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.
[1] 刘炳璋,杨泽湘.变价元素在找矿评价工作中的意义[J].四川地质学报,2007(1):66-70.[2] 谢建新,邓必阳.超声波辅助提取-HG-ICP-AES 法测定中草药雷公藤中可溶态Sb(Ⅲ) 和Sb(Ⅴ)[J].光谱学与光谱分析,2005,25(8):1347-1350.[3] Lopez A,Torralba R,Palacios M A,et al.Generation of AsH3, from As (V) in the absence of KI as prereducing agent: speciation of inorganic arsenic[J].Talanta,1992(39):1343-1348.[4] Nalan O,Mustafa S,Latif E,et al.Speciation analysis of inorganic Sb (III) and Sb (V) ions by using mini column filled with Amberlite XAD-8 resin[J].Analytica Chimica Acta,2004(505):37-41.[5] Schmidt A C,Haufe N,Otto M.A systematic study on extraction of total arsenic from down-scaled sample sizes of plant tissues and implications for arsenic species analysis[J].Talanta,2008(76):1233-1240.[6] 刘亚轩,李庆霞,董永胜.ICP-MS法在元素活动态分析中的应用[J].物探与化探,2010,34 (4):503-507.[7] Nina Ulrich.Determination of antimony species with fluoride as modifier and flow injection hydride generation inductively-coupled plasma emission spectrometry[J].Analytica Chimica Acta,2000(417): 201-209.[8] Toshio K,Akira K,Toshihiko S,et al.Determination of antimony content in natural water by graphite furnace atomic absorption spectrometry after collection as antimony (III) -pyrogallol complex on activated carbon[J].Talanta,2001(53):1117-1126.[9] 卢荫庥,王春风.塞曼效应无火焰原子吸收光谱法连续测定地球化学样品中微量铊和铟[J].物探与化探,1992,16 (4):304-312.[10] 梅俊,王秀季,汤志勇,等.氢化物发生原子荧光光谱法测定土壤中水溶态锑(Ⅲ)和锑(Ⅴ)[J].分析实验室,2004,23(3):31-33.[11] 秦德元,张新智,刘霁欣.化妆品中砷、锑无机形态的HPLC-HGAFS同测[J].生命科学仪器,2009,7(3):33-37.[12] Fuentes E,Pinochet H,Gregori I D,et al.Redox speciation analysis of antimony in soil extracts by hydride generation atomic fluorescence spectrometry[J].Spectrochimica Acta Part B,2003(58): 1279-1289.[13] 张锦茂,范凡,郭小伟,等.双道氢化物原子荧光法同时测定地球化学样品中的微量砷和锑[J].物探与化探,1984,8 (3):150-161.[14] 梅俊.氢化物发生原子荧光光谱法测定土壤中络合态锑[J].岩矿测试,2002,21(4):275-278.
