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HomeMy WebLinkAboutNC0000272_2003_Results_of_Dioxin_Monitoring_20040101 JAN 1 6 ME wnTER Ouatlr- !SEt;TIC ASHEVII.I_F_RE I RESULTS OF 2003 DIOXIN MONITORING IN FISH TISSUE Prepared for: Blue Ridge Paper Products Inc. Canton Mill Canton, North Carolina Prepared by: EA Engineering, Science, and Technology, Inc. 444 Lake Cook Road, Suite 18 Deerfield, IL 60015 January 2004 13900.03 TABLE OF CONTENTS Page Listof Tables.........................................................................................iii Listof Figures ........................................................................................v EXECUTIVE SUMMARY....................................................................... vii 1. INTRODUCTION................................................................................. 1-1 2. SAMPLING LOCATIONS ...................................................................... 2-1 3. SAMPLING OBJECTIVES ..................................................................... 3-1 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT..................... 4-1 5. SAMPLE PREPARATION...................................................................... 5-1 6. ANALYTICAL RESULTS...................................................................... 6-1 7. REFERENCES .................................................................................... 7-1 APPENDIX A: CHAIN OF CUSTODY FORMS APPENDIX B: SEVERN TRENT LABORATORY-SACRAMENTO ANALYTICAL REPORTS i LIST OF TABLES Number Title Page 2-1 Pigeon River sampling station information .......................................... 2-2 4-1 Fish collection techniques and level of effort ....................................... 4-2 4-2 Summary of fish composites collected in the Pigeon River, August2003 ............................................................................... 4-3 6-1 Summary of Pigeon River fish tissues analysis results--2003 .................... 6-2 6-2 Toxicity equivalence factors for CDD/F isomers................................... 6-3 6-3 Summary of CDD/F isomer analyses, toxicity equivalent factors, and toxicity equivalent values for the 2003 Pigeon River fish tissue composites ............................................................ 6-5 6-4 Blue Ridge Paper Canton Mill fish fillet tissue analysis results 1990-2003................................:................................................. 6-8 iii LIST OF FIGURES Number Title Page ES-1 TCDD concentrations in carp fillets collected from the Pigeon River, 1990-2003.................................................................................. viii 2-1 Sampling station locations on the Pigeon River..................................... 2-3 2-2 Sampling Station No. 1 on the Pigeon River........................................ 2-4 2-3 Sampling Station No. 2 on the Pigeon River........................................ 2-5 2-4 Sampling Station No. 3 on the Pigeon River........................................ 2-6 2-5 Sampling Station No. 4A on the Pigeon River...................................... 2-7 2-6 Sampling Station No. 4B on the Pigeon River...................................... 2-8 2-7 Sampling Station No. 5 on the Pigeon River........................................ 2-9 6-1 TCDD concentrations in carp fillets collected from the Pigeon River, 1990-2003.................................................................................6-15 6-2 TCDD concentrations in catfish fillets collected from Stations 4A and 4B in Waterville Lake, 1997-2003 ...................................................6-17 v EXECUTIVE SUMMARY Bottom feeding species were collected in 2003 from six locations in the Pigeon River and analyzed for 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD), 2,3,7,8-tetrachlorodibenzofuran (TCDF), and other CDD and CDF isomers. TCDD and TCDF concentrations in fillet composites from bottom feeders were very low (range=non-detected to 0.81 ppt) at the three riverine locations downstream of the mill. Bottom feeders used at these locations were common carp and black redhorse. TCDD concentrations in bottom feeder fillet composites at the two Waterville Lake locations were 3.4 ppt and 12.0 ppt (Stations 4A and 4B, respectively) for carp and non-detect for flathead catfish at Stations 4A and 4B. Since 1990, TCDD concentrations in common carp fillets have declined dramatically (82-99 percent) at all downstream stations (Figure ES-1). vii Figure ES-1. TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990-2003 (Stations 2 and 3). 25 20 — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — —�— Station 2 - +- ' Station 3 c 0 L15 — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — Q. L d Q. 0 10 — — — — — — — — — — — — — — — — U F 5 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - + a a —+ _ c c c — 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 YEAR a) TCDD conentrations at Station 3 were not detected, therefore, the value plotted represents the detection limit for that sample. b) TCDD concentrations at Station 2 were not detected, therefore, the value plotted represents the detection limit for that sample. c) TCDD concentrations at Stations 2 and 3 were not detected, therefore, the values plotted represent the detection limits for those samples. Figure ES-1 (Cont.). TCDD Concentrations in Carp Fillets Collected from" the Pigeon River, 1990-2003 (Stations 4A and 4B). 7a A 60 - -\- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 50 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - C \ O \ / 40 - - - - -1-/- - - - \\- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - d \ Q \ W r \ f6 \ �'30 - - - - - - - - - - - - -\- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - Q U \ F- \ 10 - - - - - - - - - - - - - - - - - -� A- - - - - - — - - - - - - - - - - - - - - A _ �A- - -� - t _ -J 0 1990 1991 1992 1993 1994 1995 1996 1997 1996 1999 2000 2001 2002 2003 YEAR —o— Station 4a — A — Station 4b I 1. INTRODUCTION This report details the results of a study conducted during 2003 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 study described herein is number 14 in a series of fish tissue surveys designed and conducted to be completely responsive to the requirements of A.(9.) Dioxin Monitoring Special Condition in Blue Ridge Paper's 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 (EA 2001a). 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, and 2003). However, selected project details were modified to be responsive to the suggestions/recommendations of the North Carolina Department of Environment and Natural Resources (NCDENR), the Tennessee Wildlife Resources Agency, U.S. EPA Region IV, and the North Carolina Department of Health and Human Services (NCDHHS). The principal change in the program was that the collection and analysis of sportfish composite samples have not been required since 2000. The 2003 study was conducted during 26-28 August, during which time biologists from EA collected and prepared fish tissue samples from six sampling locations 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. 1-1 2. SAMPLING LOCATIONS In accordance with the study plan (EA 2001 a), fish were collected from six locations on the Pigeon River. Five monitoring stations were located downstream from the Canton Mill outfall (four in North Carolina and one in Tennessee) and one control or background site was located upstream of it. Detailed sampling station information is provided in Table 2-1 and Figure 2-1. Station 1, the background site, is located at Pigeon River Mile (RM) 64.5, approximately 1.2 RM upstream from the Canton Mill outfall (Figures 2-1 and 2-2). Fish were collected from the river reach adjacent to the Canton Recreational Park(located upstream from the city of Canton). Except under extremely high flows, the Canton Mill dam blocks the movement of fishes and thereby prevents the interaction of control and downstream monitoring station fishes. Monitoring Station 2 is located upstream from Clyde,North Carolina at RM 59.0, approximately 4.3 RM downstream from the Canton Mill outfall (Figures 2-1 and 2-3). Station 3 is 11.0 RM downstream from the outfall (RM 52.3),in the vicinity of the old Rt. 209 bridge(Figures 2-1 and 2-4). 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 2-5). 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 2-6). Station 5 is located near Bluffton, Tennessee at RM 19.0, approximately 44.3 RM downstream from the Mill outfall and about 6 miles downstream of the CP&L Hydro site (Figures 2-1 and 2-7). Sampling stations were separated by at least 5.5 RM(with the exception of the Waterville Lake stations which are only 2.5 RM apart). 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. At Station 1, an approximate 0.2 RM reach was sampled which extended from just downstream of the downstream most River Road (Rt.215) Bridge to the bridge by the city park. The Station 2 sample reach was approximately 0.2 RM in length and was adjacent to a sharp bend along Old Thickety Road. The Station 3 sample reach extended approximately 0.2 RM,just upstream of the old Rt. 209 Bridge. An approximate 0.4 RM reach of Waterville Lake was sampled adjacent to and upstream of the Messer Branch-Pigeon River confluence. The Station 4B study area consisted of a 1.0 RM reach of Waterville Lake located near the Wilkins Creek-Pigeon River confluence. Sampling at Stations 4A and 4B included gillnetting near the shore along both the left and right banks of Waterville Lake. A large pool just upstream of the I- 40 Bridge was sampled at Location 5. 2-1 Table 2-1. Pigeon River Sampling Stations. Station River Station Location and Number Mile Distance from Outfall Site Descrintion/Habitat Tvoe Fish Community 1 64.5 Pigeon River upstream from Canton, Characterized by riffle,run,and pool habitats. Maximum Relative abundance dominated by minnows and darters. River NC,adjacent to Canton Recreational depth approximately 5 ft. Substrate primarily cobble and chub,green darter and rock bass are dominant. Northern hog Park(1.2 RM upstream from Canton boulders interspersed with gravel and sand. sucker,black redhorse,mirror shiner,central stoneroller, Mill outfall). greenside darter,and mottled sculpin are common. 2 59.0 Pigeon River upstream from Clyde,NC Characterized by ran and pool habitats with canopy Relative abundance dominated by redbreast sunfish,central (4.3 RM downstream from the Canton cover. Maximum depth approximately 6 ft. Substrate stoneroller,and northern hog sucker. Mill outfall). primarily cobble/gravel/sand with some boulders and bedrock 3 52.3 Pigeon River in the vicinity of the Rt. Characterized by ran and pool habitats with some Redbreast sunfish,northern hog sucker,and common carp are 209 bridge(11.0 RM downstream canopy cover. Maximum depth approximately 5 ft. dominant. Centml stoneroller is common. N from the Canton Mill outfall) Substrate primarily bedrock and boulders with some t a cobble and sand/gravellfnes deposited in pool areas. 4A 41.5 Upper Waterville Lake(2 1.8 RM Characterized by deep-water lentic habitat with bedrock Relative abundance dominated by black crappie. Bluegill, downstream from the Canton Mill covered by loose,unconsolidated bottom sediments. Maximum flathead catfish,channel catfish,and largemouth bass are outfall) depth sampled approximately 15 ft. common. Common carp are present but not common. 