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

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STUDY 1: LANDFILLS AS SOURCES<br />

(Supelco, Munich, Germany; 30 m x 0.25 mm x 0.25 μm). Samples were also me<strong>as</strong>ured in<br />

NCI to confirm FASAs. Details on instrumental conditions were reported by Dreyer et al.<br />

(2008).<br />

PFC air samples from the particle ph<strong>as</strong>e were analysed using high performance liquid<br />

chromatography (HPLC, HP100, Agilent, Waldbronn, Germany) coupled to an triplequadrupole<br />

t<strong>and</strong>em m<strong>as</strong>s spectrometer (MS/MS, Applied Biosystems, MDS SCIEX,<br />

Darmstadt, Germany) using negative electrospray ionisation <strong>and</strong> the multiple reaction<br />

monitoring (MRM) mode. Separation w<strong>as</strong> done on a Phenomenex Synergi Hydro RP 80A<br />

column (Phenomenex, Aschaffenburg, Germany) with a length <strong>of</strong> 150 mm <strong>and</strong> a inner<br />

diameter <strong>of</strong> 2 mm connected to a guard column Phenomenex Synergi 2μ Hydro RO Mercury<br />

(200 mm lengths <strong>and</strong> 2 mm inner diameter). Detailed instrumental conditions can be found in<br />

Ahrens et al. (2007).<br />

Me<strong>as</strong>urement <strong>of</strong> PBDEs <strong>and</strong> musk fragrances from g<strong>as</strong>- <strong>and</strong> particle-ph<strong>as</strong>e samples w<strong>as</strong><br />

performed separately using GC-MS in the EI mode (musk fragrances) <strong>and</strong> NCI mode<br />

(PBDEs) using the previously optimized instrumental method described in chapter 3.<br />

4.2.7 Quantification<br />

Quantification w<strong>as</strong> b<strong>as</strong>ed on peak are<strong>as</strong>. Peak integration w<strong>as</strong> done using MSD Chemstation<br />

(Agilent Technologies, version D.02.00.275) for all samples me<strong>as</strong>ured by GC-MS. HPLC<br />

samples were integrated <strong>and</strong> quantitated with Analyst (Applied Biosystems, MSD SCIEX,<br />

version 1.4.1). M<strong>as</strong>s fragments <strong>of</strong> PBDEs <strong>and</strong> musk fragrances used for quantification are<br />

listed in section 3.3.1 (musk fragrances, PBDEs) <strong>and</strong> in the supporting information (PFCs).<br />

Analyte concentrations were calculated using the internal st<strong>and</strong>ard method <strong>and</strong> a seven point<br />

calibration. Target compounds were quantified with an S/N>10 <strong>and</strong> detected with S/N>3. The<br />

PFC method quantification limits (MQL) were

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