摘要
微波消解法是测定飞灰和脱硫石膏等燃煤副产物中痕量元素含量的常用前处理方法。该文对现有微波消解方法进行总结分析,基于美国环保局Method 3052标准消解程序,研究了HNO3、HNO3-HCl和HNO3-HF-H3BO33种酸体系对脱硫石膏标准物质（FGD-2）的消解,采用电感耦合等离子质谱仪对As、Be、Cd、Co、Cr、Mn、Pb和Se含量进行测量,结果表明：采用HNO3-HF-H3BO3消解效果最好,Cr、Mn、Se等元素的回收率分别为93.5%、88.0%、97.7%。采用该方法对飞灰标准物质（GBW 08401）进行消解,As、Co、Cr、Mn、Pb和Se等元素的回收率也在90.6%~101.8%,Be和Cd的回收率较差。建立了采用HNO3-HF-H3BO3进行微波消解后,通过电感耦合等离子质谱仪测量燃煤副产物中痕量元素含量的方法。
Microwave digestion is the most common method for pretreating coal fly ash and flue gas desulfurization （FGD） gypsum before determination of the trace elements in the flow streams. This study analyzes previous microwave digestion methods. Then, the standard microwave digestion method 3052 from the US Environment Protection Agency is used to design three acid systems using HNO3, HNO3-HC1 and HNO3-HF-H3BO3 for digesting certified reference gypsum material （FGD-2）. After digestion, the As, Be, Cd, Co, Cr, Mn, Pb and Se contents are determined using inductively coupled plasma mass spectrometry （ICP-MS）. The results show that HNO3-HF-HaBOa gives the best digestion. The Cr, Mn and Se recoveries are 93.5%, 88.0% and 97.7%. Tests using a fly ash （GBW 08401） reference material also show good results with the As, Co, Cr, Mn, Pb and Se recoveries between 90.6% and 101.8%, but the Be and Cd recoveries are not good enough. This method can be used to determine the trace elements in coal fly ash and FGD gypsum by microwave digestion with HNO3-HF-H3 BO3 followed by ICP-MS analysis.
作者
朱振武
禚玉群
ZHU Zhenwu ZHUO Yuqun(Key Laboratory for Thermal Science and Power Engineering of Ministry of Education, Tsinghua University, Beijing 100084, China)
出处
《清华大学学报（自然科学版）》
EI
CAS
CSCD
北大核心
2016年第10期1072-1078,共7页
Journal of Tsinghua University(Science and Technology)
基金
国家自然科学基金项目(51376109)
关键词
痕量元素
脱硫石膏
飞灰
微波消解
ICP-MS
trace element
flue gas desulfurization （FGD） gypsum
fly ash
microwave digestion
inductively coupled plasmamass spectrometry （ICP-MS）
作者简介
朱振武（1989-），男，博士研究生。
通信作者：禚玉群，教授，E-mail：zhuoyq@tsinghua．edu．cn