4B 39.0 Lower Watervifle Lake from the dam to Characterized by deep-water lentic habitat,bedrock, Relative abundance of catch dominated by black crappie. confluence with Wilkins Creek(24.3 RM and soft bottom sediments. Maximum depth sampled Bluegill,channel catfish,and flathead catfish are common. downstream from the Canton Mill approximately 40 ft. Very steep banks with little cover. Common carp are present but not common. outfall) 5 19.0 Pigeon River near BlufRon,TN,just A single deep pool is sampled. Maximum depth Northern hog sucker is dominant. Smalhnouthbass,rockbass, upstream of 140(44.3 RM downstream approximately 8 ft. Substrate primarily boulder and cobble. black redhorse,whitetail shiner,and banded sculpin are from the Canton Mill outfall) common. Except for smalhnouth bass and rock bass, centrarchids are uncommon. Freshwater dmm,gizzard shad, and buffalo are occasionally common. Common carp are absent. 1-40 Station 5 RM 19.0 5 Bluffton TN Hartford,TN TENNESSEE N NORTH CAROLINA eK Big Hydro Plant ` o. (26.0) 11'9 S 1 XII Gt. 11 5 r"��.)ltty'en Walters Dam 4B Station 4B Station 4A RM 39.0 RM 41.5 4A Waterville Lake Fines Cre elc New Hepco Bridge FLOW ,Jonathan Creek Old Rt.209 3 Station 3 Station 2 Mill Outfall RM 52.3 RM 59.0 RM 63.3 Waynesville STP 2 Outfall Canton,NC 0 0 RM 54.7 xw Clyde Station 1 1 RM 64.5 (Control) Figure 2-1. Fish tissue sampling station locations on the Pigeon River. 2-3 " •. fl n dl' ul �/'' 4 - to••'.1, '•wi.• ./ '/ .�` • a n 'tea � n, �✓ �� ` „ c p_ �� ``,• .c Rio ,_� ` -.2800 t' • � � ` % '. ; .® ���"dam. � Aselllin¢ �Q -:- tanks� , MO J I � u ng�,lat}o __ _•� z O� L. r \ � station.^-'• _ � \ M T],75 Ise � i6h"SchF•P' � r � 2 6 F ■ �t l., `✓ O �1 1 �I Q• _ ° 00 N" rt •111 •000 G C r S .1 l' cT/ j ii `P�,�t aim• 1 e ii onq`1I > "' `` N i• �� ftltl0 j` •ove Ch . I� :f:_ IJ1..1. . 0 _ .. �4�. \.\'a../.l_ I • Figure 2-2. Sampling Station No. 1 on the Pigeon River. �O 2-4 57, �_ +J e] .J! Q o v •1��. o/,1, `.` hickey. ri n J:� '. L 1 ..-� j'r•• _ _. � ti,�'e 1 1 ��.l i47 �, ' :ir I .��.�.�_ r i��-\ \I'I ,m C/ _ �• /�., ti`J jl� i\•�^�l L "e�� a...- r`--�7rG 0 I •"':ia'{.• '� t;� �,,t f�v ~� \1l LD�'' Cert � _. r 4 Q• r ✓ \�3s 7 /o`', \J J Station 2Clk ' i - % Mn Dizs' 1. �1__r- •�� j ;� >\ . � ` _ _ �`w cur ten'sa6e r r. '`�' :. F i GFo\ ./ ._ •._ r t .Cve�L, .t: it Pei 4 BO: .•, l r� l �� �� ' ._.';. ' �"%= °`F __`•_�%, ,r—,. '� ) tom:: �� JN .-"lj'-'-'-' i Co' -� ^�_ Stamey --` d ey ove�'• 'Cam .. _ � . Figure 2-3. Sampling Station No. 2 on the Pigeon River. �O 2-5 S 04 Y��' ryFd`?'- i •f.-��QpD •ter. C-,l $ \ s � �mr�` `^ 'Da�iFs ha \.od• �%`�ct-�,C ���•� .. \ �V� is io 0'�•/4`l� fV Station 3) te �� o � •ROF ��� � ��, l n ' � j/ ', /'�� l<•I• ��. , jam/ /, � �__y 4��_ � x enARn All Figure 2-4. Sampling Station No. 3 on the Pigeon River. 2-6 �o I , J b Q n 1 r ,� o X Redm -` � � C l� \mot—_p1�E�N �� o ��I �✓/ r^\ \fir l��;ii�1"/ �/GIN � \�Yi ,^y�` Iv• �p I , 4 &g Figure 2-5. Sampling Station No. 4A on the Pigeon River. O 2-7 \\(��Ga(10 WIPER I � •rirlil t2,• � �<��: % Mz '�.� ,'�ELEV 2258 Stall on.4Bi ''� 'i ` �y / 1 (1 4 M1 :��� .il.•C`�' ? ,\ � �l� 1 fit. Figure 2-6. Sampling Station No. 4B on the Pigeon River. �O 2-8 1 I ii e 1 117 kill Station5 J Figure 2-7. Sampling station No. 5 on the Pigeon River. 29 3. SAMPLING OBJECTIVES In accordance with the study plan (EA 2001a), the goal of the fish collection effort was to collect one composite bottom feeder fillet sample at each of the six sampling stations. Each composite consisted of 5 similarly sized (shortest specimen within 75% of the length of the longest) adult individuals of the target species. Common carp (Cyprinus carpio) was the target species at Stations 2, 3, 4A, and 4B. Common carp are absent at Stations 1 and 5, so at these stations, black redhorse (Moxostoma duquesnet) was the target bottom feeder. In Waterville Lake, one additional fillet composite sample using flathead catfish was collected at Stations 4A and 4B. In addition to the fillet composites, a whole body composite consisting of 5 similarly sized common carp was collected at Station 4A in Waterville Lake. In summary, fish were collected as follows: • Bottom feeder fillet composite—one sample at all six stations • Catfish fillet composite—one sample at Stations 4A and at 4B • Common carp whole body composite--one sample from Station 4A The study plan called for the collection of catfish fillet composite samples at Stations 2 and 3 if specimens were encountered. However,no specimens were encountered at these locations in 2003. 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 2003 Pigeon River collections yielded the desired species at each sampling station. In addition, the number of specimens collected made it possible to composite individuals of similar weight and length (with larger/adult specimens preferred), and the 75 percent rule was met for all samples. 3-1 i 4. FISH COLLECTION TECHNIQUES AND LEVEL OF EFFORT V Sampling was conducted on 26-28 of August 2003. Notes were recorded at each sampling station with regard to the type of sampling gear; level of effort (time), and habitat (Table 4-1). Surface water temperature measurements at each riverine location are summarized below: Station RM Date Temp' 1 64.5 8/27 23.6 2 59.0 8/26 25.7 3 52.3 8/26 24.1 5 19.0 8/28 22.8 All fish submitted for tissue analysis were measured to the nearest millimeter (total length) and weighed to the nearest gram (wet weight). These data are summarized in Table 4-2. 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 their Sampling Guidance Manual (Versar 1984), such as electrofishing, trawling, angling, or seining. These methods are preferred over passive methods (e.g., gill nets, trap nets, trotlines) because the collection period is typically shorter (i.e., hours versus days-- thereby minimising decomposition), and because samples are collected from more definable ; areas (Versar 1984). Electrofishing was used at all stations, except 4A and 4B (Waterville Lake), where gill nets were necessary because of water depth. A boat electrofishing unit (pulsed direct current) was used to sample fish at Stations 3 and 5. The boat electrofisher was equipped with a Smith Root Type VIA electrofisher, and powered by a 240-volt, 5000W generator. A pram electrofisher, equipped with a Coffelt VVP-2C pulser and powered by a 120-volt, 1800W generator, was utilized at Stations 1 and 2. Electrofishing techniques followed those described in the National Dioxin Study (Versar 1984). Fish collection techniques and level of effort (time) expended at each of the six stations are summarized in Table 471. Total study effort involved —3.3 electrofishing-hours and —229 net- hours. Total electrofishing duration (energized time) was 45, 95, 30, and 30 minutes at Stations 1, 2, 3, and 5, respectively. 4-1 Table 4-1. Fish Collection Techniques and Level of Effort. Station Sampling sampling Number RM Date(s) Techniques Level of Effort Comments 1 64.5 27 AUG 03 Pram Electrofishing 45 min An approximate 0.2 RM reach of river was sampled;water level moderate--visibility good;characterized by riffles,runs,and pools with primarily cobble/boulder substrates interspersed with gravel and sand along margins. The entire reach was sampled using the pram. 2 59.0 27 AUG 03 Pram Electrofishing 1 It;35 min Less than 0.2 RM reach of river was sampled;water level moderate--visibility good;station characterized by ran and pool habitats with canopy cover;substrate primarily cobble/gravel with some boulders and bedrock,and sand/gravel/fines deposited along margins. Sampling involved several electrofishing passes near woody debris using the pram. 3 52.3 26 AUG 03 Boat Electrofishing 30 min An approximate 0.2 RM reach of river was sampled;water level moderate--visibility good;station characterized by runs and pools with primarily bedrock and boulder substrates,with sand/gravel/fines deposited along margins, Sampling involved several electrofishing passes over the reach utilizing a boat- mounted electrofishing unit. A lV 4A 41.5 26-27 AUG 03 (5)Gill nets --94 net-lus An approximate 0.4 RM reach of river was sampled;lake level was normal--visibility good,station characterized by moderately deep-water lentic habitat with bedrock and soft,unconsolidated bottom substrates. Sampling involved gill net setsjust off the left and right shores. 4B 39.0 26-27 AUG 03 (6)Gill nets —135 not-Ins An approximate 1.0 RM reach of river was sampled;lake level was normal--visibility good;station characterized by deep-water lentic habitats with bedrock and soft bottom substrates. Sampling involved gill nets. Effort was concentrated near the rock pile near the dam,in the small bay at the mouth of Wilkins Creek,and in the 1°small bay upriver from Wilkins Creek but along the opposite bank. 5 19.0 28 AUG 03 Boat Electrofishing 30 min An approximate 0.1 RM reach of river was sampled;water was clear and moderately low—visibility good to excellent;station was a large pool and associated shoal habitat;substrate boulder and cobble. Sampling involved several electrofishing passes over the pool using a boat-mounted electrofishing unit. 9 Table 4-2 Summary of fish composites collected at six stations in the Pigeon River,August 2003. TOTAL TOTAL LENGTH WHOLE BODY DATE STATION SPECIES (mm) WEIGHT(g) SAMPLE TYPE COMPOSITE 27 AUG 03 1 BLACK REDHORSE 420 500 FILLET R (RM 64.5) BLACK REDHORSE 373 425 BLACK REDHORSE ` 398 "0 BLACK REDHORSE 343 350 BLACK REDHORSE 346 270 MEAN 376 397 27 AUG 03 2 COMMON CARP 584 2430 FILLET R (RM 59.0) COMMON CARP 562 2350 COMMON CARP 553 1930 COMMON CARP 512 1700 COMMON CARP 552 2150 MEAN 553 2112 27 AUG 03 3 COMMON CARP 565 2330 FILLET R ON 52.3) COMMON CARP 605 2780 COMMON CARP 596 2770 COMMON CARP 555 2410 COMMON CARP 545 2130 MEAN 573 2484 26-27 AUG 03 4A FLATHEAD CATFISH 530 1830 FILLET R (RM 41.5) FLATHEAD CATFISH 574 2430 FLATHEAD CATFISH 531 1990 FLATHEAD CATFISH 521 1750 FLATHEAD CATFISH 575 2220 MEAN 546 2044 26-27 AUG 03 4A COMMON CARP 717 5700 FILLET R (RM 41.5) COMMON CARP 672 4150 COMMON CARP 680 3970 COMMON CARP 655 3500 COMMON CARP 672 4400 MEAN 679 43" 26-27 AUG 03 4A COMMON CARP 630 3300 WHOLE BODY WB ON 41.5) COMMON CARP 644 3180 COMMON CARP 594 2900 COMMON CARP 587 2680 COMMON CARP 578 2260 MEAN 607 2864 4-3 Table 4-2 (cont.). TOTAL TOTAL LENGTH WHOLE BODY DATE STATION SPECIES (mm) WEIGHT(q) SAMPLE TYPE COMPOSITE 26-27 AUG 03 4B COMMON CARP 654 3430 FILLET R (RM 39.0) COMMON CARP 713 5150 COMMON CARP 745 6800 COMMON CARP 702 5200 COMMON CARP 602 3170 MEAN 683 4750 26-27 AUG 03 4B FLATHEAD CATFISH 533 1700 FILLET R (RM 39.0) FLATHEAD CATFISH 526 1660 FLATHEAD CATFISH 513 1630 FLATHEAD CATFISH 511 1720 _ FLATHEAD CATFISH 513 1750 MEAN 519 1692 28 AUG 03 5 BLACK REDHORSE 460 1160 FILLET R (RM 19.3) BLACK REDHORSE 524 1420 BLACK REDHORSE 445 960 BLACK REDHORSE 484 1290 BLACK REDHORSE 458 1040 MEAN 474 1174 DTI u la 4-4 Ll Target species were collected at all sampling stations in 2603. Common carp, the target bottom feeder at stations 2, 3, 4A, and 4B, were collected (and prepared for fillet and/or whole body analysis) at those stations. In addition, the preferred target bottom feeding species (black redhorse) was collected from Stations 1 and 5. The physiography of the Waterville Lake Stations 4A and 4B necessitated the use of gill nets for the collection of bottom feeding species. All nets were pulled and examined on a regular basis to reduce stress or specimen mortality. All specimens submitted for analysis appeared healthy and in good condition. Lengths and weights for each fish making up each composite are provided in Table 4-2. Bottom feeder fillet composites consisted of five black redhorse at Stations 1 and 5 and five common carp at Stations 2, 3, 4A, and 4B. In addition, a second bottom feeder fillet composite, consisting of five flathead catfish, was prepared for analysis from Stations 4A and 4B. A single bottom feeder whole body composite consisting of five common carp from Station 4A was prepared for analysis (Table 4-2). All nine composites submitted for analysis in 2003 met the US EPA Region IV recommendation (Cunningham 1990) that the smallest specimen in each composite be equal to or greater than 75 percent of the total length of the largest specimen in that composite (Tables 4-2 and 6-4). 