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METHOD OPTIMISATION
3. Method optimisation for the determination of PBDEs and musk
fragrances
METHOD OPTIMISATION
3.1 Introduction
For the sampling of PBDEs and musk fragrances in ambient air, high volume samplers are the
most commonly applied sampling techniques (Lee et al. 2004; Peck and Hornbuckle 2004; Su
et al. 2007; Xie et al. 2007). However, for PBDEs and PFCs passive sampling devices were
also used (Jaward et al. 2004a; Gouin et al. 2005; Shoeib et al. 2005). PUF and XAD-2 resin
are the sorbents most typically applied to accumulate airborne PFCs, PBDEs and musk
fragrances (Agrell et al. 2004; Fromme et al. 2004; Peck and Hornbuckle 2004; Hoh and
Hites 2005; St-Amand et al. 2008; Regueiro et al. 2009). Usually, a glass fibre filter (GFF) is
additionally used to collect airborne particles.
Solvents for extraction of PUF/XAD-2/PUF and GFF include mixtures of hexane, diethyl
ether, dichloromethane and acetone (Covaci et al. 2007; Bester 2009). Soxhlet extraction is
widely used as a robust and effective extraction technique for PBDEs and musk fragrances. In
recent studies, the long extractions times and large solvent volumes were partially avoided by
the use of alternative extraction techniques, such as pressurized liquid extraction (PLE) (Wise
et al. 2005).
Synthetic musk fragrances have a sufficient vapour pressure, temperature stability and
lipophilicy and can therefore be separated by gas chromatography (GC) (Tas et al. 1997). The
numbers of analytical methods for the determination of PBDEs increased over past years and
were in most cases established on the basis of methods for chlorinated organic pollutants,
such as polychlorinated biphenyls (Covaci et al. 2003). The most applied instrumental method
is GC.
Separation of musk fragrances and PBDEs can be performed using non-polar or semi-polar
capillary columns with films containing 5 % phenyl-dimethylpolysiloxane (DB-5 MS, HP-5
MS) and 100 % methyl-polysiloxane (DB-1 MS) (Strandberg et al. 2001; Stevens et al. 2003;
Bester 2004; Covaci et al. 2005; Gouin et al.2005). Frequently, a length of 30 m and inner
diameters of 0.25 mm with film thickness 0.25 μm is used. However, for determination of
thermo-labile BDE209 it is suggested to apply columns with a lengths of 15 m or even shorter
(Bjorklund et al. 2004; Kierkegaard et al. 2009).
Except for on-column inlets, all currently available inlets have been successfully applied in
the analysis of musk fragrances since these substances are not thermo-labile (Rimkus 1999;
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