Landfills and waste water treatment plants as sources of ... - GKSS

METHOD OPTIMISATION
3.3 Extraction experiments
3.2.5 Extraction method for PBDEs and musk fragrances of gas-phase samples
Prior to the extraction experiments, precleaned PUF/XAD-2/PUF cartridges (n=3) were
spiked with 50 μL of an internal standard solution containing mass-labelled MBDE27,
MBDE47, MBDE99, MBDE153, MBDE183 as well as both musk fragrances AHTN D3 and
MX D15 (c=200 pg μL -1 ). PUF/XAD-2/PUF cartridges were cold-column extracted in three
cycles (1 h, 1 h, 30 min) using hexane/acetone 1:1 (v:v). After each cycle, solvent was blown
out with nitrogen. The volume of the solvent (approximately 450 mL) was reduced using
Synchore polyvap (Büchi, Essen, Germany) at a temperature of 45 °C and 415-380 mbar.
Samples were further evaporated to 150 μL by a gentle stream of nitrogen. Finally, extracts
were transferred to GC vials. Prior to the measurements using GC-MS, 50 μL of an injection
standard solution ( 13 C HCB and Fluoranthene D10, c=400 pg μL -1 ) was added to the samples.
For quantification a seven point calibration was used (2, 4, 10, 20, 50, 80, 100, 200 pg μL -1 ).
Linearity of calibration was checked as described in DIN 32645 (1994). Peaks were
quantitated based on their peak areas and calculated using the internal standard method.
3.2.6 Extraction method for PBDEs and musk fragrances of particle-phase samples
Accelerated solvent extraction (ASE)
GFF (n=3) were folded and filled into extraction cells (stainless steel, volume= 22 mL) of an
accelerated solvent extractor (ASE, ASE 200, Dionex, Idstein, Germany). 50 μL of an internal
standard solution containing mass-labelled MBDE27, MBDE47, MBDE99, MBDE153,
MBDE183 as well as both musk fragrances AHTN D3 and MX D15 (c=200 pg μL -1 ) was
added. Remaining space in the cells was filled up with precleaned diatomite (Fluka,
Germany). Filters were extracted with hexane/acetone and pressurized to 140 bar at 100 °C.
Two static cycles (5 min, hold time 5 min) were performed. After the first extraction cycle
cell volume was rinsed and refilled with solvent. The purge time was set to 60 s. The volume
of the extract (about 35 mL) was reduced to 1 mL using Synchore polyvap. Extracts were
further concentrated to 150 μL under a gentle stream of nitrogen. Prior to the measurement
using GC-MS, 50 μL of an injection standard solution containing 13 C HCB and
Fluoranthene D10 (c=400 pg μL -1 ) was added to the samples. For quantification a seven point
calibration was used (2, 4, 10, 20, 50, 80, 100, 200 pg μL -1 ). Linearity of calibration was
checked as described in DIN 32645 (1994). Peaks were quantitated based on their peak areas
and calculated using the internal standard method.
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