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Full text: R&D-Project - Identification of organic compounds in the North and Baltic Seas

140 
Additionally, a Varian triple quadrupole mass spectrometer (Wallnut Creek, USA) was 
used. Gas chromatographic separations were carried out on a CP-3800 gas 
chromatograph (Varian, Wallnut Creek, USA) applying a capillary of 15 m length and 
0.25 mm ID coated with a film of 0.25 pm DB5-MS (5 % phenyl-methylpolysiloxane, 
J&W Scientific, Folsom, USA). An injector temperature of 275 °C and Helium as 
carrier gas (flow 2 ml/min) were used. The temperature programme was as follows: 100 
°C for 1 min, then with 50 °C/min to 300 °C, isothermal for 4 min. Splitless injections 
(splitless time 1.5 min) of 2.5 pi sample volume were carried with a Pal autosampler 
(CTC Analytics, Zwingen, Switzerland). 
The following EI-MS/MS conditions were applied: Electron energy 70 eV, filament 
current 300 pA, resolution of quadrupole 1 at 0.8 u and of quadrupole 3 at 1.2 u, Ar as 
collision gas at a pressure of 0.12-0.15 Pa (0.9-1.1 mTorr). The selected ions to be 
fragmented as well as further parameters are given in Table 44. The precursor ion m/z 
383 [M-C1] + and the product ion m/z 276 [M-4C1] + were selected for the internal 
standard 1 ’Cio-/ra/7.s'-chlordane (collision energy -21 V). 
Table 44: Selected precursor and product ions for the determination of the total PCA content by EI- 
MS/MS with an ion trap and triple quadrupole mass spectrometer. Important instrument parameters and 
the masses for the internal standard 13 Ci 0 -fran.s-chlordane are also given. 
Precursor ion 
(m/z) 
Product ion 
(m/z) 
Ion trap 
Triple quadrupole 
Excitation am 
plitude (V) 
Excitation “storage 
level” (m/z) 
Collision energy 
(V) 
91 [C 7 H V ] + 
53 [C 4 H 5 ] + 
2,0 
39,9 
-16,0 
102 [C 5 H 7 C1] + 
65 [C 5 H 5 ] + 
0,6 
44,7 
-10,0 
102 [C 5 H 7 C1] + 
67 [C 5 H 7 ] + 
* 
* 
-18,0 
383 [M-ClT 
276 [M-4C1] + 
0,85 
169,0 
-21,0 
*not detectable in the ion trap. 
5.6.9 Quantification of chlordanes by ECNI-LRMS 
Gas chromatographic separations were 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
	        
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