor: . 1 Prep Date....: 08/31/11 Analysis Date....: 09/08/11 ' Prep Dutch#....: 1243088 Instrument ID....: 111)5 In1Ha1 WgtfVol: 10.45 g Analyst ID....: Grandllold S.Virginia i REPORTING ES11MATE77 PARAMETER RESULT LiMiT DETECTION LIMIT UNITS Percent Lipids 3.0 % f i QUALIFIERS I1 \ 1 i 1 \\4macsgll\QDSApps\S00 SmdsEDL_Ri._Repun.tpt 92M011 - Evergreen Packaging Sample ID: SITE 4A COMMON CARP Trace Level Organic Compounds SW8468290 , Lot-Sample#..... GIB230506-002 Work Order#....: MLXBFIAA Matrix_.: BIOLOGICAL Date Sampled.._: 08/01/11 Date Received....: 08/23/11 Dilution Factor. I Prep Date:..: 08/31/11 Analysis Date._.: 09/08/11 Prep Batch#....: 1243098 instrument ID_..: I ID5 Initial Wgt/Vol: 10.66 g Analyst ID....: Grandfield S.Virginia REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS Percent Lipids 8.6 % OUALTFMRS \\gsacsgll\QDSAppMOG_StodED1,R1-Rgmrtapt 9t23/2011 G1H230506 TestAmerlca West Sacramento(916)373-5600 6 of 831 Evergreen Packaging Sample ID: SITE 4B CHANNEL CAT Trace Level Organic Compounds SW846 8290 Lot-Sample#.._: GIH230506-003 Work Order#....: ZALX801AA Matrix...: BIOLOGICAL, Date Sampled..... 08/02/11 Date Received....: 08/23/11 Dilution Factor: 1 Prep Date....: 08/31/11 Analysis Date....: 09/08/11 Prep Batch#.._: 1243088 Instrument iD....: I 1 D5 Initial WguVol: 10.14g Analyst ID....: Grandfleld S.Virginia REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS Percent Lipids 12 % QUALIFIERS r i J i _ k�gsacsgll\QDSAppsISQG_smdEDL_RLltepodapt V23/2011 GIH230606 TestAmerlca West Sacramento(916)373-5600 7 of 831 Evergreen Packaging Sample ID: SITE 4B COMMON CARP Trace Level Organic Compounds S WS46 9290 Lot-Sample#...... G1H230506-004 Work Order#.„.: hUMHIAA Matrix.„.: BIOLOGICAL Date Sampled....: 08/02/11 Date Received....: 08/23/11 Dilution Factor: 1 Prep Date....: 08/31/11 Analysis Date._ 09/08/11 Prep Batch#....: 1243088 Instrument ID.„.: 11D5 InftialWgtrVol: 10.4g Analyst ID....: Grandfield'S.Virginia REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS Percent Lipids 15 QUALIFIERS • %kq,,,qlllQDSApps1SOG_St,&EDL—RL_Reponipt 9123/2011 G111230506 TestAmerica West Sacramento(916)373-5600 8 of 631 Evergreen Packaging Sample ID: SITE 4B COMMON CARP WB Trace Level Organic Compounds SW846 8290 Lot-Sample P/....: GIH230506-005 Work Order#....: MLXBJIAA Matrix....: BIOLOGICAL Date Sampled._.: O8/02111 Date Received....: 08/23/11 Dilution Factor: 1 Prep Date-: 08/31/11 Analysis Date....: 09/08/11 Prep Batch N...... 1243088 Instrument ED—.: I lD5 Initial Wgt/frol: 10.1 g Analyst ID....: Grandfield S.Virginia REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS Percent Lipids 27 1/O OUALiFIERS %\gsacsglllQDSApps)SOG_StnMDL_RL Rcponspt 91232011 GIH230506 TestAmerica West Sacramento(916)373-5600 9 of 831 Evergreen Packaging Sample ID: SITE 4A CHANNEL CAT Trace Level Organic Compounds SW846 8290 Lot-Sample#._.: GIH230506-001 Work Order#....: MLX8ElAC Matrix....: BIOLOGICAL Date Sampled...: 08/01/11 Date Received...: 0823111 Dilution Factor: 0.95 Prep Date...: 08/31/11 Analysis Date._.: 09/19/11 Prep Batch#....: 1243094 Instrument ID....: 3D5 Initial Wgt/Vol: 10.45 g Analyst D)...: Michael Ng REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS 2,3,7,8-TCDD ND 0.96 0.24 pg/g Toud TCDD ND 0.96 0.24 Pg/g 1,2,3,7,8-PeCDD ND 4.8 0.13 pg/g TotalPeCDD ND 4.8 0.13 pg/g 1,2,3,4,7,8-HpCDD ND 4.8 0.15 pg/g 1,2,3,6,7,8-HxCDD ND 4.8 0.60 pg/g 1,2,3,7,8,9-14xCDD ND 4.8 0.16 Pg/g Total HxCDD ND 4.8 0.6D pg/g 1,2,3,4,6,7,8-HpCDD ND 4.8 1.6 PS/9 Total HpCDD ND 4.8 1.6 pg/g OCDD 7.6 1 9.6 0.17 pg/g 2,3,7,8-TCDF ND 0.96 0.046 pg/g TotWTCDF ND 0.96 0.41 Pg/g 1,2,3,7,8-PeCDF ND 4.8 0.10 pg/g 2,3,4,7,E-PeCDF ND 4.8 0.10 PA Total PeCDP ND 4.8 0.10 Pg/g 1,2,3,4,7,8-HxCDF ND 4.8 0.11 pg/g 1,2,3,6,7,8-HxCDF 3.7 1 4.9 0.068 P919 2,3,4,6,7,8-HxCDF ND 4.8 0.07E Pg/g 1,2,3,7,8,9-HxCDF ND 4.8 0.095 pg/g Total HxCDF 3.7 4.8 0.080 pllg 1,2,3,4,6,7,8-HpCDF ND 4.8 0.20 P919 1,2,3,4,7,8,9-HpCDF ND 4.8 0.24 Pg/g Total HpCDF ND 4.8 0.24 PClg OCDF ND 9.6 0.27 P9/9 kYgmcNlllQDSApps1900_StndIEDL RL_Reponzp[9/23/2011 G1H230506 TestAmerica West Sacramento(916)373-6600 10 of 831 Evergreen Packaging Sample ID: SITE 4A CHANNEL CAT Trace Level Organic Compounds SW846 8290 Lot-Sample#..... GIH230506-001 Work Order#....: MLXSEIAC Matrix...: BIOLOGICAL Date Sampled...: 08/01/11 Date Received.,_: 08/23/11 Dilution Factor: 0.95 Prep Date....: WWII I Analysis Date....: 09/19/11 Prep Dutch#....: 1243084 Instrument ID....: 3135 Initial Wgtfvol: 10.45 g Analyst ID.... Michael Ng PERCENT RECOVERY INTERNALSTANDARDS RECOVERY LIMITS 13C-2,3,7.8-TCDD 96 40-135 13G1,2,3,7,8-PeCDD 87 40-135 13C-1,2,3,6,7,8-HxCDD 87 40-135 13C-1,2,3,4,6,7,8-HpCDD 83 40-135 13C-OCDD 80 40-135 13C-2,3,7,8-TCDF 92 40-135 13C-1,23,7,8-PeCDF 87 40-135 13C-1,2,3,4,7,8-HxCDF 87 40-135 13C-1,2,3,4,6,7,E-HpCDF 91 40-135 QUALIFIERS ' I Estimated Result. r Ogsacsgll\QDSAppsISOG_SmdML_RL_Repon.cpt W232011 GlHZ30506 TestAmerlca West Sacramento(916)373-5600 11 of 831 Evergreen Packaging Sample ID: SITE 4A COMMON CARP Trace Level Organic Compounds SW846 8290 Lot-Sample N_. GIH230506-002 Work Ordertl. Nff"lAC Matrix....: BIOLOGICAL, Date Sampled_..: 08/01/11 Date Received...: 08/23/11 Dilution Factor; 0.93 Prep Date....: 08/31/11, Analysis Date....: 09/19/11 Prep Batch 0....: 1243084 Instrument ID..... 3D5 loltial Wgt/Vol: 10.66 g Analyst ED....c . Michael Ng REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS 2,3,7,8-TCD1) 0.83 _ J 0.94 0.065 Pgfg Total TCDD 0.83 0.94 0.065 P919 1,2,3,7,8.PeCDD ND 4.7 0.23 13E18 Total PeCDD ND 4.7 0.23 Pgfg. 1,2,3,4,7,8-HxCDD ND 43 0.82 Pg/g 1,2,3,6,7,8-HxCDD 32 J 4.7 0.093 119/9 1,2,3,7,8,9-HxCDD ND 4.7 0.71 PA Total HxCDD 32 4.7 0.095 pgfg 1,2AA6,7,8-HxCDD 21 4.7 0.22 Pgfg Total HpCDD 29 4.7 6.22 pgfg /- OCDD 73 9.4 036 pgfg 2,3,7,8-TCDF 2.5 CON 0.94 022 Pgf9 Total TCDF 4.7 0.94 0.10 pgfg 1,2.3,7,8.PeCDF ND 4.7 1.7 PA 2,3,4,7,8-PeCDF ND 4.7 1.3 PA Total PeCDF ND 4.7 1.7 p8/8 1,2,3,4,7,8-HxCDF ND 4.7 1.4 PA 1,V,6,7,8-4xCDF 10 4.7 0.068 pg1g 2,3,4,6,7,8-HxCDF ND 4.7 0.077 138/9 1,2,3,7,8,9-HxCDF ND 4.7 0.094 P919 Total HxCDF 10 4.7 0.080 Pgfg 1,2,3,4,6,7,8-HpCDF, 43 J 4.7 0.27 PA 1,2,3,4,7,8,9-HpCD15 ND 4.7 0.32 P919 Total HpCDF 43 4.7 0.29 pgfg OCDF 8.1 J 9.4 0.16 pg'g \`q.a qll\QASAppASOG_Smd\EDL-tL_RVOMWt 9/232011 G1 H230506 TestAmerica West Sacramento(916)373-5600 12 of 831 Evergreen Packaging Sample ID: SITE 4A COMMON CARP Trace Level Organic Compounds SW846 8290 Lot-.Sample#....: GIH230506-002 Work Order#....: MLX8FIAC Matrix....: BIOLOGICAL Date Sampled....: 08/01/11 Date Received.._: 08/23/11 Dilution Factor: 0.93 Prep.Date....: 08/31/11 Analysis Date....: 09/19/11 Prep Batch#....: 1243084 Instrument ID—.* 3D5 Initial WgUVol: 10.66 g Analyst ID....: Michael Ng PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIhIITS 13C-2,3,7.8-TCDD 67 40-135 13C-1,2,3,7,8-PeCDD 65 40-135 13C-1,2,3,6,7,8-HxCDD 71 40- 135 13C-1.2,3,4,6,7,8-HpCDD 67 40-135 13C-OCDD 67 40-135 13C-2,3,7,8-TCDF 66 40-135 13C-1,2,3,7:8-PeCDF 66 40-135 1361,2,3,4,7,8.HxCDF 73 40-135 13C-1,2,3,4,6,7,8-HpCDF 70 40-135 OUALIFIERS CON Confirmation analysis. I Estimated Result l \\gsacsgll\QDSApps\SGG-Smd\EDL-Rt�RgwrLrpt 9/23/2011 G1H230506 TestAmerica West Sacramento(916)373-5600 13 of 831 Evergreen Packaging Sample 7D: SITE 4B CHANNEL CAT Trace Level Organic Compounds SW946 8290 Lot-Sample#-...: GIH230506-003 WorkOrder#__: MLX8GIAC Matrix...: BIOLOGICAL Date Sampled....: 08/02/11 Date Received....: 08/23/11 Dilution Factor: 0.98 Prep Date....: 08/31/11 Analysis Date....: 09/20/11 Prep Batch 0....: 1243084 Instrument ID....: 3D5 Initial WgHvol: 10.14 g Analyst m...: Michael Ng REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNTTS 2�3,7,8-TCDD 1.7 0.99 0.060 p919 Total TCDD 1.7 0.99 0.060 pg/g 1,2,3,7,8-PeCDD ND 4.9 1.2 Wit Total PeCDD ND 4.9 1.2 Pg(g 1,2,3,4,7,8-HxCDD ND 4.9 1.2 pg/g 1,2,3,6,7,8-HxCDD 3.7 J 4.9 0.087 pg/g 1,2,3,7,8,9-HxCDD ND 4.9 0.57 pg/g Total HxCDD 3.7 49 0.099 pg/g 1,2,3,4,6,7,8-HpCDD 13 4.9 0.16 pg/g Total HpCDD 16 4.9 0.16 P919 OCDD 37 9.9 0.25 PR/g 2,3,7,8-TCDF 1.8 CON 0.99 0.24 PF/g Total TCDF 4A 0.99 0.068 pg/g 1,2,3,7,8-PeCDF ND 4.9 1.1 pg/g 2,3,4,7,8-PeCDF ND 4.9 1.5 pglg Total PeCDF ND 4.9 1.5 Pg/g 1,2,3,4,7,8-HxCDF ND 4.9 0.92 pg/g 1,2,3,6,7,8-HxCDF 3.1 J 4.9 0.066 Pgf9 2,3,4,6,7,8-HxCDF ND 4.9 0.075 pg/g 1,2,3,7,8,9-HxCDF ND 4.9 0.091 pgfg Total HxCDF 3.1 49 0.077 pg/g 1,2,3,4,6,7,8-HpCDF ND 4.9 1.4 pg/g 1,2,3,4,7,8,9-HpCDF ND 4.9 0.23 pg/g Total HpCDF ND 4.9 1.4 PA OCDF ND 9.9 0.39 pg(g %%gsacsgll%QDSAppsISOG_Stnd%DL RL-Rq*mrpt 9/23/2011 GIH230506 TestAmerica West Sacramento(916)373-5500 14 of 831 Evergreen Packaging Sample ID: SITE 4B CHANNEL CAT Trace Level Organic Compounds SW946 5290 Loot-Sample#....: GIH230506-003 Work Order#._.: MLXBGIAC Matrix....: BIOLOGICAL Date Sampled....: 08/02/11 Date Received....: 08/23/11 Dilution Factor: 0.98 Prep Date....: 08/31/11 Analysis Date_..: 09/20/11 Prep Batch#....: 1243084 Instrument ID....: 3D5 Initial Wgt(Vol: 10.14 g Analyst ID....: M)chael Ng PERCENT RECOVERY INTERNALSTANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 77 40-135 13C-1,2,3,7,8-PeCDD 75 40-135 13C-1,2,3,6,7,8-HxCDD 67 40-135 13C-1,%3A,6,7,8-HpCDD 73 40-135 13C-OCDD 67 40-135 13C-2,3,7,8-TCDF 75 40-135 13C-1,2,3,7,8-PeCDF 79 40-135 13C-1,2,3,4,7,8-HxCDF 74 40-135 13C-1,2,3,4,6,7,8-HQCDF 76 40-135 QUALIFIERS CON Confimnation analysis. _ I Estimated ResolL &Lsacsgll lQDSApps1500_StndeDL-RL-Report ryt 9/2312011 G1 HZ30506 TestAmerlca West Sacramento(916)373-660 15 of 831 Evergreen Packaging Sample ID: SITE 4B COMMON CARP Trace Level Organic Compounds SW846 9290 Lot-Sample#_..: GIR230506-004 Work Order#.