Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds

In this study, poly (styrene-divinylbenzene) (PS-DVB) adsorbents were synthesized by using suspension polymerization method. The modifications on highly cross-linked porous PS-DVB resin consisted of (i) Friedel-Crafts acylation reaction using stearoyl chloride as an acylation agent to produce PS-DVB...

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Main Author:	Siregar, Sri Hilma
Format:	Thesis
Language:	English
Published:	2005
Subjects:	QD Chemistry
Online Access:	http://eprints.utm.my/id/eprint/4450/1/SriHilmaSiregarMFS2005.pdf
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spelling	my-utm-ep.44502018-01-28T08:23:57Z Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds 2005-09 Siregar, Sri Hilma QD Chemistry In this study, poly (styrene-divinylbenzene) (PS-DVB) adsorbents were synthesized by using suspension polymerization method. The modifications on highly cross-linked porous PS-DVB resin consisted of (i) Friedel-Crafts acylation reaction using stearoyl chloride as an acylation agent to produce PS-DVB heptadecyl ketone, (ii) Chloromethylation reaction to produce chloromethyl PS-DVB in the presence of chloromethyl styrene, and (iii) Williamson ether reaction using sodium metal and octadecanol as reaction agents to produce octadecoxy methyl PS-DVB. The synthesized adsorbents were characterized by Fourier transform infrared (FTIR), scanning electron microscopy (SEM), nitrogen adsorption analysis and thermogravimetric analysis (TGA). Solid phase extraction (SPE) studies of selected organic test compounds, namely nitrobenzene, 2-chlorophenol, benzaldehyde, butyrophenone, and p-cresol were carried out using SPE tubes packed with the synthesized adsorbents. Commercial SPE adsorbents were also used for comparison. The recoveries obtained for the home-made PS-DVB were in the range of 7% to 72% with relative standard deviations of 1% to 10%. Increased percentages of recovery (35%-83%) with the relative standard deviations of 2%-7% were obtained using PSDVB heptadecyl ketone. Highest recovery percentages (67%-100%) were obtained using commercial C18-silica adsorbent. Breakthrough volume determinations for the various adsorbents showed that highest breakthrough volume was achieved for PSDVB heptadecyl ketone adsorbent, i.e. 30.60 mL of 20 ppm nitrobenzene and 20.47 mL of 20 ppm 2-chlorophenol. Lowest breakthrough volume was obtained for octadecoxy methyl PS-DVB adsorbent (1.03 mL of 20 ppm nitrobenzene and 1.00 mL of 20 ppm 2-chlorophenol). PS-DVB heptadecyl ketone has been proven suitable to be used as SPE adsorbent in the future. 2005-09 Thesis http://eprints.utm.my/id/eprint/4450/ http://eprints.utm.my/id/eprint/4450/1/SriHilmaSiregarMFS2005.pdf application/pdf en public masters Universiti Teknologi Malaysia, Faculty of Science Faculty of Science
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	QD Chemistry
spellingShingle	QD Chemistry Siregar, Sri Hilma Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds
description	In this study, poly (styrene-divinylbenzene) (PS-DVB) adsorbents were synthesized by using suspension polymerization method. The modifications on highly cross-linked porous PS-DVB resin consisted of (i) Friedel-Crafts acylation reaction using stearoyl chloride as an acylation agent to produce PS-DVB heptadecyl ketone, (ii) Chloromethylation reaction to produce chloromethyl PS-DVB in the presence of chloromethyl styrene, and (iii) Williamson ether reaction using sodium metal and octadecanol as reaction agents to produce octadecoxy methyl PS-DVB. The synthesized adsorbents were characterized by Fourier transform infrared (FTIR), scanning electron microscopy (SEM), nitrogen adsorption analysis and thermogravimetric analysis (TGA). Solid phase extraction (SPE) studies of selected organic test compounds, namely nitrobenzene, 2-chlorophenol, benzaldehyde, butyrophenone, and p-cresol were carried out using SPE tubes packed with the synthesized adsorbents. Commercial SPE adsorbents were also used for comparison. The recoveries obtained for the home-made PS-DVB were in the range of 7% to 72% with relative standard deviations of 1% to 10%. Increased percentages of recovery (35%-83%) with the relative standard deviations of 2%-7% were obtained using PSDVB heptadecyl ketone. Highest recovery percentages (67%-100%) were obtained using commercial C18-silica adsorbent. Breakthrough volume determinations for the various adsorbents showed that highest breakthrough volume was achieved for PSDVB heptadecyl ketone adsorbent, i.e. 30.60 mL of 20 ppm nitrobenzene and 20.47 mL of 20 ppm 2-chlorophenol. Lowest breakthrough volume was obtained for octadecoxy methyl PS-DVB adsorbent (1.03 mL of 20 ppm nitrobenzene and 1.00 mL of 20 ppm 2-chlorophenol). PS-DVB heptadecyl ketone has been proven suitable to be used as SPE adsorbent in the future.
format	Thesis
qualification_level	Master's degree
author	Siregar, Sri Hilma
author_facet	Siregar, Sri Hilma
author_sort	Siregar, Sri Hilma
title	Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds
title_short	Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds
title_full	Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds
title_fullStr	Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds
title_full_unstemmed	Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds
title_sort	synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2005
url	http://eprints.utm.my/id/eprint/4450/1/SriHilmaSiregarMFS2005.pdf
_version_	1747814530911567872

Synthesis and methods development of adsorbents based on poly (styrene-divinylbenzene) derivatives for solid phase extraction of aromatic compounds

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