论文部分内容阅读
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%。
Limestone samples were pretreated by microwave digestion and the mineral elements such as Si, Ca, Al, Fe, Mg, K, Ti, Sr and Mn in limestone were determined by ICP-OES. GBW07120 and GBW07214a as limestone standard material. The effects of HNO3, HNO3 / HF and HNO3 / HF + H3BO3 on the elemental recoveries of different digestion acid microwave digestion limestone samples were compared. By comparing the measured value with the standard value of the sample, the sample digestion is the most complete after using HNO3 / HF + H3BO3. A two-step microwave-assisted digestion method was established for the decomposition of 0.2g limestone with 9mL HNO3 and 1mL HF followed by the addition of 10mL4% (w / v) H3BO3 to neutralize excess HF and fluoride precipitation. The method of detecting two kinds of limestone reference material, the elemental recovery rate between 88.5% -104.1%, RSD were less than 3%.