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P507负载泡塑分离-电感耦合等离子体质谱法同时测定化探样品中银钨钼

Simultaneous Determination of Ag, W and Mo in Geochemical Exploration Samples by ICP-MS Using P507 Loaded Foam for Separation

  • 摘要: 电感耦合等离子体质谱法(ICP-MS)测定化探样品中的Ag时,由于受到Zr、Nb氧化物离子91Zr16O和93Nb16O的严重干扰,直接测定时低含量Ag的分析结果误差较大,需要将干扰元素分离才能得到较准确的结果。当前应用P507萃淋树脂分离样品溶液中Zr和Nb等干扰元素已经成功应用于化探样品中Ag的测定。本文将此方法进一步改进,用氢氟酸、硝酸、高氯酸和逆王水敞开溶样,通过P507负载泡塑进行振荡吸附,实现了化探样品中Ag和内标元素Rh与干扰元素Zr的有效分离,应用ICP-MS可同时测定Ag、W和Mo。标准样品的测定结果准确可靠,方法检出限为Ag 0.0045 μg/g,W 0.023 μg/g,Mo 0.060 μg/g,均低于多目标地球化学调查(1:250000)样品分析的检出限。P507负载泡塑分离流程操作简便,无交叉污染,一次振荡可处理100件样品,其分析效率显著优于P507萃淋树脂交换柱,更加适合大批量化探样品Ag与W、Mo及微量元素的同时测定。

     

    Abstract: When determining Ag in geochemical exploration samples by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), the molecular ions 91Zr16O and 93Nb16O can seriously interfere with the isotopes 107Ag and 109Ag and need to be separated out to obtain accurate results. The application of P507 levextrel resin to separate the interfering elements of Zr and Nb was recently successfully conducted to in the determination of Ag in exploration samples. In this study, this method was improved by using P507 loaded foam to absorb the interference elements with vibration and in measuring Ag, W and Mo by ICP-MS. The sample was digested by HF, HNO3, HClO4 and reverse aqua regia in an open system. The results of reference materials agree well with the certified values. The detection limits of Ag, W and Mo are 0.0045 μg/g, 0.023 μg/g, 0.060 μg/g, respectively, which are lower than the detection limits of multi-target geochemical exploration (1: 250000). The proposed method is more simple and rapid than the method of P507 levextrel resin and can be used for routine determination of Ag, W, Mo and trace elements in large amounts of geochemical exploration samples.

     

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