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

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METHOD OPTIMISATION 3.3 Results 3.3.1 Determination of mass-to-charge ratio of PBDEs and musk fragrances Table 10: Mass-to-charge-ratio (m/z) of PBDEs and musk fragrances determined with GC-MS in the EI and NCI mode, respectively. MW: molecular weight, TI: Target Ion, Q1: Qualifier 1, Q2: Qualifier 2. 32 EI mode NCI mode Analyte MW TI Q1 Q2 TI Q1 Q2 13 C HCB 291 290 255 - 290 256 - ADBI 244 229 244 173 - - - AHMI 244 229 244 187 - - - MX D15 294 294 248 - - - - HHCB 258 243 213 258 - - -- ATII 258 215 173 258 - - - AHTN D13 271 246 261 - - - - MX 297 282 297 - - - - AHTN 258 243 258 159 - - - MK 294 279 294 128 - - - Fluoranthene D10 212 212 106 - 212 211 - BDE28 407 248 408 139 327 328 326 MBDE28 419 260 418 150 339 337 338 MBDE47 498 338 498 228 417 419 415 BDE47 486 326 486 406 407 405 404 BDE100 565 404 564 484 405 403 484 MBDE99 577 416 576 496 417 415 496 BDE99 565 404 564 484 405 403 484 BDE154 644 484 644 404 564 562 563 MBDE153 656 496 656 416 496 494 498 BDE153 644 484 644 404 564 562 563 MBDE183 734 574 734 414 574 576 572 BDE183 722 562 724 484 564 562 484 MBDE 209 972 - - - 495 497 - BDE209 960 - - - 487 489 485 3.3.2 Optimisation of the GC oven program In order to asses the selectivity of the chromatographic process, separation factor � for each analyte was calculated using following equation: �= k2/k1, whereas k1 and k2 are the retention times of two peaks succeeding one another. For example, in the case where �=1, the two compounds are not separated, whereas �=1.10 means that compounds differ in 10 % of relative retention time and are well separated. Table 11 displays � values of each analyte at the tested parameters from section 3.2.3. It should be noted that mass-labelled PBDEs were observed at same retention times as their native substances and are therefore not discussed separately.
METHOD OPTIMISATION Table 11: Separation factors (�) of PBDEs and musk fragrances obtained by experiments A-E as well as direct comparison of � values of pairs of analytes that were problematic to separate (for details see 3.2.3). Separation factor � Analyte Experiment A Experiment B Experiment C Experiment D Experiment E 13 C HCB - - - - - ADBI 1.00 1.00 1.00 1.00 1.02 AHMI 1.04 1.04 1.03 1.03 1.08 MX D15 1.08 1.08 1.07 1.06 1.16 HHCB 1.00 1.00 1.00 1.00 1.00 ATII 1.00 1.00 1.00 1.00 1.00 AHTN D13 1.01 1.01 1.01 1.01 1.02 MX 1.00 1.00 1.00 1.00 1.00 AHTN 1.00 1.00 1.00 1.00 1.00 MK 1.11 1.09 1.08 1.07 1.16 Fluoranthene D10 1.06 1.05 1.05 1.05 1.07 BDE28 1.12 1.09 1.10 1.08 1.12 BDE47 1.14 1.09 1.11 1.10 1.09 BDE100 1.09 1.05 1.07 1.06 1.05 BDE99 1.02 1.01 1.02 1.02 1.01 BDE154 1.06 1.04 1.05 1.05 1.04 BDE153 1.03 1.02 1.03 1.03 1.02 BDE183 1.08 1.09 1.10 1.11 1.08 ADBI, AHMI 1.04 1.04 1.03 1.03 1.08 HHCB, AHTN 1.00 1.01 1.01 1.01 1.03 BDE100, BDE99 1.02 1.01 1.02 1.02 1.02 BDE154, BDE153 1.03 1.02 1.03 1.03 1.03 Separation factors of musk fragrances ranged from 1.00 to 1.16 in all experiments. However, low retention factors of most musk fragrances (ADBI, HHCB, ATII, AHTN D13, MX, and AHTN) were observed in experiments A-D. Experiment E revealed elevated retention factors for some musk fragrances, such as AHMI and MK. Retentions factors of musk fragrances with same m/z were slightly elevated in experiment E. For PBDEs significant differences in retentions factors could not be observed in one of the experiments. For musk fragrances and PBDEs peak abundances were elevated with increasing heating rates. Concurrently, decreasing peak widths were detected at higher heating rates. Fronting or tailing of musk fragrances during different oven parameters were not observed. However, a slight tailing was detected for low brominated congeners BDE28 and BDE47 in all experiments. 3.3.3 Optimisation of the GC inlet parameters Figure 1 displays peak abundances of native musk fragrances and PBDEs obtained by injections of standard solution at different oven and inlet temperature settings as described in table 8 (section 3.2.4). Settings at low oven temperatures (50 °C, 60 °C) resulted in low peak abundances. Maximum peak abundances were observed for the most volatile analytes (ADBI 33
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 46 and 47: METHOD OPTIMISATION used as carrier
Page 48 and 49: METHOD OPTIMISATION 3.3 Extraction
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
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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
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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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