Landfills and waste water treatment plants as sources of ... - GKSS
Landfills and waste water treatment plants as sources of ... - GKSS
Landfills and waste water treatment plants as sources of ... - GKSS
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METHOD OPTIMISATION<br />
Figure 6: Improvements <strong>of</strong> sensitivity (%) <strong>of</strong> PBDEs <strong>and</strong> musk fragrances after optimisation <strong>of</strong><br />
PTV inlet on the b<strong>as</strong>is <strong>of</strong> previous PTV inlet settings in section 3.2.2<br />
Further objective w<strong>as</strong> the optimisation <strong>of</strong> an instrumental method that is sensitive for PBDEs<br />
<strong>and</strong> musk fragrances. Due to the high LOD <strong>and</strong> LOQ in the EI mode for higher brominated<br />
PBDE congeners it w<strong>as</strong> not possible to determine these compounds at low concentration<br />
levels. Thus the objective to develop a simultaneous detection method w<strong>as</strong> not achieved <strong>and</strong><br />
NCI mode w<strong>as</strong> selected <strong>as</strong> the adequate ionisation mode for PBDEs. For further analysis,<br />
PBDEs had to be separately determined in the NCI mode <strong>and</strong> musk fragrances in the EI<br />
mode. Finally, following optimized inlet parameter were used: Initial inlet temperature 70 °C,<br />
initial oven temperature 60 °C, final inlet temperature 300 °C, inlet heating rate 400 °C, initial<br />
oven temperature: 60 °C. Final optimized oven temperature programs <strong>and</strong> final<br />
chromatograms are displayed in table 15 <strong>and</strong> figure 7, respectively.<br />
Table 15: Final oven temperature programs for the determination <strong>of</strong> PBDEs <strong>and</strong> musk<br />
fragrances using GC-MS<br />
NCI (PBDEs)<br />
EI (Musk fragrances)<br />
heating rate final temperature hold time heating rate final temperature hold time<br />
°C min -1 °C min °C min -1 °C min<br />
30 130 0 30 130 0<br />
5 170 3 5 170 3<br />
5 200 0 5 200 0<br />
15 300 20 15 300 5<br />
41