4-5 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 at each station (plus a catfish composite for each station in Waterville Lake as well as a common carp whole body composite 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 collected and 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 the scales (or removing skin from catfishes) and then making an incision behind the opercula (on both sides of the fish) from the base of the spine (behind the skull) to just below the pectoral fin. Care was taken to cut through the epaxial muscle without puncturing the rib cage or gut lining. A second incision was made along the length of the spine to the caudal fin on both sides of the fish. The epaxial muscle was then gently cut away from the rib cage to obtain a fillet. In this fashion, all flesh and skin was obtained from head to tail on both sides of the fish. Fillet knives were solvent rinsed (hexane and acetone) between fish from different stations. Each composite sample was wrapped in aluminum foil (dull side toward sample), labeled, and placed on dry ice. Right side fillets were sent to Severn Trent Laboratory for analysis; left side fillets were retained by Blue Ridge personnel as back-up fillets. All individual specimens (fillets or whole bodies) composing a single composite sample were placed together in a water-tight plastic bag labeled with the station name, sample number, and the number of specimens in that composite. All labels contained the following information: • sample identification number, sample location and station identification, sampling team initials, date of sample collection, O species name, • sample type (i.e., fillet or whole body) 5-1 A chain-of-custody form was filled out for each cooler of samples submitted for analysis. Each form included composite-specific information and instructions. Copies of all chain-of-custody records are provided in Appendix A. All samples were frozen solid prior to shipment to the analytical laboratory. The frozen samples were packed on dry ice, shipped via overnight delivery on 2 September and were - received, still frozen, at Severn Trent Laboratory - Sacramento on 3 September 2003. L � I . I � i 3 I i �J L! 5-2 6. ANALYTICAL RESULTS The fish tissue samples were received at Severn Trent Laboratory (STL) - Sacramento, California.under chain-of-custody on 3 September 2003. Once received at the laboratory, samples were compared to the chain-of-custody record to verify the contents of each shipping container. Each individual fish or fillet within a composite was homogenized separately by STL personnel, and equal aliquots of the homogenate from each fish were removed to constitute the composite. Dioxin and furan analyses were performed using high resolution Gas Chromatography/Mass Spectrometry (GSIMS) 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 Canton Mill NPDES permit. 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 2003 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 NCDHHS considers only fillet results when issuing health advisories. Concentrations of 2,3,7,8-TCDD in bottom feeder composite fillet samples were below the level of detection at Stations 1, 2, 3, 4A (flathead catfish), 4B (flathead catfish), and 5 (Table 6-1).. Concentrations of 2,3,7,8-TCDD were detectable only in common carp composite fillet samples from Stations 4A (3.4 ppt) and 4B (12.0 ppt). Furan isomer (2,3;7,8-TCDF) analysis results indicated a concentration range from non-detect [Stations 1, 2, 4A (flathead catfish), and 4B (flathead catfish)] to 3.5 ppt (common carp at Station 4B). 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 and 1983) and Cordle (1983)]. NCDHHS has identified a dioxin evaluation level of 3 ppt in fillet samples, expressed as average toxicity equivalent (TEQ) (NCDEHNR 1991). The TEQ of each chlorodibenzo dioxin and furan (CDD/F) isomer is based on the toxicity equivalence factor (TEF) (WHO 1997 and Table 6-2) as described in the 2001 Study Plan (EA 2001b). The TEQ value is calculated assuming additivity of effects from the individual congeners of dioxins and furans and is expressed as an "equivalent amount of 2,3,7,8-TCDD" (NCDEHNR 1991). The measured concentration of each CDD/F isomer, when multiplied by its appropriate TEF, yields the TEQ 6-1 Table 6-1. Summary of Pigeon River Fish Tissue Analysis Results,2003. Station Percent Number Sample ID Species Composite/Sample Type 2,3,7,8-TCDDtat 2,3,7,8-TCDF(a) Livid 1 LOC 1 BLACK RE Black redhorse 5 fillet samples ND(DL=0.20) ND(DL=0.15) 2.2 2 LOC 2 CARP Common carp 5 fillet samples ND(DL=0.18) ND (DL=0.39) 3.2 3 LOC 3 CARP Common carp 5 fillet samples ND(DL=0.31) 0.81t'> 6.6 4A LOC 4A FH. CATFISH Flathead catfish 5 fillet samples ND(DL=0.35) ND (DL=0.98) 2.5 LOC 4A CARP Common carp 5 fillet samples 3.4 3.4 16.0 LOC 4A CARP-WB Common carp 5 whole body samples 1.9 1.5 11.0 4B LOC 4B FH. CATFISH ` Flathead catfish,.". 5 fillet samples ND(DL=0.20) . ND(DL=0.16) 3.4 } t' LOC 4B CARP Common carp 5 fillet samples 12.0 3.5 22.0 N 5 LOC 5 BLACK RE Black redhorse 5 fillet samples ND (DL=0.19) 0.66ro1 6.1 (a) Units=ppt(parts per trillion)or pg/g(picogram per gram) (b) Estimated result. Result is less than the reporting limit Table 6-2. Toxicity Equivalence Factors for CDD/F Isomers. DIOXIN DIBENZOFURAN Isomer(°) TEF(") Isomer(') TEP) 2,3,7,8-TCDD 1 2,3,7,8-TCDF 0.1 1,2,3,7,8-PeCDD I 1,2,3,7,8-PeCDF 0.05 2,3,4,7,8-PeCDF 0.5 1,2,3,4,7,8-HxCDD 0.1 1,2,3,4,7,8-HxCDF 0.1 1,2,3,7,8,9-HxCDD 0.1 1,2,3,7,8,9-HxCDF 0.1 1,2,3,6,7,8-HxCDD 0.1 1,2,3,6,7,8-HxCDF 0.1 2,3,4,6,7,8-HxCDF 0.1 1,2,3,4,6,7,8-HpCDD 0.01 1,2,3,4,6,7,8-HpCDF 0.01 1,2,3,4,7,8,9-HpCDF 0.01 OCDD 0.0001 OCDF 0.0001 (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. 6-3 of that isomer (the toxic concentration of that isomer relative to the toxicity of 2,3,7,8-TCDD). In cases where CDD/F concentrations were below the level of detection, a value of zero was used in the TEQ calculation. The TEQ calculation and summarization schemes presented in Table 6-3 followed methods used by NCDHHS (NCDEHNR 1991). Bottom feeder fillet TEQ values were below the NCDHHS limit of 3 ppt for all stations, except 4A and 4B in Waterville Lake. Although the TEQ values for carp fillet composites at Stations 4A and 4B (8.6 and 20.0 ppt, respectively) exceeded the level of concern, the TEQ value for flathead catfish fillets from the same locations were < 0.01 and 0.0 ppt, respectively. In addition, the common carp whole body composite at Station 4A was also below the NCDHHS limit of 3 ppt. Table 6-4 illustrates the decline in 2,3,7,8 TCDD concentrations in carp fillet samples from 1990 through 2003. Since 1990, 2,3,7,8 TCDD concentrations in carp fillets declined dramatically (82-99 percent) at all sampling stations (Table 6-4, Figure 6-1). The concentrations of 2,3,7,8 TCDD in carp fillets from all stations in 2003 were similar to those observed in 2002, except at Station 4B. Concentrations of 2,3,7,8 TCDD in carp fillets at Station 4B appear to have increased slightly in recent years (Figure 6-1), with a similar, but less pronounced trend at Station 4A. The increases in TCDD concentrations observed in carp fillets since 1999 may be due in part to environmental conditions, specimen size, and/or dioxin biouptake/depuration rates of individual carp submitted for analysis rather than representing a real increase in dioxin concentrations in Waterville Lake. Regarding specimen size, on average, the size of the carp submitted for fillet analysis from Waterville Lake has increased in recent years, particularly at Station 4B. For example, during the period 1999-2003, the mean weight of carp analyzed at Stations 4A and 4B was 3.193 kg and 5.042 kg, respectively, compared to only 2.673 kg (Station 4A) and 3.207 kg (Station 4B) for the period 1994 through 1999 (EA 1994, 1995, 1996, 1997, 1998, 2000, 2001b, 2001c, and 2003). In addition, three of the five fish submitted for analysis at Station 4B in 2003 were greater than 700mm, and one fish was 745mm and weighed 6800 grams, the largest fish ever submitted for fillet analysis. In contrast to carp fillets, TCDD concentrations in catfish fillets from Stations 4A and 4B have - declined since 1999 (Figure 6-2). Thus, despite modest increases in recent years that may be an artifact associated with the size of the specimens collected, the concentration of 2, 3, 7, 8 TCDD in carp fillets from Waterville Lake has declined by 82-87 percent from 1990 through 2003 (Figure 6-1). 6-4 Table 6-3. Summary of CDD/F Isomer Analyses, Toxicity Equivalent Factors and Toxicity Equivalent Values for the 2003 Pigeon River Fish Tissue Composites. STATION 1 STATION 2 STATION 3 BLACK REDHORSE - Fillet COMMON CARP - Fillet COMMON CARP - Fillet CDD/F ISOMERS TEF(c) Results(a) TEQ(b) Results TEQ Results TEQ Dibenzodioxin 2,3,7,8-TCDD 1.0 0.20 * 0.000 0.18 * 0.000 0.31 * 0.000 1,2,3,7,8-PeCDD 1.0 0.48 * 0.000 0.48 * 0.000 0.56 * 0.000 1,2,3,4,7,8-HxCDD 0.1 0.34 * 0.000 0.40 * 0.000 0.42 * 0.000 1,2,3,6,7,8-HxCDD 0.1 0.28 * 0.000 0.59 * 0.000 0.69 * 0.000 1,2,3,7,8,9-HxCDD 0.1 0.29 * 0.000 0.35 * 0.000 0.36 * 0.000 112,3,4,6,7,8-HpCDD 0.01 0.48 * 0.000 2.10 * 0.000 3.1(d) 0.031 OCDD 0.0001 1.60 * 0.000 11.00 0.001 10.0(d) 0.001 Dibenzofuran O\ 2,3,7,8-TCDF 0.1 0.15 * 0.000 0.39 * 0.000 0.81(d) 0.081 1,2,3,7,8-PeCDF 0.05 0.23 * 0.000 0.26 * 0.000 0.30 * 0.000 2,3,4,7,8-PeCDF 0.5 0.23 * 0.000 0.26 * 0.000 0.26 * 0.000 1,2,3,4,7,8-HxCDF 0.1 0.22 * 0.000 0.29 * 0.000 0.22 * 0.000 1,2,3,6,7,8-HxCDF 0.1 0.18 * 0.000 0.25 * 0.000 0.19 * 0.000 2,3,4,6,7,8-HxCDF 0.1 0.22 * 0.000 0.30 * 0.000 0.23 * 0.000 1,2,3,7,8,9-HxCDF 0.1 0.25 * 0.000 0.34 * 0.000 0.26 * 0.000 1,2,3,4,6,7,8-HpCDF 0.01 0.43 * 0.000 0.37 * 0.000 0.41 * 0.000 1,2,3,4,7,8,9-HpCDF 0.01 0.51 * 0.000 0.43 * 0.000 0.48 * 0.000 OCDF 0.0001 0.61 * 0.000 0.67 * 0.000 0.59 * 0.000 Total TEQ 0.00 0.00 0.11 Table 6-3 (cont.) STATION 4A FLATHEAD CATFISH - Fillet COMMON CARP - Fillet COMMON CARP - WB CDD/F ISOMERS TEF(c) Results (a) TEQ(b) Results TEQ Results TEQ Dibenzodi.oxin 2,3,7,8-TCDD 1.0 0.35 * 0.000 3.40 3.400 1.90 1.900 1,2,3,7,8-PeCDD 1.0 0.83 * 0.000 2.50 2.500 1.70 * 0.000 1,2,3,4,7,8-HxCDD 0.1 0.61 * 0.000 1.70 * 0.000 0.34 * 0.000 1,2,3,6,7,8-HxCDD 0.1 0.50 * 0.000 7.70 0.770 5.00 0.500 1,2,3,7,8,9-HxCDD 0.1 0.52 * 0.000 1.40 * 0.000 0.91 * 0.000 1,2,3,4,6,7,8-HpCDD 0.01 1.40 * 0.000 24.00 0.240 21.00 0.210 OCDD 0.0001 6.4(d) 0.001 92.00 0.009 81.00 0.008 Dibenzofuran 2,3,7,8-TCDF 0.1 0.98 * 0.000 3.40 0.340 1.50 0.150 ON 1,2,3,7,8-PeCDF 0.05 0.48 * 0.000 1.90 * 0.000 0.69 * 0.000 ' 2,3,4,7,8-PeCDF 0.5 0.48 * 0.000 2.6(d) 1.300 1.70 * 0.000 D\ 1,2,3,4,7,8-HxCDF 0.1 0.43 * 0.000 1.40 * 0.000 0.82 * 0.000 1,2,3,6,7,8-HxCDF 0.1 0.36 * 0.000 1.20 * 0.000 0.73 * 0.000 2,3,4,6,7,8-HxCDF 0.1 0.44 * 0.000 0.71 * 0.000 0.26 * 0.000 1,2,3,7,8,9-HxCDF 0.1 0.50 * 0.000 0.30 * 0.000 0.29 * 0.000 1,2,3,4,6,7,8-HpCDF 0.01 0.67 * 0.000 2.30 * 0.000 1.40 * 0.000 1,2,3,4,7,8,9-HpCDF 0.01 0.79 * 0.000 0.69 * 0.000 0.71 * 0.000 OCDF 0.0001 1.00 * 0.000 0.50 * 0.000 0.51 * 0.000 Total TEQ 0.00 8.56 2.77 Table 6-3 (cont.) STATION 4B STATION 5 FLATHEAD CATFISH - Fillet COMMON CARP - Fillet BLACK REMORSE - Fillet CDD/F ISOMERS TEF(c) Results (a) TEQ(b) Results TEQ Results (a) TEQ(b) Dibenzodioxin 2,3,7,8-TCDD 1.0 0.20 * 0.000 12.00 12.000 0.19 * 0.000 1,2,3,7,8-PeCDD 1.0 0.50 * 0.000 3.7(d) 3.700 0.58 * 0.000 1,2,3,4,7,8-HxCDD 0.1 0.37 * 0.000 3.1(d) 0.310 0.35 * 0.000 1,2,3,6,7,8-HxCDD 0.1 0.38 * 0.000 11.00 1.100 0.29 * 0.000 1,2,3,7,8,9-HxCDD 0.1 0.32 * 0.000 1.80 * 0.000 0.30 * 0.000 1,2,3,4,6,7,8-HpCDD 0.01 0.54 * 0.000 30.00 0.300 0.55 * 0.000 OCDD 0.0001 0.96 * 0.000 76.00 0.008 0.74 * 0.000 Dibenzofuran 2,3,7,8-TCDF 0.1 0.16 * 0.000 3.50 0.350 0.66(d) 0.066 1,2,3,7,8-PeCDF 0.05 0.26 * 0.000 1.40 * 0.000 0.28 * 0.000 0� 2,3,4,7,8-PeCDF 0.5 0.26 * 0.000 4.4(d) 2.200 0.28 * 0.000 1,2,3,4,7,8-HxCDF 0.1 0.26 * 0.000 1.60 * 0.000 0.22 * 0.000 1,2,3,6,7,8-HxCDF 0.1 0.22 * 0.000 1.80 * 0.000 0.19 * 0.000 2,3,4,6,7,8-HxCDF 0.1 0.27 * 0.000 0.93 * 0.000 0.23 * 0.000 1,2,3,7,8,9-HxCDF 0.1 0.31 * 0.000 0.30 * 0.000 0.26 * 0.000 1,2,3,4,6,7,8-HpCDF 0.01 0.50 * 0.000 2.40 * 0.000 0.37 * 0.000 1,2,3,4,7,8,9-HpCDF 0.01 0.59 * 0.000 0.76 * 0.000 0.44 * 0.000 OCDF 0.0001 0.54 * 0.000 0.30 * 0.000 0.63 * 0.000 Total TEQ 0.00 19.97 0.07 (a) Units = ppt (parts per trillion) or pg/g picogram per gram) . (b) Dioxin Toxic Equivalent Concentration using methodology from U.S. EPA (1989) . (c) Toxicity Equivalent Factors from World Health Organization (WHO 1997) . (d) Estimated result. Result is less than reporting limit. (*) CDD/F isomer concentrations were below the level of detection, therefore a value of zero was applied to the TEQ calculation. , Table 6-4. Blue Ridge Paper Canton Mill Fish Fillet Tissue Analysis Results, 1990-20031a). 1990 Results(b) 1991 Results(b) Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDDt°t 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 358471 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 408463 2.4 4A Bluegill 5 178-192 ND(1.2) 4A Largemouth bass 7 313-468 3.0 RM 41.5 Bluegill 5 153-174 ND(0.63) RM 41.5 Black crappie 10 173-216 ND(0.63) rn Common carp 1 574 27 Common carp 10 502-688 23 00 4B Bluegill 5 183-196 0.76 4B Bluegill 5 186-212 ND(0.34) RM 39.0 Largemouth bass 2 279400 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 2 Sl1-539 1.7 Total Fish Filleted 57 138 Table 6-4 (cont.). 1992 Resultst°t 1993 Results(l) Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDD(`) Station Species Fish Range(ram) 2,3,7,8-TCDDt`f 1 Rock bass 10 147-194 ND(0.085) 1 Rock bass 10 185-208 ND(0.10) RM 64.5 Redbreast sunfish 10 147-182 ND(0.075 RM 64.5 Redbreast sunfish 5 148-203 ND(0.12) Black redhorse 6 365-441 1.4 Black redhorse 10 365-410 ND(0.80) 2 Redbreast sunfish 10 I80-220 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 Cornmon 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 carp 10 492-622 29 Common carp 10 525-611 19 0 4B Bluegill 10 182-212 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-&0 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 Smalhnouth bass 9 212-281 ND(0.13) Smallmouth buffalo 5 428-510 0.61 Smallmouth buffalo 5 450-550 ND(0.41) Total Fish Filleted 158 162 Table 6-4 (cont.). 1994 Results rot 1995 Res ilts(e) Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDDt'1 Station Species Fish Range(mm) 2,3,7,8-TCDDt°t 1 Rock bass 6 156-185 ND(0.083) 1 Rock bass 10 162-205 ND(0.10) RM 64.5 Redbreast sunfish 10 155-197 ND(0.10) RM 64.5 Rock bass 10 150-220 ND(0.26) Black redhorse 3 367-435 ND(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 10 160-210 ND(0.092) RM 59.0 Redbreast sunfish 10 161-188 ND(0.16) Common carp 10 490-590 0.99 Comon carp 10. 435-664 1.7 3 Redbreast sunfish 10 148-196 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 281439 2.0 RM 41.5 Bluegill 10 185-205 ND(0.084) RM 41.5 Bluegill 10 167-199 ND(0.26) p� Common carp 10 465-591 3.4 Common carp 10 520-615 5.8 p 4B Black crappie 10 200-215 ND(0.084) 4B Largemouth bass 9 248-391 0.68 RM 39.0 Black crappie 10 195-220 ND(0.062) RM 39.0 Bluegill 8 158-216 ND(0.34) Common carp 10 520-635 6.6 Common carp 4 532-626 11.0 5 Redbreast sunfish 6 129-289 ND(0.075) 5 Smallmouth 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) Sm illmouth 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 Results(s) 1997 Resultsa) Number of Length Number of Length Station Species Fish Range(ram) 2,3,7,8-TCDDt`t Station Species Fish Range(mm) 2,3,7,8-TCDDt0 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 5 184-190 ND(0.13) 3 Redbreast sunfish 5 187-202 ND(0.18) RM 52.3 Redbreast sunfish 5 165-185 ND(0.13) RM 52.3 Redbreast sunfish 5 164-195 ND(0.18) 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 cmpppie 5 215-231 ND(0.27) RM 41.5 Black crappie 5 215-229 ND(0.18) RM 41.5 Black crappie 5 220-230 ND(0.10) Common carp 5. 562-632 4.2 Common carp 5 570-655 2.3 Channel catfish 5 418-482 2.0 4B Black crappie 5 223-258 ND(0.11) 4B Black crappie 5 226-241 ND(0.17) RM 39.0 Largemouth bass 5 278-310 ND(0.13) RM 39.0 Largemouth bass 5 270-360 ND(0.21) 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 19.0 Smallmouth bass 5 278-367 ND(0.27) Smaurnouth buffalo 5 451-555 ND(0.12) Smallmouth buffalo 5 406-525 ND(0.22) Total Fish Meted 89 Total Fish Filleted 99 Table 6-4 (cont.). 1998 Resultsrot 1999 ResultsrDt Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDDW Station Species Fish Range(nun) 2,3,7,8-TCDDt°I 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 5 164-180 ND(0.37) Black redhorse 5 340-396 ND(0.18) Black redhorse 5 352-427 ND(0.33) 2 Redbreast sunfish 5 164-177 ND(0.20) 2 Redbreast sunfish 5 167-190 ND(0.37) RM 59.0 Redbreast sunfish 5 166-193 ND(0.28) RM 59.0 Redbreast sunfish 5 158-178 ND(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 Redbreastsunfish 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) Channel catfish 5 425482 0.83 N 4B Black crappie 5 233-252 ND(0.15) 4B Black crappie 5 233-244 ND(0.27) RM 39.0 Largemouth bass 5 259-330 ND(0.17) RM 39.0 Largemouth bass 5 276-305 ND(0.32) Common carp 5 563-686 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 Results(b) 2001 Resultst'o Number of Length Number of Length Station Species Fish Range(mm) 2,3,7,8-TCDD(0 Station Species Fish Range(mm) 2,3,7,8-TCDD(`) 1 Redbreast sunfish 5 137-148 ND(0.48) 1 Black redhorse 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 cup 5 456-555 ND(0.27) RM 59.0 Redbreast sunfish 5 164-181 ND(0.43) RM 59.0 Common carp 5 505-592 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(0.32) RM 52.3 Common carp 5 514-569 ND(0.53) 4A Black crappie 5 212-241 ND(0.29) 4A Channel catfish 5 476-612 1.2 RM 41.5 Black crappie 5 220-241 ND(0.24) RM 41.5 Common carp 5 528-668 1.3 Common carp 4 559-604 1.1 Channel catfish 5 435-487 ND(0.70) w 4B Black crappie 5 213-231 ND(0.41) 4B Flathead catfish 5 405-463 ND(0.29) RM 39.0 Black crappie 5 220-230 ND(0.37) RM 39.0 Common carp 5 654-723 5.6 Common carp 4 593-712 4.4 Flathead catfish 5 407450 ND(0.42) 5 Rock has 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(0.35) Total Fish Filleted 98 Total Fish Filleted 40 Table 6-4 (cont.). 2002 Resul[st� 2003 Results(b) Number of Length Number of Length , , , Station Species Fish Range(mm) 2378-TCDDt`t ng Station Species Fish Range(man) 2,3,7,8-TCDDW RM 164 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 RM 52.3 Common carp 5 575-632 ND(0.22) 3 Common carp 5 545-605 ND(0.31) 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) 'A 4B Common carp 5 647-670 6.6 RM 39.0 Flathead catfish 5 418-505 ND(0.22) 4B Common carp 5 511- RM 39.0 Flathead catfish 5 511-533 533 ND ND(DL=0.20) RM 19.0 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 (a) Survey conducted by EA Engineering,Science,and Technology. Analyses conducted by ENSECO Laboratories 1990-1994,Quanterm Laboratories 1995- 1999,Sevem Trent Laboratories in 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(picogram per gram) ND =Non-detectable at the detection limit in parentheses. f—I --j -- �---� �-_ _- - - - — — - — --- -- Figure 6-1. TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990-2003 (Stations 2 and 3). 2s 20 — — — — — — — — — — — — — — — — — — — — — — — — —�— Station 2 - +- Station 3 c 0 y15 — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — w L d 0 Q- I y r � O. a10 — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — G V 5 — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — �i a a b c c c c 0 \ — + — _ — + 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 YEAR a) TCDD conentrations at Station 3 were not detected, therefore, the value plotted represents the detection limit for that sample. b) TCDD concentrations at Station 2 were not detected, therefore, the value plotted represents the detection limit for that sample. c) TCDD concentrations at Stations 2 and 3 were not detected, therefore, the values plotted represent the detection limits for those samples. Figure 6-1 (Cont.). TCDD Concentrations in Carp Fillets Collected from the Pigeon River, 1990-2003 (Stations 4A and 4B). 70 s \ eo \- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - \ \ 50 — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — C i / O_ \ / ' L ` 40 — — — — —t - - - - -` — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — N \ O1 W \ Q30 — — — — — — — — — — — — —\— — — — — — — — — — — — — — — — — — — — — — — — G � FU— \ 20 \ — — — — — — — — -�10 — — — — — — — — — — — — — — — —\- - —\- - - - - - ' A`�y - - - - - - - - - - - - - - - - - -��— 0 --------------------------------------------- •� ~ •• r 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 YEAR —• — Station 4a — . — Station 4b Figure 6-2. TCDD Concentrations in Catfish Fillets Collected from Stations 4A and 4B in Waterville Lake, 1997-2003. 2.50 2.00 .. \ —0—Station 4A --A—Station 4B C O 1.50 w O1 a \ 0 ACa 1.00 \ F \\ a . / b \ 0.50 a ,� ---- ----- __ a 0.00 1997 1998 1999 2000 2001 2002 2003 YEAR a) TCDD concentrations at Stations 4A and 4B were not detected,therefore,the values plotted represent the detection limits for those samples. b) TCDD concentrations at Station 4B were not detected,therefore,the value plotted represents the detection limit for that sample. 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 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 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 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 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 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 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 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 1997 Dioxin Monitoring in Fish Tissue. EA Report No. 13353.01, prepared for Champion International Corporation, Canton, North Carolina. November. 7-1 EA Engineering, Science, and Technology, Inc. 1998. Results of 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 1999 Dioxin Monitoring in Fish Tissue. EA Report No. 13478.01, prepared for Champion International Corporation, Canton, North Carolina. January. EA Engineering, Science, and Technology, Inc. 2001a. Study Plan for Pigeon River Dioxin Monitoring in Fish Tissue. Prepared for Blue Ridge Paper Products, Canton, North Carolina. November. EA Engineering, Science, and Technology, Inc. 2001b. Results of 2000 Dioxin Monitoring in Fish Tissue. EA Report No. 13745.01, prepared for Blue Ridge Paper Products, Canton, North Carolina. January. EA Engineering, Science, and Technology, Inc. 2001c. Results of 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 2002 Dioxin Monitoring in Fish Tissue. EA Report No. 13900.02, prepared for Blue Ridge Paper Products, Canton, North Carolina. January. Food and Drug Administration. 