4-甲基-2-戊酮萃取分离-电感耦合等离子体质谱法测定高纯硒中17种杂质元素
发布时间：2018-08-30 09:05
【摘要】：利用电感耦合等离子体质谱法(ICP-MS)测定5N~6N(纯度为99.999%~99.999 9%)高纯硒中痕量杂质元素时,硒的基体效应明显,影响结果的准确性。采用硝酸溶解高纯硒,经4-甲基-2-戊酮选择性萃取硒后,对水相进行测定,建立了电感耦合等离子体质谱法测定高纯硒中的Li、Be、B、Sc、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、As、Sr、Cd、Ba、Pb共17种痕量杂质元素的方法。实验表明,萃取时当盐酸浓度为7mol/L、MIBK体积为20mL和萃取时间为2min时,水相中硒的质量浓度低于5mg/L,此时硒基体对测定的影响可忽略。方法中各元素校准曲线的线性关系均大于0.999 5,各待测元素的方法检出限为0.2~7.0ng/g。按照实验方法对高纯硒样品中这17种杂质元素进行测定,测定结果的相对标准偏差(RSD,n=6)在5.0%~11.2%之间,加标回收率在91%~103%之间。
[Abstract]:In the determination of trace impurities in high purity selenium by inductively coupled plasma-mass spectrometry (ICP-MS), the matrix effect of selenium is obvious and the accuracy of the results is affected. A method for the determination of Li,Be,B,Sc,Ti,V,Cr,Mn,Co,Ni,Cu,Zn,As,Sr,Cd,Ba,Pb in high purity selenium by inductively coupled plasma mass spectrometry (ICP-MS) after selective extraction of selenium by 4-methyl-2-pentanone was developed. The results show that when the concentration of hydrochloric acid is 7 mol / L ~ (MIBK) and the extraction time is 2min, the mass concentration of selenium in aqueous phase is less than 5 mg / L, and the effect of selenium matrix on the determination is negligible. The calibration curve of each element is linear more than 0.999, and the detection limit of each element is 0.2ng / g. The relative standard deviation (RSD,n=6) of the 17 impurity elements in high purity selenium samples was between 5.0% and 11.2%, and the recovery rate was between 91% and 103%.
【作者单位】： 成都理工大学;
【分类号】：O657.63;TQ125.2
本文编号：2212619
[Abstract]:In the determination of trace impurities in high purity selenium by inductively coupled plasma-mass spectrometry (ICP-MS), the matrix effect of selenium is obvious and the accuracy of the results is affected. A method for the determination of Li,Be,B,Sc,Ti,V,Cr,Mn,Co,Ni,Cu,Zn,As,Sr,Cd,Ba,Pb in high purity selenium by inductively coupled plasma mass spectrometry (ICP-MS) after selective extraction of selenium by 4-methyl-2-pentanone was developed. The results show that when the concentration of hydrochloric acid is 7 mol / L ~ (MIBK) and the extraction time is 2min, the mass concentration of selenium in aqueous phase is less than 5 mg / L, and the effect of selenium matrix on the determination is negligible. The calibration curve of each element is linear more than 0.999, and the detection limit of each element is 0.2ng / g. The relative standard deviation (RSD,n=6) of the 17 impurity elements in high purity selenium samples was between 5.0% and 11.2%, and the recovery rate was between 91% and 103%.
【作者单位】： 成都理工大学;
【分类号】：O657.63;TQ125.2
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