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

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Acknowledgements First and farmost, thanks are to ‘God’ for my life through all tests in the past years. You have made my life more bountiful. May your name be exalted, honoured, and glorified. My sincere gratitude goes to Prof. Dr. Nikolai Kuhnert for his continuous supervision, advice, support and inspiration as well as for his confidence he gifted to work in generous freedom. Thanks for being able to work with modern analytical techniques and to attend interesting international conferences. I’m so glad to have come to know him. I’d like to deeply thank the Fond für Angewandte Umweltforschung des Landes Bremen and the Bremer Entsorgungsbetriebe (BEB Company) for the support given to this project. I would like to thank my dear wife Adal for support and love through out the study years, my parents Mahmoud and Salwa Hourani, my brothers Wassim, Ibrahim and Hamzi, and my sisters Fatemah and Kawkab, all my dear friends and in particular Hany Nour. My sincere love and gratitude goes for Dr. Ursula Zimoch whose splendid care and support were more than intriguing for me during my study. Needless to say how much gratitude I owe to Prof. Dr. Angela Danil De Namor for continued support and advice. Without her contribution this Ph.D study wouldn’t have been achieved. I am tempted to individually thank all my colleagues in our laboratory in as much as thanks to Mrs Anja Müller, for the technical support.
This work has been carried out under the supervision of Prof. Dr. Nikolai Kuhnert in the analytical and organic laboratory of Chemistry Department at Jacobs University Bremen in Germany. Abstract The lack of a routine characterization method for non-volatile hydrocarbons has been an ongoing problem preventing mass spectrometry from the analysis of these hydrocarbons within many sources. Non-polar hydrocarbons are still difficult to be detected by mass spectrometry. Although several studies targeted this problem, lack of self-ionization has been limiting the ability of mass spectrometry to examine these hydrocarbons. A novel identification method for saturated straight-chain hydrocarbons in light shredder waste fraction under atmospheric pressure chemical ionization mass spectrometry (APCI-MS) has been developed. Ionization of alkanes under nitrogen gas source favoured hydrogen abstraction producing majorly (M-H) + ions which are strictly corresponding to their respective series of n-alkanes between n-decane (C10) and n-tetracontane (C40). The method is shown to produce intact gas phase ions of n- alkane in both reference and real life waste samples. APCI-MS 2 fragmentation data assisted in the structural verification of the n-alkanes investigated in both standard and waste mixtures. Additionally the total chemical composition of the light shredder waste fraction was translated by the same method. The mass spectrum displayed a bimodal distribution of odd and even mass ions with a molecular weight distribution range of m/z 200-900 Da. Molecular formulas for a 1000 unsaturated hydrocarbon compounds suggested a dehydrogenation process. The molecular masses were plotted on a Kendrick plot which was successfully employed for monitoring sample degradation. Another selection of high mass linear, branched and cyclic hydrocarbons, reported to be notoriously difficult to ionize, were examined during this study. Using optimized APCI conditions all of these analytes could be ionized without the use of an additional
Page 1 and 2: Development of a Novel Mass Spectro
Page 3: Declaration of Authorship I ,Nadim
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 and 46: Introduction including determinatio
Page 47 and 48: Introduction 1.5 Scope and Signific
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
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Results and Discussion experiment.
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Results and Discussion Intens. [%]
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Results and Discussion common featu
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Results and Discussion 3.2 APCI-TOF
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Results and Discussion These compou
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Results and Discussion Ions were pr
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Results and Discussion procedure ba
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Results and Discussion to produce m
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Results and Discussion 519.5863 519
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Results and Discussion Higher mass
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Results and Discussion isolated fro
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Results and Discussion 3.4.5 Tandem
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Results and Discussion injected int
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Results and Discussion 3.4.8 Quanti
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Results and Discussion Int. x 10000
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Results and Discussion Table 3.6 Qu
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Results and Discussion assessment o
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Results and Discussion hydrocarbons
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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
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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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Development of a Novel Mass Spectrometric ... - Jacobs University

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