1981. FDA advises Great Lake 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. 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. 7-2 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. 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. 7-3 APPENDIX A CHAIN OF CUSTODY FORMS ... . . . ` _ _ - y� _ ._ _ . - _ .a � ..;1:. '; t 'i � - _] _ ! �- 1 �_1 Y � -- - - _ 0 Chain of STL Custody Record Severn Trent Laboratories, Inc. STL4124 (09D1) Client ain Project Manager Dale Ch of Custody Number, lue W 'v Pc,, g✓ S'c-e v✓� a 28 03 Address / Telephone Number Area Code)/F Number Lab Number `e _ MO' t.1 ST . ?'??— 6 G 7 y Page— of City/, rr Stale Lp Code Pfier;/Waybillftmbef Contact Lab Contact Analysis(Aflach list if (,._L-1 n 'TJ:1 NC e lR h i e mores ace is needed Project Name and Location(State) a T S� {�Z • can i�� 1 ( u �— � � Special Instructional Contra Purchase OrdedOuote No. Matrix Containers& � ? Conditions of Receipt Preservatives Is o Sample I.D.No.and Description Date Time :� g Q o o A � N t (Containers for each sample maybe combined an one line) a � ,p', � � _ _ � Z, 0 Lam SlrKk RN 5 A F)JAS "130 G�ti s'��C Ctl •Z Car •11�03 00 3 8 sxG o f s so u 8/ab o3 -oc Cu��is 8 x� 03 /03� 6 I Lur 8 s 63 a En ] lack- K4 S 28 n ONO _ RE EI1 ED!;0000 (I01{ j JfE C3 2003 I ibie Hazard identification Sample Disposal d r ( lee may p !assessed it are retained Nan-Hazard ❑ Flammable ❑ Skin Irritant ❑ Poison 8 ❑ Unknown ❑Return To Client ❑ Disposal By Lab ❑Archive For_Months I han'1 rRetnnT-'- --•- Turn Around Time Required CC Requirements(Specify) ❑24 Hours ❑ 48 Hours ❑ 7 Days ❑ 14 Days - 1121 Days ❑Other — I Relinquished By Date Time I. c iv By Date Time �8 " o /3' 2.Relinquis ed By a Date Time 2.Received y Dale Time 8 a o 3.Relinquished By Dale Time 3.Recaiv y ale Time Comments A m DISTRIBUTION: WHITE-Returned to Client with Report: CANARY-Slays with the Sample; PINK-Field Copy A Ut Chain of STL Custody Record Severn Trent Laboratories, Inc. STL4124 (0e01) Client Projecl Manager Date - Chain of CUaledy Number Ri 'e � G�� S, z.� za 03 129069 Address Telephone Numbe (Area CodeallF rc Number Lab Num er 5 i S,Zg - ed - C Z7y Page o/ City Slate Zip Code Site Contact Lab Contact Analysis(Attach list it I mores ace is needed ca v.4-o C 28 IL e ohic b Project Name and Location(State) CerrleryWayblll Number Pre .r R;dt� fits tA� ' sh i+ m Speciallnstructions/ Con acVPurchase Order/Quote No. Containers& f, b Conditions of Receipt Matrix Preservatives gg $ O r Sample I.D.No.and Description Date Time § h o o AR (Containers for each sample may be combined on one line) '�' X y y .`� i rV z i A 2 LdG — ar •• (l� o�C '1 Y& g 0-0 (c, lh'•,e hr SS r/, . N S e.Gt lhr r,S )tt'tn o.�C ��! Sr m 3 m 0 o r m m w V W N e) o v " :JitlDMOx----- o L �c9Cr�^ 1 Possible Hazard Identification Sample Disposal (A lee may be assessed if samples are retained Non-Hazard El Flammable ❑Skin Irritant ❑ Poison ❑ Unknown ❑Return To Client ❑ Disposal By lab El Archive For__Months longer than I monlh) Turn Around Time Required DC Requirements(Specily) ❑ 24 Hours ❑48 Hours ❑ 7 Days ❑ 14 Days ❑21 Days ❑ Other 1. elinquishedB rime 1.Received 9y ` Dfalta w Time 2 efi wished ey G D7{e� /ma� 2.Received By Date Tlme 3.Relinq ed By Date Time J.Received y Date Tim-L� Comments u o` � DISTRIBUTION: WHITE-Returned to Client with Report; CANARY.Stays with the Sample: PINK-Field Copy A N APPENDIX B SEVERN TRENT LABORATORY-SACRAMENTO ANALYTICAL REPORT STL September 30,2003 STL SACRAMENTO PROJECT NUMBER: G3I030256 PO/CONTRACT: 266777 Melanie Samuels Gardner Blue Ridge Paper Products Inc 175 Main Street P.O. Box 4000 Canton,NC 28716 Dear Ms. Samuels Gardner, This report contains the analytical results for the samples received under chain of custody by STL Sacramento on September 3, 2003. These samples are associated with your Pigeon River 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 Severn Trent Laboratories, Inc. STL Sacramento •880 Riverside Parkway,West Sacramento,CA 95605 Atn tlofSevern Trent plc Tel 916 373 5600 Fax 916 3721059•www.sti-inc.com TABLE OF CONTENTS STL SACRAMENTO PROJECT NUMBER G31030256 Case Narrative STL Sacramento Quality Assurance Program Sample Description Information Chain of Custody Documentation BIOLOGIC, 8290,Percent Lipids Samples: 1 through 9 Sample Data Sheets BIOLOGIC, 8290,Dioxins/Furans, Samples: 1 through 9 Sample Data Sheets Method Blank Report Laboratory QC Reports CASE NARRATIVE STL SACRAMENTO PROJECT NUMBER G3I030256 There were no anomalies associated with this project. GM30256 STL Sacramento 916-373-5600 1 of 645 O tN ACCOR C. �O STL Sacramento Certifications/Accreditations Alaska I UST-O55 Ore on CA 200005 - '6�x1:�1n20naii:`c41`^ +, 'aupv'u°.z IPB[1rI5..IVanidi Lv .itr.�S'}•;F(.I.�Q..1�.72P S,NYy,v„`m -, - "e'• wj .tt liken-k'F'AZ0�:1,6 Arkansas NA South Carolina 87014001 MORv ' "'Fe�a's�.�% ; `� Connecticut PH-0691 . i_ iatO R :1I�itrin�.'lI+f`•r..I�nvj;�n�sx0 0p16778 ar FOdai,k `� Y vE6JP Geo is 960 West Vir inia 9930C,3 3rY4 fq"k f'w NAEik vvf ekWISGdnd rx.X .,e ' 962U468M^vRra' Louisiana' 01944 NFESC NA {l. ''vK' 4.•! i'm"."•,1,•Yif K erg 7q .n .- s n,^ Y-:}" 9,J s s; 4 ";."•; r s NevadaiT .CA.D94�...a»f .r$ aUSACEakF,c New Jerse CA005 USDA Foretan Plant 37-82605 _ - ,x��� �ew,+Y,o[I�' .'"' cffxa �{m�stn1'656fm`�`� �'�i aid DA>F'� l tt"+ .o0 -awffS `NELAP accredited. A more detailed parameter list is available upon request. 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 used to evaluate the precision of the process. Duplicate Sample(DU): Different aliquots of the same sample are analyzed*to evaluate the precision of an analysis. Surrogates: Organic compounds not expected to be detected in field samples, which behave similarly to target analyzes. 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. Revised 919103 PAS . G3030256 STL Sacramento 916-373-5600 2 of 645 Sample Summary G31030256 WO# Sample# Client Sample ID Sampling Date Received Date FXHV 1 1 LOC 1 BLACK RH SR FILLETS 8/27/2003 02:30 PM 9/3/2003 09:15 AM FXHV7 2 LOC 2 CARP 5R FILLETS 8/26/2003 01:00 PM 9/3/2003 09:15 AM FXHWC 3 LOC 3 CARP 5R FILLETS 8/26/2003 10:50 AM 9/3/2003 09:15 AM FXHWE 4 LOC 4A CARP 5R FILLETS 8/26/2003 05:00 PM 9/3/2003 09:15 AM FXHWJ 5 LOC 4A FH CATFISH 5R FILLETS 8/27/2003 10:30 AM 9/3/2003 09:15 AM FXHWM 6 LOC 4B CARP 5R FILLETS 8/26/2003 06:30 PM 9/3/2003 09:15 AM FXHWQ 7 LOC 4B FH CATFISH 5R FILLETS 8/27/2003 09:28 AM 9/3/2003 09:15 AM FXHWX S LOC 5 BLACK RH 5R FILLETS 8/28/2003 08:30 AM 9/3/2003 09:15 AM FXHW4 9 LOC 4A CARP WHOLE FILLETS 8/26/2003 05:00 PM 9/3/2003 09:15 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 slated limit. - This report must not be reproduced,except in full,without the written approval of the laboratory. - Results for the following parameters are never reported on a dry weight basis:color,comosivity,density,flashpoint,ignitability, layers,odor,paint filter test,pH,porosity,pressure,reactivity,redox potential,specific gravity,spot tests,solids,solubility, temperature,viscosity,and weight (i3030256 STL Sacramento 916-373-5600 3 of 645 • 7 L3 .1 ki_j . >TL Sacramento -LIENT I. G Q PM-54c— LOG B LOTS( (QUANTIMS ID) L`/ (a QU07EJ_;d�.�LOCATION �V> Initials' �Date" DATE RECEIVED �� 3 3 TIME RECEIVED DELIVERED BY 0"FEDEX ❑ CA OVERNIGHT ❑ CLIENT. .,, ❑ AIRBORNE ❑ GOLDENSTATE ❑ DHL ❑ UPS ❑ BAX.GLOBAL ❑ GO-GETTERS ❑ STL COURIER. ❑ COURIERS ON DEMAND: ❑OTHER ,USTODY SEAL STATUS ErINTACT ❑BROKEN N/A ,;USTODY SEAL 1(S) iHIPPPING CONTAIN ER(S)J�'STL ❑ CLIENT ❑ N/A TEMPERTURE RECORD (IN 00 IR '1;.A 2 ❑ ❑ OTHER ,Oc I(S) TEMPERATURE BLANK ;AMPLE TEMPERATURE a--O £u� COLLECTOR'S NAME: ❑Verified from CDC �,61\10t on CDC )H MEASURED ❑YES ❑ ANOMALY 10'N/A . LABELEDBY..................................................._...................................... ABELSCHECKED BY........".............................."................................... SHORT HOLD TEST NOTIFICATION SAMPLE RECEIVING WEfCHEM ] N/A VOA-Encores 0 N/A ' ] METALS NOTIFIED OF FILTER/PRESERVE VIA VERBAL & EMAIL.P/N/A ] COMPLETE SHIPMENT RECEIVED IN GOOD CONDITION WITH ❑ WA APPROPRIATE TEMPERATURES, CONTAINERS, PRESERVATIVES r]Clouseau ❑TEMPERATURE EXCEEDED (2 0-6 °Cl ❑ N/A ]WET ICE ❑ BLUE ICE ❑GEL PACK ❑ PM NOTIFIED ❑ NO COOLING AGENTS USED totes: 33i0302tEgAVE'NO SPACES BLANK. USE.N/A'IF-NOT APPLiCA§LTt.-SMMAIl tUdB Att)ON1A'�ENTRIES.., ...: . . DA1858tODNEK,._:•„�.,,,•,_ 6.0f645. BIOLOGIC, 8290, Di0XMSIFUMS G3i030256 STL Sacramento 916-373-5600 7 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 1 BLACK RH 5R FILLETS Trace Level Organic Compounds Lot-Sample #. . .: G3I030256-001 Work Order #...: FXHV11AA Matrix. ... . ....: BIOLOGIC Date Sampled. .. : 08/27/03 Date Received.. : 09/03/03 Prep Date. ... ..: 09/09/03 Analysis Date.. : 09/13/03 Prep Batch #. .. : 3252577 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 2.2 SW846 8290 G=30256 STL Sacramento 916-373-5600 8 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 1 BLACK RH 5R FILLETS Trace Level Organic Compounds Lot-Sample #.. .: G3I030256-001 Work Order #...: FXHVIIAC Matrix... . -. ...: BIOLOGIC Date Sampled. . . : 08/27/03 Date Received..: 09/03/03 Prep Date. . . . ..: 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #...: 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD ND 0.20 pg/g SW846 8290 Total TCDD ND 0.20 pq/g SW846 8290 1,2,3,7,8-PeCDD ND- 0.48 pg/g SW846 8290 Total PeCDD ND 0.46 pg/g SW846 8290 1,2,3,4.,7,8-HXCDD ND 0.34 pg/g SW846 8290 1,2,3,6,7,8-HXCDD ND 0.28 pq/g SW846 8290 1,2,3,7,8,9-HpCDD ND 0.29 pg/g SW846 8290 Total HxCDD ND 0.34 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD ND 0.48 pg/g SW846 8290 Total HpCDD ND 0.48 pg/g SW846 8290 OCDD ND 1.6 pg/g SW846 8290 2,3,7,8-TCDF ND 0.15 pg/g SW846 8290 Total TCDF ND 1.2 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.23 pq/q SW846 8290 2,3,4,7,8-PeCDF ND 0.23 pg/g SW846 8290 Total PeCDF ND 0.23 pg/g SW846 8290 1,2,3,4,7,8-HpCDF ND 0.22 pg/g SW846 8290 1,2,3,6,7,8-HXCDF ND 0-18 pg/g SW846 8290 2,3,4,6,7,8-HXCDF ND 0.22 pg/g SW846 8290 1,2,3,7,8,9-HXCDF ND 0.25 pg/g SW846 8290 Total HxCDF ND 0.30 pg/g SW846 8290 1,2,3,4,6,7,8-HeCDF ND 0.43 pq/q SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.51 pg/g SW846 8290 Total HpCDF ND 0.51 pg/g SW846 8290' OCDF ND 0.61 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 70 (40 - 135) 13C-1,2,3,7,8-PeCDD 70 (40 - 135) 13C-1,2,3,6,7,8-HpCDD 62 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 68 (40 - 135) 13C-OCDD 57 (40 - 135) 13C-2,3,7,8-TCDF 65 (40 - 135) 13C-1,2,3,7,8-PeCDF 73 (40 - 135) 13C-1,2,3,4,7,8-HXCDF 69 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 64 (40 - 135) NOTE(S) : The-Tmis-reporting limit for the TCDF homologue series has been raised due to the presare of a dipheneyl ether(DPE). No Gagging is required. Goiv30256 STL Sacramento 916-373-5600 9 of 645 M 10 01 0099-ELE-916 olueweMS IIS 9SZOEN^9 06Za 9baMs 8 Z'E sPidzZ �aaoaad aoHS3W SSIM .LIWI'I S'If153X uaiswvRvd T caogoed uozanlia LLSZSZ£ = "# Rogea; dead EO/ET/6o z"aiea szsdle¢y C0160160 =- - - - - -a4ea dead EO/EO/60 = -PaAiaOaa area EO/9Z/Eo = " �.PaleS GILa JI'JO'IOIfi ="" ' - •"xca�eW VYTLAHxa ="'# Tap-To $aom Z00-95ZoEOI£`J = " '# oldwes-:10Z spanodwoJ Oraefiao IanaffI a0eay sSam-TA us dHVD Z Jo'I =a2 aldnes :Ina?ZJ JNI Ssanaoxd Maw ED= Harla BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 2 CARP 5R FILLETS Trace Level Organic Compounds Lot-Sample #. __: G31030256-002 Work Order #.. .: PXHV71AC Matrix- . . --- - -- : BIOLOGIC Date Sampled--- : 08/26/03 Date Received.