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Appendix 1: Screening studies of POPs in bottom sediments from the P az watercourse Appendix 1 Methods for determination of POPs and selected trace elements in sediment and fish tissue samples from Pasvik area The following persistent pollutants have been determined in the bottom sediment and fish samples: - - chlorinated pestcides and industrial organochlorines: DDT-group (o,p'- and p ,p ’-DDE, o,p'- and p ,p ’-DDD, o,p - and p ,p ’-DDT), HCH (a-, P- and y- isomers of HCH), Hexachlorobenzene (HCB), chlordanes (Heptachlor, Heptachlor epoxide, Oxychlordane, trans - and cis -Nonachlors, , trans - and cis -Chlordanes), mirex, endrin and dieldrin; - ortho-substituted congeners of polychlorinated biphenyls; - planar and non-ortho-substituted congeners of PCBs (IUPAC): # 77, 81, 105, 114, 118, 123, 126, 156, 157, 167, 169, 189, as well as PCB congeners # 170 and 180; - toxaphene compounds Parlar-26, Parlar-50, Parlar-62; - brominated flame-retardants 2,4,4'-TrBDE (#28); 2,2',4,4'-TeBDE (#47); 2,2',4,4',5-PBDE (#99); 2,2',4,4',6-PBDE (#100); 2,2’,4,4’,5,5’- HeBDE (#153); 2,2’,4,4’,5,6-HeBDE (#154); 2,2’,3,4,4’,5,6-HpBDE (#183); - polychlorinated dibenzo- p -dioxines and dibenzofurans (PCDD/PCDF); - -40 individual polycyclic aromatic hydrocarbons (PAHs), included alkyl-homologues and 16 PAHs recommended by EPA Samples have been analyzed in the analytical batches, which included laboratory procedural blanks, spiked blank samples and samples o f standard reference material o f mussel tissue SRM 2977 o f NIST, US and dogfish muscle certified reference material for trace metals DORM-2, National Research Council Canada. To control recovery o f analytes surrogate isotope-labelled substances have been used, which were introduced into samples before extraction. Extracts have been analyzed using GC/MS. Sub-samples were analysed for quality control purpose at analytical laboratory o f University of Michigan (Environmental Health Sciences). Sample p rep a ra tio n fo r analysis of POPs Before analysis samples were refrozen and homogenized. The samples o f bottom sediments were dried. Extraction o f bottom sediments was carried out in Soxhlet apparatus using solvent mixture benzene-ethanol during 16 hours. Determinations o f PCBs, chlorinated pesticides and toxaphenes, PCDD/PCDFs, PBDEs and planar congeners o f PCBs were carried out from the same extract. Base digestion and ultrasonic extraction procedures were used to determine PAHs. Schemes o f clean-up for all types o f extracts are presented in Figures 1.1, 1.2, 1.3 and 1.4. E x trac tion of fish tissues samples Ex trac tion of PCBs, PBDEs, PCDD/Fs, OCPs and toxaphenes POPs from fish tissue samples were extracted by column extraction method. As extragent the mixture o f solvents - hexane : dichlormethane = 1:1 (v/v) was used. Lipid content was determined by gravimetric method from 10% o f extract volume. The 50 % o f extract volume was used for clean up for PCDD/Fs and PBDEs analysis. The 15 % o f extract volume was used for clean up for planar congeners o f PCB analysis. The 25 % o f extract volume was used for clean up for another POPs analysis. Ex trac tion of PAHExtraction o f PAH from the samples o f the tissues o f fish was carried out using base digestion with methanol and 50% KOH solution. The analytes from base solution were extracted with two portions o f hexane in separatory funnel. Rapport APN- 514.3665.01 31