| 氢化物发生-原子荧光光谱法测定氟石中锑 |
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| 引用本文： | 金宇,刘曙,李晨,林苗.氢化物发生-原子荧光光谱法测定氟石中锑[J].冶金分析,2014,34(5):64-67. |
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| 作者姓名： | 金宇 刘曙 李晨 林苗 |
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| 作者单位： | 1. 上海出入境检验检疫局, 上海 200135; 2. 东华大学化学化工与生物工程学院, 生态纺织教育部重点实验室, 上海 201620 |
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| 基金项目： | 质检公益性课题(201310065) |
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| 摘 要： | 采用HNO3、HF和HClO4消解氟石样品, 通过加热挥发溶液中酸来控制反应体系酸度和去除试液中的F-, 以L-半胱氨酸为预还原剂, 在60 ℃的温度下进行还原反应30 min, 使溶液中的Sb还原为Sb, 用氢化物发生-原子荧光光谱法测定氟石中总锑含量。结果表明, F-存在下, 不会影响Sb的荧光强度, 但会显著影响Sb的荧光强度, 对总锑的测定存在干扰, 添加L-半胱氨酸或硫脲-抗坏血酸, 都不能消除F-对Sb荧光强度的影响。方法检出限为0.024 μg/L。选取6种不同氟石样品进行测定, 测定结果的相对标准偏差在3.3%～8.0%范围(n=6), 回收率在94%～106%之间, 锑的测定值与ICP-MS法测定值相符。
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| 关 键 词： | 氢化物发生 原子荧光光谱法 氟石 锑 |
| 收稿时间： | 2013-11-14 |
Determination of antimony in fluorspar by hydride generation-atomic fluorescence spectrometry |
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| JIN Yu,LIU Shu,LI Chen,LIN Miao.Determination of antimony in fluorspar by hydride generation-atomic fluorescence spectrometry[J].Metallurgical Analysis,2014,34(5):64-67. |
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| Authors: | JIN Yu LIU Shu LI Chen LIN Miao |
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| Affiliation: | 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;2. College of Chemistry, Chemical Engineering and Biotechnology, Key Laboratory of Science and Technology of Eco-Textile, Ministry of Education, Donghua University, Shanghai 201620, China |
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| Abstract: | A new method was described for the determination of total antimony in fluorspar by hydride generation-atomic fluorescence spectrometry. The samples were dissolved in HNO3+HF+HClO4 mixed acid. Through heating until fumes of perchloric acid disappearing, system acidity was controlled and F- in the sample solution was removed. L-cysteine was added under 60 ℃ for 30 min to pre-reduce Sb from the pentavalent state to the trivalent state. The results indicated that F- could not interfere with the fluorescence signals of Sb but could significantly interfere with the fluorescence signals of Sb, i.e., it would interfere with the determination of total antimony. Even after the addition of L-cysteine or thiourea-ascorbic acid, the interference of F- in the determination of total antimony still could not be eliminated. The detection limit was 0.024 μg/L. Six different fluorspar samples were determined. The relative standard deviations (RSDs) were 3.3%-8.0% (n=6). |
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| Keywords: | hydride generation atomic fluorescence spectrometry fluorspar antimony |
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