137
A triple quadrupole mass spectrometer was applied in the ECNI mode (1200L, Varian,
Walnut Creek, USA). Regular performance optimisation of both quadrupoles was
carried out. The temperature of the transfer line was 280 °C, of the ion source 200 °C
and of the manifold 40 °C. Methane was used as reagent gas (99,995 %, Carbagas,
Switzerland) at a pressure of 7.3 mbar (5.5 Torr). The dwell time was 0.25 ms per ion
group. Table 42 and Table 43 summarised the selected masses in the selected ion
monitoring mode.
Table 43: Mass-to-charge ratios of ion selected for the internal standards e-HCH and n C w -trans-
chlordane as well as for other polychlorinated compounds included during method development. The
ECNI-MS mode was applied.
Compound
Ion
m/z
m/z most abundant
isotope
a-HCH
[M-Clf
253
255
e-HCH
[M-Clf
253
255
’ C i o -'' ' v -C h 1 o rd a n e
[MP
416
420
r/.v-Chlordane
[M]-
406
410
rz.v-Xonachlor
[M]-
440
444
Heptachlor
[M-2C1]"
299
302
Octachloronaphthalene
[M-2C1]"
332
334
p,p’-DDT
[M+H-3C1] -
248
248
PCB 153
[M]-
358
360
Toxaphene #44
[M-Clf
373
377
Toxaphene #62
[M-Clf
373
377
rra/z.v-Chlordane
[Mf
406
410
rra/z.v-\o nach lor
[Mf
440
444
5.6.6 Quantification of PCAs by ECNI-HRMS
A comparison between ECNI-HRMS and ECNI-LRMS combined with the newly
developed clean-up was carried out to ensure, that the latter has the necessary selectivity
for PCA. The ECNI-HRMS measurements were carried out at the Norwegian Institute
for Air Research (Kjeller, Norway). Results obtained by LRMS and HRMS were well
comparable (see chapter 5.3.3.3).