-.: MLX8HIAC Matrix._.: BIOLOGICAL Date Sampled....: 08/02/11 Date Received....: 08/23/11 Dilation Factor: 0.96 Prep Date...: 08/31/11 Analysis Date..: 09/20/11 Prep Batch#....: 1243084 Instrument D)_.: 3D5 Initial Wgt/Vol: 10.4 g Analyst LD....: Michael Ng REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS 2,3,7,8-TCDD 1.1 0.96 0.043 pg/g Total TCDD 1.1 0.96 0.043 pgfg - 1,2,3,7,8-PeCDD ND 4.8 0.20 pg/g Total PeCDD ND 4.8 0.20 pg/g 1,2,3,4,7,8-HXCI)D ND 4.8 1.2 pg/g 1,2,3,6,7,8-HxCDD 3.9 J 4.8 0.050 pg/g 1,2,3,7,8,9-HxCDD ND 4.8 0.68 p9(9 Total HxCDD 3.9 4.8 0.057 pg/g 1,2A,4,6,7,8-HpCDD 19 4.8 (,20 pg/g Total HpCDD 22 4.8 0.20 p9t9 OCDD 52 9.6 0.27 pg/g 2,3,7,8-TCDF 2.6 CON 0.96 0.20 pg/g Total TCDF 4.4 0.96 0.078 pg/g 1,2,3,7,8-PeCDF ND 4.8 1.7 pg/g 2,3,4,7,8-PeCDF ND 4.8 1.6 pg/g Total PCCDF ND 4.8 1.7 118/9 1,2,3,4,7,8-HXCDF ND 4.8 1.2 pglg 1,2,3,6,7,8-HzCDF 8.4 4.8 0.11 pg/g 2,3,4,6,7,8-NxCDF ND 4.8 0.12 pg/g 1,2,3,7,8,9-NxCDF ND 4.8 0.15 P919 Total HzCDF 8.4 4.8 0.12 pg/g 1,2,3,4,6,7,8-HpCDF ND 4.8 1.2 pg/g 1,2,3,4,7,8,9-HpCDF ND 4.8 0.20 pg/g Total HpCDF ND 4.8 1.2 Pg/g , OCDF ND 9.6 0.26 pg/g %)gncsglllQDSApps\SOG_Smd1EDt-RL-Reporupt 9/2312011 GIK230505 TestAmerlea West Sacramento(916)373-5600 16 of 831 Evergreen Packaging Sample ID: SITE 4B COMMON CARP Trace Level Organic Compounds SW846 8290 Lot-Sample#....: GIH2305D6-004 WorkOrder#....: MLX8HIAC Matrix.... BIOLOGICAL Date Sampled—*. 08/02/11 Date Received....: 08/23/11 Dilution Factor. 0.96 Prep Date....: 08/31/11 Analysis Date...: 09/20/11 Prep Batch#....: 1243094 Instrument M_.: 3D5 Initial Wgt/Vol: 10A g Analyst ID._: Michael Ng PERCENT RECOVERY EMRNAL STANDARDS- RECOVERY LIMITS 1362,3,7.E-TCDD 86 40-135 13C-1,2,3,7,8-PeCDD 78 40-135 13C-1,2,3,6,7,8-HxCDD 82 40-135 1361,2,3.4,6,7;8-HpCDD 78 40-135 ,. 13C-OCDD 70 40-135 13C-2,3,7,8-TCDF 84 40-135 13C-1,2,3,7,8-PeCDF 80 40-135 13C=1,2,3,4,7,8-HxCDF 81 40-135 1361,2,3,4,6,7,8-HpCDF 82 40-135 QUALIFIERS CON Confimudonanalysis: J Funimated Resale Ngsar gll\QDSApps%SOG_Smd1E0L RL_ReporLrpt 9/23/2011 GIH230506 TestAmerica West Sacramento(915)373-5600 17 of 831 1 Evergreen Packaging Sample ED: SITE 4B COMMON CARP WB Trace Level Organic Compounds SW846 8290 Lot-Sample H. GIH230506-005 Work Order 0...... MLX8JIAC Matrix....: BIOLOGICAL Date Sampled...: 08/02/11 Date Received...: 08/23/11 Dilution Factor: 0.99 Prep Date...: 09/31/11 Analysis Date...: 09/20/11 Prep Batch#....: 1243084 InstrumentID....: 3D5 Initial Wgt/Vol: 10.1 g Analyst ID.._: Michael Ng REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS 2,3,7,8-TCDD 23 0.99 0.065 pg/g Total TCDD 23 0.99 0.065 pg/9 1,2,3,7,8•PeCDD 25 J 5.0 032 pg/g Total PeCDD 25 5.0 032 pg/g 1,2,3,4,7,8-HxCDD ND 5.0 2.3 pg/g 1,2,3,6,7,8-HxCDD 7.0 5.0 0.094 p9f9 1,2,3,7,8,9-HxCDD ND 5.0 1.0 PY/B Total HxCDD 7.0 5.0 011 PP/g 1,2,3,4,6,7,8-HpCDD 35 5.0 0.29 p9/g Total HpCDD 53 5.0 0.29 pg/g OCDD 200 9.9 0.42 JI& 2,3,7,8-TCDF 6.0 CON 0.99 0.29 119/9 Total TCDF 11 0.99 0.098 pg/g 1,2,3,7,8-PeCDF 3.6 J 5.0 0.23 pg/g 2,3,4,7,&PeCDF 3.0 J 5.0 0.24 pg/g Total PeCDF 6.6 5.0 0.24 pg/g 1,2,3,4,7,8-HxCDF 2.7 J 5.0 0.093 pg/g 1,2,3,6,7,8-HxCDF 20 5.0 0.075 p9/g 2,3,4,6,7,8-HxCDF ND 5.0 0.085 P919 1,2,3,7,8,9-HxCDF ND 5.0 0.10 P919 Total HxCDF 23 5.0 0.088 P& 1,2,3,4,6,7,8-HpCDF 3.1 J 5.0 030 W9 1,2,3,4,7,8,9-HpCDF ND 5.0 0.36 pg(g Total HpCDF 3.1 5.0 032 P919 OCDA ND 9.9 0.34 P919 L \lgsacsgll\QDSApps\S00_Smd%EDL_R1lteponzpt 9/23/2011 GIH230506 TestAmerica West Sacramento(916)373-5600 18 of 831 Evergreen Packaging Sample ID: SITE 4H COMMON CARP VVB Trace Level Organic Compounds SW846 8290 Lot-Sample#„..: GIH230506-005 Work Order#....: MLX8JIAC Matrix...: BIOLOGICAL, Date Sampled...: 08/02/11 Date Received....: 08/23/11 Dilution Factor: 0.99 Prep Date...: 08/31/11 Analysis Date....: 09/20/11 Prep Batch 9....: 1243084 Instrument JD._.: 3D5 Initial Wgt/Vol: 10.1 g Analyst ID....: Michael Ng PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 70 40-135 I3C.1,2,3,7,8-PecDD 64 40-135 13C-1,23,6,7,8-HxCDD 73 40-135 13C-1,2.3,4,6,7,8-HpCDD 70 40-135 13C-OCDD 67 40-135 13C-2,3,7,8-TCDF 71 40-135 13C-1,2,3,7,8-PeCDF 66 40-135 13C-1,2,3,4,7,8-HxCDF 77 40-135 13C-1,23,4,6,7,8-HpCDF 73 40-135 OUALIFIERS - CON Confumafion analysis. I Fstimatcd Resu1L @gsacsgi 11QDSApps1.SOG_Smd1EDL,RL-lepaa-cpt 9/23/2011 Gt H230506 TestAmerica West Sacramento(916)373-5600 19 of 831 t , QC DATA ASSOCIATION SUMMARY GIR230506 Sample Preparation and Analysis Control Numbers ANALYTICAL LEACH PREP SAMPLE# MATRIX METHOD BATCH # BATCH # MS RUN# 001 BIOLOGIC SW846 8290 1243084 BIOLOGIC SW846 8290 1243088 002 BIOLOGIC SW846 8290 1243084 BIOLOGIC SW846 8290- 1243088 003 BIOLOGIC SW846 8290 1243084 BIOLOGIC SW846 8290 1243088 004 BIOLOGIC SW846 8290 1243084 BIOLOGIC SW846 8290 1243088 005 BIOLOGIC SW846 8290 1243084 BIOLOGIC SW846 8290 1243088 f GIH230506 TestAmerica West Sacramento(916)373-6600 20 of 831 Method Blank Report Trace Level Organic Compounds SW846 8290 Lot-Sample 9....: GIH310000-084B Work Order9._: ML57W1AA Matrix-_: BIOLOGICAL Date Sampled....: 08/01/11 Date Received....: 08/23/11 Dilution Factor: I Prep Date....: 08/31/11 Analysis Date....: 09/03/11 Prep Batch 5....: 1243084 Instrument ID_..: 4D5 Initial WgWol: log Analyst ID...: Michael Ng REPORTING ESTIMATED PARAMETER RESULT LIMIT DETECTION LIMIT UNITS 2,3,7,8-TCDD ND 1.0 0.027 PP/8 Total TCDD ND 1.0 0.027 139/8 1,2,3,7,8-PeCDD ND 5.0 0.14 P918 Total PeCDD NO 5.0 0.14 pg19 1,2,3,4,7,8-HxCDD ND 5.0 0.22 F%/8 1,2,3,6,7,8-HxCDD NO 5.0 0.19 p8/9 1,2,3,7,8,9-HxCDD ND 5.0 0.19 P919 Total HxCDD ND 5.0 0.22 i' P919 1,2.3,4,6,7,8-HxCDD ND 5.0 0.43 p8/8 Total HpCDD ND 5.0 0.43 pg/g OCDD NO 10 0.99 pg/g 2,3,7,8-TCDF ND 1.0 0,20 pg/g Total TCDF ND 1.0 0.20 pg/g 1,2,3,7,8-PeCDF ND 5.0 0.077 Pg1g 2,3,4,7,8-PeCDF NO 5.0 0.085 P818 Total PeCDF ND 5.0 0.085 PA 1,2,3,4,7,8-HxCDF NO 5.0 0.10 pg1g 1,2,3,6,7,8-HxCDF ND 5.0 0.094 pB/8 2,3A,6,7,8-HxCDF ND 5.0 0.10 pg/g 1,2,3,7,8,9-HxCDF ND 5.0 0.11 PA Total HxCDF ND 5.0 0.11 p8/g 1,2,3,4,6,7,8-HpCDF ND 5.0 0.18 13918 1,2,3,4,7,8,9-HxCDF ND 5.0 0.21 139/8 Total HpCDF ND 5.0 0.21 pg/g OCDF NO 10 0.20 pP/g %t4mcsglltQDSApps150G_Smd1EDIiRL,tcPmtrPt 9123/Ml1 GIR230506 TestAmerica West Sacramento(916)373-5600 21 0£831 Method Blank Report Trace Level Organic Compounds SWS"8290 Let-Sample#—.. GIH310OW-094B Work Order#.._: W57WIAA Matrix....: BIOLOGICAL Date Sampled....: 08/01/11 Date Received_..: 08/23/11 Dilution Factor: 1 Prep Date—: 08/31/11 Analysis Date...: 09/03/11 Prep Batch# 1243094 Instrument ID....: 4135 Initial Wgt/Vol: 108 Analyst ID....: Michael Ng PERCENT RECOVERY INTERNALSTANDARDS RECOVERY LEMTS 13C-2,3,7,8-TCDD 71 40-135 13C-1,2,3,7,8-PeCDD 69 40-135 13C-1,2,3,6,7,8-HxCDD - 84 40-135 13C-1,2,3,4,6.7,8-HpCDD 69 40-135 ' 13C-OCDD 69 40-135 13C-2,3,7,8-TCDF 71 40-135 13G1,2,3,7,8-PeCDF 71 40-135 13C-1.2.3,4,7,8-HxCDF 72 40-135 13C-1,2,3,4,6,7,8-HpCDF 72 40- 135 OUALIFIERS --, Results and repotting limits have been adjusted for dry weight t � Pq=c qll\QDSApps\SQG_Smd1EDL—RL-Rewaipt 9/23/2011 G1H230506 TeslAmerlca West Sacramento(916)373-6600 22 of 831 LABORATORY CONTROL SAMPLE DATA REPORT Trace Level Organic Compounds Client Let#...: G1H230506 Work Order#...: AIL57WIAC-LCS Matrix.._.....: BIOLOGICAL LCS MtSample#: GIH310DOO-084 Prep Date......: 08/31/11 Analysis Date_: 69/03/11 Prep Batch#...: 1243094 Dilution Factor: 1 AnalystED—..: Michael Ng Instrument ID..: 4D5 Method__: SW846 8290 Initial WgtlVol: log SPIKE MEASURED PERCENT RECOVERY PARAMETER AMOUNT AMOUNT UNITS RECOVERY LIMITS 2,3,7,8-TCDD 20.0 18.8 pg/g 94 (50-150) 1,2,3,7,8-PeCDD loor 953 pg/g 95 (SO-ISO) 1,2,3,4,7,8-HxCDD 100 90.9 pg/g 91 (50-150) 1,2,3,6,7,8-I1xCDD 100 93.8 pg/g 94 (50-150) 1,2,3,7,8,9-HxCDD 100 93.8 pg/g 94 (50-150) 1,2,3,4,6,7,8-HpCDD 100 100 pg/g 100 (50-150) OCDD 200 215 pg/g 107 (50-150) 2,3,7,8-TCDF 20.0 21.3 pg/g 107 (50-150) 1,2,3,7,8-PeCDF 100 103 pg/g 103 (50-150) 2,3,4,7,8-PeCDF 100 109 pg/g 168 (50-150) 1,2,3,4,7,8-13xCDF 100 102 pg/g 102 (50-150) ?.