微波消解ICP-MS测试大理岩中的锆和铪

Determination of Zirconium and Hafnium in the Marble by Microwave Digestion and ICP- MS Test

提出了地质中大理岩样品通过加入盐酸与硝酸后用微波消解,经过微波消解溶解好的样品用电感耦合等离子质谱仪测试得到锆和铪含量的方法。为了验证方法的可靠性,本方法进行了加标回收实验,得到锆的回收率在99.9%~101.60%,铪的回收率在96.8%~102.8%。通过检出限实验得到锆的检出限为0.001μg/g,铪的检出限为0.02μg/g。进行了样品前处理方法的选择;进行了分析元素适用质量数的选择;进行了消解试剂的选择;进行了国家标准样品分析,RSD在5%以内。

The geological marble samples by adding hydrochloric acid and nitric acid with microwave digestion and after microwave digestion dissolved samples with inductively coupled plasma mass spectrometry test method of zirconium and hafnium content. The reliability of the method was validated,the method was determined in standard addition recovery experiments,zirconium recovery was in the 99. 9% ~ 101. 60%,hafnium recovery rate was in the 96. 8% ~102. 8%. The detection limit obtained zirconium detection limit was 0. 001 μg / g,the detection limit was 0. 02 μg / g hf.The selection of sample pretreatment method was carried out,the selection of the number of the applicable mass of elements was analyzed,and the selection of digestion reagent was carried out. The analysis of the national standard sample was carried out,and the RSD was less than 5%.