-: 09/03/03 Prep Date. . .. .. : 09/09/03 Analysis Date.. : 09/13/03 Prep Batch ##---- 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD ND 0.18 pg/g SW846 8290 Total TCDD ND _ 0.18 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 0.48 pg/g SW846 8290 Total PeCDD ND 0.48 pg/g SW846 8290 1,2,3,4,7,8-HXCDD ND 0.40 pg/g SW846 8290 1,2,3,6,7,8-HxCDD ND 0.59 pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 0.35 pg/g SW846 8290 Total HxCDD ND 0.59 pg/g SW846 8290 112,3,4,6,7,8-HpCDD ND 2.1 pg/g SW846 8290 Total HpCDD ND 2.1 pg/g SW846 8290 OCDD 11 pg/g SW846 8290 2,3,7,8-TCDF ND 0.39 pg/g SW846 8290 Total TCDF ND 0.39 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.26 pg/g SW846 8290 2,304,7,8-PeCDF ND 0.26 pg/g SW846 8290 Total PeCDF ND 0.26 pg/g SW846 8290 1,2,3,4,7,8-HxCDF NO 0.29 pg/g SW846 8290 1,2,3,6,7,8-HXCDF ND 0.25 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.30 pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 0.34 pg/g SW846 8290 Total HxCDF NO 0.47 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 0.37 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF NO 0.43 pg/g SW846 8290 Total HpCDF NO 0.43 pq/q SW846 8290 OCDF ND 0.67 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 79 (40 - 135) 13C-1,2,3,7,8-PeCDD 81 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 72 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 71 (40 - 135) 13C-OCDD 61 (40 - 135) 13C-2,3,7,8-TCDF 74 (40 - 135) 13C-1,2,3,7,8-PeCDF 75 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 72 (40 - 135) 13C-1,2,3,4,6,7, 8-HpCDF 71 (40 - 135) GoiJ30256 STL Sacramento 916-373-5600 11 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 3 CARP 5R FILLETS Trace Level Organic Compounds Lot-Sample #.__ : G3I030256-003 Work Order #. .. : FXHWCIAA Matrix--- ------ BIOLOGIC Date Sampled. . . : 08/26/03 Date Received- .: 09/03/03 Prep Date.. . . . - : 09/09/03 Analysis Date.. : 09/13/03 Prep Batch #. . .: 3252577 Dilution Factor: I DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 6.6 & SW846 8290 b..030256 STL Sacramento 916-373-5600 12 of 645 SP910 EL 0098-ELE-91.6 oluaweioes 11S 9SZOENpO '1R�� 1%$H¢ +a'T�i]0J3Yiy1•uwn10> 5'=a W01J iA!591]IfOJ 1PU UO.W U9UW=RIM PUO •JAUMPU Z) 'nwq 3uluodai Pg11wy1 ssal st 116Ag'11=1 patRumsg L = (S)RION (SET - OP) P9 dQJdH-8'L'9 It,'£'Z'T-J£T (SET - OP) OL 'dQJdH-8'L'b'E'Z'i-JET (SET - OP) OL 3QJad-8'L'E'Z'i-J£T (SEC - OP) L9 dQJZ-8'L'E'Z-JET (SET - OP) PS QQJO-J£T (SEE - OP) L9 QQOdH-8'L'9'P'E'Z'T-JET (SET - OP) £9 QQOXH-8'L'9'£'Z'T-JET (SET - OP) OL 032)ad-8'4 'E'Z'T-JET (SET - OP) EL QQJZ-8'L 'E'Z-JET SZIWI'I Auahoosu SQdvawzs 'T aHazNI XdaAODEH ZNamiad 06ZB 9P8MS b/bd 6S"0 QN acoo o6Z8 9118MS b/bd 8P•0 QN dQJdH Te-4oL 06Z8 9P8MS b/5d 819-0 (IN 9QJdH-6'8'L'P'E'Z'T 06Z8 9PBMS 6/bd 11110 QN dQJdH-8'L'9'P'£'ZIT o6Z8 91WBMS 5/bd 9L'O QN dQJxH Te,4oZ 06Z8 9P8MS b/bd 9Z•0 QN dQJdH-6'8'L'E'Z'I 06ZS 9P8MS b/bd EZ'O cm dQ3dH-8'L'9'P'E'Z 06ZB 9P8MS s/.6d 61•0 QN SQJXH-9'L'9'E'Z'i o6Z8 9118MS b/bd ZZ'0 QN daJxH-8'L'P'£'Z'T 06Z8 9P8MS b/bd OE'0 (N 3QJad Ta3o.1 06ZB 9P8MS b/Hd 9Z"o QN daoad-8'L'P'E'Z 06ZB 9P8MS b/sd OE"0 QN dQJad-8'L'E'Z'T 06Z8 9P8MS b/bd 18"0 dOz)Z Ta:10Z 06ZS 9P8MS b/bd P TS'O 2lQJZ-8'L'E'Z o6Z8 9i8MS b/bd t OT QQJo 06ZO 9PSMS b/bd T'E QQJdH TEgoZ o6Z8 9P8MS b/bd t TIE Q®dH-8'L'9'VIE'Z'T 062E 9P8MS b/bd 69.0 QN aQJxH TeaoZ 06Z8 9P8MS 5/5d 9E-0 QN QQJXH-6'8'L'E'Z'T 06Z8 9PBMS .6/bd 69'0 (IN QQJxH-8'L'9'E 'Z'T o6Z8 9PBMS b/Bd Z31'0 QN QQOXH-8'L'P'E'L'I o6Z8 91v8MS 5/15d 89'0 QN QQJad Tv2oZ 06Z8 9P814S b/bd 9S-0 QN QQJad-B'L'E'Z'I 06ZB 9PBMS 5/Bd T£'O UN QQJZ TugoZ o6Z8 9PBMS S/bd TU O QN QQJZ-8'L'E'Z QOHZ3W SZINfl ZIWI'I Z'SIlSa-d d3Z2wvzivd NOIZ03Z3Q i =.xo�oed uor;nTiQ ELSZSZ£ = " "# gogEu dasd EO/ET/60 c '-agea szs. l=v E0160160 :- -aqua de;rd EO/EO/60 = "PaAiaoag agrG EO/9Z/80 =-- -paTdmes ageQ JI°JO'IOIS °---- ---- -wragvx JKTJMHXd = ' "'# 3aPY0 NaOM £00-9SZ0£OIEO :"_#k aTdmES-qoQ spunodmoJ z)iu f=O TanaZ aO221 sZB:P a us di3HJ E oui :QI aidmes 7ua-cT3 JNI SzollaoSd 2IIdYd SD= ancia BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4A CARP SR FILLETS Trace Level Organic Compounds Lot-Sample #._. : G3I030256-004 Work Order #_. .: FXHWEIAA Matrix. . ... ....: BIOLOGIC Date Sampled. . . : 08/26/03 Date Received. . : 09/03/03 Prep Date--- --- : 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #. . . : 3252577 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 16 SW846 0290 G�030256 STL Sacramento 916-373-5600 14 of 645 BLUE RIDGE PAPER PRODtiCTS INC Client Sample ID: LOC 4A CARP 5R FILLETS Trace Level Organic Compounds Lot-Sample #. _.: G3I030256-004 Work Order #. ..: FXHWEIAC Matrix. ... .. ... BIOLOGIC Date Sampled_ _ . : 08/26/03 Date Received.-: 09/03/03 Prep Date.... . . : 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #.. . : 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD 3.4 Total TCDD Pg/9 SW846 8290 3.4 pg/g SW846 8290 1,2,3,7,8-PeCDD 2_5 pg/g SW846 8290 Total PeCDD 2.5 pg/g SW846 8290 1,2,3,4, 7,8-HxCDD ND 1.7 pg/g SW846 8290 1,2,3,6,7,8-HxCDD 7.7 pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 1.4 pg/g SW846 8290 Total HXCDD 7.7 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD 24 pg/g SW846 8290 Total HpCDD 34 Pg/g SW846 8290 OCDD 92 Pg/g SW846 8290 2,3,7,8-TCDF 3_4 CON pg/g SW846 8290 Total TCDF 3.4 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 1.9 pg/g SW846 8290 2,3,4,7,8-PeCDF 2.6 J pg/g SW846 8290 Total PeCDF 2-6 pg/g SW846 8290 1,2,3,4,7,8-HxCDF ND 1.4 pg/g SW846 8290 1,2,3,6,7,E-HXCDF ND 1.2 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.71 pg/g SW846 8290 1,2,3,7,8,9-HpCDF ND 0.30 pg/g SW846 8290 Total HxCDF ND 2.3 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 2.3 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.69 pg/g SW846 8290 Total HpCDF ND 2.3 pg/g SW846 8290 OCDF ND 0.50 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3, 7,8-TCDD 74 (40 - 135) 13C-1,2,3,7,8-PeCDD 76 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 68 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 70 (40 - 135) 13C-OCDD 65 (40 - 135) 13C-2,3,7,8-TCDF 72 (40 - 135) 13C-1,2,3,7,8-PeCDF 73 (40 - 135) 13C-1,2,3,4,7,8-HpCDF 69 (40 - 135) 13C-1,2,3,4,6,7, 8-HpCDF 76 (40 - 135) NOTE(S) - CON Cognation amlysis. 1 Fztinated result.Re Wt is less than the reporting limit. G�.J30256 STL Sacramento 916-373-5600 15 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4A PH CATFISH 5R FILLETS Trace Level Organic Compounds Lot-Sample #. . .: G31030256-005 Work Order #.. .: FXHWJIAA Matrix. . . .. .. . . : BIOLOGIC Date Sampled.. .: 08/27/03 Date Received. .: 09/03/03 Prep Date.. . ... : 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #. . .: 3252577 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 2.5 & SW846 8290 Got030256 STL Sacramento 916-373-5600 16 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4A PH CATFISH SR FILLETS Trace Level Organic Compounds Lot-Sample #--- : G3I030256-005 Work Order #.. .: FXHWJIAC Matrix. . . .. . . . .: BIOLOGIC Date Sampled. . . : 08/27/03 Date Received..: 09/03/03 Prep Date. . . ...: 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #.- . : 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD ND 0.35 pg/g SW846 8290 Total TCDD ND 0.35 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 0.83 pg/g SW846 8290 Total PeCDD ND 0.83 pg/g SW846 8290 1,2,3,4,7,8-HxCDD ND 0.61 pg/g SW846 8290 1,2,3,6,7,8-HxCDD ND 0.50 pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 0.52 pg/g SW846 8290 Total HxCDD ND 0.61 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD ND 1.4 pg/g SW846 8290 Total HpCDD ND 1.4 OCDD pg/g SW846 8290 6.4 a pg/g SW846 8290 2,3,7,8-TCDF ND 0.98 pg/g SW846 8290 Total TCDF ND 0.98 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.48 pg/g SW846 8290 2,3,4,7,8-PeCDF ND 0.48 pg/g SW846 8290 Total PeCDF ND 0.48 pg/g SW846 8290 1,2,3,4,7,8-HxCDF ND 0.43 pg/g SW846 8290 1,2,3,6,7.,8-HXCDF ND 0.36 pg/g SW846 8290 2,3,4,6,7,E-HXCDP ND 0.44 pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 0.50 pg/g SW846 8290 Total HxCDF ND 0.74 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 0.67 pg/g SW846 8290 1,2,3,4,7,8,9-HeCDF ND 0.79 pg/g SW846 8290 Total HpCDF ND 0.79 pg/g SW846 8290 OCDF _ ND 1.0 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3, 7,8-TCDD 54 (40 - 135) 13C-1,2,3,7,8-PeCDD 52 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 44 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 48 (40 - 135) 13C-OCDD 41 (40 - 135) 13C-2,3,7,8-TCDF 50 (40 - 135) 13C-1,2,3,7,8-PeCDF 51 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 45 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 48 (40 - 135) NOTE(S) • 1 Estimated rmlt.Result is less than the reposing limi[. w030256 STL Sacramento 916-373-5600 17 of 645 BLUE RIDGE PAPER pRODucrS INC Client Sample ID: LOC 4A CARP WHOLE FILLETS Trace Level Organic Compounds Lot-Sample #.. .: G3I030256-009 Work Order #. . .: FXHW41AA Matrix--- - -- --- BIOLOGIC Date Sampled. . .: 08/26/03 Date Received.. : 09/03/03 Prep Date... . .. . 09/09/03 Analysis Date..: 09/13/03 Prep Batch #-. . : 3252577 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 11 $ SW84G 8290 Go,030256 STL Sacramento 916-373-5600 24 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4A CARP WHOLE FILLETS Trace Level Organic Compounds Lot-Sample #.. . : G3I030256-009 Work Order #. . .: FXHW41AC Matrix. ... .. ...: BIOLOGIC Date Sampled. . .: 08/26/03 Date Received. . : 09/03/03 Prep Date.. . . ..: 09/o9/03 Analysis Date.. : 09/13/03 Prep Batch #.. . : 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD 1.9 pg/g SW846 8290 Total TCDD 1-9 Pg/g SW846 8290 1,2,3,7, 8-PeCDD ND 1.7 pg/g SW846 5290 Total PeCDD ND 1.7 pg/g SW846 8290 1,2,3,4,7,8-HxCDD ND 0.34 pg/g SW846 8290 1,2,3,6,7,8-HXCDD 5.0 pg/g SW846 8290 1,2,3,7,8,9-14XCDD ND 0.91 T Pg/g SW846 8290 Total HxCDD 8.0 pg/g SW846 8290 1,2,3,4,6,7,8-EPCDD 21 pg/g SW846 8290 Total HpCDD 28 pg/g SW846 8290 OCDD 81 Pg/g SW846 8290 2,3,7,8-TCDF 1.5 CON pg/g SW846 6290 Total TCDF 1-5 Pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.69 pg/g SW646 8290 2,3,4,7,8-PeCDF ND 1.7 pg/g SW846 8290 Total PeCDF ND 1.7 pg/g SW846 8290 1,2,3,4,7,8-HxCDF ND 0.82 pg/g SW846 8290 1,2,3,6,7,8-HxCDF ND 0.73 Pg/g SW846 8290 2,3,4,6,7,8-HXCDF ND 0.26 pg/g SW846 8290 1,2,3,7,8,9-HXCDF ND 0.29 Pg/g SW846 8290 Total HxCDF ND 1.8 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 1.4 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0-71 pg/g SW846 3290 Total HpCDF ND 1.4 pg/g SW846 8290 OCDF ND 0.51 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 71 (40 - 135) 13C-1,2,3,7,8-PeCDD 79 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 74 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 70 (40 - 135) 13C-OCDD 64 (40 - 135) 13C-2,3,7,8-TCDF 69 (40 - 135) 13C-1,2,3,7,8-PeCDF 72 (40 - 135) 13C-1,2,3,4, 7,8-HxCDF 75 (40 - 135) 13C-1,2,3,4, 6,7,8-HpCDF 68 (40 - 135) NOTE(S) - CON Conn tion amlysis. (,c�J30256 STL Sacramento 916-373-5600 25 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4B CARP 5R FILLETS Trace Level Organic compounds Lot-Sample #.. .: G31030256-006 work Order #--- : FXHWMIAA Matrix... . ... .