-%3,6,7,8-HpCDF 100 114 pg/g 114. (50-150) 3,4,6,7,8-HxCDF 100 107 pgJg 107 (50-150) =2,3,7,8,9-HxCDF 100 109 pg/g 109 (50-150) 1,2,3,4,6,7,8•HpCDF 100 110 pg/g 110 (50-150) 1,2,3,4,7,8,9-I1pCDF 100 106 Wig 106 (50-150) OCDF 7.00 243 pg/g 122 (50-150) PERCENT RECOVERY, INTERNALSTANDARD RECOVERY LIMITS 13C-2,3,7,E-TCDD 82 (40- 135) 1341,2,3,7,8-PeCDD 82 (40- 135) 13C-1,2,3,6,7,8-HxCDD 89 (40-135) 1341,2,3,4,6,7,8-HpCDD 73 (40- 135) 13C-OCDD 72 (40 135) 13C-2,3,7.8-TCDF 83 (40-135) 13C-1,2,3,7,8-PeCDF 82 (40-135) 13C-1,2,3.4,7,8-HpCDF 82 (40-135) 13C-1,2,3,4,6,7,8-HpCDF 79 (40- 135) Notes: Calculations=pnfoanedlcfoa:mandingto avoid mandoRertominralddatcdn alts. Bold prim denotes co Wpammdws - 1�asq IIIQDSAppsISOG SidISOG Stnd laded mvl.rpt 9/2312011 G1H230506 TestAmerlca West Sacramento(916)373 600 23 of 631 • Vista Analytical Laboratory November 29, 2011 Vista Project I.D.: 33436 Mr. Nick McCracken Evergreen Packaging 175 Main Street Drop 56A Canton,NC 28716-4331 Dear Mr. McCracken, Enclosed are the results for the four fish tissue samples received at Vista Analytical Laboratory on November 2, 2011 under your Project Name "Waterville Lake - Fish Tissue". This work was authorized under your Purchase Order No. 423393. These samples were extracted and analyzed using EPA Method 8290 for tetra-through-octa chlorinated dioxins and furans. A standard turnaround time was provided for this work. Vista Analytical Laboratory is committed to serving you effectively. If you require additional information,please contact me at 916-673-1520 or by email at calvin@vista-analytical.com. Thank you for choosing Vista as part of your analytical support team. Sincerely, a1c, � Calvin Tanaka Senior Scientist K eea q a'sr.4402N.yz` Vista Analytical lnboromry certtfres that the report herein m en meets all the rnquiremtssr/forth hyNF.LACfor those applicable lest melhodr.Results relate only to the sam cs as received b the laboratory.-This re ri should not be reproduced exce t in ! +4 Y P!' Y P^ P P jw - Z�l w6hout the written approval of Vista Analytical Laboratory t sy Vista Analytical Laboratory 1104Windfield Way El Dorado Hills,CA 95762 ph:916-673-1520 I fx:916-673-0106 I wwww.vista-analytical.com c ` Table of Contents CaseNarrative............................................................................................. I Tableof Contents........................................................................................ 2 SampleInventory......................................................................................... 3 AnalyticalResults........................................................................................ 4 Qualifiers..................................................................................................... I 1 Certifications............................................................................................... 12 SampleReceipt............................................................................................ 13 Project 33436 Page 2 of 15 Section I: Sample Inventory Report Date Received: 11/2/2011 r Vista Lab.ID Client Sample ID 33436-001 Site 4A channel cat L-fillets (5) 33436-002 Site 4A common carp L-fillets (5) 33436-003 Site 4B channel cat L-fillets (5) 33436-004 Site 4B common carp L-fillets (5) Proiect33436 Page 3 of 15 ANALYTICAL RESULTS Project 33436 Page 4 of 15 Method Blank EPA Method 8290 Matrix: Tissue QC Batch No.: 4106 Lab Sample: 0-MB001 Sample Size: 10.0 g Date Extracted: 21-Nov-11 Date Analyzed DB-5: 23-Nov-11 Date Analyzed DB-225: NA Analyte Cone. (pW9) DL a EMPC b Qualifiers Labeled Standard %R LCL-UCLd Oualifiers 2,3,7,8-TCDD.:----'---__..ND _..._ _.0.0542 IS_.. 13C 2;3,7;8^TCDD_ _ . _ ._ .._.-81.0-- -_. 40 135__ 1,2,3,7,8-PeCDD ND 0.0868 13C 1 2 3,7,8-PeCDD 84.8 40 135 1,2,3,4,7,8_HxCDD, D, .._ - _ 0 150__. ____..:...,. _. _. 13C_1,2 3 4 7,8 HXCDD_ .__ _96 2 . 40 -135_ ---- _ 1,2,3,6,7,8-HxCDD ND _ 0_168 __. 13C 123,6,7,8-HxCDD 95.4 40- 135 ._-ND .._.___-- 0.152_..---- -__ ___... _- `-- --.---13C-1 2 3,7,8,9 HxCDD_ __ 95 5 ._..,_ 40. 135_„ 1,2 3 4,6 7 8 HpCDD ND 0.0875 - 13C 1 2 3,4,6,7,8-HpCDD 93.7 40- 135 0165 J _.._ - _. 13C;OCDD .. _. 81:4 _40- 135_ _- ---- TCDF ND 0.0374 _ p_13C 2 3,7,8-TCDF 89.1 40- 135 _ _ r - _. _ �> 00,335 w— �� -..> . 13C12,3;7,8_-PeCDF — r 91_3 _ 40 _135 _. YND_ _0.00338 —_ 13C 2 3 4,7,8-PeCDF 89.2 40- 135 1,2;3,4,9,8 HxCDF__.__.,., 00316___-y—.---_- 40_135_ - _.-NDy0.0318 13C 1,2,3,6,7,8-HxCDF^ W - �96.7 40e 135 - - 2,3,4,6,7,8-HxCDF__------ND----... --,-0.0403 _ _;1_3G_2 3, A7,8 HzCDF - 84_2 40.135 1,2,3,7,8,9-HxCDF ND 0.0547 _ --^_` - 13C-1,2,3,7,8,9-HHxCDF^ 81.1 40- 135 1,2;3y4,6,7,8 HpCDF__----_ ND_ __ _: 0_0629 ._» - ._ � n__��a ,_. 13C_1,2;3 467;8HpCDF- ,_.,. -,70 3 J_ 40135 1,2,3,4,7 8 9,HpCDF _ ND 0.0601 13C 1 2,3,4,7,8,9_HpCDF 75.7 40 135 0.0704 CRS 37C1-2,3,7,8-TCDD 90.1 40- 135 Totals Toxic Equivalent Quotient(TEQ)Data e Total TCDD�_K_ , ND�. 0116 m._ TEQ(Mm) -_ ___j.0000495 Total PeCDD ND 0.179 Total HXCDDLL __ND _,. 01412 :.. aS-ple specifc estimated detechon>limtr4-___ __...e..m._ t _ ...._. Total HpCDD ND 0,0875 b Estimated maximum possible concentration Total TCDF ND:.______ 0 0374 c Method detection limit _ _ __._..---_-_ ._..__.___�..____. ._ ...,._._.�.. _.__ --.._._ __ I.--I-------,-- _._.—_,_.. __- Total PeCDF ND 0.0336 d.Lower control limit-upper control limit. Total:HXCDF , 1ID , _ 0396 _ e TEgl a ed on Q(05),World_HeafthOrganr�a i n Toxic Equivalent Factors(WHO) Total HpCDF ND 0.0615 Analyst: FEB Approved By: Calvin Tanaka 29-Nov-201109:56 Project33436 Page 5 of 15 OPR.Results: - - - EPA Method 8290 Matrix: Tissue QC Batch No.: 4106 Lab Sample: 0-OPR001 Sample Size: 10.0 g Date Extracted: 21-Nov-11 Date Analyzed DB-5: 23-Nov-11 Date Analyzed DB-225: NA Analyte Spike Cone. Cone.(ng/mL) OPR Limits Labeled Standard %R LCL-UCL Qualifier 2 3 7,8:TCDD 10.0 8.65 7 13 IS 13C 2 3 7 8 TCDD . 86.8 40 135 1,2,3,7,8-PeCDD 50.0 46.2 35-65 13C 1,2,3,7,8-PeCDD 88.9 40- 135 1 2,3;4,7,8 HxCDD 50-0 46.9 35 65 13C.1,2,3,4,7,8 HxCDD 97.9 40_135 1,2,3,6,7,8-HxCDD 50.0 45.2 35-65 13C-1,2,3,6,7,8-HxCDD 101 40- 135 1,2,3;7,8,9-HxCDD 50:0 46.4 35 -65 13C 1;2,3 7,8,9 HxCDD 99.3 40 135 1,2,3,4,6,7,8-HpCDD 50.0 42.9 35 -65 13C-1,2,3,4,6,7,8-HpCDD 90.0 40- 135 OCDD, 100 96.6 70- 130 13C OCDD 78.8 40 135 2,3,7,8-TCDF 10.0 -8.25 ,7_13_-_ 13C-2,3,7,8-TCDF 93.6 _...: _40- 135 1;2;3,7,8 PeCDF yv 50.0 42 8 - 35 65T _ ��13C 1,2,37;8-PeCDF•. �_ ,_-,- _97.8 40 135' _ 50.0 42.4 35 -65 13C-2,3,4,7,8-PeCDF 95.5 40- 135 - 1,2,3y4,7,8-HxCDF 50.0 46:0• - 35-65 P3C 1 2 3 47,8-HxCDF . 92.6 40 135 : _ 1,2,3,6,7,8-HxCDF 50.0 43.0 35-65 13C-1,2,3,6,7,8-HxCDF 97.0 40- 135 23 4 6-7 8 HxCDF' 50.0 .44.3 T.` _ 35 65 _ 13C-2;3 4 6 7,8 HxCDF 86.3. 40135- `1,2,3,7,8,9-HxCDF 50.0 43.6 35-65 13C-1,2,3,7,8,9-HxCDF 85.5 40- 135 v- _---- - - 1,2,3,4,E 7 8 HpCDF 50'.0 47.1 35-65 13C 1 2,3,4 6,7 8 H CDF`' 72`2 40 135, __ .--- _.p .__ 1,2,3,4,7,8,9-HpCDF 50.0 47.0 35-65 13C-1,2,3,4,7,8,9-HpCDF 74.4 40- 135 OCDF 100 86.4 70= 130 13C-OCDF 74.5 40- 135 CRS 37C1-2,3,7,8-TCDD 94.4 40- 135 Analyst: Approved By: Calvin Tanaka 30-Nov-2011 13:13 Project 33436 Page 6 of 15 Sample 1D: Site 4A channel cat L-fillets(5) EPA Method 8290 Client Data Sample Data Laboratory Data Name: Evergreen Packaging Matrix: Tissue Lab Sample: 33436-001 Date Received: 2-Nov-11 Project: Waterville Lake-Fish Tissue Sample Size: 10.1 g QC Batch No.: 4106 Date Extracted: 21-Nov-11 Date Collected: 1-Aug-11 o Date Analyzed DB-5: Date Analyzed DB-225: Time Collected: 1452 /oLipids: 2.95 Yz 23-Nov-11 Y NA Analyte Conc. (pg/g) DL a EMPCb Qualifiers Labeled Standard %R LCL-UCLd Oualifiers IS 13C-2 3 7 8-TCDD__ 80.4 40-135___ _..- _ - 1 2 3,7,8 PeCDD 4_._ ND . --- _. 0.304 13C-1 2 3 7,8=PeCDD 79.3 40- 135 _1,2;3,4,7,8_HxCDD___0.169i. 7,8-HxCDD 135, _.,_. _ _93 0 40`= ' _ --- 1,2,3,6,7,8_HxCDD 0.768 _ __ . _ -_._._J __. yl3C-1 2 3 6,7,8-HxCDD 90.8 40- 135 1,2;3,7,8,9_HxCDD ND _. . .__._ ._ _..._0;187 _-- __ . . __ ..--_-- 13C-1,2,3,7,8;9-HxCDD___.. _ . _ 89 8 40- 135 1,2,3,4,6,7,8-HpCDD.. 0.727 _ 7._—_ . ,13C�1,2,3,4,6,7,8-HpCDD - 88.8 40- 135 _ OCDD__ , _ --_-- 1.34 _.1.3C_0CDD_ _ _ __.____ .. _ _ ___ 742-- _40. 135__.