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

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Contents 2.2.2 Preparation of Oxidation Products from Shredder Extract ........................................34 2.3 MS Operating Conditions ..............................................................................................34 2.4 Graphical Presentation of the Used Instruments .............................................................36 3 Results and Discussion ............................................................................................... 37 3.1 APCI-TOF-MS of Standard n-Alkanes ..........................................................................37 3.2 APCI-TOF-MS of a Variety of Hydrocarbons ................................................................44 3.3 Pathway of Ionisation of Hydrocarbon Standards under APCI Conditions ......................49 3.4 Light shredder Waste Analysis ......................................................................................53 3.4.1 (+)APCI-TOF-MS of Waste Sample ........................................................................53 3.4.2 Calibration ..............................................................................................................57 3.4.3 Identification of Polychlorinated Biphenyls (PCBs) in (-) APCI-TOF-MS ...............63 3.4.4 Tandem MS Measurements .....................................................................................65 3.4.5 Tandem MS of Derivatised Compounds ..................................................................76 3.4.6 Tandem MS of PCBs ...............................................................................................77 3.4.7 Oxidative Degradation of Complex Mixture of Shredder Waste ...............................79 3.4.8 Quantification .........................................................................................................84 3.5 Application of the Methodology to Other Complex Mixtures .........................................88 3.5.1 Analysis of Solid Waste from Lebanon ....................................................................88 3.5.2 Analysis of Car Motor Oil .......................................................................................91 3.5.3 Analysis of Asphaltenes ..........................................................................................96 3.6 Kendrick Plot and Interpretation of Complex Data from Various Complex Mixtures ......98 3.6.1 Light Shredder Waste ..............................................................................................98 3.6.1.1 Kendrick Plot for PCBs ................................................................................... 106 3.6.1.2 Kendrick Plot for Oxidation Products .............................................................. 108 3.6.2 Lebanon Waste...................................................................................................... 109 3.6.3 Oil sample ............................................................................................................. 110 3.6.4 Asphaltenes ........................................................................................................... 112 Conclusions ................................................................................................................. 114 References ................................................................................................................... 116
List of Figures List of Figures Figure 1-1 Examples of aliphatic and aromatic hydrocarbons in crude oils.................................. 8 Figure 1-2 Range of ionisation techniques employed with different types of compounds ...........10 Figure 1-3 Matrix-assisted laser desorption/ionization (MALDI) ...............................................12 Figure 1-4 Complex data management ......................................................................................19 Figure 1-5 Schematic description of the atmospheric pressure chemical ionisation (APCI) interface and the mechanism of ion formation in the corona discharge region .....................21 Figure 1-6 Kendrick mass defect vs nominal Kendrick mass for odd mass ions in crude oil sample. Note the visual vertical separation of compound classes (O, O 2 , O 3 S) and types (e.g., compounds with different number of rings plus double bonds) based on mass defect and the simultaneous visual horizontal distribution of number of CH 2 groups for a given compound class and type. 105 ................................................................................................................26 Figure 1-7 Shredding Plant ........................................................................................................27 Figure 1-8 Light shredder waste fraction set for biological treatment in a prepared unit. ............28 Figure 1-9 UCM feature of hydrocarbon content of light shredder waste in GC .........................29 Figure 2-1 Instruments used in the study ..................................................................................36 Figure 3-1 APCI mass spectrum in positive ion mode of dodecane (C 12 H 26 ) showing (M-3) + H 2 O ion as product ion at m/z 185.2 ...........................................................................................38 Figure 3-2 APCI mass spectrum in positive ion mode of tridecane (C 13 H 28 ) showing (M-3) + H 2 O ion as product ion at m/z 199.2 ...........................................................................................38 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...............................................................................................................39 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 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 ).....................................................................................40 Figure 3-6 APCI mass spectrum of model mixture of n-alkanes injected using n-pentane ..........41 Figure 3-7 APCI-MS spectrum in positive ion mode of C7-C40 showing (M-1) + ions of n-alkanes ..........................................................................................................................................42 Figure 3-8 APCI mass spectrum of n-paraffin mixture ...............................................................43 Figure 3-9 APCI mass spectrum of C12-C60 .............................................................................43 Figure 3-10 Structures of various hydrocarbons investigated by APCI-TOF-MS ........................45
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: Contents Contents Declaration of Au
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 and 56: Results and Discussion experiment.
Page 57 and 58: Results and Discussion Intens. [%]
Page 59 and 60:
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 Intens. [%]
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Results and Discussion Ions were pr
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Page 71 and 72:
Results and Discussion procedure ba
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Page 75 and 76:
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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Page 83 and 84:
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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.,
Page 137 and 138:
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
Page 149 and 150:
345.3511 C 25 H 45 345.3516 1.5 349
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