Development of a Novel Mass Spectrometric ... - Jacobs University

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Introduction uV (x100,000) Chromatogram 1.75 1.50 1.25 1.00 0.75 0.50 0.25 0.00 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0 32.5 35.0 37.5 min Figure 1-9 UCM feature of hydrocarbon content of light shredder waste in GC The scientific question that needs to address urgently is about the composition of the hump. Whether the hump contains only hydrocarbons has remained a matter of speculation rather than experimental proof and no detailed information exists on the actual composition, presumably varying dramatically between samples. If other non HC components are present the KW 4 does not then determine HCs and should not be used as legally binding procedure for measuring HC contamination. The resulting challenge is to develop an alternative method to reliably measure HCs in shredder waste or any other source of heavy long chain HCs. Resulting from this problem the specific aim of the project is to establish the chemical content of the UCM in light shredder waste and once adequately characterized develop a reliable method for the determination and quantification of HCs alternative to KW 4.As well the study aims at evaluating the extent of UCM weathering or biodegradation of the waste. The project however seeks to devise and develop an MS-based methodology capable of analysing and characterizing a complex mixture of hydrocarbons within the light shredder waste. 29
Introduction 1.5 Scope and Significance of this Work The aim of this work is to develop, adapt and evaluate a new MS-based methodology for the analysis of hydrocarbons. Besides general method development and validation, the following problems and applications should be addressed At first task it should be investigated if model hydrocarbons compounds can be analysed using mass spectrometry. The following step will involve applying the developed method for the analysis of light shredder waste sample. The major goal is to explore the chemical composition of shredder waste. The ability to provide a quantitative figure about selected hydrocarbons needs to be devised. Validation of the method requires testing similar complex hydrocarbon mixtures. The possibilities to differentiate complex data from each other by using tools available in literature need to be established. Finally the comparability of results obtained by different spectrometries should be investigated as by their advantages and limitations. After this promising scope of this study, a general synopsis of the study significance is illustrated in the following description. This thesis describes investigations undertaken into the nature of the UCM of light shredder waste. The results and discussion section comprises six parts. The first two parts involves the ionisation of n-alkanes and other various branched and cyclic hydrocarbons by a newly developed mass spectrometry method. In the third part the mechanism of the ionisation was discussed. The fourth part comprises the analysis of the chemical content of the light shredder waste. This included exploring the molecular level details of the complex mixture. The fifth part investigates the application of the developed methodology into other different complex mixture comprising similar types of hydrocarbons. The final part explains the management of the complex data. The utility of graphical tool to help simplify the spectral data was demonstrated. 30
Page 1 and 2: Development of a Novel Mass Spectro
Page 3 and 4: Declaration of Authorship I ,Nadim
Page 5 and 6: This work has been carried out unde
Page 7 and 8: Contents Contents Declaration of Au
Page 9 and 10: List of Figures List of Figures Fig
Page 11 and 12: List of Figures Figure 3-39 MS 2 fr
Page 13 and 14: List of Tables List of Tables Table
Page 15 and 16: Abbreviations Abbreviations APCI AP
Page 17 and 18: Abbreviations UV VGOs VOCs VRs ultr
Page 19 and 20: Introduction Analytical chemistry h
Page 21 and 22: Introduction 1.2 Presence and Fate
Page 23 and 24: Introduction aliphatic hydrocarbons
Page 25 and 26: Introduction Figure 1-1 Examples of
Page 27 and 28: Introduction Figure 1-2 Range of io
Page 29 and 30: Introduction fractions. 42 Another
Page 31 and 32: Introduction 1.3.5 APLI Other crude
Page 33 and 34: Introduction products). Other molec
Page 35 and 36: Introduction Other studies performe
Page 37 and 38: Introduction APLI-FT ICR-MS Crude o
Page 39 and 40: Introduction spectrometry in as muc
Page 41 and 42: Introduction catalytic processing t
Page 43 and 44: Introduction Figure 1-6 Kendrick ma
Page 45: Introduction including determinatio
Page 49 and 50: Experimental e) Other model mixture
Page 51 and 52: Experimental 2.2.2 Preparation of O
Page 53 and 54: Experimental 2.4 Graphical Presenta
Page 55 and 56: Results and Discussion experiment.
Page 57 and 58: Results and Discussion Intens. [%]
Page 59 and 60: Results and Discussion common featu
Page 61 and 62: Results and Discussion 3.2 APCI-TOF
Page 63 and 64: Results and Discussion These compou
Page 67 and 68: Results and Discussion Ions were pr
Page 71 and 72: Results and Discussion procedure ba
Page 75 and 76: Results and Discussion to produce m
Page 77 and 78: Results and Discussion 519.5863 519
Page 79 and 80: Results and Discussion Higher mass
Page 87 and 88: Results and Discussion isolated fro
Page 93 and 94: Results and Discussion 3.4.5 Tandem
Page 97 and 98:
Results and Discussion injected int
Page 99 and 100:
Results and Discussion Intens. [%]
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Results and Discussion 3.4.8 Quanti
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Results and Discussion Int. x 10000
Page 105 and 106:
Results and Discussion Table 3.6 Qu
Page 107 and 108:
Results and Discussion assessment o
Page 109 and 110:
Results and Discussion hydrocarbons
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Page 113 and 114:
Page 115 and 116:
Page 117 and 118:
Results and Discussion of n-alkanes
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Results and Discussion flow (in I2)
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Results and Discussion Other intere
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Results and Discussion Figure 3-80
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Results and Discussion KMD 2.4 2.2
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Results and Discussion KMD 1.1 1 Le
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Results and Discussion 3.6.4 Asphal
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Conclusions In conclusion we could
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References References 1. Fay, R. M.
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References 23. Colavecchia, M. V.,
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References 47. Dzidic, I., Petersen
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References Hydroconversion Processe
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References 91. Golovlev, V. V., All
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Appendix Light shredder waste Meas.
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419.4592 C 30 H 59 419.4611 4.6 421
Page 147 and 148:
Liqui Moly car motor oil Meas. m/z
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345.3511 C 25 H 45 345.3516 1.5 349
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