Development of a Novel Mass Spectrometric ... - Jacobs University
Development of a Novel Mass Spectrometric ... - Jacobs University Development of a Novel Mass Spectrometric ... - Jacobs University
Experimental 2 Experimental 2.1 Chemicals and Model Standards a) Standard low mass n-alkanes such as Octane, nonane, decane, undecane, dodecane, tridecane, tetradecane, pentadecane and hexadecane were purchased from Sigma Aldrich (Bremen, Germany). Higher mass n-alkanes like octadecane, eicosane, henicosane, docosane, tricosane, tetracosane, pentacosane, hexacosane, octacosane, dotricontane, hexatriacontane, tetracontane, dotetracontane, tetratetracontane, octatetracontane, pentacontane, tetrapentacontane and hexacontane all of analytical grade, were purchased from Sigma Aldrich. b) Different model mixtures of n-alkanes were also purchased from the same company. i) C7-C40 Saturated Alkanes (1 mg/ml in hexane) ii) C8-C40 Alkanes Calibration Standard (500 µg/ml in dichloromethane) iii) C10, C20-C40 Alkane Standard Mixture (50 mg/l in n-heptane) iv) C21-C40 Alkane Standard Solution (40 mh/l in toluene) v) C12-C60 Quantitative Linearity Standard (0.01 % (w/w) in cyclohexane) vi) n-Paraffin Mix C18, C20, C22, C24 Analytical Standard (2 % (w/w) in octane) c) Other deuterated standards such as deuterated tetracosane [(D-24), (C 24 D 50 )] and deuterated dotriacontane [(D-32), (C 32 D 66 )] d) Other individual standards were purchased from Chiron Company (Chiron.no). These standards were 2,6,10,14-tetramethyl nonadecane, 2,6,10,14,18-pentamethyl heneicosane, n-tetradecyl cyclohexane, n-octadecyl cyclohexane, n-octyl benzene, n-nonyl benzene, n-tetradecyl benzene, and n-octadecyl benzene, each in 1 mg/ml isooctane solution. 5-α-Cholestane, squalane, squalene, phytane, and 1-phenyl decane all of analytical grade were also purchased from Sigma Aldrich. 31
Experimental e) Other model mixture purchased also from Aldrich Company is the polychlorinated biphenyls (PCBs), PCB Congener Mix 1. Decachlorobiphenyl (C 12 Cl 10 ) was purchased from the same company. f) The list of solvents and derivatisation agents include n-pentane, n-heptane, chloroform, isooctane, methanol, dichloromethane and toluene. Deuterium oxide (D 2 O), silver trifluoroacetate (CF 3 COOAg) and chromium trioxide (CrO 3 ) were also supplied. Last, the purification material florisil (100-200 mesh) was purchased from Aldrich Company as well. 2.2 Preparation of Samples 2.2.1 Alkane Standards and Shredder Waste Samples Preparation Preparation of model standards was done by dissolving or diluting a known quantity of separate alkanes. The prepared solution was always diluted prior to injection to meet the concentration needed for mass spectrometry around mM concentration. Model mixtures of n-alkanes was prepared by mixing equimolar ratios of the separate alkane standards. Standard model mixture purchased from Sigma Aldrich company were diluted to mM concentration before measurement. For example 20 µl were taken from C7-C40 alkane standard (1mg/l) and diluted into a 1 ml of n-heptane solvent before injection. Preparation of light shredder waste samples was achieved by few but important steps. Most of the common analytical steps are related to the separation and purification of analytes of interest from a sample matrix prior to their measurement. After frequent treatments of huge amounts of upcoming light shredder waste in the BEB Company, samples are cropped for analytical investigation. Although the shredder waste itself is homogenous by nature, samples are taken from different locations of the same treated shredder waste portion. In our laboratory, the sample was dried and sieved by a normal sieve to get rid of bulk pieces of plastic, small wires and others that are removed. Next the sieved waste are grounded into fine particles (around µm) by a Fritsch Mill. 32
- 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: Introduction 1.5 Scope and Signific
- 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 65 and 66: Results and Discussion Intens. [%]
- Page 67 and 68: Results and Discussion Ions were pr
- Page 69 and 70: Results and Discussion Intens. [%]
- Page 71 and 72: Results and Discussion procedure ba
- Page 73 and 74: 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 81 and 82: Results and Discussion Intens. [%]
- Page 83 and 84: Results and Discussion Intens. [%]
- Page 85 and 86: Results and Discussion Intens. [%]
- Page 87 and 88: Results and Discussion isolated fro
- Page 89 and 90: Results and Discussion Intens. [%]
- Page 91 and 92: Results and Discussion Intens. [%]
- Page 93 and 94: Results and Discussion 3.4.5 Tandem
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- Page 97 and 98: Results and Discussion injected int
Experimental<br />
2 Experimental<br />
2.1 Chemicals and Model Standards<br />
a) Standard low mass n-alkanes such as Octane, nonane, decane, undecane,<br />
dodecane, tridecane, tetradecane, pentadecane and hexadecane were purchased<br />
from Sigma Aldrich (Bremen, Germany). Higher mass n-alkanes like octadecane,<br />
eicosane, henicosane, docosane, tricosane, tetracosane, pentacosane, hexacosane,<br />
octacosane, dotricontane, hexatriacontane, tetracontane, dotetracontane,<br />
tetratetracontane, octatetracontane, pentacontane, tetrapentacontane and<br />
hexacontane all <strong>of</strong> analytical grade, were purchased from Sigma Aldrich.<br />
b) Different model mixtures <strong>of</strong> n-alkanes were also purchased from the same<br />
company.<br />
i) C7-C40 Saturated Alkanes (1 mg/ml in hexane)<br />
ii) C8-C40 Alkanes Calibration Standard (500 µg/ml in dichloromethane)<br />
iii) C10, C20-C40 Alkane Standard Mixture (50 mg/l in n-heptane)<br />
iv) C21-C40 Alkane Standard Solution (40 mh/l in toluene)<br />
v) C12-C60 Quantitative Linearity Standard (0.01 % (w/w) in cyclohexane)<br />
vi) n-Paraffin Mix C18, C20, C22, C24 Analytical Standard (2 % (w/w) in octane)<br />
c) Other deuterated standards such as deuterated tetracosane [(D-24), (C 24 D 50 )] and<br />
deuterated dotriacontane [(D-32), (C 32 D 66 )]<br />
d) Other individual standards were purchased from Chiron Company (Chiron.no).<br />
These standards were 2,6,10,14-tetramethyl nonadecane, 2,6,10,14,18-pentamethyl<br />
heneicosane, n-tetradecyl cyclohexane, n-octadecyl cyclohexane, n-octyl benzene,<br />
n-nonyl benzene, n-tetradecyl benzene, and n-octadecyl benzene, each in 1 mg/ml<br />
isooctane solution. 5-α-Cholestane, squalane, squalene, phytane, and 1-phenyl<br />
decane all <strong>of</strong> analytical grade were also purchased from Sigma Aldrich.<br />
31