微波消解-氢化物发生原子荧光光谱法同时测定钨矿中砷汞

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摘要以盐酸硝酸（5+3）的混酸为消解液,微波消解钨矿样品,然后采用氢化物发生原子荧光光谱法(HG-AFS)同时测定钨矿中砷和汞。对微波消解程序进行优化,并探讨了共存离子对测定砷、汞的干扰。由于钨基体在酸性消解液中形成钨酸沉淀,而实际样品中其他共存离子浓度均低于允许浓度,因此,基体和共存元素对待测元素几乎没有影响。砷、汞的测定下限分别为0.20 mg/kg和0.10 mg/kg。选择不同钨矿石进行精密度考察,相对标准偏差（RSD,n=6）在1.3％～6.2％范围内；加标回收试验表明,回收率在82％～101％之间。对钨矿石标准样品进行分析,砷的测定值与认定值一致。

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	雷美康
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	杨靖

关键词 ：钨矿 , 微波消解 , 氢化物发生原子荧光光谱法 , 砷 , 汞

Abstract： With mixed HCl-HNO₃ (5+3) as digestion solution, tungsten ore samples were dissolved by microwave digestion. Then hydride generation-atomic fluorescence spectrometry was used to determine arsenic and mercury in tungsten ore. The microwave digestion procedure was optimized. In addition, the interference of the coexistent ions on the determination of arsenic and mercury was discussed. Since tungsten matrix formed tungstic acid precipitation in acid digestion solution and the concentration of other coexistent ions in the actual sample was lower than the allowable concentration, so the matrix and coexistent elements did not impact the testing elements. The low limit of determination of arsenic and mercury is 0.20 mg/kg and 0.10 mg/kg, respectively. Different tungsten ores were chosen to study its precision, with RSD (n=6) between 1.3% and 6.2%. The standard addition recovery test indicated the recovery was between 82% and 101%. A study was conducted on the determination of arsenic in certified reference material of tungsten ore, with the found value consistent with the certified value.

Key words： tungsten ore microwave digestion hydride generation-atomic fluorescence spectrometry arsenic mercury

收稿日期: 2012-03-13

ZTFLH:

O657.31

基金资助:出入境检验检疫行业标准制（修）订计划项目（2009B647）

作者简介: 雷美康（1982-）,男,工程师,硕士,主要从事分析检测工作;E-mail：leimeikang@163.com

引用本文:

雷美康,彭芳,曹培林,梅凯,杨靖. 微波消解-氢化物发生原子荧光光谱法同时测定钨矿中砷汞[J]. 冶金分析, 2013, 33(4): 44-47. LEI Mei-kang,PENG Fang,CAO Pei-lin,MEI Kai,YANG Jing. Simultaneous determination of arsenic and mercury in tungsten ore by microwave digestion-hydride generation-atomic fluorescence spectrometry. , 2013, 33(4): 44-47.

链接本文:

http://47.93.29.245/Jweb_yjfx/CN/ 或 http://47.93.29.245/Jweb_yjfx/CN/Y2013/V33/I4/44


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