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Speciation of Inorganic Antimony in Food and Water Samples by Flow Injection On-line Nano γ-Alumina Micro-column Solid-Phase Extraction Coupled with Slotted Tube Atom Trapping Flame Atomic Absorption Spectrometry

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Abstract

Nano γ-alumina, with ultra-high specific surface area (387.2 m2 g−1), has been synthesized and used as a promising adsorbent material in solid-phase extraction. A simple, sensitive, and economic method was developed for speciation of inorganic antimony by slotted tube atom trapping flame atomic absorption spectrometry (STAT-FAAS) after flow injection on-line nano γ-alumina micro-column solid-phase extraction. In this method, Sb(III)–diethyldithiocarbamate (DDTC) complexes produced on-line from DDTC and Sb(III) were adsorbed by the synthesized γ-alumina nanoparticles in a micro-column, then eluted by 1.0 mol L−1 HNO3 in methanol, whereas Sb(V) remained in aqueous solution. The total inorganic Sb was determined by the same procedure after Sb(V) was reduced with thiourea. Under optimal conditions, the enrichment factor was 56.5 and the detection sensitivity was improved 40-fold for antimony by STAT-FAAS compared to conventional FAAS. The limit of detection was 6.0 ng L−1 for Sb(III) and 8.2 ng L−1 for Sb(V), respectively. The intra-day precision (RSDs, n = 11) were 2.8 % for Sb(III) and 3.5 % for Sb(V), respectively, and the inter-day precision (n = 3) were 7.1 % for Sb(III) and 8.4 % for Sb(V), respectively. The recoveries for the spiked samples were 93–107 %. The proposed method was applied to speciation of inorganic antimony in water and food samples successfully.

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Acknowledgments

The authors gratefully acknowledge the financial support provided by the project funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions, the Science and Technology Project of Xuzhou City (XF11C050), and the Natural Science Foundation of Jiangsu Education Committee (11KJB150018).

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  1. Jiangsu Key Laboratory of Green Synthetic Chemistry for Functional Materials, School of Chemistry and Chemical Engineering, Jiangsu Normal University, 101 Shanghai Road, Xuzhou, 221116, People’s Republic of China

    Jiuying Tian, Tao Huang & Jusheng Lu

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  1. Jiuying Tian
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  2. Tao Huang
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Correspondence to Jusheng Lu.

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Tian, J., Huang, T. & Lu, J. Speciation of Inorganic Antimony in Food and Water Samples by Flow Injection On-line Nano γ-Alumina Micro-column Solid-Phase Extraction Coupled with Slotted Tube Atom Trapping Flame Atomic Absorption Spectrometry. Food Anal. Methods 6, 1080–1089 (2013). https://doi.org/10.1007/s12161-012-9513-4

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