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

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Results and Discussion Intens. [%] C15 227.2 +MS 80 60 40 20 0 C10 135.1 149.1 157.2 163.1 177.2 C12 185.2 191.2 C13 199.2 213.2 241.3 253.1 263.2 140 160 180 200 220 240 260 m/z C14 C16 Figure 3-3 APCI mass spectrum in positive ion mode of a mixture containing decanes (C 10 H 22 ), dodecane (C 12 H 26 ), tridecane (C 13 H 28 ), tetradecane (C 14 H 30 ), pentadecane (C 15 H 32 ) and hexadecane (C 16 H 34 ) showing (M-3) + H 2 O ions at m/z 157.2, 185.2, 199.2, 213.2, 227.2 and 241.3 respectively. Intens. [%] 100 (M-1) + 505.6 +MS 80 60 (M-3) + H 2 O 521.6 40 20 0 257.2 285.3 409.4 309.3 353.4 (M-3) + 465.5 597.6 250 300 350 400 450 500 550 600 650 m/z 663.4 Figure 3-4 APCI mass spectrum in positive ion mode of hexatricontane (C 36 H 74 ) showing an (M-1) + and (M-3) + H 2 O at m/z 505.6 and 521.6 respectively 39
Results and Discussion Intens. [%] 50 505.6 521.6 +MS 40 30 20 449.5 465.5 561.6 577.6 10 0 535.5 479.5 407.4 421.4 435.5 493.3 549.6 591.6 617.7 425 450 475 500 525 550 575 600 m/z Figure 3-5 APCI mass spectrum in positive ion mode of dotriacontane (C 32 H 64 ), hexatricontane (C 36 H 74 ) and tetracontane (C 40 H 82 ) These reported measurement were my starting steps before I tried to optimise solvent. These measurements were absolutely considered novel hits because it is well known that n-alkanes are difficult to be ionised. As far as the effect of other solvents over the ionisation process in APCI was concerned, two further experiments were performed. Two solutions of model n-alkane mixture of the higher mass range (C20 to C40) were prepared and injected as direct infusions in n-pentane and chloroform as the APCI reagent. None of the two solvents afforded better results compared to those with n-heptane. Figure 3-6 shows the mass spectra of few analytes in the aforementioned range in n-pentane. n-Pentane was seen to enhance fragmentation potential of alkanes by possibly increasing the efficiency of collisions of reagent ions with the neutral n-alkane analytes inside the APCI source. To this end, the appearance of such n-alkane species is in agreement with the results summarized in the introduction in particular the study performed by Bell et al.. 78 The latter’s study of a set of low mass n- alkanes produced (M-1) + , (M-3) + and (M-3) + H 2 O. The results of individual model n-alkanes were summarised in table 3.1. 40
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 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: Results and Discussion experiment.
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 65 and 66: Results and Discussion Intens. [%]
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 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 111 and 112:
Results and Discussion Intens. [%]
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
Page 127 and 128:
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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