Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB)
Poly(styrene-divinyl benzene) (PS-DVB) resin is an attractive adsorbent for extraction and separation of various types of compounds due to its stability over the pH range of 1-14. However, PS-DVB resin is known to have hydrophobic surfaces that highly retain non-polar compounds while poorly retain p...
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| Format: | Monograph |
| Language: | English |
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Universiti Teknologi Malaysia
2005
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| Online Access: | http://eprints.utm.my/2716/ http://eprints.utm.my/2716/1/74091.pdf |
| _version_ | 1848890415289204736 |
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| author | Sanagi, Mohd. Marsin Abu Naim, Ahmedy Hussain, Asiah Siregar, Sri Hilma Sarjadi, Mohd. Sani Abd. Aziz, Norsyariza |
| author_facet | Sanagi, Mohd. Marsin Abu Naim, Ahmedy Hussain, Asiah Siregar, Sri Hilma Sarjadi, Mohd. Sani Abd. Aziz, Norsyariza |
| author_sort | Sanagi, Mohd. Marsin |
| building | UTeM Institutional Repository |
| collection | Online Access |
| description | Poly(styrene-divinyl benzene) (PS-DVB) resin is an attractive adsorbent for extraction and separation of various types of compounds due to its stability over the pH range of 1-14. However, PS-DVB resin is known to have hydrophobic surfaces that highly retain non-polar compounds while poorly retain polar compounds. To improve its use in the separation or extraction of polar compounds, PS-DVB resin must be chemically or physically bonded to hydrophilic groups to reduce its hydrophobic surface. The objectives of this project were to modify PS-DVB phases by introducing moieties that can increase the dispersive forces and lower the hydrophobicity of the PS-DVB phases and to examine the characteristics and applications of the modified PS-DVB adsorbents. The PS-DVB adsorbents were prepared by suspension polymerization method with polyvinyl alcohol as the suspension stabilizer at a stirring speed of 1000 rpm for 20 h. In the first approach (Volume 1), the synthesized PS-DVB adsorbents were subjected to modifications that 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 FTIR spectroscopy, SEM, nitrogen adsorption analysis and thermogravimetric analysis. Solid phase extraction (SPE) studies of test compounds, namely nitrobenzene, 2- chlorophenol, benzaldehyde, butyrophenone, and p-cresol were carried out using SPE tubes packed with the synthesized adsorbents. 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 PS-DVB heptadecyl ketone. Highest recovery percentages (67%-100%) were obtained using commercial C18-silica adsorbent. Highest breakthrough volume was achieved for PS-DVB 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.
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| first_indexed | 2025-11-15T20:41:42Z |
| format | Monograph |
| id | utm-2716 |
| institution | Universiti Teknologi Malaysia |
| institution_category | Local University |
| language | English |
| last_indexed | 2025-11-15T20:41:42Z |
| publishDate | 2005 |
| publisher | Universiti Teknologi Malaysia |
| recordtype | eprints |
| repository_type | Digital Repository |
| spelling | utm-27162017-10-11T01:35:51Z http://eprints.utm.my/2716/ Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB) Sanagi, Mohd. Marsin Abu Naim, Ahmedy Hussain, Asiah Siregar, Sri Hilma Sarjadi, Mohd. Sani Abd. Aziz, Norsyariza QD Chemistry Poly(styrene-divinyl benzene) (PS-DVB) resin is an attractive adsorbent for extraction and separation of various types of compounds due to its stability over the pH range of 1-14. However, PS-DVB resin is known to have hydrophobic surfaces that highly retain non-polar compounds while poorly retain polar compounds. To improve its use in the separation or extraction of polar compounds, PS-DVB resin must be chemically or physically bonded to hydrophilic groups to reduce its hydrophobic surface. The objectives of this project were to modify PS-DVB phases by introducing moieties that can increase the dispersive forces and lower the hydrophobicity of the PS-DVB phases and to examine the characteristics and applications of the modified PS-DVB adsorbents. The PS-DVB adsorbents were prepared by suspension polymerization method with polyvinyl alcohol as the suspension stabilizer at a stirring speed of 1000 rpm for 20 h. In the first approach (Volume 1), the synthesized PS-DVB adsorbents were subjected to modifications that 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 FTIR spectroscopy, SEM, nitrogen adsorption analysis and thermogravimetric analysis. Solid phase extraction (SPE) studies of test compounds, namely nitrobenzene, 2- chlorophenol, benzaldehyde, butyrophenone, and p-cresol were carried out using SPE tubes packed with the synthesized adsorbents. 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 PS-DVB heptadecyl ketone. Highest recovery percentages (67%-100%) were obtained using commercial C18-silica adsorbent. Highest breakthrough volume was achieved for PS-DVB 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. Universiti Teknologi Malaysia 2005-12-31 Monograph NonPeerReviewed application/pdf en http://eprints.utm.my/2716/1/74091.pdf Sanagi, Mohd. Marsin and Abu Naim, Ahmedy and Hussain, Asiah and Siregar, Sri Hilma and Sarjadi, Mohd. Sani and Abd. Aziz, Norsyariza (2005) Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB). Project Report. Universiti Teknologi Malaysia, Skudai, Johor. (Unpublished) |
| spellingShingle | QD Chemistry Sanagi, Mohd. Marsin Abu Naim, Ahmedy Hussain, Asiah Siregar, Sri Hilma Sarjadi, Mohd. Sani Abd. Aziz, Norsyariza Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB) |
| title | Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB) |
| title_full | Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB) |
| title_fullStr | Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB) |
| title_full_unstemmed | Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB) |
| title_short | Development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (PS-DVB heptadecyl ketone, chloromethyl PS-DVB, and octadecoxy methyl PS-DVB) |
| title_sort | development and application of new modified poly(styrene-divinylbenzene) adsorbents and chromatography stationary phases -volume 1 (ps-dvb heptadecyl ketone, chloromethyl ps-dvb, and octadecoxy methyl ps-dvb) |
| topic | QD Chemistry |
| url | http://eprints.utm.my/2716/ http://eprints.utm.my/2716/1/74091.pdf |