- : BIOLOGIC Date Sampled. . . : 08/26/03 Date Received..: 09/03/03 Prep Date. .. ...: 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #. .. : 3252577 Dilution Factor: I DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 22 $ SW846 8290 6.030256 STL Sacramento 916-373-5600 18 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4B CARP SR FILLETS Trace Level Organic Compounds Lot-Sample #. ..: G31030256-006 Work Order #.. .: FXHPIMIAC Matrix. .... . . .. : BIOLOGIC Date Sampled. . . : 08/26/03 Date Received..: 09/03/03 Prep Date.. .... : 09/09/03 Analysis Date.. : 09/13/03 Prep Batch #. . .: 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TC10D 12 pg/g SW846 8290 Total TCDD 12 pg/g SW846 8290 1,2,3,7,8-PeCDD 3.7 T pg/g SW846 8290 Total PeCDD 3.7 pg/g SW846 8290 1,2,3,4,7,8-HxCDD 3-1 T pg/g SW846 8290 1,2,3,6,7,8-HxCDD 11 pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 1.8 pg/g SW846 8290 Total HxCDD . 14 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD 30 pg/g SW846 8290 Total HxCDD 35 pg/g SW846 8290 OCDD 76 pg/g SW846 8290 2,3,7,8-TCDF 3.5 CON pg/g SW846 8290 Total TCDF 3.5 CON pg/g SW846 8290 1,2,3,7,8-PeCDF ND 1.4 pg/g SW846 8290 2,3,4,7,8-PeCDF 4.4 .T pg/g SW846 8290 Total PeCDF 7.2 pg/g SW846 8290 1,2,3,4,7,8-HXCDF ND 1.6 pg/g SW846 8290 1,2,3,6,7,8-HxCDF NO 1.8 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.93 pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 0.30 pg/g SW846 8290 Total HxCDF ND 5.5 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 2.4 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.76 pg/g SW846 8290 Total' HpCDF ND 2.4 pg/g SW846 8290 OCDF ND 0.30 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 81 (40 - 135) 13C-1,2,3,7,8-PeCDD 81 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 63 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 71 (40 - 135) 13C-OCDD 69 (40 - 135) 13C-2,3,7,8-TCDF 74 (40 - 135) 13C-1,2,3,7, 8-PeCDF 80 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 65 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 67 (40 - 135) NOTE(S) - J Fstitnated result.Result is less than the reporting limit. CON Confirmation Mlysis. The"Totals'reporting limit for the Hen Furan homologue=in has been raised due to the presence of a diphenyl e9w(DP6). No nagging is necessary. G.n,30256 STL Sacramento 916.373-5600 19 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4B FE CATFISH SR FILLETS Trace Level Organic Compounds Lot-Sample #. ..: G31030256-007 Work Order #. ..: FXHWQIAA Matrix-- -- -- ---: BIOLOGIC Date Sampled. . .: 08/27/03 Date Received. . : 09/03/03 Prep Date.. . ... : 09/09/03 Analysis Date. .: 09/13/03 Prep Hatch #. ..: 3252577 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 3.4 9W846 8290 631030256 STL Sacramento 916-373-5600 20 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 4B PH CATFISH SR FILLETS Trace Level Organic Compounds Lot-Sample #...: G3I030256-007 Work Order #---: FXHWQIAC Matrix- -- -- - - --: BIOLOGIC Date Sampled. . . : 08/27/03 Date Received.. : 09/03/03 Prep Date... . .. : 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #. . .: 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3, 7,8-TCDD ND 0.20 pg/g SW846 8290 Total TCDD ND 0.20 pg/g SW846 8290 1,2, 3,7,E-PeCDD ND 0.50 pg/g SW846 8290 Total PeCDD ND 0.50 pg/g SW846 8290 1,2,3,4,7,8-HXCDD ND 0.37 pg/g SW846 8290 1,2,3,6,7,8-HXCDD ND 0.38 pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 0.32 pg/g SW846 8290 Total HxCDD ND 0.38 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD ND 0.54 pg/g SW846 8290 Total HpCDD ND 0.54 pg/g SW846. 8290 OCDD ND 0.96 pg/g SW846 8290 2,3, 7,8-TCDF ND 0.16 pg/g SW846 8290 Total TCDF ND 0.46 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.26 pg/g SW846 8290 2,3,4,7,8-PeCDF ND 0.26 pg/g SW846 8290 Total PeCDF ND 0.26 pg/g SW846 8290 1,2,3,4,7,8-HxCDF ND 0.26 pg/g SW846 8290 1,2,3,6,7,8-HxCDF ND 0.22 pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.27 pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 0.31 pg/g SW846 8290 Total HxCDF ND 0.31 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 0.50 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.59 pg/g SW846 8290 Total HpCDF ND 0.59 pg/g SW846 8290 OCDF ND 0.54 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 71 (40 - 135) 13C-1,2,3,7,8-PeCDD 75 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 66 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 67 (40 - 135) 13C-OCDD 56 (40 - 135) 13C-2,3,7,8-TCDF 71 (40 - 135) 13C-1,2,3,7,8-PeCDF 71 (40 - 135) 13C-1,2,3,4,7, 8-HxCDF 62 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 64 (40 - 135) W030256 STL Sacramento 916-373-5600 21 of 645 BLUE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 5 BLACK RH SR FILLETS Trace Level Organic Compounds Lot-Sample #. . .: G3I030256-008 Work Order #.-. : FXHWXIAA Matrix... . . . ...: BIOLOGIC Date Sampled. -. : 08/28/03 Date Received. .: 09/03/03 Prep Date. . . . . .: 09/09/03 Analysis Date. -: 09/13/03 Prep Batch #. ..: 3252577 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD Percent Lipids 6.1 g SN846 8290 G-J30256 STL Sacramento 916-373-5600 22 of 645 13LDE RIDGE PAPER PRODUCTS INC Client Sample ID: LOC 5 BLACK RH SR FILLETS Trace Level Organic Compounds Lot-Sample #.__ : G3I030256-008 Work Order #.. .: FXHWXIAC Matrix. . . .. . ...: BIOLOGIC Date Sampled. .-: 08/28/03 Date Received.. : 09/03/03 Prep Date. .. . .. . 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #.. . : 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD ND 0.19 Pg/g SW846 8290 Total TCDD ND 0.19 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 0.58 Pg/g SW846 8290 Total PeCDD ND 0.58 pg/g SW846 8290 1,2,3,4,7,8-HpCDD ND _ 0.35 pg/g SW846 8290 1,2,3,6,7,8-HxCDD ND 0.29 pg/g SW846 8290 1,2,3,7,8,9-HXCDD ND 0.30 pg/g SW846 8290 Total HxCDD ND 0.35 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD ND 0.55 pg/g SW846 8290 Total HpCDD ND OCDD 0.55 pg/g SW846 6290 ND 0.74 pg/g SW846 8290 2,3,7,8-TCDF 0.GG CON,J Total TCDF 0_66 Pg/g SW846 8290 Pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.28 Pg/4 SW846 6290 2,3,4,7,8-PeCDF ND 0.28 Pg/g SW846 8290 Total PeCDF ND 0.28 pg/g SW846 8290 1,2,3,4,7,8-HXCDF ND 0.22 Pg/g SW846 8290 1,2,3,6,7,8-HxCDF ND 0.19 Pg/g SW846 8290 2,3,4,6,7,8-HxCDF ND 0.23 Pg/g SW846 8290 1,2,3,7,8,9-HxCDF ND 0.26 pg/g SW846 8290 Total HxCDF ND 0.26 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDF ND 0.37 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.44 pg/g SW846 8290 Total HpCDF ND 0.44 OCDF ND Pg/g SW846 8290 0.63 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 75 (40 - 135) 13C-1,2,3,7,8-PeCDD 75 (40 - 135) �l3C-1,2,3,6,7,8-HxCDD 72 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 71 (40 - 135) 13C-OCDD 67 (40 - 135) 13C-2,3,7,8-TCDF 69 (40 - 135) 13C-1,2,3,7,8-PeCDF 74 (40 - 135) 13C-1,2,3,4,7,8-HxCDF 71 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 68 (40 - 135) NOTE(S) : CON conGm„um,analysis. J Estimated result.Result is less than the repotting limit W,030256 STL Sacramento 916-373-5600 23 of 645 QC DATA ASSOCIATION SIM MARY G3I030256 Sample Preparation and Analysis Control Numbers ANALYTICAL LEACH PREP SAMPLE# MATRIX METHOD BATCH # BATCH # MS RUN# 001 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 - 3252577 002 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 003 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 004 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 005 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 006 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 007 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 008 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 009 BIOLOGIC SW846 8290 3252573 BIOLOGIC SW846 8290 3252577 G-J30256 STL Sacramento 916-373-5600 26 of 645 METHOD BLANK REPORT Trace Level Organic Compounds Client Lot #.. . : G32030256 Work Order #.. . : FXXLJIAA Matrix.. .. . .. ..: BIOLOGIC MB Lot-Sample #: G32090000-573 Prep Date... ...: 09/09/03 Analysis Date- .: 09/13/03 Prep Batch #.. .: 3252573 Dilution Factor: 1 DETECTION PARAMETER RESULT LIMIT UNITS METHOD 2,3,7,8-TCDD ND 0.18 pg/g SW846 8290 Total TCDD ND 0.18 pg/g SW846 8290 1,2,3,7,8-PeCDD ND 0.40 pg/g SW846 8290 Total PeCDD ND 0.40 pg/g SW846 8290 1,2,3,4,7,8-HXCDD ND 0.37 pg/g SW846 8290 1,2,3,6,7,8-HxCDD ND 0.31 pg/g SW846 8290 1,2,3,7,8,9-HxCDD ND 0.32 pg/g SW846 8290 Total HxCDD ND 0.37 pg/g SW846 8290 1,2,3,4,6,7,8-HpCDD ND 0.40 pg/g SW846 8290 Total HpCDD ND 0.40 pq/g SW846 8290 OCDD ND 0.66 pg/g SW846 8290 2,3,7,8-TCDF ND 0.13 pg/g SW846 8290 Total TCDF ND 0.13 pg/g SW846 8290 1,2,3,7,8-PeCDF ND 0.25 pg/g SW846 8290 2,3,4,7,8-PeCDF ND 0.25 pg/g SW846 8290 Total PeCDF ND 0.25 pg/g SW846 8290 1,2,3,4,7,8-HxCDF ND 0.21 pg/g SW846 8290 1,2,3,6,7,8-HxCDF ND 0.18 pq/g SW846 8290 2,3,4, 6,7,8-HxCDF ND 0.22 pg/g SW846 8290 1,2,3,7,8,9-HXCDF ND 0.25 pg/g SW846 8290 Total HxCDF ND 0.25 pg/g SW846 8290 1,2,3,4,6,7,8-HeCDF ND 0.37 pg/g SW846 8290 1,2,3,4,7,8,9-HpCDF ND 0.43 pg/g SW846 8290 Total HpCDF ND 0.43 pg/g SW846 8290 OCDF ND 0.64 pg/g SW846 8290 PERCENT RECOVERY INTERNAL STANDARDS RECOVERY LIMITS 13C-2,3,7,8-TCDD 77 (40 - 135) 13C-1,2,3,7,8-PeCDD 79 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 75 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 75 (40 - 135) 13C-OCDD 66 (40 - 135) 13C-2,3,7,8-TCDF 72 (40 - 135) 13C-1,2,3,7,8-PeCDF 74 (40 - 135) 13C-1,2,3,4,7, 8-HxCDF 75 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 73 (40 - 135) NOTE(S) : Calculations are performed before rounding to avoid round-off errors in oaleular j results. W030256 STL Sacmmento 916-373-5600 27 of 645 LABORATORY CONTROL SAMPLE EVALUATION REPORT Trace Level Organic Compounds Client Lot #___ : G3I030256 Work Order #...: FXXLJ3.AC Matrix---- --- - - BIOLOGIC LCS Lot-Sample#: G3I090000-573 Prep Date. .. . . . : 09/09/03 Analysis Date.. : 09/13/03 Prep Batch #. . .: 3252573 Dilution Factor: 1 PERCENT RECOVERY PARAMETER RECOVERY LIMITS METHOD 2,3,7,8-TCDD 103 (50 - 150) SW846 8290 1,2,3,7,8-PeCDD 104 (50 - 3.50) SW846 8290 1,2,3,4,7,8-HxCDD 120 (5D - ISO) SW846 8290 1,2,3,6,7,8-HxCDD 96 (50 - 150) SW846 8290 1,2,3,7,8,9-HxCDD 107 (50 - 150) SW846 8290 112,3,4,6,7,8-HpCDD 95 (50 - 3.50) SW846 8290 OCDD 99 (50 - 3.50) SW846 8290 2,3,7,8-TCDF 102 (50 - 150) SW846 8290 1,2,3,7,8-PeCDF 96 (50 - 150) SW846 6290 2,3,4,7,8-PeCDF 100 (50 - 3.50) SW846 8290 1,2,3,4,7,8-HxCDP 94 (50 - 150) SW846 8290 1,2,3,6,7,8-HxCDF 93 (50 - 150) SW846 8290 2,3,4,6,7,8-HxCDF 99 (50 - 150) SW846 8290 1,2,3,7,8,9-HxCDF 99 (50 - 350) SW846 8290 1,2,3,4,6,7,8-HpCDF 93 (50 - 250) SW846 8290 1,2,3,4,7,8,9-HpCDF 87 (50 - 3.50) SW846 8290 OCDF 96 (50 - 150) SW846 8290 PERCENT RECOVERY INTERNAL STANDARD RECOVERY LIMITS 13C-2,3,7,8-TCDD 78 (40 - 135) 13C-1,2,3,7,8-PeCDD 79 (40 - 135) 13C-1,2,3, 6,7,8-HxCDD 73 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 76 (40 - 135) 13C-OCDD 66 (40 - 135) 13C-2,3,7,8-TCDF 73 (40 - 135) 13C-1,2,3,7,8-PeCDF 76 (40 - 135) 13C-1,2,3,4,7,8-HXCDF 74 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 70 (40 - 135) NOTE(S) - Calculations are performed before rounding to avoid roLMpff errors in calculated results. Bold print denota cannot parameters G=30256 STL Sacramento 916-373-5600 28 of 645 LABORATORY CONTROL SAMPLE DATA REPORT Trace Level Organic Compounds Client Lot #.