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

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STUDY 2: WASTE WATER TREATMENT PLANTS AS SOURCES Figure 18: Sampling locations of two WWTPs: WA and WB and the corresponding RFs (RA, RB). 5.2.2 Chemicals Except for HHCB (51 % purity), all solvents, native and mass-labelled analytical standards and gases were of highest purity. A detailed table of all compounds, suppliers and qualities is listed in supporting information. 5.2.3 Extraction of semi-volatile PFCs, PBDEs and musk fragrances in gas-phase samples PFCs in gas-phase samples were extracted according to the method of Dreyer et al. (2008). Details on sample preparation can be found in section 4.2.3. Gaseous PBDEs and musk fragrances extraction procedures are described in section 3. Briefly, PUF/XAD-2/PUF cartridges were cold extracted three times (1 h, 1 h, 30 min) using MTBE/acetone 1:1 (v:v) for PFCs and hexane/acetone 1:1 (v:v) for PBDEs and musk fragrances. The volume of the extracts was reduced to 150 μL and extracts were transferred to measurement vials. Prior to the measurement, 50 μL of an injection standard solution containing 13 C HCB and TCB D3 (c=400 pg μL -1 ; PFC analysis) or 13 C HCB and Fluoranthene D15 (c=400 pg μL -1 , PBDEs and musk fragrance analysis) was added. 68
STUDY 2: WASTE WATER TREATMENT PLANTS AS SOURCES 13 13 -1 C PFUnDA and C PFDoDA (c=200 pg μL ; PFCs) or MBDE27, MBDE47, MBDE99, MBDE153, MBDE183, AHTN D3 and MX D15 (c=200 pg μL -1 ; PBDEs and musk fragrances) was added to correct for analyte losses during sample handling and extraction. The volume of the extracts was reduced to about 1 mL. PBDE and musk fragrance extracts were purified by silica gel and alumina oxide. Samples were eluted with hexane and hexane/DCM. The eluates were evaporated and transferred to measurement vials. Prior to the GC-MS measurements, 50 μL of an injection standard solution containing Fluoranthene D15 and 13 C HCB (c=400 pg μL -1 ) was added. PFC samples were spiked with 50 μL of an injection standard solution containing EtFOSAA D5 (400 pg μL -1 ). After spiking PFC extracts with the injection standard, white solids was formed. Therefore, sample vials were centrifuged at 5000 rpm for 15 min (Hettich, Universal 320, Tuttlingen, Germany). The remaining liquid fraction was measured. 5.2.5 Instrumental analysis Semi-volatile and volatile PFCs were measured by GC-MS using the PCI and SIM mode. Samples were also measured in NCI to confirm FASAs. Chromatographic separation was performed on a Supelco Wax column (30 m x 0.25 mm x 0.25 μm). Ionic PFCs were analysed by HPLC-MS/MS using an ESI source (MRM mode). Separation was performed by a Phenomenex Synergi Hydro RP 80A column connected to a guard column. Measurement of PBDEs was performed by GC-MS. MS was run in the NCI using SIM mode. Separation was conducted using a HP5-MS column (15 m x 0.25 mm x 0.25 μm). For determination of musk fragrances GC-MS was operated in the EI mode (SIM). Analytes were separated by HP-5 MS column (30 m x 0.25 mm x 0.25 μm). Detailed instrumental conditions of GC-MS and HPLC MS/MS can be obtained from Dreyer et al. (2008) and Ahrens et al. (2007) for PFCs and section 3 for PBDEs and musk fragrances. 5.2.6 Quantification Peak integration was performed using MSD Chemstation (version D.02.00.275) for all samples analysed by GC-MS. HPLC-MS/MS peaks were integrated with Analyst software (version 1.4.1). Mass fragments that were used for determination and quantification are presented in section 3.3.1 (PBDEs and musk fragrances) and in the supporting information (PFCs). The internal standard method was used for the calculation of analytes. Target compounds were quantified with an S/N>10 and detected with S/N>3. The PFC method quantification limits (MQL) were
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ISSN 0344-9629 Landfills and waste
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Die Berichte der GKSS werden kosten
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Deponien und Kläranlagen als Quell
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TABLE OF CONTENTS VI 4.2.5 Extracti
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LIST OF FIGURES Figure 20: Proporti
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LIST OF TABLES Table S6: Table of r
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ABBREVIATIONS BDE47 2,2',4,4'-Tetra
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ABBREVIATIONS MW molecular weight M
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2 INTRODUCTION
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INTRODUCTION 175 chemicals classifi
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INTRODUCTION Table 1 cont. Analytes
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INTRODUCTION Table 3: Polycyclic mu
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INTRODUCTION Mabury 2006). This inc
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INTRODUCTION 1.3 Physico-chemical p
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INTRODUCTION 1.4 Environmental conc
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INTRODUCTION Chen et al. 2007a; Har
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INTRODUCTION prevent xenobiotica fr
Page 36 and 37: INTRODUCTION al. 2009c) and being d
Page 38 and 39: INTRODUCTION Table 6: Selection of
Page 40 and 41: INTRODUCTION 1.5 Sources Sources of
Page 42 and 43: OBJECTIVES 2. Objectives In recent
Page 44 and 45: METHOD OPTIMISATION Simonich et al.
