【引用本文】 黄靖, 王英滨, 周冠轩, 等. 微波消解-电感耦合等离子体发射光谱法测定粉煤灰中的镓[J]. 岩矿测试, 2020, 39(1): 92-98. doi: 10.15898/j.cnki.11-2131/td.201905190065
HUANG Jing , WANG Ying-bin , ZHOU Guan-xuan , et al. Determination of Gallium in Coal Fly Ash with Microwave Digestion and Inductively Coupled Plasma Optical Emission Spectrometry[J]. Rock and Mineral Analysis, 2020, 39(1): 92-98. doi: 10.15898/j.cnki.11-2131/td.201905190065

微波消解-电感耦合等离子体发射光谱法测定粉煤灰中的镓

中国地质大学(北京)数理学院, 北京 100083

收稿日期: 2019-05-19  修回日期: 2019-09-01 

基金项目: 中国神华科学技术研究院合作研究基金(3-4-2014-140)

作者简介: 黄靖,硕士研究生,化学专业。E-mail:2019170017@cugb.edu.cn。。

Determination of Gallium in Coal Fly Ash with Microwave Digestion and Inductively Coupled Plasma Optical Emission Spectrometry

School of Science, China University of Geosciences(Beijing), Beijing 100083, China

Received Date: 2019-05-19
Revised Date: 2019-09-01

摘要:粉煤灰中镓元素含量为12~230μg/g,测定粉煤灰中的镓对实现粉煤灰高附加值利用具有重要的意义。传统敞口酸溶法作为样品的预处理方法存在局限性,如需使用大量氢氟酸,对分析仪器腐蚀大,溶样时间长,在开放容器中易造成元素损失和环境污染。微波消解法具有消解完全、元素损失量少、消解时间短等优点,可以有效解决酸溶法的不足。本文选取内蒙古某电厂采集的粉煤灰,采用硝酸-氢氟酸-盐酸-高氯酸微波消解法对粉煤灰样品进行预处理,电感耦合等离子体发射光谱法测定元素含量。结果表明:使用硝酸-氢氟酸-盐酸-高氯酸(5:1:5:1),消解温度190℃,消解时间30min,微波功率1400W时,镓被浸出完全。方法检出限为0.004mg/L,精密度为1.7%,加标回收率为95.1%~100.9%。本方法在体系中引入盐酸,减少了氢氟酸的用量,显著缩短了除氟时间,降低了对分析仪器的损害,且操作方便,可应用于粉煤灰中微量元素镓的测定。

关键词: 粉煤灰, , 微波消解, 硝酸-氢氟酸-盐酸-高氯酸, 电感耦合等离子体发射光谱法

Determination of Gallium in Coal Fly Ash with Microwave Digestion and Inductively Coupled Plasma Optical Emission Spectrometry

KEY WORDS: coal fly ash, gallium, microwave digestion, nitric acid-hydrofluoric acid-hydrochloric acid-perchloric acid, inductively coupled plasma-optical emission spectrometry

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微波消解-电感耦合等离子体发射光谱法测定粉煤灰中的镓

黄靖, 王英滨, 周冠轩, 马真乾