THE DETERMINATION OF ANTIMONY (III) AND ANTOMONY (V) IN GEOLOGICAL SAMPLES BY HYDRIDE GENERATION-ATOMIC FLUORESCENCE SPECTROMETRY
HAO Zhi-hong1, YANG Fan1,2, XING Xia1, TANG Zhi-yong3, ZHANG Qin1
1. Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Sciences, Langfang 065000, China;
2. College of Earth Scie- nce and Resources, China University of Geosciences, Beijing 100083, China;
3. Faculty of Material Science and Chemical Engineering, China University of Geosciences, Wuhan 430074, China
Abstract:A method for the determination of antimony (Ⅲ) and antimony (Ⅴ) in geological samples (stream sediments) by hydride generation-atomic fluorescence spectrometry was developed in the paper. 4.8 mol/L HCl could be used as the extractant with ultrasonic-assisted extraction. In the medium of 0.24 mol/L hydrochloric acid, antimony (Ⅲ) could be alternatively determined with 6 g/mL sodium citrate as the masking agent for Sb (V). Then antimony (Ⅴ) could be figured out by the subtraction method. The detection limit of the method was 0.075×10-6 for Sb (Ⅲ) and 0.097×10-6 for Sb (Ⅴ), and the relative standard deviation was 1.1% and 0.64% (n=11) for 40 ng/mL Sb (Ⅲ) and 40 ng/mL Sb(Ⅴ) standard solution. The proposed method was applied to the determination of antimony (Ⅲ) and antimony (Ⅴ) in geological samples, and a comparison between the extraction results and the aqua regia dissolution results shows that the extraction rate of antimony was higher than 80%, the recoveries were in the ranges of 83%~107% and 98%~114% for Sb (Ⅲ) and Sb (V) respectively.
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