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

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METHOD OPTIMISATION used as carrier gas at a constant flow of 1.3 mL min -1 . 2 μL of a standard solution (c=1 ng μL -1 ) of each target analyte was injected to the GC-MS using EI in the full scan mode. For PBDE m/z determination in the NCI mode (full scan) a 15 m HP-5 MS column with same diameter and film thickness as described above was also used. The following oven program was applied: initial temperature 40 °C, 30 °C min -1 to 130 °C; 2 °C min -1 to 240 °C; 30 °C min -1 to 300 °C, hold for 20 min). This assured the elution of all analytes in the chromatogram. The fragment occurring in highest abundance was depicted as target ion (TI). In addition to each TI, at least one qualifier ion (Q) was selected according to abundance and m/z difference to TI. 3.2.3 Optimisation of the oven program In order to achieve a sufficient chromatographic separation for all analytes, the oven temperature program was optimized. 2 μL of a standard solution containing all native and mass-labelled PBDEs and musk fragrances (c=800 pg μL -1 ) was injected to GC-MS (EI mode, full scan). Separation was conducted on a HP-5 MS capillary column (Agilent, 30 m x 0.25 mm x 0.25 μm). During optimisation, special attention was given to those substances that were detected with similar m/z. Particularly, these are musk fragrances (ADBI, AHMI m/z = 229 and HHCB, AHTN m/z = 243) as well as PBDE congeners (BDE99, BDE100 m/z = 404 and BDE154, BDE153 m/z = 484). Furthermore, attention was given to fronting and tailing of peaks. Initial oven temperature (60 °C, hold for 2 min) and (30 °C min -1 to 130 °C) were fixed parameters and not changed during the experiments. Temperature program for musk fragrances (ramp ��) and PBDEs (ramp ��) were evaluated stepwise. An overview about oven temperature programs tested in this study is presented in table 8. 28
METHOD OPTIMISATION Table 8: Overview about oven temperature programs. Parameters printed in bold were changed during experiments. Exp. Ramp I Ramp II Ramp III A 30 °C min -1 to 130 °C, hold 2 min 5 °C min -1 to 200 °C 10 °C min -1 to 300 °C, hold 20 min B 30 °C min -1 to 130 °C, hold 2 min 10 °C min -1 to 200 °C 10 °C min -1 to 300 °C, hold 20 min C 30 °C min -1 to 130 °C, hold 2 min 15 °C min -1 to 200 °C 15 °C min -1 to 300 °C, hold 20 min D 30 °C min -1 to 130 °C, hold 2 min 20 °C min -1 to 200 °C 20 °C min -1 to 300 °C, hold 20 min E 30 °C min -1 to 130 °C, hold 2 min 5 °C min -1 to 170 °C, hold 3 min 5 °C min -1 to 200 °C 15 °C min -1 to 300 °C, hold 20 min 3.2.4 Optimisation of the inlet program Inlet temperature was optimized in three steps as suggested by Godula et al. (2001). For three steps 2 μL of a standard solution containing all native and mass-labelled PBDEs and musk fragrances (c=800 pg μL -1 ) were injected. GC-MS was operated in the EI mode using the selected ion monitoring mode (SIM). Inlet parameters were adjusted according to table 9. Table 9: Overview about the inlet temperature programs. Parameters printed in bold were adjusted during the three steps. Step A B C Initial inlet temperature (°C) Inlet heating rate (°C min -1 ) Final inlet temperature (°C) Pulse pressure (psi) Pulse time (min) Initial oven temperature (°C) 50 300 300 40 2 40 60 300 300 40 2 40, 50 70 300 300 40 2 40, 50, 60 60 300 200 40 2 50 60 300 250 40 2 50 60 300 300 40 2 50 60 100 300 40 2 50 60 200 300 40 2 50 60 300 300 40 2 50 60 400 300 40 2 50 60 500 300 40 2 50 3.2.5 Determination of the instrumental detection and quantification limits For determination of the instrumental limits of detection (LOD) and limits of quantification (LOQ) of PBDEs and musk fragrances 2 μL of a standard solution containing native and mass-labelled analytes were spiked to the GC system. Ionisation modes were EI and NCI. In order to include thermo-labile BDE209 in the analysis, a 15 m HP-5 MS capillary column was used in the NCI mode. PBDEs and musk fragrances in the EI mode were separated on a 30 m HP-5 MS capillary column. LOD and LOQ were determined using optimized oven and inlet settings from section 3.4. The LOD was set to signal-to-noise ratio (S/N) of 3, the LOQ was set to S/N=10. 29
Page 1: ISSN 0344-9629 Landfills and waste
Page 4 and 5: Die Berichte der GKSS werden kosten
Page 6 and 7: Deponien und Kläranlagen als Quell
Page 8 and 9: TABLE OF CONTENTS VI 4.2.5 Extracti
Page 10 and 11: LIST OF FIGURES Figure 20: Proporti
Page 12 and 13: LIST OF TABLES Table S6: Table of r
Page 14 and 15: ABBREVIATIONS BDE47 2,2',4,4'-Tetra
Page 16 and 17: ABBREVIATIONS MW molecular weight M
Page 18 and 19: 2 INTRODUCTION
Page 20 and 21: INTRODUCTION 175 chemicals classifi
Page 22 and 23: INTRODUCTION Table 1 cont. Analytes
Page 24 and 25: INTRODUCTION Table 3: Polycyclic mu
Page 26 and 27: INTRODUCTION Mabury 2006). This inc
Page 28 and 29: INTRODUCTION 1.3 Physico-chemical p
Page 30 and 31: INTRODUCTION 1.4 Environmental conc
Page 32 and 33: INTRODUCTION Chen et al. 2007a; Har
Page 34 and 35: 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 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
Page 80 and 81: STUDY 1: LANDFILLS AS SOURCES conce
Page 82 and 83: STUDY 1: LANDFILLS AS SOURCES influ
Page 84 and 85: STUDY 2: WASTE WATER TREATMENT PLAN
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STUDY 2: WASTE WATER TREATMENT PLAN
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CONCLUSIONS AND OUTLOOK BDE183 were
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REFERENCES wastewater treatment/pol
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REFERENCES Capuano, F. Cavalchi, B.
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REFERENCES Dreyer, A. Temme, C. Stu
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REFERENCES Harada, K. Nakanishi, S.
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REFERENCES Kallenborn, R. Gatermann
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REFERENCES sexual development, and
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REFERENCES Oros, D. R. Hoover, D. R
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REFERENCES Rimkus, G. (1995): Nitro
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REFERENCES Smithwick, M. Mabury, S.
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REFERENCES USEPA (2006): 2010/2015
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REFERENCES Zhao, Y.-X. Qin, X.-F. L
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SUPPORTING INFORMATION Figure S3: H
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SUPPORTING INFORMATION Table S1: Ta
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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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