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A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA

In this study, a simple sample preparation method was developed for the determination of tri-and hexavalent chromium in water samples. It utilizes a pre-heated customized glass tube (CGT), to supply the heat energy required for the reaction of Cr(III) with ammonium pyrrolidinedithiocarbamate (APDC)....

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Main Authors: Salihu, Simon Olonkwoh, Bakar, Nor Kartini Abu
Format: Article
Published: Elsevier 2018
Subjects:
Q Science (General)
QD Chemistry
Online Access:http://eprints.um.edu.my/20802/
https://doi.org/10.1016/j.talanta.2018.01.041
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spelling my.um.eprints.208022019-04-03T08:47:10Z http://eprints.um.edu.my/20802/ A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA Salihu, Simon Olonkwoh Bakar, Nor Kartini Abu Q Science (General) QD Chemistry In this study, a simple sample preparation method was developed for the determination of tri-and hexavalent chromium in water samples. It utilizes a pre-heated customized glass tube (CGT), to supply the heat energy required for the reaction of Cr(III) with ammonium pyrrolidinedithiocarbamate (APDC). The products of the Cr complexes, tris(1-pyrrolidinecarbodithioato)chromium(III) and bis(1-pyrrolidinecarbodithioato)[1-pyrrolidinecarbodithio(thioperoxoato)]chromium(III) were chromatographed with Shimadzu LC-20AT and Zobax Eclipse C18 (150 mm × 4.6 mm, 5 µm) column using ACN: Water, (7:3, v/v) as the mobile phase. The concentration of Cr(III) ranged from 0.06 mgL−1 to 0.09 mgL−1 and that of Cr(VI) was between 0.02 mg L−1 to 0.04 mgL−1 in the samples. Percentage recoveries from spiked real samples were between 87% (tap water) to 110% (wastewater) for Cr(III) and 92% (pond water) to 117% (tap water) for Cr(VI). The limits of detection (LODs) were 0.0029 mg L−1 and 0.0014 mg/L−1 for Cr(III) Cr(VI) respectively. While the limits of quantitation (LOQs), were 0.0098 mg L−1 and 0.0047 mg L−1 for Cr(III) and Cr(VI) respectively. Method precision (RSD (%)) was 3.3% and 3.5% for Cr(III) and Cr(VI) respectively. The developed method was applied for the speciation analysis of chromium in drinking water, tap water, wastewater, river water, and pond water samples. Our findings proved the method is simple and inexpensive. The method was validated by the analysis of a certified reference material (CRM) SLRS-4. The percentage recovery and RSD(%) from the spiked CRM were 91% and 115% and 0.32% and 1.4% for Cr(III) and Cr(VI) respectively. Elsevier 2018 Article PeerReviewed Salihu, Simon Olonkwoh and Bakar, Nor Kartini Abu (2018) A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA. Talanta, 181. pp. 401-409. ISSN 0039-9140 https://doi.org/10.1016/j.talanta.2018.01.041 doi:10.1016/j.talanta.2018.01.041
institution Universiti Malaya
building UM Library
collection Institutional Repository
continent Asia
country Malaysia
content_provider Universiti Malaya
content_source UM Research Repository
url_provider http://eprints.um.edu.my/
topic Q Science (General)
QD Chemistry
spellingShingle Q Science (General)
QD Chemistry
Salihu, Simon Olonkwoh
Bakar, Nor Kartini Abu
A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA
description In this study, a simple sample preparation method was developed for the determination of tri-and hexavalent chromium in water samples. It utilizes a pre-heated customized glass tube (CGT), to supply the heat energy required for the reaction of Cr(III) with ammonium pyrrolidinedithiocarbamate (APDC). The products of the Cr complexes, tris(1-pyrrolidinecarbodithioato)chromium(III) and bis(1-pyrrolidinecarbodithioato)[1-pyrrolidinecarbodithio(thioperoxoato)]chromium(III) were chromatographed with Shimadzu LC-20AT and Zobax Eclipse C18 (150 mm × 4.6 mm, 5 µm) column using ACN: Water, (7:3, v/v) as the mobile phase. The concentration of Cr(III) ranged from 0.06 mgL−1 to 0.09 mgL−1 and that of Cr(VI) was between 0.02 mg L−1 to 0.04 mgL−1 in the samples. Percentage recoveries from spiked real samples were between 87% (tap water) to 110% (wastewater) for Cr(III) and 92% (pond water) to 117% (tap water) for Cr(VI). The limits of detection (LODs) were 0.0029 mg L−1 and 0.0014 mg/L−1 for Cr(III) Cr(VI) respectively. While the limits of quantitation (LOQs), were 0.0098 mg L−1 and 0.0047 mg L−1 for Cr(III) and Cr(VI) respectively. Method precision (RSD (%)) was 3.3% and 3.5% for Cr(III) and Cr(VI) respectively. The developed method was applied for the speciation analysis of chromium in drinking water, tap water, wastewater, river water, and pond water samples. Our findings proved the method is simple and inexpensive. The method was validated by the analysis of a certified reference material (CRM) SLRS-4. The percentage recovery and RSD(%) from the spiked CRM were 91% and 115% and 0.32% and 1.4% for Cr(III) and Cr(VI) respectively.
format Article
author Salihu, Simon Olonkwoh
Bakar, Nor Kartini Abu
author_facet Salihu, Simon Olonkwoh
Bakar, Nor Kartini Abu
author_sort Salihu, Simon Olonkwoh
title A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA
title_short A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA
title_full A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA
title_fullStr A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA
title_full_unstemmed A simple method for chromium speciation analysis in contaminated water using APDC and a pre-heated glass tube followed by HPLC-PDA
title_sort simple method for chromium speciation analysis in contaminated water using apdc and a pre-heated glass tube followed by hplc-pda
publisher Elsevier
publishDate 2018
url http://eprints.um.edu.my/20802/
https://doi.org/10.1016/j.talanta.2018.01.041
_version_ 1643691384018829312
score 13.211869

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