沉淀分离-电感耦合等离子体质谱法测定方铅矿中铊

• 作 者: 代小吕 董利明 赵欣 孙朝阳 郑存江
• 机 构: 浙江省地质矿产研究所,中国环境监测总站,
• 出 处: 分析试验室
• 发表日期: 2016年03期
• 关键词: 沉淀分离 泡沫塑料 四极杆 检出限 沉淀 样品 清液 稀散元素 拖尾 原子吸收光谱法

当高浓度Pb共存时,采用四极杆ICP-MS测定Tl,由于~(204)Pb、~(206)Pb的强峰拖尾,分别干扰~(203)Tl、~(205)Tl的测定,使测定结果偏高。本文采用样品分解后加入硫酸,使大量Pb以PbSO_4沉淀形式与Tl分离,分取清液稀释后用ICP-MS测定,解决了测定方铅矿中Tl时Pb的干扰问题。方法检出限(3σ)为0.002μg/g,相对标准偏差(n=12)为3.5%~7.5%。通过与传统泡沫塑料吸附富集-石墨炉原子吸收光谱法比对验证,方法准确可靠。

When the high concentration of Pb coexists, the determination of Tl by quadrupole ICP-MS will interfere with the determination of ~ (203) Tl and ~ (205) Tl due to the strong tailing of ~ (204) Pb and ~ , So that the measurement results are high. In this paper, after the sample is decomposed, sulfuric acid is added, so that a large amount of Pb is separated from Tl in the form of PbSO_4 precipitation. The supernatant is diluted and measured by ICP-MS, which solves the problem of Pb interference when determining Pb in galena. The detection limit (3σ) was 0.002 μg / g and the relative standard deviation (n = 12) was 3.5% -7.5%. The method is accurate and reliable by comparison with traditional foam plastic absorption and enrichment - graphite furnace atomic absorption spectrometry.