Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water

In this work, a sample preparation method based on dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for the extraction of polycyclic aromatic hydrocarbons (PAHs), namely phenanthrene and fluoranthene from water sample. In this m...

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Main Author:	Sharef A., Sarra Younes
Format:	Thesis
Language:	English
Published:	2011
Subjects:	Q Science (General)
Online Access:	http://eprints.utm.my/id/eprint/28697/1/SarraYounesSharefAMFS2011.pdf
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spelling	my-utm-ep.286972018-05-27T06:39:00Z Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water 2011 Sharef A., Sarra Younes Q Science (General) In this work, a sample preparation method based on dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for the extraction of polycyclic aromatic hydrocarbons (PAHs), namely phenanthrene and fluoranthene from water sample. In this method, a mixture of carbon tetrachloride, CCl4 (extraction solvent) and acetone (disperser solvent) was injected using a syringe into 5 mL water sample to form emulsion where the PAHs were extracted into the fine droplets of extraction solvent. The solution was then centrifuged for 3 min at 3000 rpm and the fine droplets were sedimented at the bottom of centrifuge tube. Sedimented phase (1 ?L) was injected into the GC-MS for separation and determination of PAHs. The effects of various extraction parameters namely extraction solvent type, disperser solvent type, volume of extraction solvent, and volume of disperser solvent were investigated. The optimized conditions for DLLME of selected PAHs were carbon tetrachloride as extraction solvent, 60 ?L of extraction solvent (CCl4), acetone as disperser solvent and 1 mL of disperser solvent (acetone). The correlation coefficient (r2) of the calibration curve for phenanthrene and fluoranthene were 0.9993 and 0.9973, respectively. The limits of detection (LODs) obtained for phenanthrene and fluoranthene were 0.0008 ?g/mL and 0.0006 ?g/mL, respectively. The proposed method proved to be reproducible with relative standard deviations (RSDs) of 10.69 % and 9.72 % for phenanthrene and fluoranthene, respectively. The analyte recoveries were 100.5 – 107.8 %. The concentration of was 0.02-0.15 ?g/mL. It was found that phenanthrene and fluoranthene were present in lake water sample at concentrations of 3.47×10-3 and 2.69×10-3 ?g/mL. The DLLME method combined with GC-MS proved to be an efficient method and was applied successfully for the determination of PAHs from water sample 2011 Thesis http://eprints.utm.my/id/eprint/28697/ http://eprints.utm.my/id/eprint/28697/1/SarraYounesSharefAMFS2011.pdf application/pdf en public masters Universiti Teknologi Malaysia, Faculty of Science Universiti Teknologi Malaysia, Faculty of Science
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	Q Science (General)
spellingShingle	Q Science (General) Sharef A., Sarra Younes Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water
description	In this work, a sample preparation method based on dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for the extraction of polycyclic aromatic hydrocarbons (PAHs), namely phenanthrene and fluoranthene from water sample. In this method, a mixture of carbon tetrachloride, CCl4 (extraction solvent) and acetone (disperser solvent) was injected using a syringe into 5 mL water sample to form emulsion where the PAHs were extracted into the fine droplets of extraction solvent. The solution was then centrifuged for 3 min at 3000 rpm and the fine droplets were sedimented at the bottom of centrifuge tube. Sedimented phase (1 ?L) was injected into the GC-MS for separation and determination of PAHs. The effects of various extraction parameters namely extraction solvent type, disperser solvent type, volume of extraction solvent, and volume of disperser solvent were investigated. The optimized conditions for DLLME of selected PAHs were carbon tetrachloride as extraction solvent, 60 ?L of extraction solvent (CCl4), acetone as disperser solvent and 1 mL of disperser solvent (acetone). The correlation coefficient (r2) of the calibration curve for phenanthrene and fluoranthene were 0.9993 and 0.9973, respectively. The limits of detection (LODs) obtained for phenanthrene and fluoranthene were 0.0008 ?g/mL and 0.0006 ?g/mL, respectively. The proposed method proved to be reproducible with relative standard deviations (RSDs) of 10.69 % and 9.72 % for phenanthrene and fluoranthene, respectively. The analyte recoveries were 100.5 – 107.8 %. The concentration of was 0.02-0.15 ?g/mL. It was found that phenanthrene and fluoranthene were present in lake water sample at concentrations of 3.47×10-3 and 2.69×10-3 ?g/mL. The DLLME method combined with GC-MS proved to be an efficient method and was applied successfully for the determination of PAHs from water sample
format	Thesis
qualification_level	Master's degree
author	Sharef A., Sarra Younes
author_facet	Sharef A., Sarra Younes
author_sort	Sharef A., Sarra Younes
title	Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water
title_short	Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water
title_full	Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water
title_fullStr	Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water
title_full_unstemmed	Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water
title_sort	dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Universiti Teknologi Malaysia, Faculty of Science
publishDate	2011
url	http://eprints.utm.my/id/eprint/28697/1/SarraYounesSharefAMFS2011.pdf
_version_	1747815681890451456

Dispersive liquid-liquid microextraction-gas chromatography-mass spectrometric determination of polycylic aromatic hydrocarbons in water

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