- 2,3,7,8-TCDF_ __ ND -� 0.0427 _ m- _ __.13C 2 3----TCDF T_81 7 40�135 , . — ------ 1,2,3,V PeCDF,-- _- ND_`._ _ , _ 0A442_y __. ...j.. _ ___ _ -1`3C-1 2 3 7,8-PeCDF._", ._.. _ _;:82 6_._ 40-135 2,3,4,7,8_PeCDF _ 0,256J_..., 13G23,4,7,8;PeCDF v 814 40_135 _ 78 8 _40-- 13.3 1,2,3,6,7,8-HxCDF _ 0 0638 - __ _.- ___---__.__-_.- .____.. .__- J- ___..__. 13C-1 2 3 6,7,8 HxCDF� 86.1 40- 135 . .___ 2,3,4;6,7,8-HxCDF _ - OA742 _ _ - �_. _.,.._ _ _ _ _ J_.- __13G2 3,4,6;7,8 HxCDF"-___ 83_4 40 ,135 1,2 3,7,8 9 HxCDF _ -.> ._._.. __ _ _ . , 0.0566 ._�__.._. .__. 13C 1 23,7.8,9-HxCDF _ _-____75;5_ 40- 135 1,2,3,46,7,8 HpCDF,._;ND`" 0.0852 s R--.�. _ _ _ 13C 1,2,3 4 6,7 8 HpCDF.:__. _:64 6 40'-135 1,2,3A7,8,2-4P F ._ ND _..._ 0.0829 y_. _ _ .__- 13C_1 2 3,4,7,8,9-HpCDF _ 70.3 40- 135 OCDF - - 1VD--. , .. -- -- - -0 0590 ,— .s. .. . 13C-OCDF_ _.. -._ .._ _69 7 40, 135 CRS 37C1-2,3,7,8-TCDD 92.5 40- 135 Totals Toxic Equivalent Quotient(TEQ)Data e Total TC ------_ . -0300_ — - _ TEQ(Min) �_0.500 :_- -- - - -- -_ .._ __ Total PeCDD ND Total'.HxCDD._ ,,--0.937- _ _ a Sample specific estimated detection limit. Total H CDD 0.727 b.Estimated maximum possible concentration. Total,TCDF__. ND _ _0;0427 c.Method detechontimit. Total PeCDF 0.256 d Lower control limit upper control limit. _Total HXCDF_-_ 0:222 _ ._,.. _ _ _.. _ e TEQbased on(2005)World'Health C rgawzatmn Toxic Equivalent Factors(WHO)— _. ._ .. _ .. __. _ _. _ ___.._,_._..�___... .. ,. .d__ Total HpCDF ND 0.0840 Analyst: ANP Approved By: Calvin Tanaka 30-Nov-2011 13:13 Proiect 33436 Page 7 of 15 Sample ID: Site 4A common carp L-fillets (5) EPA Method 8290 Client Data Sample Data Laboratory Data Name: Evergreen Packaging Matrix: Tissue Lab Sample: 33436-002 Date Received: 2-Nov-11 Project: Waterville Lake-Fish Tissue Date Extracted: 21-Nov-1 I Sample Size: 5.14 g QC Batch No.: 4106 Date Collected: 1-Aug-11 o Date Analyzed DB-5: Date Analyzed DB-225: Time Collected: 1602 /oLipids: 11.7 yz 23-Nov-11 y NA Analyte Cone. (pg/g) DL a EMPCb Qualifiers Labeled Standard %R LCL-UCLd Oualifers 2,3,7,8_TCDD , 13C-2,3,7,8-TCDD 1. _ _ 82.3 40- 135 1.24 IS 1,2,3,7,8-PeCDD 1.52 -_ _ _ _ _ J_ _ 13C-1,2,3,7,8-PeCDD 80.6 40- 135 l,2,3,4;7,87HxCDD. _ 1.05 _-- - J.. l3C 1,2,3,4,7,8-HxCDD 94.8. 40- 135 1,2,3,6,7,8-HxCDD , 4.09 __ - J _ _ 13C-1,2,3,6,7,8_HxCDD 92.2 40- 135 1,2,3,7,8,9-HxCDD - _.0.664__ _ -- _ -. ._.,.- _ - _ J. 13C-1,2,3,7,8,9-HxCDD 88.5 40-135- _ 1,213,4,6,7,8-HpCDD 11.0 _-__-_, __ -13C-1,2,3,4,6,7,8-HpCDD_ 86.8 40- 135 OCDD - -- 29.4 ._ B - - - _13C-OCDD - .. 70.2 40- 135 2,3,7,8-TCDF _,.. 2.21 _. - - - --- ----- -. ___.._._ .-_--- -.-.- - 13C 2,3,7,8-TCDF - -__ _ - --.82.2 40-_135 - 1,2;3,7,8-PeCDF-_- 0,M13 _ - __- _ -_- -- - , , . J , .- 13G1 2,3,7,8-PeCDF _ 84.8_ ,_40,- 135 2,3,4,7,8-PeCDF 1.51 J_ ._ 13C 2 3 4,7,8-PeCDF 82.4 40- 135 1,2,3,4,7,8-HXCDF 0.987 .. _ -. _ _- J - - -_- _ 13C-1,2,3,4,7,8.HxCDF_- _ _-_ 79.9 40__135 - 1,2,3,6,7,8-HxCDF _- _0.854 J _ 13C 1 2 3,6,7,8-HXCDF 81.1 40- 135 2,3,4,6,7,8-HxCDF _ 0.416 _ _ - J 13C 23,4,6,7,8-HxCDF 84.7 _ 40_135 _ 1,2,3,7,8,9-HxCDF ,ND 0.0928 _- _ _ 13C-1,2,3,7,8,9 HxCDF 73.9 40- 135 1,2,3,4;6,7,8-HpCDF-_ 2.00 _ _ - _ - __J_._ - _13C-1,2,3,4,6,7,8-HpCDF 63.4 40- 135 1,2,3,4,7,8,9-HpCDF_ _ND _ 0.120_ _ _ 13C-1,2,3,4,7,8,9-HpCDF 68.7 40- 135 OCDF ND 0.135 13C-OCDF 67:0_ 40- 135 CRS 37C1-2,3,7,8-TCDD 92.2 40- 135 Totals Toxic Equivalent Quotient(TEQ)Data e Total TCDD.--- ------1.24 -- - - - - TEQ(Min):. 4.40 Total PeCDD 1.52 1.72 Total HxCDD .,5.81- --a._Sample specific estimated detection limit. Total HpCDD 11.0 b.Estimated maximum possible concentration. Total TCDF - 2.21 _ _ - _ - _ c..Method detection limit. _ Total PeCDF 2.64 _ d.Lower control limit-upper control limit. Total HxCDF 2.87 ,.. _ _ 3.00. _ _ e_.T_EQ based on.(2005)World Health Organization Toxic Equivalent Factors.(WHO) Total H CDF 2.00 Analyst: ANP Approved By: Calvin Tanaka 29-Nov-2011 09:56 Project 33436 Page 8 of 15 Sample iD: Site 413 channel cat L-fillets (5) EPA Method 8290 Client Data Sample Data Laboratory Data Name: Evergreen Packaging Matrix: Tissue Lab Sample: 33436-003 Date Received: 2-Nov-11 Project: Waterville Lake-Fish Tissue Sample Size: 10.0 g QC Batch No.: 4106 Date Extracted: 21-Nov-11 Date Collected: 2-Aug-11 P Time Collected: 1100 %Li ids: 5.79 Date Analyzed DB-5: 23-Nov-11 Date Analyzed DB-225: NA Analyte Conc. (pg/g) DL a EMPCb Qualifiers Labeled Standard %R LCL-UCLd Oualifiers 2,3;7,8-TCDD - 0;273. J IS 13C-2,3,7,8-TCDD 82.0 40- 135 1,2,3,7,8-PeCDD 0.363 J 13C-1,2,3,7,8-PeCDD 80.1 40- 135 _1,2,3,4,7,8 HxCDD 0.149 J _ _13C 1,2,3,4,7,8--HxCDD - _ _ 953 40- 135 1,2,3,6,7,8-HxCDD 0.715 J 13C-1,2,3,6,7,8-HxCDD 89.0 40- 135 1,2,3,7,8,9-HxCDD_ _ ND 0.117 13C71,2,3,7,8,9-HxCDD - _ 90.4 - 40- 135 1,2,3,4,6,7,8-HpCDD 0.589 __ -,--J.- l3C-1,2,3,4,6,7_,8-HxCDD 87.1 40- 135 OCDD 1.31 J,B - - 13C-OCDD 68.0 40- 135 . 2,3,7,8-TCDF. . --- -_ND- -- - - 0.0494 _--_ ---_.. _ 1.3C-2,3,7,8-TCDF . ._ _-- --. . 80.7 40- 135 1,2,3,7,8-PeCDF ND 0.0520 _- l.3C-1,2,3,7,8-PeCDF -- 86.5 40- 135 2,3,4,7,8-PeCDF - ND 0.218 _._ 13C-2,3,4,7,8-PeCDF 84.2 40- 135 1,2,3,4,7,8-HxCDF- ND - _ . _ 0.0560 --- __ 13C-1,2',3,4,7,8-HxCDF .__' _- 84.3 40- 135 1,2,3,6,7,8-HXCDF 0.0764 _ -_ - . - J. _ _ 13C 1 2 3,6,7,8 HxCDF 81.7 40- 135 2,3A6,7,8-HxCDF, ND 0.03.93 13C 2,3,4,6,7,8-HxCDF _ - 85,5 - 40- 135 1,213,7,8,9-HxCDF_ -_ND 0.0560 13C-1,2,3,7,8,9-HxCDF 76.1 40- 135 l,2,3,4A7,8-HpCDF--- -0.170 13C l 2 3,4,6,7,8-HpCDF - -, 64.8 40- 135---- 1,2,3,4,7,8,9-HpCDF ND 0.0570 13C-1,2,3,4,7,8,9-HpCDF 67.3 40- 135 OCDF _ - ND .- 0.0880 13C-OCDF 64.9 40- 135 CRS 37CI-2,3,7,8-TCDD 90.8 40- 135 Totals Toxic Equivalent Quotient(TEQ)Data e Total_TCDD - _ 0.273 ____---_- __ TEQ (Min):., 0.738 Total PeCDD 0.363 -Total HxCDD - _ ,0.864_ _ _ _ _- - - _ - _ _-d..Sample specific estimated detection limit. Total HpCDD 0.589 b.Estimated maximum possible concentration. Total TCDF ND 0.0494 C.Method detection limit Total PeCDF ND 0.270 d.Lower control limit-upper control limit. Total HxCDF ., _0.0764 _ - _ - -0.132 _---_-_ - _ e.TEQ based on(2005)World Health Organization Toxic Equivalent Factors_(WHO) Total HpCDF 0.170 Analyst. ANT Approved By: Calvin Tanaka 29-Nov-2011 09:56 Project 33436 Page 9 of 15 Sample ID: Site4B common carp L-fillets (5) EPA Method 8290 Client Data Sample Data Laboratory Data Name: Evergreen Packaging Matrix: Tissue Lab Sample: 33436-004 Date Received: 2-Nov-1 I Project: Waterville Lake-Fish Tissue Sample Size: 5.12 g QC Batch No.: 4106 Date Extracted: 21-Nov-11 Date Collected: 2-Aug-I I o Date Analyzed DB-5: Date Analyzed DB-225: Time Collected: 1400 /oLipids: 17.8 Y 23-Nov-11 Yz NA Analyte Cone. (pglg) DL a EMPCb Qualifiers Labeled Standard %R LCL-UCLd Oualifiers 2,3,7;8-TCDD 2.63-,._ IS 13C72,3,7,8-TCDD 81.2 40- 135 _- 1,2,3,7,8-PeCDD 1.88 J 13C-1,2,3,7,8-PeCDD 78.0 40- 135 1,2,3,4,7,8-HxCDD 1.57_1 - - _ _- .J - - _ - _, 13C-1,2,3,4,7,8-HxCDD_. - 87.0 40-.135_-- 1,2,3,6,7,8-HxCDD _ - 5.63 _- _ _ 13C-1 2,3,6,7,8-HxCDD 88.0 40- 135 1,2,3,7,8,9-HxCDD 0.989y J_ -13C-1,2,3,7,8,9-HxCDD _ __ _ -86.6 40- 135 1,2,3,4,6,7,8-HpCDD 13.7 13C-1 2 3,4,6,7,8-HPCDD 87.8 40- 135 OCDD _ _ 34.1 B 13C-OCDD 69.9 40--135 2,3,7,8-TCDF . -_ _3.20 13C-2,3,7,8-TCDF 79.8 40- 135 1,2,3,7;8-PeCDF- 1.26- J' 13C-11213,7,8_PeCDF _ - 82.2 40-135-_ 2,3,4,7,8-PeCDF -- 2.23 Y _-__ - ___- __ __- . J__ _- - 13C-2 3 4,7,8_PeCDF 81.0 40- 135 1,2,3,4,7,8-HxCDF 13C_ __'1.38 __ __- __. _ _... - . . - J 1,2,M,7,8-HxCDF - _ ___- - 77.8 40- 135 1,2,3,6,7,8-HxCDF_ .- 1.16 _ -_-- _ _-_7 --___ -- 13C-1,2,3,6,7,8-HxCDF 79_9 40- 135 2,3,4,6,7,8-HxCDF _ ND 0.460 _ - -- - _ _ _ 13C-2,3,4,6,7,8-HxCDF 79.1 40--135 1,2,3,7,8,9_HxCDF DID 0.310 13C-1,2,3,7,8,9_HxCDF 72.9 40- 135 1,2,3,4,6,7,8 HpCDF_ 2,12, - - - _ _ __-_ J__ _ 13C-1 2,3 4,6,7,8-H CDF 63.0 _40- 135 . 1,2,3,4,7,8,9-4pCDF - ND 0.114 13C-1,2,3,4,7,8,9-HpCDF 70.1 40- 135 OCDF - - ND - 0.142 13C-OCDF 66.7 40- 135 - CRS 37C1-2,3,7,8-TCDD 88.6 40- 135 Totals Toxic Equivalent Quotient(TEQ)Data e Total TTCDD_ z'63 --- . -- TEQ(Min): . _._ ._6:78 - . Total PeCDD 1.88 Total HxCDD_- 8.19 a.Sample specific estimated detection limit. Total H CDD 14.2 b.Estimated maximum possible concentration. Total TCDF 3.51 ._ _- _ _ - ___ _- - c.Method detection limit. - -. Total PeCDF 3.84 4.09 d.Lower control limit-upper control limit. Total HxCDF- 3.16 3.62 e.T_EQ based on(2005)World Health Organization Toxic Equivalent Factors.