不同酸体系对微波消解法测量燃煤副产物中痕量元素的影响

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清华大学辅仁网/2017-07-07

朱振武, 禚玉群

清华大学热科学与动力工程教育部重点实验室, 北京 100084

Effect of acid systems for determination of trace elements in coal combustion byproductsusing microwave digestion method

ZHU Zhenwu, ZHUO Yuqun

Key Laboratory for Thermal Science and Power Engineering of Ministry of Education, Tsinghua University, Beijing 100084, China

摘要:

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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-H₃BO₃ 3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。

关键词 ：痕量元素,脱硫石膏,飞灰,微波消解,ICP-MS

Abstract：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-HCl 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-H₃BO₃ 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-H₃BO₃ followed by ICP-MS analysis.

Key words：trace element flue gas desulfurization (FGD) gypsum fly ash microwave digestion inductively coupled plasma mass spectrometry (ICP-MS)

收稿日期: 2015-12-04 出版日期: 2016-10-25

ZTFLH:

X773

通讯作者:禚玉群,教授,E-mail:zhuoyq@tsinghua.edu.cnE-mail: zhuoyq@tsinghua.edu.cn

引用本文:

朱振武, 禚玉群. 不同酸体系对微波消解法测量燃煤副产物中痕量元素的影响[J]. 清华大学学报（自然科学版）, 2016, 56(10): 1072-1078.
ZHU Zhenwu, ZHUO Yuqun. Effect of acid systems for determination of trace elements in coal combustion byproductsusing microwave digestion method. Journal of Tsinghua University(Science and Technology), 2016, 56(10): 1072-1078.

链接本文:

http://jst.tsinghuajournals.com/CN/10.16511/j.cnki.qhdxxb.2016.22.041或 http://jst.tsinghuajournals.com/CN/Y2016/V56/I10/1072

图表:

表１标准微波消解程序

表２燃煤副产物微波消解程序

表３ ICP-MS测量的定量限

表４ FGD-2脱硫石膏标准物质ICP-MS测量结果

表５ GBW 08401飞灰标准物质ICP-MS测量结果

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