微波消解-电感耦合等离子体发射光谱法同时测定煤飞灰中6种主要元素  

Determination of 6 Main Elements in Coal Fly Ash by Microwave Digestion-Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：包倩倩 张勤 冯向东 Bao Qianqian;Zhang Qin;Feng Xiangdong(Zhejiang Energy Group P&DCo.,Ltd.,Hngzhou 311121;Key Research Laboratory of High Eficiency Energy Saving and Polutant Contro1 Technology in Thermal Power Generation of Zhejiang Province,Hangzhou 311121;Zhejiang Zheneng Lanxi Power Co.,Ltd.,Lanxi 321100,China)

机构地区：[1]浙江浙能技术研究院有限公司,浙江杭州311121 [2]浙江省火力发电高效节能与污染物控制技术研究重点实验室,浙江杭州311121 [3]浙江浙能兰溪发电有限责任公司,浙江兰溪321100

出　　处：《广东化工》2021年第9期270-271,229,共3页Guangdong Chemical Industry

摘　　要：对不同消解温度和HNO3+HF、HNO3+HCl+HF两种酸体系及用量进行考察,建立了一种微波消解-电感耦合等离子体发射光谱法同时测定飞灰中6种主要元素Al、Ca、Mg、Fe、Mn、Si的分析方法。试样微波消解的程序为:取0.1 g飞灰试样,加入5 mL HNO3、1 mL HCl和1 mL HF,15 min加热到155℃保持30 min,冷却后再加入10 mL 5%(W/V)H3BO3溶液进行第二步消解,消解程序同第一步。溶液定容至100m L,取上清液上机测定。该方法测定煤飞灰标准物质GBW08401中6种主要元素,结果与标准值基本一致。该方法用酸量少,消解温度低,准确度高,加标回收率在92.43%~101.03%之间,各元素检测的RSD均小于5%。The different digestion temperature, HNO3+HF, HNO3+HCl+HF two acid systems and their dosages were investigated, and a microwave digestion-inductively coupled plasma emission spectrometry method was established to simultaneously determine the six main elements Al, Ca, Analysis methods of Mg, Fe, Mn, Si. The procedure for microwave digestion of the sample is as follows: take a 0.1 g fly ash sample, add 5 mL HNO3, 1 mL HCl and 1 mL HF, heat it to 155 ℃ for 15 minutes for 30 minutes, and then add 10 mL 5 %(W/V) H3 BO3 solution after cooling. Perform the second step of digestion, the digestion procedure is the same as the first step. The volume of the solution was adjusted to 100 mL, and the supernatant was taken on the machine for determination. This method is used to determine the six main elements in coal fly ash standard material GBW08401, and the results are basically consistent with the standard values. This method uses less acid, has low digestion temperature and high accuracy. The recovery rate of standard addition is between 92.43 % and 101.03 %, and the RSD of each element detection is less than 5 %.

关 键 词：微波消解 电感耦合等离子体发射光谱 飞灰 主要元素 

分 类 号：TQ[化学工程]