(WHO) Total HpCDF 2.12 Analyst: ANP Approved By: Calvin Tanaka 29-Nov-2011 09:56 Project 33436 Page 10 of 15 DATA QUALIFIERS & ABBREVIATIONS B This compound was also detected in the method blank. D Dilution E The amount detected is above the High Calibration Limit. P The amount reported is the maximum possible concentration due to possible chlorinated diphenylether interference. H Recovery was outside laboratory acceptance limits. I Chemical Interference J The amount detected is below the Low Calibration Limit. * See Cover Letter Conc. Concentration r DL Sample-specific estimated detection limit r� MDL The minimum concentration of a substance that can be measured and reported with 99% confidence that the analyte concentration is greater than zero in the matrix tested. EMPC Estimated Maximum Possible Concentration NA Not applicable RL Reporting Limit—concentrations that correspond to low calibration point ND Not Detected TEQ Toxic Equivalency Unless otherwise noted, solid sample results are reported in dry weight. Tissue samples are reported in wet weight. Project 33436 Page 11 of 15 CERTIFICATIONS Accrediting Authority Certificate Number State of Alaska, DEC CA413-2008 State of Arizona AZ0639 State of Arkansas, DEQ 08-0443-0 State of Arkansas, DOH Reciprocity through CA State of California — NELAP Primary AA 02102CA State of Colorado N/A State of Connecticut PH-0182 State of Florida, DEP E87777 State of Indiana Department of Health C-CA-02 Commonwealth of Kentucky 90063 State of Louisiana, Health and Hospitals -LA08000 State of Louisiana, DEQ 01977 State of Maine 2008024 State of Michigan 9932 State of Mississippi Reciprocity through CA Naval Facilities Engineering Service Center NFESC413 State of Nevada CA004132007A State of New Jersey CA003 State of New Mexico Reciprocity through CA State of New York, DOH 11411 State of North Carolina 06700 State of North Dakota, DOH R-078 State of Oklahoma D9919 State of Oregon CA200001-006 State of Pennsylvania 68-00490 State of South Carolina 87002001 State of Tennessee TN02996 State of Texas T104704189-08-TX U.S. Army Corps of Engineers N/A State of Utah CA16400 Commonwealth of Virginia 00013 State of Washington C1285 State of Wisconsin 998036160 State of Wyoming 8TMS-Q Project 33436 Page 12 of 15 ChalnAW Temperature on Receipt• TestAmedca -334�(,,wec Custody Record . Drinking Water? Yes .No qp Tf{E LEADMIN ENVIRONMENTAL TESTING - TAL4124l10an Client �.r• /'fit Pro ect_:Menaget ,�/� / " Datez, Chain of Custody Number �✓ Yee 117� l 1��a�Rr . �y w'�N I1�lc o : . . : � g�©z_ r1 073907 Addiess Telephone Nu er(Area Code)IF&Number s Lab Number yris A`11� Qi7 .�710✓ 7 ( Page � of Cly Stale Tp ode; Site—Contact Lab Contact Analysis(Attach listif ' i,/ N, 2,g /� more space Is needed) Pm)ect N me and cabo (S te) ,; 1O .,,,.Waybill Number - rtn�� �"9 F � AS �G�U'll I. ." "` I�'S�L }�v Special Instructions/ Contmct/Pwchase OrdedQuote No: - Containers& ' _1 �,N;W -Conditions of Receipt (} �Z?�f Matrix U Preservatives w ja Sample I.D.No.and Description Date Time ph 8 8 o (Containers for each samplemay be combined on one line) ;� h rSj `i = i 6 qz 6 i' it;o x 1� 4 eL a ` -/ l t-a o X sj� .S legs,1, .� GDw�tMor�e iT�� -�i.� lqao }C x kColt,D;4te Possible Hazard ldemblication - Sample Disposal (A fee maybe assessedffsamples are retained ❑ Nan-Hazard 0 r-7ammabie ❑ Skfn Irritant ❑ Poison B ❑ Unknown ❑Return To Client ❑ Disposal ByLab ❑Archive FDr—'Months longeriban;I mo_pth) Turn Around rime Required - -QC Requirements(Spec(fy) ❑24Hours Q 4B Hmm; ❑,7Days ❑ 14 Days ❑21 Days ❑,Other ` 1. ' qu/she By' - Date Time 1,Recei y, ; ` Dale Time Dg`D2 ►.l 6 �a flQaz It 15W 2.RallholPhed 9k I i ,Ime 2.Received By " - > ' Date Time 9.Relingui oVL Date -- =Time- y Dat 77me i do ►t z l� oa15 Commence; � e^- _ /.t_ C ♦/L/ ewY�eti /� ,I.ut AG�(/G ✓e page n oz n PtmR�i 0 WHITE-AetumetltoClfentwithRepart; CA A Y-Stays wit theSam p `N -geld Copy �• SAMPLE LOG-IN CHECKLIST �/IStq 1 L Analytical Laboratory Vista Project# I�� TAT (7 G GI' _C Date/Time Initials: Location: W F- ,'- Samples Arrival: I�Ao / L/��' 68 55 Shelf/Rack; A Date/Time Initials: Location: -2 Logged In: O� �' J l I � Shelf/Rack: Delivered By: edEx UPS On Trac DHL Hand Other Delivered Preservation: Ice Blue Ice Dry Ice None Temp °C Time: Thermometer ID: IR-1 YES/ NO NA Adequate Sample Volume Received? Holding Time Acceptable? Shipping Containers Intact? Shipping Custody Seals Intact? Shipping Documentation Present? Airbill I Trk# 7216 8885 6566 Sample Container Intact? Sample Custody Seals Intact? Chain of Custody/ Sample Documentation Present? COC Anomaly/Sample Acceptance Form completed? If Chlorinated or Drinking Water Samples. Acce table Preservation? Na2SZOa Preservation Documented? CDC Sample, None Container Shipping Container Vista I Retain Return I Dispose Comments: Sample Login 3/7007 nuh Project 33436 Page 14 of 15 a Chain of Custody Anomaly/Sample Acceptance Form %lient: Evergreen Packaging Project Number 33436 Contact: Nick McCracken Date Received: Nov 2 2011 Fax Number: Documented by/date: i 11 2/1t Please review the following information and complete the Client Authorization section. To comply with NELAC regulations,we must receive authorization before proceeding with sample analysis. Thank You. (Fax # 916-673-0106 ) The following information or item is needed to proceed with analysis: ❑ Complete Chain-of-Custody ❑ Preservative ❑ Collector's Name ❑ Test Method Requested ❑ Sample Identification ❑ Sample Type ❑ Analyte List Requested ❑ Sample Collection Date/Time ❑ Sample Location The following anomalies were noted. Authorization is needed to proceed with the analysis. Temperature outside 12°C range Samples Affected: / 'Temperature outside °C Ice presennt?nq Yes No Sample ID Discrepancy Samples Affected t�00 ,GJOUoc.� Sample holding time missed Samples Affected Custody seals broken Samples Affected Insufficient Sample Size Samples Affected Sample Container(s)Broken Samples Affected Incorrect,Container Type Samples Affected Other (' ('n � Label To- : - Sth 4A glut ngj oaf 2-�r1/ef5 C Ca4 - oo1 Anna C05 - n ar C r Uo 00 -L - qA -5-0/it yB Channel caf CCa4 -cV/ -ira aa4"-L'yB 'q,$60nmen Carp AA-f-CCCikP -oa/Aru aotl gao6 �d2/u Client Authorization Proceed With Analysis: S NO Signature and Date Client Comments/Instructions: Si{ E ILA wd( LISL L. "I 2 (f4tr Fffol ) Vista Analytical Laboratory El Dorado Hills,CA 95762 Phone:(916)673-1520 Fax:(916)673-0106 Project 33436 Page IS of 15 APPENDIX C BLUE RIDGE PAPER CANTON MILL FISH FILLET TISSUE ANALYSIS RESULTS, I990-2004 33 APPENDIX C Table 6-4. Blue Ridge Paper Canton Mill Fish Fillet Tissue Results. 1990-2004 r From: EA Engineering, Science, and Technology, Inc. December 2004 36 Table 6-4. Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 1990-2004(a). 1990 Resultsa'1 1991 ResultsOl Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDD(') Station Species Fish Range(mm) 2,3,7,8-TCDDt°t 1 Rock bass 5 151-197 ND(0.15) 1 Rock bass 10 151-190 ND(0.40) RM 64.5 Rock bass 5 153-213 ND(0.15) RM 64.5 Redbreast sunfish 10 106.178 ND(0.33) Black redhorse 2 380.383 ND(0.20) Black redhorse 5 358-471 ND(0.35) 2 Redbreast sunfish 5 185-196 1.4 2 Redbreast sunfish 8 154-189 0.87 RM 59.0 Redbreast sunfish 5 148-201 3.4 RM 59.0 Redbreast sunfish 8 154-202 0.93 Common carp 1 517 19.7 Common carp 10 491-570 9.7 3 Redbreast sunfish 5 188-203 0.79 3 Redbreast sunfish 10 176-209 ND(0.89) RM 52.3 Redbreast sunfish 5 191-198 2.6 RM 52.3 Bluegill 6 164-197 ND(0.83) Common carp 2 489-555 4.2 Common carp 10 409-463 2.4 4A Bluegill 5 178-192 ND(1.2) 4A Largemouth bass 7 3I3-468 3.0 RM 41.5 Bluegill 5 153-174 ND(0.63) RM 41.5 Black crappie 10 173-216 ND(0.63) Common carp 1 574 27 Common carp 10 502-688 23 4B Bluegill 5 183.196 0.76 Q Bluegill 5 186-212 ND(0.34) RM 39.0 Largemouth bass 2 279-400 ND(1.8) RM 39.0 Bluegill 5 190-208 ND(0.62) Common carp 4 551-638 66 Common carp 10 532-605 40 5 Redbreast sunfish 10 143-223 0.98 RM 16.5 Spotted bass 2 266-368 ND(0.35) Common ca 2 511-539 1.7 Total Fish Filleted 57 138 Table 6-4 (cont.). 1992 Results(w 1993 Results9l) Number of Length Number of Length Station Species Fish Range(ram) 2,3,7,8-TCDDt°t Station Species Fish Range(ram) 2,3,7,8-TCDDt`> 1 Rock bass 10 147-194 ND(0.085) 1 Rack 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 redhorse 6 365441 1.4 Black redhorse 10 365.410 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) 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 10 183-200 ND(0.29) RM 52.3 Redbreast sunfish 7 180-213 ND(0.36) Common carp 10 438.600 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 emp 10 492-622 29 Common carp 10 525-611 19 4B Bluegill 30 182-212 ND(0.23) 4B Largemouth bass 10 190-310 ND(0,12) RM 39.0 Largemouth bass 5 215-332 ND(0.19) RM 39.0 Bluegill 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) Smallmoutlt buffalo 5 428-510 0.61 Smallmouth buffalo 5 450-550 ND(0.41) Total Fish Filleted 158 162 r- r Table 6-4 (cont.). 