微波消解-ICP-OES测定石灰石样品中的多种元素

Determination of Multi-Element in Limestone by ICP-OES with Microwave Digestion

采用微波消解预处理石灰石样品,并利用ICP-OES测定石灰石中Si、Ca、Al、Fe、Mg、K、Ti、Sr和Mn等矿物元素含量。以GBW07120和GBW07214a作为石灰石标准物质。对比了HNO3,HNO3/HF和HNO3/HF+H3BO33种不同消解用酸微波消解石灰石样品后对元素回收率的影响。通过检测值与样品标准值的对比,使用HNO3/HF+H3BO3后样品消解最完全。建立了用9mLHNO3和1mLHF分解0.2g石灰石,再加入10mL4%(W/V)的H3BO3中和过量的HF及氟化物沉淀的两步微波加热消解方法。本方法检测2种石灰石标准物质时,元素回收率在88.5%—104.1%之间,RSD均小于3%。

Microwave digestion was applied in the pre-treatment of limestone sample,and the contents of nine mineral elements（Si,Ca,Al,Mg,Fe,K,Ti,Sr and Mn）in limestone were determined by inductively coupled plasma-optical emission spectrometry（ICP-OES）.GBW 07120 and GBW 07214a were used as limestone standard reference materials.The effect of three acids（HNO3,HNO3/HF and HNO3/HF＋H3BO3）on element recovery was studied.The results showed that limestone sample was completely decomposed with HNO3/HF＋H3BO3.This method achieved good recoveries for all elements in the two limestone standard reference materials.The recoveries of nine elements were from 88.5% to 104.1% and all RSD of tests were below 3%.