Page 46 and 47: METHOD OPTIMISATION used as carrier
Page 48 and 49: METHOD OPTIMISATION 3.3 Extraction
Page 50 and 51: METHOD OPTIMISATION 3.3 Results 3.3
Page 52 and 53: METHOD OPTIMISATION AHMI). For less
Page 54 and 55: METHOD OPTIMISATION 3.3.5 Extractio
Page 56 and 57: METHOD OPTIMISATION 3.4 Discussion
Page 58 and 59: METHOD OPTIMISATION partly due to h
Page 60 and 61: METHOD OPTIMISATION Figure 7: Final
Page 62 and 63: STUDY 1: LANDFILLS AS SOURCES volat
Page 64 and 65: STUDY 1: LANDFILLS AS SOURCES On ea
Page 66 and 67: STUDY 1: LANDFILLS AS SOURCES (Supe
Page 68 and 69: STUDY 1: LANDFILLS AS SOURCES Table
Page 70 and 71: STUDY 1: LANDFILLS AS SOURCES 52 c
Page 74 and 75: STUDY 1: LANDFILLS AS SOURCES 4.3.2
Page 78 and 79: STUDY 1: LANDFILLS AS SOURCES 4.5 D
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Page 82 and 83: STUDY 1: LANDFILLS AS SOURCES influ
Page 84 and 85: STUDY 2: WASTE WATER TREATMENT PLAN
Page 106 and 107: CONCLUSIONS AND OUTLOOK BDE183 were
Page 108 and 109: REFERENCES wastewater treatment/pol
Page 110 and 111: REFERENCES Capuano, F. Cavalchi, B.
Page 112 and 113: REFERENCES Dreyer, A. Temme, C. Stu
Page 114 and 115: REFERENCES Harada, K. Nakanishi, S.
Page 116 and 117: REFERENCES Kallenborn, R. Gatermann
Page 118 and 119: REFERENCES sexual development, and
Page 120 and 121: REFERENCES Oros, D. R. Hoover, D. R
Page 122 and 123: REFERENCES Rimkus, G. (1995): Nitro
Page 124 and 125: REFERENCES Smithwick, M. Mabury, S.
Page 126 and 127: REFERENCES USEPA (2006): 2010/2015
Page 128 and 129: REFERENCES Zhao, Y.-X. Qin, X.-F. L
Page 130 and 131: SUPPORTING INFORMATION Figure S3: H
Page 132 and 133: SUPPORTING INFORMATION Table S1: Ta
Page 134 and 135: SUPPORTING INFORMATION Table S2: Ma
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SUPPORTING INFORMATION Table S5: Ta
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SUPPORTING INFORMATION Table S7: Bl
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SUPPORTING INFORMATION Table S11: P
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SUPPORTING INFORMATION Figure S7: S
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SUPPORTING INFORMATION Figure S7 co
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SUPPORTING INFORMATION Table S16: T
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SUPPORTING INFORMATION Table S19: M
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ERKLÄRUNG DER SELBSTSTÄNDIGEN VER
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