1994 Resultstw 1995 Results(c) Number of Length Number of Length Station Species Fish Range(nun) 2,3,7,8-TCDDW Station Species Fish Range(mm) 2,3,7,8-TCDDt°t 1 Rack bass 6 156-195 ND(0.083) 1 Rock bass 10 162-205 ND(0.10) RM 64.5 Redbreast sunfish 10 155-197 ND(0.10) RM 64.5 Rock bass 10 150-220 ND(0.26) Black redhorse 3 367-435 ND(0.096) Black redhorse 7 375-464 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 10 166-210 ND(0.092) RM 59.0 Redbreast sunfish 10 161-189 ND(0.16) Common carp 10 490.590 0.99 Comma carp 10 435-664 1.7 3 Redbreast sunfish 10 148-196 ND(0.15) 3 Redbreast sunfish 10 170-206 ND(0.18) RM 52.3 Redbreast sunfish 10 158-210 ND(0,074) RM 52.3 Redbreast sunfish 10 154-202 ND(0.20) Common carp 10 456-565 0.74 Common carp 10 391-571 1.2 4A Black crappie 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 carp 30 465-591 3.4 Common carp 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(034) Common carp 10 520-635 6.6 Common carp 4 532-626 11.0 5 Redbreast sunfish 6 129.289 ND(0.075) 5 Smallmoudr bass 9 280.423 ND(0.11) RM 19.0 Smallmouth bass 9 234-442 ND(0.11) RM 19.0 Redbreast sunfish 7 163-192 ND(0.15) Smalhnout4 buffalo 9 440-520 ND(0.089) Black redhorse 7 440-481 ND(0.45) Total Fish Filleted 163 156 Table 6-4 (cont.). 1996 Resultsul) 1997 ResultsP) Number of Length Number of Length Station Species Fish Range(aim) 2,3,7,S-TCDDW Station Species Fish Range(mm) 2,3,7,8-TCDD(-) 1 Redbreast sunfish 5 154-185 ND(0.13) 1 Redbreast sunfish 5 144-161 ND(0.11) RM 64.5 Rock bass 5 160.208 ND(0.085) RM 64.5 Rock bass 5 162-194 ND(0.23) Black redhorse 5 401-440 ND(0.089) Black redhorse 4 291-424 ND(0.22) 2 Redbreast sunfish 5 179-187 ND(0.10) 2 Redbreast sunfish 5 183-200 ND(0.26) RM 59.0 Redbreast sunfish 5 183-191 ND(0.12) RM 59.0 Redbreast sunfish 5 160-181 ND(0.12) Common carp 5 543-580 1.5 Common carp 5 506-615 1.4 3 Redbreast sunfish 5 194-190 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) 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(D,10) Common carp 5 562-632 4.2 Common carp 5 570-655 2.3 Channel catfish 5 418-482 2.0 0 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(0.21) Common carp 5 470.623 4.0 Common carp 5 605-690 11.0 Flathead catfish 5 430-540 0.62 5 Rock bass 4 169-186 ND(0-077) 5 Rock bass 5 143.214 ND(0.15) RM 19.0 Smallmouth bass 5 315-454 ND(0.12) RM 10.0 Smallmouth bass 5 278-367 ND(0.27) Smallmouth buffalo 5 451-555 ND(0.12) Smallmouth buffalo 5 406-525 ND(0,22 Total Fish Filleted 89 Total Fish Filleted 99 l i i Table 6-4 (coat.). 1998 Results" 1999 Resuitst°) Number of Length Number of Length Station Species Fish Range(rare) 2,3,7,8 TCDDW Station Species Fish Range(mm) 2,3,7,8-TCDDW 1 Redbreast sunfish 5 145.176 ND(0.19) 1 Redbreast sunfish 5 141-177 ND(0.21) RM 64.5 Rock bass 5 158.179 ND(0.29) RM 64.5 Rock bass 5 164-I80 ND(0.37) Black redhorse 5 340-396 ND(0.18) Black redhorse 5 352-427 ND(0.33) 2 Redbreast sunfish 5 164-M ND(0.20) 2 Redbreast sunfish 5 167-190 ND(0.37) RM 59.0 Redbreast sunfish 5 166.193 ND(0.28) RM 59.0 Redbreast sunfish 5 158-178 ND(0.29) Common carp 5 551-661 1.3 Common carp 5 544-615 ND(0.27) 3 Redbreast sunfish 5 168-193 ND(0.34) 3 Redbreast sunfish 5 169-189 ND(0.36) RM 52.3 Redbreast sunfish 5 167-200 ND(0.22) RM 52.3 Redbreast sunfish 5 162-176 ND(0.37) Common carp 5 449-550 ND(0.38) Common carp 5 500-591 0.57 4A Black crappie 5 220.240 ND(0.49) 4A Black crappie 5 220-268 ND(0.18) RM 41.5 Largemouth bass 5 227-330 ND(0.15) RM 41.5 Black crappie 5 219.244 ND(0.08) Common carp 5 585-621 1.6 Common carp 5 574-645 0.58 Channel catfish 5 416-458 ND(0.28) Charnel catfish 5 425-482 0.83 413 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 5 563-686 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 Rock bass 5 170-203 ND(0.29) 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 Table 6-4 (cont.). 2000 Resuhsol) 2001 ResuhS(d) Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDD(°) Station Species Fish Range(mm) 2,3,7,8-TCDDt°t 1 Redbreast sunfish 5 137-148 ND(0.48) 1 Black wilhorse 5 312-407 ND(0.25) RM 64.5 Rock bass 5 162-186 ND(0.45) RM 64.5 Black redhorse 5 357-396 ND(0.38) 2 Redbreast sunfish 5 169-176 ND(0.31) 2 Common carp 5 456-555 ND(0.27) RM 59.0 Redbreast sunfish 5 164-181 ND(0.43) RM 59.0 Common carp 5 505-582 ND(0.42) 3 Redbreast sunfish 5 169-181 ND(0.43) 3 Common carp 5 504-615 ND(0.35) RM 52.3 Redbreast sunfish 5 186-199 ND(032) RM 52.3 Common carp 5 514-569 ND(0.53) 4A Black crappie 5 212-241 ND(0.29) 4A Channel catfish 5 476-612 1.2 RM 41.5 Black crappie 5 220.241 ND(0.24) RM 41.5 Common carp 5 529-668 1.3 Common carp 4 559-604 1.1 Channel catfish 5 435-487 ND(0.70) 4B Black crappie 5 213-231 ND(0.41) 4B Flathead catfish 5 40SA63 ND(0.29) RM 39.0 Black crappie 5 220-230 ND(0.37) RM 39.0 Common carp 5 654-723 5.6 Common carp 4 593-712 4.4 Flathead catfish 5 407.450 ND(0.42) 5 Rock bass 5 - 171-198 ND(0.45) 5 .Black redhorse 5 437-497 ND(0.26) RM 19.0 Smallmouth bass 5 209-238 ND(0.31) RM 19.0 Black redhorse 5 427-476 ND 0.3 Total Fish Filleted 98 Total Fish Filleted 40 Table 6-4 (cont.). 2002 Results"? 2003 Results(h) Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDD") Station Species Fish Range(moo) 2,3,7,8-TCDDt4 RM 1 64.5 Black redhorse 5 372-431 ND(0.14) 1 Black redhorse 5 343-420 ND(0.20) RM 64.5 2 Common carp 5 517-548 ND(0.28) 2 Common carp 5 512-584 ND(0.18) RM 59.0 RM 59.0 3 Common carp 5 575-632 ND(0.22) 3 Common cup 5 545-605 ND(0.31) RM 52.3 RM 52.3 4A Common carp 5 523-648 2.2 4A Common carp 5 655-717 3.4 RM 41.5 Channel catfish 5 425-475 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) RM519 0 Black redhorse 5 430-489 ND(0.14) 5 Black redhorse 5 445-524 ND(DL=0.19) RM 19.0 Total Fish Filleted 40 Total Fish Filleted 40 Table 6-4 (cont.). 2004 Resultstd Number of Length Station Species Fish Range(min) 2,3,7,8-TCDDtn 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 369453 ND(0.17) 3 Common carp 5 597.609 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) 5 Black redhorse 5 420-480 ND(0.13) RM 19.0 Total Fish Filleted 40 (a) Survey conducted by EA Engineering,Science,and Technology. Analyses conducted by ENSECO Laboratories 1990-1994,Quanterra Laboratories 1995-1999,Sevem Trent Laboratories iu 2000- 2003. (b) Survey conducted in August. (c) Survey conducted in August and September. (d) Survey conducted in September. (e) Units=ppt(parts per trillion)or pg/g(pioogram per gram) ND =Non-detectable at the detection limit in parentheses. APPENDIX D 2006 REVISIONS TO DIOXIN MONITORING PLAN 34 WA Michael F.Easley,Governor 0 9 William G.Ross Jr.,Secretary \0[� Q North Carolina Department of Environment and Natural Resources fiJ Alan W.Klimek,P.E.Director Division of Water Quality p .� Coleen H.Sullins,Deputy Director uality nn E C E June 6, 2006 JUN 12 Mr. Paul S. Dickens Manager, Environmental Affairs BLUE RIDGE PAPER PRODUCTS INC Blue Ridge Paper Products BHS DEPARTMENT P.O. Box,4000 Canton,North Carolina 28716 Subject: Revisions to Dioxin Monitoring Plan Blue Ridge Paper Products NPIDES 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. • 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 continents please feel free to contact Mark Hale at 919/733- 6946. nc(�r e immie verton ironmental Sciences Section cc: Roger Edwards -ARO Dr. Luanne Williams—NCDHHS Susan Wilson -DWQ Permits — John Crutchfield—Progress Energy g Ao.x ENR N.C.Division of Water Quality 1617 Nail Service Center Raleigh,North Carolina 27699-1617 (919)733-7015 Customer Service 1-877-623-6748 BLUE RIDGE ac py i PAPER PRODUCTS INC. Certified Mail Return Receipt Requested 7099 3220 0007 0371 6235 30 March 2006 Mr.Mark Hale Environmental Biologist Environmental Services Section Division of Water Quality North Carolina Department of Environment and Natural Resources _ 1621 Mail Service Center Raleigh, North Carolina 27699-1621 Subject: Study Plan Revision Dioxin Monitoring in Fish Tissue—Waterville Lake March 2006 NPDES No. NC0000272 Blue Ridge Paper Products Inc. Canton Mill Dear Mr. Hale— The subject study plan revision is enclosed for Division of Water Quality(DWQ)review and approval. Background The Blue Ridge Paper Products Inc. mill in Canton,North Carolina has completed biological monitoring for dioxin in fish in the Pigeon River for the past 16 years. This annual biological monitoring is a requirement of the Canton Mill's NPDES permit. The permit requires that we follow.a study plan approved by the DWQ for this work. Dioxin in fish sample collection and reporting for 2002 through 2005 was conducted under the December 2001 Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue prepared by EA Engineering, Science and Technology. EA Engineering completed the dioxin in fish sampling and reporting for years 2002 thru 2004. In 2005, Blue Ridge Paper contracted with the University of Tennessee, Knoxville(UTK)Department of Forestry, Wildlife and Fisheries for the dioxin in fish tissue work. UTK followed the 2001 Study Plan for the 2005 dioxin in fish sampling and report. The 2005 report was submitted to the DWQ on 20 Feb 2006. 