79
As can be seen from Table 22, octachloronaphthalene (OCN) has a yield, which
sometimes is more similar to the PC A compounds. Therefore, OCN was used as
additional and alternative internal standard in case of a low recovery of 13 Cio-trans-
chlordane.
Chlordanes
As already discussed before, frans-nonachlor cannot be collected completely in the PCA
fraction. Tests of the two clean-up steps for biota gave good recoveries of 77-90 % (see
Table 23). /ran.s-Nonachlor could be recovered to 75 % in the pre- and PCA-fraction.
Therefore, both were quantified.
However, cis- heptachlorepoxide was non-detectable, and the yield for trans-hepta-
chlorepoxide was poor. The reason is degradation by the silica gel coated with sulphuric
acid. Since this step is essential for a clean extract, these compounds could not be
determined.
Overall chlordane recoveries of the complete extraction and clean-up method were also
tested with both sea-sand and air-dried sediment from the site UE 67 (Gauss 332, TOC
0.12 %). Here, clean-up by silica gel coated with sulphuric acid could be omitted for
chlordane analysis. Recoveries of the internal standards and the analytes were compa
rable and in average >10%.
Table 23: Relative recoveries [%] of selected chlordane compounds in biota after the two clean-up steps
(column chromatography with silica gel/sulphuric acid and adsorption chromatography with Florisil ®).
Samples of 10 g were spiked with 10 ng of each compound in 10 jal of cyclohexane.
Compound
Pre-fraction
PCA-fraction
ISTD
13 Ci 0 -frani-chlordane
4
80
e-hexachlorocyclohexane
Chlordanes
79
<1
frans-chlordane
2
77
r/.v-chlordane
2
77
r/.v-nonachlor
1
90
frans-nonachlor
29
46
Oxychlordane
<1
85
rz.v-heptachlorepoxide
<1
24
frans-heptachlorepoxide
<1
<1