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

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

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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

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

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