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

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Results and Discussion Intens. [%] 100 (M-3) + +MS 2 (465.8) 447.4 80 409.4 60 40 167.0 181.0 353.4 381.4 367.4 395.4 (M-3) + H 2 O 465.8 20 0 100 150 200 250 300 350 400 450 m/z Figure 3-18 APCI-MS 2 spectrum of C32 showing (M-3) + fragment at m/z 447.4 from precursor ion at m/z 465.8 corresponding to (M-3) + H 2 O Intens. +MS 2 (425) [%] 100 (M-1) + (M-1) + H 2 O 425.1 407.3 158.9 369.1 50 0 188.9 215.0 271.0 313.1 299.1 351.1 381.1 150 200 250 300 350 400 450 m/z Figure 3-19 APCI-MS 2 spectrum of C29 showing (M-1) + fragment at m/z 407.3 from precursor ion at m/z 425.1 corresponding to (M-1) + H 2 O 3.4 Light shredder Waste Analysis 3.4.1 (+)APCI-TOF-MS of Waste Sample After the detailed and necessary groundwork knowledge about the ionisation of the standard hydrocarbons in the previous section was attained, I have moved into the analysis of hydrocarbon content within the complex mixture of light shredder waste. Concerning the waste sample I have employed an optimised extraction 53
Results and Discussion procedure based on the KW 04 method. 108,110 I found that addition of acetone during extraction, enhanced the penetration of n-heptane (main solvent). Using an automatic Soxhlet extraction, it was found that six hours were the optimum extraction time needed for hydrocarbon intake. Next, the extracted waste samples were measured as direct infusions in n-heptane using the APCI-TOF MS method similar to the one used for the analysis of reference standards. Figure 3-20 shows a mass spectrum of light shredder waste sample initially extracted with Heptane/Acetone. Figure 3-21 shows a waste sample which was extracted with n- heptane only. The former spectrum reflected a higher degree of complexity which was characterised by a large number of significant peaks compared to the sample of figure 3-21. By similar mass spectra comparisons, I was also able to screen the effectivity of florisil in purifying the heptane extract from polar species. Mass spectra (a), (b) and (c) in Figure 3-22 shows that when more grams of florisil are used during purification course, the sample is better cleaned. Intens. [%] 100 80 369.4 411.4 397.4 425.4 453.4 +MS 60 40 273.3 315.3 467.5 481.5 495.5 509.5 551.5 20 701.8 0 200 250 300 350 400 450 500 550 600 650 m/z Figure 3-20 APCI (+) mass spectrum of waste sample extracted using n- heptane/Acetone 54
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Development of a Novel Mass Spectro
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Declaration of Authorship I ,Nadim
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This work has been carried out unde
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Contents Contents Declaration of Au
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List of Figures List of Figures Fig
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List of Figures Figure 3-39 MS 2 fr
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List of Tables List of Tables Table
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Abbreviations Abbreviations APCI AP
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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
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 69: Results and Discussion Intens. [%]
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 101 and 102: Results and Discussion 3.4.8 Quanti
Page 103 and 104: 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
Page 117 and 118: Results and Discussion of n-alkanes
Page 119 and 120: 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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