__ : G31030256 Work Order #_.. : FXXLJIAC Matrix. . ... ... . : BIOLOGIC LCS Lot-Sample#: G3I090000-573 Prep Date. . .. . .: 09/09/03 Analysis Date. .: 09/13/03 Prep Batch #. .. : 3252573 Dilution Factor: 1 SPIKE MEASURED PERCENT PARAMETER AMOUNT AMOUNT UNITS RECOVERY METHOD 2,3,7,8-TCDD 20.0 20.7 pg/g 3.03 SW846 8290 1,2,3,7,8-PeCDD 100 104 pg/g 104 SW846 8290 1,2,3,4,7,8-HxCDD 100- 120 pg/g 120 SW846 8290 1,2,3,6,7,8-HxCDD 100 96.4 pg/g 96 SW846 8290 1,2,3,7,8,9-11xCDD 100 107 pg/g 107 SW846 8290 1,2,3,4,6,7,8-HpMD 100 95.1 pg/g 95 SW846 8290 OCDD 200 198 Pg/g 99 SW846 8290 2,3,7,8-TCDF 20-0 20.3 Pg/g 102 SW846 8290 1,2,3,7,8-PeCDF 100 96.3 pg/g 96 SW846 8290 2,3,4,7,8-PeCDF 100 99.6 pg/g 100 SW846 8290 1,2,3,4,7,8-HxCDF 100 94.2 pg/g 94 SW846 8290 1,2,3,6,7,8-HxCDF 100 92.9 pg/g 93 SW846 8290 2,3,4,6,7,E-HxMF 100 98-8 pg/g 99 SW846 8290 1,2,3,7,8,9-HxCDF 100 99.0 pg/g 99 SW846 8290 1.2,3.4.6,7.8-HpCDF 100 93.2 pg/g 93 SW846 B290 1,2,3,4,7,8,9-HpCDF 100 67.2 Pg/g 87 SW846 8290 OCDF 200 192 pg/g 96 SW846 8290 PERCENT RECOVERY INTERNAL STANDARD RECOVERY LIMITS 13C-2,3,7,8-TCDD 78 (40 - 135) 13C-1,2,3,7,8-PeCDD 79 (40 - 135) 13C-1,2,3,6,7,8-HxCDD 73 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDD 76 (40 - 135) 13C-OCDD 66 (40 - 135) 13C-2,3,7,8-TCDF 73 (40 - 135) 13C-1,2,3,7,8-PeCDF 76 (40 - 135) 13C-1,2,3,4,7,8-HXCDF 74 (40 - 135) 13C-1,2,3,4,6,7,8-HpCDF 70 (40 - 135) NOTE(S) - Calculations are performed before rounding to avoid murd.off error in calculated resin¢. Bold prior dumles control parameters G=30256 STL Sacramento 916-373-5600 29 of 645 r BLUE* RIDGE PAPER PRODUCTS INC. April 17, 2002 R 0 d N - 4122M "I Mr. Don Anderson U.S. Environmental Protection Agency WATER OUAUTY SECTI7ri Mail Code 4303 HEVIL E REGIONAL OFFICL T , Room 195A, East Tower 401 M Street, SW Washington, D.C. 20460 Re: SIMCO's RDP Color Reduction Method Dear Mr. Anderson: Blue Ridge Paper Products Inc. is writing in response to your request for information concerning the SIMCO Products Inc. color removal trials conducted at the Canton Mill in the fall of 2000. This process is similar to other polyamine/flocculant treatment methods that were evaluated in preparation for the 2001 Color Removal Technology Assessment prepared by Jacobs Engineering Group, Inc., which was submitted to North Carolina DENR on February 27, 2001 in connection with the renewal of the Mill's NPDES permit. A copy of the SIMCO report dated October 30, 2000 is attached for your convenience. The SIMCO color removal process is called the Rapid Decolorization Process (RDP) and involves a dual stage process. The initial stage involves mixing the colored wastewater with SIMCOFLOC CAT-30 to form a Colorant/Cat complex. The second stage involves mixing the Colorant/Cat complex with SIMCO COUPLER ANP-30 to form an "insoluble precipitate." SIMCO reports the precipitate or flocculent is then removed from solution by conventional sludge techniques. While at the mill, SIMCO conducted bench scale trials on sewer 6A, the bleach plant acid sewer; sewer 3A, the bleach plant alkaline filtrates and the Pine Fiberline brownstock process wastewater; and the Primary Influent. The summary of the results and estimated product costs, on an actual and not a design basis, are shown below. Color(PPM) Stream Flow (MGD) Untreated Treated % Removal Ap27 Yearly Cost 6A 3.8 243 173 29 2.7 million' 3A 1.4 1454 683 53 3.0 million' Pri. Influent 24.0 180 Ill 38 5.8 million' I These are chemical costs only and do not include the capital or other operating costs of the RDP treatment and sludge dewatering system. 175 Main Street • P.O. Box 4000 Canton, North Carolina 28716 Phone: 828-646-6700 • Fax: 828.646-6892 Raising Your Expectations BLUE RIDGE PAPER PRODUCTS INC. f The color concentrations used in this analysis are based on the true color test method using a spectrophotometer at 465 nanometers using Platinum Cobalt color standards. The application rate and cost estimate was based on laboratory data generated at the Canton Mill and product costs from SIMCO. SIMCO also took composite samples from the following sources with them to their laboratory for further evaluation: Primary Influent, 6A sewer, CRP purge, Mixed Liquor from the aeration basin, and Secondary Effluent. The Mixed Liquor and Secondary Effluent samples were not evaluated due to "logistics," according to the SIMCO report. A summary of the results reported to the Canton Mill by SIMCO is shown below. Stream Use /1 * Cost per Million Gallons Cost per Year Primary Influent 0.04 $529.00 $4.83 Million 6A sewer** 0.12 $1,587.00 $2.31 Millions CRP Purge** 2.50 $33,072.00 $0.24 Millions *This use level is for the CAT-30 and the ANP separately. ** These appear to reduce the color level by 65% or more. [* and ** footnotes as they appear in original SIMCO communication] SIMCO's report stated that the CRP purge color appeared to be reduced by 65% or more. Blue Ridge does not know what method was used to determine this value, and we question whether the method used for color measurement can be directly compared to the approved method utilized at the mill. The SIMCO technology was not considered feasible for the following reasons. After evaluating the SIMCO report, Blue Ridge decided not to pursue the CAT-30/ANP technology. The Canton Mill approach to color reduction is and has been focused on pollution prevention and the implementation of technologies that do not generate additional solid waste (i.e., sludge). Blue Ridge has conducted extensive color reduction trials using other precipitation technologies, which we believe generate a sludge similar to that generated by the SIMCO process. Based upon our experience with those technologies, dewatering such sludge for disposal is difficult and capital intensive. In addition to the deterioration in sludge quality,we have found that the color"removed"by precipitation technologies in individual sewers dissociates in the main Mill sewer and returns to the wastewater; thus, the color is not actually removed from the wastewater. Our research indicates that if any color precipitation technology is feasible for the CRP, it will likely require a separate sludge dewatering system. In addition to major concerns regarding sludge quality and color dissociation, the potential color reduction from the CRP purge stream is not as large as appears from the SIMCO report. A purported 65% color reduction in the CRP purge does not translate into an equivalent color reduction in the Secondary Effluent,because the Wastewater 'Not including capital and non-chemical operating costs of RDP treatment and sludge dewatering. BLUE RIDGE PAPER PRODUCTS INC. Treatment Plant (WWTP)has been proven to preferentially remove brown color sources at a rate averaging 62 - 70% (duplicated by separate studies). Therefore, there would not be an incremental 65%reduction of CRP purge stream color as a result of the application of the SIMCO process, and any color reduction achieved would be at a potentially high capital and operating cost in addition to annual chemical costs of$240,000. The Canton Mill is actively working toward additional improvements in color performance, and, we are interested in all technically, operationally and economically feasible concepts. Currently, the Canton Mill is investigating several technologies for color removal in the CRP purge stream. In accordance with Section A.(8), paragraph 9 of the mill's 2001 NPDES Permit, a report will be submitted December 1, 2004 evaluating all technologies studied, including SIMCO's CAT-30/ANP products. Blue Ridge entered into an agreement with SIMCO in good faith to assess the effectiveness of its process to remove color from the Canton Mill's wastewater. It is Blue Ridge's opinion that the SIMCO process does not meet the feasibility criteria for application at the Canton Mill. In addition, we are concerned about the qualifications of SIMCO as a potential business partner for Blue Ridge. For all of the above reasons, we have determined that the SIMCO process is not appropriate for the Canton Mill. If you have further questions regarding this issue,please call me at(828) 646-2033. Sincerely, VBobWilli Director—Regulatory Affairs Blue Ridge Paper Products Inc. Attachment xc: Keith Haynes Mike Myers Forrest Westall r SIMCO PRODUCTS .INC., ' MANUFACTURING CHEMISTS Mr . Derric Brown 10/30/00 Blue _ Ridge Paper Products : Canton NC 28716 Re: Removal of contaminates in,pulp/paper waste water . WASTE WATER: Five samples of waste water were: provided for study using the RDP method to remove color -as well as other non colorant materials . Two of the samples Involved- waste streams-•that were' not 'considered for this study' due,: to logistics, one at t•he -aeration pond and the : other.";;af;: the <secondary clarifiers The waste streams cons idered ;w6re' the primary influent (P), the 6A influent (A);, the CRP: Purge 'inf:luent• -(CP) . FLOW: AND COLORANT VALUE: ? Stream P is a flow that: lag'approx.a 26, mll'lion gallons/day and •is a combinat•!on of all flows: to .ri'nclude :both A .and CP. Stream A is a flow that Is approx. -4: mi.11ion gallons/day'• and contributes about 26SK- ofaL"e:"color' =observed 'in flow P.: ' Stream CP is a flow that: is approx. : 20I000•. gal:lons/day and contributes about 6-8% of A he 'color• obser.ved : l* flow P. PURPOSE OF STUDY: The approach in this 'study.; is•'to remove-.color - and non colorant chemicals that. .are:.contained :,in'the :waste -water in a manner as to maximize thq,.eiiectiveiess while minimizing the cos't'. ' Th9 RDP method will: be-':used to. complex and encapsulate -colorant materials such as. ;li:glns- and non colorants -such as metals, cresols, etc. Our main focus Is' to re.duce , the color of the. waste water by 60% -pr"better' with• the ;-lydea:. that further * operations .will also reduce- A he color . PO Box 17903 Greenville,SC-29606 •. (864) 862-6705 Fax (864) 862-2472 e-mail: simcopro@beltsouth.net • webslte:www.simcoinc.com j SIMCO PRODUCTS INC. MANUFACTURING CHEMISTS 2 METHOD OF APPLICATION: A one liter sample of P and A and- a . 5• liter sample of hot CP were treated first with SIMCOFLOC CAT-30 stirred to mix then treated - with .SIMCO Coupler ANP and atirred again. They were then allowed' to sit to allow the floc to settle . Aliquots of P and A were removed and the color reduction compared to the untreated controls . The CP sample was diluted 30/1 then compared to a. 30/1 diluted control . RESULTS OF STUDY: Table I shows the usage level to remove approximately 50% of the color or better and the cost associated with that removal . Table I Waste 'Stream *Use Cost Cost g/l mil gal Year P . 04 $ 529. 00 $ '4. 83 million A ** .12 8 1587. 00 2. 31 million CP** 2 . 50 8 330.72. 00 0. 24 million * This use level is for the CAT-30 and• the ANP separately. ** These appear to reduce the,:color level by 65% or more. : . CONCLUSIONS: This study shows that 5'0% or. more color can be removed at `fairly low levels of usage. . 98%6 of the color can be removed but - at several times the cost.. The study, however, needs to Pe repeated at the Blue Ridge location to verify the findings and to. optimize the results . PO Box 17903 •' Greenville,SC 29606 (864) 862-6705 Fax (864) 862-2472 e-mail: simcopro@bellsouth.net • website:www.simcoinc.com 1 • tiMCO PRODUCTS iNC - MANUFACTURING CHEMISTS 3 Ii there are any other questions,' 'please do not hesitate to contact me at my direct number- : (864'. 862-7010) Beat Regards Dr . Joseph A. Pacifici .Technical Director . , cc: Dan Sims- • Robert - Wi111ams Melanie• Rageri✓ "Randy Medford John Pryately e PO Box 17903 Greenville, SC 29606• • (864) 862-6705 Fax (864) 862-2472 e-mail:simcopro@bellsouth.net •• website:www.simcoinc.com