7 175 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 in 2000 and have remained below analytical detection levels since that time. Dioxin fish tissue sample concentrations in sport fish species from all sampling locations in.the Pigeon River became non- detect in the mid-1990s. Based on annual fish tissue sampling, the State of North Carolina lifted the dioxin in fish advisory for the Pigeon River upstream of Waterville Lake in August 2001. The State of Tennessee lifted the dioxin in fish advisory for the Tennessee portion of the Pigeon River in January 2003. The only fish advisory remaining is for carp in Waterville Lake. Dioxin levels in carp collected from Waterville Lake since 2000 continue to be at or near analytical detection levels and are below the North Carolina Department of Health and Human Services (NC DHHS) dioxin toxicity equivalent(TEQ) fish advisory action level of 4 parts per trillion(ppt). The NC DHHS has indicated that two consecutive years of TCDD TEQ levels in carp of 3 ppt or less would provide basis for lifting the public health advisory for consumption of carp from Waterville Lake (e-mail correspondence from Dr. Luanne Williams,DHHS to Blue Ridge Paper dated 9 Mar 2006). The TCDD TEQs for carp fillet composite samples from Stations 4A&4B in Waterville Lake for the last two years are as follows: Year Station 4A Station 4B 2004 2.5 ppt 2.2 ppt 2005 2.1 ppt 3.6 ppt Study Plan Revision Blue Ridge Paper proposes the following changes to the 2001 biological monitoring Study Plan: 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- 3/30/06, 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 dickep@blueridgelaper.com rogerg@blueridgenaper.com Enclosures: Study Plan Revision Dioxin Monitoring in Fish Tissue- Waterville Lake March 2006 Prepared by University of Tennessee for Blue Ridge Paper Products Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue December 2001 Prepared by EA Engineering for Blue Ridge Paper Products cc(w/enclosures): Bryn Tracy- NC DENR DWQ, ESS Susan Wilson—NC DENR DWQ, Permits Sergei Cherinkov—NC DENR DWQ, Permits Roger Edwards—NC DENR DWQ, ARO Keith Haynes - NC DENR DWQ, ARO Dr. Louanne Williams—NC DHHS Larry Wilson—UTK Billy Clarke—Roberts & Stevens John Crutchfield—Progress Energy Blue Ridge Paper Products Inc 175 Main Street a PO Box 4000 Canton, North Carolina 28716 o 828-646-2000 Raising Your Expectations BLUE RIDGE I�fi PAPER PRODUCTS INC. STUDY ELAN REVISION DIOXIN MONITORING IN FISH TISSUE Waterville Lake Prepared for: Blue Ridge Paper Products, Inc. Canton Mill Canton,North Carolina ` NPDES No.NC 0000272 Prepared by: J.Larry Wilson,Ph.D. Departments of Forestry,Wildlife and Fisheries University of Tennessee Knoxville,Tennessee March 2006 Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page I 1 INTRODUCTION The Blue Ridge Paper Products Inc. Canton Mill conducts annual biological monitoring of dioxin in fish in the Pigeon River under conditions of the NPDES permit for the mill. This monitoring for years 2002 thru 2005 was in accordance with the December 2001 Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue prepared by EA Engineering, Science and Technology(EA 2001a). This document details changes for dioxin in fish monitoring beginning in 2006. The 2001 study plan is incorporated by reference. The specific changes to the 2001 study plan include: 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 Paper Products Inc.Canton Mill Page 2 each year is dependent on physical river conditions and the natural diversity and abundance of target fishes at each location. The field investigators will be equipped with an array of collecting gear, which will enable sampling of all habitats regardless of river conditions. The US EPA recommends active methods of fish collection in the Sampling Guidance Manual (Versar 1984), such as electrofishing, trawling, angling, or seining. These are preferred over passive methods (e.g., gill nets, trap nets, trot lines) because samples are.collected from more defineable areas (Versar 1984). Electro- fishing may be used at both locations (4A and 4B); gill nets may also,be used in areas where water depth will limit the electro-fishing gear. A boat electrofishing unit(pulsed direct current, Smith Root Type VIA electro-fisher powered by a 240-volt, 5000-Watt generator) will be provided. Electro-fishing techniques will follow those described in the National Dioxin Study (Versar 1984). All gill nets will be pulled and examined on a regular basis to reduce specimen stress or mortality, and specimens submitted for analysis will be selected for good health and condition. Fish collection techniques and level of effort (time) expended at both locations (4A and 4B) will be recorded. Total study effort for the 4A/4B collections in 2005 took 460 gill-net hours and approximately six hours of electro-fishing over a four-day period to obtain the necessary specimens. Channel catfish were easily caught, but common carp were extremely difficult to collect,particularly in the lower portion of the lake (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 4B O 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 making an incision behind the opercula (on both sides of the fish) from the base of the spine(behind the skull) to just below the pectoral fin. Care will be taken to cut through the epaxial muscle without puncturing the rib cage or gut lining. A second incision will be made along the length of the spine to the caudal fin on both sides of the fish. The muscle will be cut away from the rib cage to obtain a fillet. Fillet knives will be solvent rinsed(hexane and acetone) between fish from different locations. Each composite sample will be wrapped in aluminum foil (dull side toward sample), labeled, and placed on dry ice. One side fillets will be sent to 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 Sevem Trent Laboratory (STL)—Sacramento for analysis.The back-up fillets will be retained in a freezer at the Canton Mill until laboratory analytical results for the composite fillet samples are received and verified; the back-up fillet samples will then be destroyed. SAMPLE ANALYSIS The composite fillet fish tissue samples received by STL will be analyzed for dioxin(2,3,7,8- TCDD), furan (2,3,7,8-TCDF) and related isomers using EPA Method 8290 (US EPA 1994). Percent lipids will also be determined for each composite sample. STL will provide laboratory analytical reports including QA/QC summaries and completed chain-of-custody forms documenting receipt by the lab. REPORTING Results of 2006 dioxin in fish tissue sampling from Waterville Lake will be submitted to the NC DENR within 180 days of the completion of field work as required by the Blue Ridge Paper NPDES permit. The fish tissue sampling and analytical report will follow the general format of prior year reports. Dioxin toxicity equivalent(TEQ) levels will be calculated for all 17 chlorodibenzo dioxin and furan (CDD/F) isomers included in EPA Method 8290. The TEQ of each detectable isomer will be calculated based on the toxicity equivalent factor(TEF) for the isomer provided by the World Health Organization(WHO 1997). The measured concentration of each CDD/F isomer will be multiplied by its appropriate TEF to obtain a concentration of the isomer equivalent to the toxicity of 2,3,7,8-TCDD, the most toxic of the CDD/F isomers. Non- detectable concentrations will be treated as zero values for TEQ calculation. As requested by the Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 4 NC DHHS (Williams 2006), the TEQ results for the last two years will be presented in a columnar, side-by-side format to allow easy comparison against health advisory action levels. References EA Engineering,Science, and Technology Inc. 1990. Study Plan for the Monitoring of Dioxin in Fish Tissue. EA Report No. 11370.01,prepared for Champion International Corporation, Canton, North Carolina. EA Engineering,Science,and Technology Inc. 1991. Results of the 1990 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.02,prepared for Champion International Corporation, Canton,North Carolina. EA Engineering,Science,and Technology Inc. 1992. Results of the 