138
Gas chromatographic separations were carried out with an HP 5890II gas
chromatograph (Hewlett Packard, Palo Alto, USA) equipped with a split/splitless
injector and a capillary of 25 m length and 0.20 mm ID coated with a 0.33 pm film of
HP-1 (100 % dimethylpolysiloxane, Hewlett Packard, Palo Alto, USA). A sample
volume of 1 pi was injected in the splitless mode (splitless time 2 min). The injector
temperature was 260 °C. He (99,999 %) was used as carrier gas at an inlet pressure of
138 kPa. The temperature programme was as follows: 150 °C for 2 min, then with
7 °C/min to 260 °C, isothermal for 8 min and finally with 10 °C/min to 280 °C,
isothermal for 13 min.
A VG Autospec (Micromass, Manchester, UK) mass spectrometer was employed in the
ECNI-mode. Argon was applied as reagent gas at an ion source pressure of 2-10" 5 mbar.
The mass resolution was 12'000 at an acceleration voltage of 6 kV. The ion source
temperature was set to 170 °C, the filament current to 0.3-1 mA and the electron energy
to 25-40 eV. Perfluorokerosene was used for mass calibration. The most abundant
isotope signals of the [M-Cl]" ions were recorded in the selected ion mode for PC As,
and [M]" or [M-4C1-2H]" ions for 1 ’Cio-/ra/7.v-chlordanc. The dwell time per ion was
50 ms.
5.6.7 Group pattern determination of PCAs by CH4/CH2CI2-NICI
Gas chromatographic separations was carried out on an HP 5890II gas chromatograph
(Hewlett Packard, Palo Alto, USA), equipped with a Hewlett Packard 7673 auto
sampler. A fused silica capillary was employed of 15 m length and 0.25 mm ID coated
with a 0.25 pm film of DB5-MS (5%-phenyl-95%-methylsiloxane, J&W Scientific,
Folsom, USA). The injected volume was 1.5 pi in the splitless mode (2 min splitless
time). The injector temperature was 275 °C. He was used as carrier gas (99,999 %
purity, Carbagas, Switzerland) at a head pressure of 68,9 kPa (10 psi). The following
temperature programme was employed: 100 °C isothermal for 2 min, with 10 °C/min to
260 °C, isothermal for 10 min.