239
7 List of Tables and Figures
Table 1 : Salinity of sea water samples [practical salinity unit] in the North Sea 43
Table 2: TOC in sediments [mg/g] 44
Table 3: Sampling sites of the monitoring campaign WH242 in August/September 2002 48
Table 4: Sampling sites of the monitoring campaign WH255 in August/September 2003 49
Table 5: Sampling sites of the monitoring campaign WH267 in August/September 2004 49
Table 6: International Rubin code of fish species abbreviations 50
Table 7: Detailed logging data of the catches 50
Table 8: Physical-chemical properties of selected PCAs 54
Table 9: Aquatic toxic properties of sPCAs and mPCAs 55
Table 10: Overview of sPCA levels in selected environmental matrices at the start of this project 56
Table 11: log K 0 w values of main chlordane compounds (Simpson et ai, 1995) 57
Table 12: Comparison of quantification of s- and mPCAs in spiked fish (mackerel) and naturally exposed
fish livers using four different mass spectrometric methods (single measurements). Spikes 1 and
2 contained 1500 ng in total (150 ng/g assuming a sample weight of 10 g) of sPCA with 55.5 %
Cl content and spike 3 contained 1500 ng each of sPCAs and mPCAs with Cl contents of
55.5 % and 52 %, respectively. The relative deviations from the spiked amount are given in
parenthesis 65
Table 13: Quantification of three sPCA solutions (overall amount 1500 ng) with variable chlorine content
with a sPCAs reference standard of 55 % Cl and 63 % Cl content using ECNI, CH4/CH2C12-
NICI-LRMS and EI-MS/MS. Relative deviations are given in parenthesis 66
Table 14: PCA quantification of different sPCA mixtures (51-69 % Cl) by ECNI with total response
factors corrected for the chlorine content. The chlorine contents calculated from ECNI-LRMS
measurements are indicated in brackets. The expected amount, the measured amount and the
relative error are given. Deviations between expected and found chlorine content are caused by
the presence of additives which are not detectable by ECNI 69
Table 15: Comparison of sPCA determination in fish liver by ECNI according to Tomy et al. (1997)
using three commercial references of different chlorine content (51 %, 55 % and 63 %) and via
the total response factor approach. Calculated chlorine contents are given in brackets 69
Table 16: Comparison of quantification of chlordanes [ng/g dw] in sediments by ECNI (two instruments)
and EI-MS/MS. The fraction of the Florisil clean-up is assigned, where the compound is
present 72
Table 17: Instrumental (mass spectrometric) limits of detection (LOD) at a signal-to-noise ratio (S/N) of
3:1 and limits of quantification (LOQ, S/N 10:1) for total sPCA, single sPCA groups, total
mPCA and single mPCA groups. Injection volumes were 1-1.5 pi 73
Table 18: Instrumental (mass spectrometric) limits of detection at a signal-to-noise ratio (S/N) of 3:1 and
limits of quantification (S/N 10:1) for single chlordane compounds in pg/pl. Compared are two
measuring techniques (ECNI, EI-MS/MS) as well as two mass spectrometers (HP 5989B and
Varian 1200 L). Injection volumes were 1-1.5 pi 73
Table 19: Fractionation of the single PCA congeners CioHi 6 Cl6 and Q3H20CI8 from PCB 153,
toxaphene #62 and frans-chlordane by Florisil column clean-up. Relative distributions are given
(prefraction: 60 ml of n-hexane followed by 5 ml of dichloromethane, PCA-fraction: 60 ml of
dichloromethane) 75
Table 20: Fractionation behaviour of the Florisil® clean-up for chlordane compounds carried out on two
different batches. Relative recoveries [%] of the total amounts are given. Tetrachloro- (TCN),
octachloronaphthalene (OCN), the chlordane compound MC8 and 4,5-dichlorochlordene were
evaluated as internal standards (ISTD) 76
Table 21: Relative recoveries [%] of selected sPCA/mPCA compounds and the internal standard 13 Ci 0 -
trans-chlordane after stepwise and complete clean-up of spiked sun flower oil or mackerel
muscle tissue (spiked amount: 1.5-25 pg of sPCA or 1.5-20 pg of mPCA mixture) 77
Table 22: Relative recoveries [%] of selected sPCA/mPCA compounds and the internal standards 13 Cio-
frans-chlordane, octachloronaphthalene (OCN) and MC8 (a chlordane congener). Extraction as
well as a stepwise and complete clean-up of spiked sea sand and sediments were tested (spiked