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6.6 Appendix
6.6.1 Reagents and solvents
The reagents and solvents were of the highest purity available. The following solvents
were used: acetone (Merck, SupraSolv®), dichloromethane, /7-hexane (Baker, Ultra resi-
analyzed) methanol (Baker, Hplc-analyzed). Deionized water was obtained from an
ultra-filtration system (Millipore milli-Q academic A10, 18.2 Milcm).
All glassware was washed twice with acetone, dried, and then washed twice with n-
hexane. After that the glassware was heated at 180°C for 5 h.
6.6.2 GC-MS method for the determination of Chlorpyrifos, Endosulfan
and Trifluralin
All analyses were carried out with a Trace GC capillary gas chromatograph coupled to
a Trace MS mass spectrometer (both Thermo Finnigan). Analyses were conducted with
the following parameters:
Column:
Carrier gas:
Oven temperature:
Injector:
Interface temperature:
Detection mode:
ZB-5 from Phenomenex (5 % Phenyl-, 95 %
dimethylpolysiloxan) 30 m x 0.25 i. d. x 0.25 pm; 1 m
precolumn ZB-5
Helium 1.5 mL/min
40 °C, 1 min isotherm; linear temperature gradient
(5.5 °C/min to 320 °C; then 10 min isotherm)
PTV splitless (Inlet temperature: 50 °C; split flow:
30 ml/Min; splitless time: 1 Min; injection phases:
injection: 40 kPa, 50 °C, 50 mL/Min , 0.01 Min;
evaporation: 140 kPa, 14.5 °C/s, 60 °C, 0.5 Min; transfer:
210 kPa, 14.5 °C/Min, 280 °C, 10 Min)
280 °C
NCI
Reagent gas:
Source temperature:
Emission current:
Dwell time per mass:
Methane
130 °C (NCI)
150 pA
50 ms