1991 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.03,prepared for Champion International Corporation, Canton,North ,Carolina. EA Engineering,Science,and Technology Inc. 1993a. Results of the 1992 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.05,prepared for Champion International Corporation, Canton,North Carolina. April. EA Engineering,Science,and Technology Inc. 1993b. Results of the 1993 Dioxin Monitoring in Fish Tissue. EA Report No. 11370.06,prepared for Champion International Corporation,Canton, North Carolina. December. EA Engineering,Science,and Technology Inc. 1994. Results of the 1994 Dioxin Monitoring in Fish Tissue. EA Report No. 1.1370.07,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 1995. Results of the 1995 Dioxin Monitoring in Fish Tissue. EA Report No. 13043.01,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science;and Technology Inc. 1996. Results of the 1996 Dioxin Monitoring in Fish Tissue. EA Report No. 13176.01,prepared for Champion International Corporation,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 1997. Results of the 1997 Dioxin Monitoring in Fish Tissue. EA Report No. 13353.01,prepared for Champion International Corporation,Canton,North Carolina. November. EA Engineering,Science,and Technology Inc. 1998. Results of the 1998 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01,prepared for Champion International Corporation, Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2000. Results of the 1999 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01,prepared for Champion International Corporation, Canton,North Carolina. January. EA Engineering,Science,and Technology Inc. 2001a. Study Plan for Pigeon River Dioxin Monitoring in Fish tissue. Prepared for Blue Ridge Paper Products,Canton,North Carolina. November. Study Plan—2006 Dioxin Monitoring in Fish Tissue,Waterville Lake University of Tennessee for Blue Ridge Paper Products Inc.Canton Mill Page 5 EA Engineering,Science,and Technology Inc. 2001b. Results of the 2000 Dioxin Monitoring in Fish Tissue. EA Report No. 13745.01,prepared for Blue Ridge Paper Products, Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2001c. Results of the 2001 Dioxin Monitoring in Fish Tissue. EA Report No. 13900:01,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2003. Results of the 2002 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.02,prepared for Blue Ridge Paper Products,Canton,North Carolina. December. EA Engineering,Science,and Technology Inc. 2004. Results of the 2003 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.03,prepared for Blue Ridge Paper Products,Canton,North Carolina. January. Henry,A.G. and J.L.Wilson. 2006. Results of 2005 Dioxin Monitoring in Fish Tissue. Center for Environmental Biotechnology and Department of Forestry,Wildlife and Fisheries, University of Tennessee,Knoxville,Tennessee. U.S.Environmental Protection Agency(US EPA). 1994. Analytical Procedures and Quality Assurance for Multimedia Analysis of Polychlorinated Dibenzo-para-dioxins and 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 H Health Assessment of 2,3,7,8-Tetrachlorodibenzo-P-dioxin(TCDD and Related Compounds. copy , EA Project 13900.01 , r STUDY PLAN FOR PIGEON RIVER DIOXIN MONITORING IN FISH TMUE Prepared for., Blue Ridge Paper Products Canton, NC Prepared by. EA Engineering, Science, and Technology 444 Lake Cook Road, Suite 18 Deerfield, IL 60015 I December2001 TABLE OF CONTENTS Page I..........Introduction .................................................................................... 1-1 2. Station Locations .............................................................................. 2-1 3. Fish Collection Techniques and Target Species .......................................... 3-1 4. Sample Preparation ........................................................................... 4-1 5. Analysis of Fish Tissue Samples ............................................................ 5-1 6. Quality Assurance ............................................................................. 6-1 7. Project Schedule ................................................................................ 7-1 8. Monitoring Report ............................................................................. 8-1 9. References ...................................................................................... 9-1 r � r i 1. INTRODUCTION This study plan details the materials and methods that will be used to amorally 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 1-40 Station 5 RM 19.0 5 Bluffton TN-- (19.3f d�Hartford,TN TENNESSEE N ^ ^ NORTH N; CAROLINA GteeK I v / N qt9 Hydro Plant I( (26.0) A Il0 Itd - A o A N. Ot. I� en5 Walters Dam— B Station 46 Station 4A RM 39.0 RM 41.5 4 Waterville Lake Fines Creek New Hepco Bridge FLOW Jonathan Creelr Old Rt.209 3 Station 3 Station Mill Outfall RM 52.3 RM 50.0 RM 63.3 Waynesville STP— 2 Outfall Canton,NC a RM 50A �\eG�ee Clyde Station 1 1 RM 64.5 (Control) Figure 2-1. Fish tissue sampling station locations on the Pigeon River. J r TABLE2-1 PIGEON RIVER SAMPLING STATIONS Station River Station Location and N ti ntber Mile Distance from Outfall Site Deccrintion/Habitat Tyne Fish Community 1 64.5 Pigeon River upstream from Canton, Characterized by riffle,ran,and pool habitats. Maximum Relative abundance dominated by minnows and darters. River NC,adjacent to Canton Recreational depth approximately 6 fa Substrate primarily cobble and chub,greenfin darter and rock bass arc dominant. Northern hog Pak(1.2 RM upstream from Canton boulders interspersed with gravel and sand. sucker,black redhorse,mirror shiner,redbreast sunfish,central Mill outfall), stoncroller,greenside darter,and mottled sculpin arc 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 (4.3 RM downstream from the Canton cover. Maximum depth approximately 5 ft. Substrate stoncroller,and northern hog sucker. Mill outfall). primarily cobblelgravellsand with some boulders and bedrock. 3 52.3 Pigeon River in the vicinity of the Rt. Characterized by riffle,mn,and pool habitats with some Redbreast sunfish,northern Ihog sucker,and common carp are 209 bridge(11.0 RM downstream canopy cows. Maximum depth approximately 5 ft. dominant. Central stoncroller is common. from the Canton Mill outfalt) Substrate primarily bedrock and boulders with some cobble and sand/gravel/fncs deposited in pool areas. 4A 41.5 Upper Waterville lake(21.8 RM Characterized by deep-water lentic habitat,bedrock, Relative abundance dominatedby black crappic. Bluegill, downstream from the Canton Mill and soft bottom sediments. Maximum depth sampled Flathead catfish,channel catfish,largemouth bass,and common outfall) approximately 14 ft. carp are common. 4B 39.0 lower Waterville lake(24.3 RM Characterized by deep-water lentic habitat,bedrock, Relative abundance of catch dominated by black crappim downstream from the Canton Mill and soft bottom sedimmts Maximum depth sampled Bluegill,channel catfish,Flathead catfish,and carp am common. outfall) approximately 40 ft. Very steep banks with little cover. 5 19.0 Pigeon River near Bluffton,TN,just Characterized by deep,pools and runs with some shallow Central stoncroller and northern hog sucker are dominant. upstream of 140(44.3 RM downstream riffles. Maximum depth approximately 6 to 8 tit. Substrate Smalimouth bass,whitetail shiner,telescope shiner,greenside from the Canton Mill outfall) primarily bedrock,boulder,and cobble. darter,and banded sculpin are common. Except for smallmou(h bass and rock bass,centrarchids are uncommoon. J 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 f In summary,fish will be collected as follows: o Bottom feeder fillet composite—one sample at all six stations Catfish fillet composite—one sample at Stations 4A and at 4B c 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 4 7 ti 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 obtahi 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. t , T 8 1 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: ® Sample identification number, m Station identification, o Sampling team initials, o Date of sample collection, a Species name, O Sample type(i.e.,fillet or whole body) ( a 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 Dibenzofurans by High-Resolution Gas Chromatography/High- Resolution Mass Spectrometry(Method 8290). World Health Organization(WHO). 1997. Exposure and Human Health Reassessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) and Related Compounds: Part II Health Assessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin(TCDD) and Related Compounds. fi 13