Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique

Solid Phase Extraction (SPE) is a very powerful technique for clean-up and pre-concentration of the sample. Even though there is no universal method for SPE, there have been an increasing demand for a reliable and accurate forensic trace analysis. Samples received by a forensic laboratory are often...

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Main Author:	Mahmod, Anizah
Format:	Thesis
Language:	English
Published:	2016
Subjects:	QD Chemistry
Online Access:	http://eprints.utm.my/id/eprint/77833/1/AnizahMahmodMFS2016.pdf
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spelling	my-utm-ep.778332018-07-04T11:49:28Z Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique 2016-04 Mahmod, Anizah QD Chemistry Solid Phase Extraction (SPE) is a very powerful technique for clean-up and pre-concentration of the sample. Even though there is no universal method for SPE, there have been an increasing demand for a reliable and accurate forensic trace analysis. Samples received by a forensic laboratory are often in small amounts and there is a need to develop methods that are capable to detect lower concentration. The objectives of this study were to develop, evaluate and compare an SPE procedure as a pre-concentration step with conventional cotton swabbing method for analysis of ions in explosive residue. Four samples of pyrotechnics were analysed in this study. The samples were Mercun Bola (MB), Mercun Ketupat (MK), Happy Bomb (HB) and Monster Bomb (MS). The results of this study showed that all six standard cations (lithium, sodium, ammonium, potassium, magnesium and calcium) were successfully separated within 45 minutes using Metrosep C4 column (250 x 4 mm i.d) with 5 µm particle size. The eluent used were 0.7 mmol/L dipicolinic acid and 1.7 mmol/L nitric acid with a flow rate of 1.0 mL/min and pressure of 9.5 MPa. The calibration graph gave a good linearity with r2 = 0.992. The detection limits were 0.32 µg/L to 1.32 µg/L and quantitation limits in the range of 1.26 µg/L to 4.4 µg/L. The SPE method was optimized using several parameters before the method was applied to post-blast residues. The SPE cartridge used was Supelco MCAX with 500 mg sorbent bed packed with sulfonilic functional group. The SPE parameters that have been chosen were sample flow rate, type of eluents and volume of eluent. The results indicated that SPE procedure gave good pre-concentration of the analytes of interest with the preconcentration factor in the range of 7 to 74. 2016-04 Thesis http://eprints.utm.my/id/eprint/77833/ http://eprints.utm.my/id/eprint/77833/1/AnizahMahmodMFS2016.pdf application/pdf en public http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:94714 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 Mahmod, Anizah Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique
description	Solid Phase Extraction (SPE) is a very powerful technique for clean-up and pre-concentration of the sample. Even though there is no universal method for SPE, there have been an increasing demand for a reliable and accurate forensic trace analysis. Samples received by a forensic laboratory are often in small amounts and there is a need to develop methods that are capable to detect lower concentration. The objectives of this study were to develop, evaluate and compare an SPE procedure as a pre-concentration step with conventional cotton swabbing method for analysis of ions in explosive residue. Four samples of pyrotechnics were analysed in this study. The samples were Mercun Bola (MB), Mercun Ketupat (MK), Happy Bomb (HB) and Monster Bomb (MS). The results of this study showed that all six standard cations (lithium, sodium, ammonium, potassium, magnesium and calcium) were successfully separated within 45 minutes using Metrosep C4 column (250 x 4 mm i.d) with 5 µm particle size. The eluent used were 0.7 mmol/L dipicolinic acid and 1.7 mmol/L nitric acid with a flow rate of 1.0 mL/min and pressure of 9.5 MPa. The calibration graph gave a good linearity with r2 = 0.992. The detection limits were 0.32 µg/L to 1.32 µg/L and quantitation limits in the range of 1.26 µg/L to 4.4 µg/L. The SPE method was optimized using several parameters before the method was applied to post-blast residues. The SPE cartridge used was Supelco MCAX with 500 mg sorbent bed packed with sulfonilic functional group. The SPE parameters that have been chosen were sample flow rate, type of eluents and volume of eluent. The results indicated that SPE procedure gave good pre-concentration of the analytes of interest with the preconcentration factor in the range of 7 to 74.
format	Thesis
qualification_level	Master's degree
author	Mahmod, Anizah
author_facet	Mahmod, Anizah
author_sort	Mahmod, Anizah
title	Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique
title_short	Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique
title_full	Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique
title_fullStr	Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique
title_full_unstemmed	Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique
title_sort	analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2016
url	http://eprints.utm.my/id/eprint/77833/1/AnizahMahmodMFS2016.pdf
_version_	1747817842182455296

Analysis of inorganic cations in low explosive residue using solid phase extraction as a pre-concentration technique

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