过氯乙烯滤膜采样测定空气和废气中铀的分析方法研究

摘要/Abstract

摘要： 利用微波消解-ICP-MS法,针对过氯乙烯滤膜采集空气和废气中铀含量的分析,建立了过氯乙烯滤膜微波消解体系。结果表明,优选硝酸作为消解酸溶液,消解程序优化后,本方法铀加标回收率在98.4%～102.0%之间,检出限为2×10^-3 ng/m³(按采样体积10 m³、定容体积50 mL计),检出限的放射性活度浓度为6×10^-8 Bq/m³(以天然铀计)。应用该方法分析实际空气样品中铀含量,相对标准偏差为3.18%。该方法前处理时间短,结果可靠,能够实现空气和废气样品中铀含量的快速、稳定、高效、准确的分析测试。

关键词: 过氯乙烯滤膜, 铀, 微波消解, ICP-MS

Abstract: In this paper, the optimum and most appropriate microwave digestion system was established for the analysis of uranium in air and waste gas samples collected with polyvinyl chloride filter membrane, using a microwave digestion-ICP-MS method. Results showed that, when nitric acid was used as the optimized digestion acid, the uranium standard addition recovery rate was 98.4% to 102.0%, the detection limit was 2×10^-3 ng/m³ (10 m³ of sample volume, 50 mL of constant volume) and radioactivity concentration of uranium detection limit was 6×10^-8 Bq/m³ (based on natural uranium). The uranium content in atmosphere samples was analyzed using the established method and its relative standard deviation (RSD) was 3.18%. Rapid pre-treatment and reliable data were implemented by this method which meets the requirements of fast, stable, efficient and accurate in analysis of the concentration of uranium in air and waste gas samples.

Key words: polyvinyl chloride filter membrane, uranium, microwave digestion, ICP-MS

中图分类号:

O657.4

张晓燕, 张桂芬, 郝悦, 孔淮, 曹昆武. 过氯乙烯滤膜采样测定空气和废气中铀的分析方法研究[J]. 辐射防护, 2021, 41(5): 410-414.

ZHANG Xiaoyan, ZHANG Guifen, HAO Yue, KONG Huai, CAO Kunwu. Research on analysis methods of uranium in air and waste gas samples collected with polyvinyl chloride filter membrane[J]. RADIATION PROTECTION, 2021, 41(5): 410-414.

参考文献

[1] 朱寿彭,李章.放射毒理学[M].苏州:苏州大学出版社,2004:147-165.
[2] 徐颖,尹亮亮,陈飞,等.多级大气颗粒物中超痕量铀的HR-ICP-MS分析方法研究[J].中华放射医学与防护杂志,2017,37(3):212-215.
XU Y,YIN L L,CHEN F,et al.HR-ICP-MS method for the determination of ultratrace uranium in multi-stage atmospheric particles[J].Chin J Radiol Med Prot,2017,37(3):212-215.
[3] Zytoon M A,Aburas H M,Abdulsalam M I.Determination of ⁴⁰K,²³²Th and ²³⁸U activity concentration in ambient PM2.5 aerosols and the associated inhalation effective dose to the public in Jeddah City,Saudi Arabia[J].J Environ Radioact,2014,129:148-156.DOI:10.1016/j.jenvrad.2014.01.003.
[4] 中华人民共和国环境保护部.环境样品中微量铀的分析方法:HJ 840—2017[S].北京:中国环境科学出版社,2017.
[5] 中华人民共和国环境保护部.空气和废气颗粒物中铅等金属元素的测定电感耦合等离子体质谱法:HJ 657—2013[S].北京:中国环境科学出版社,2013.
[6] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.锆及锆合金化学分析方法第14部分铀量的测定极谱法:GB/T 13747.14—2017[S].北京:中国标准出版社,2017.
[7] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.六氟化铀分析方法第6部分铀的测定:GB/T 14501.6—2008[S].北京:中国标准出版社,2008.
[8] 中国市场监督总局,中国国家标准化管理委员会.食品安全国家标准食品中放射性物质天然钍和铀的测定:GB 14883.7—2016[S].北京:中国标准出版社,2016.
[9] 中华人民共和国国家卫生和计划生育委员会.尿中总铀和铀-235/铀-238比值的分析方法电感耦合等离子体质谱法(ICP-MS):WS/T 549—2017[S].北京:中国标准出版社,2017.
[10] 张霖琳,刀谞,王超,等.微波消解ICP-MS法测定空气颗粒物中54种元素[J].环境化学,2014,33(1):154-156.
ZHANG L Y,DAO X,WANG C,et al. Determination of 54 elements in air atmospheric particles by ICP-MS with microwave digestion[J].Environmental Chemistry,2014,33(1):154-156.
[11] 张敏会,王露,徐瑞,等.微波消解-电感耦合等离子体质谱法测定大气PM2.5中金属元素[J].分析试验室,2017,36(7):841-844.
ZHANG M H,WANG L,XU R,et al.Determination of metalelements in PM2.5 by inductively coupled plasma mass spectrometry and microwave digestion[J].Chinese Journal of Analysis Laboratory,2017,36(7):841-844.
[12] 刘宇栋,孙国娟.石墨消解－电感耦合等离子体原子发射光谱法测定废气中锡[J].冶金分析,2016,36(6):60-63.
LIU Y D,SUN G J.Determination of tin in waste gas by inductively coupled plasma atomic emission spectrometry with graphite digestion[J].Metallurgical Analysis,2016,36(6):60-63.
[13] 黎阳明,段学新.大气颗粒物中金属元素测定消解方法浅探[J].环境科学导刊,2016,35(3):105-108.
LI Y M,DUAN X X.Discussion on digestion method for determining metal elements in atmospheric particulate[J].Environmental Science Survey,2016,35(3):105-108.
[14] 谢华林.ICP-AES法测定大气颗粒物中的金属[J].环境科学与技术,2001,(6):25-26.
XIE H L.Determination ofmetals in atmosphere by ICP-AES[J].Environmental Science & Technology,2001,(6):25-26.
[15] 赵晓亮,孙杰,李俊华,等.消解体系对TSP滤膜重金属测定的影响研究[J].环境科学与技术,2017,40(9):83-89.
ZHAO X L,SUN J,LI J H,et al.Effect of microwave digestion systems on the heavy metals determination in TSP colleted by PTFE filter[J]. Environmental Science & Technology,2017,40(9):83-89.
[16] 郭晓爽,杨婧,付强,等.微波消解体系与聚四氟乙烯滤膜对PM2.5中重金属测定的影响[J].中国环境监测,2014,30(4):129-133.
GUO X S,YANG J,FU Q,et al.Effect microwave digestion system and PTFE filter on quantitative research of heavy metals in PM2.5[J].Environmental Monitoring in China,2014,30(4):129-133.
[17] 曹雷,任妍冰,姚远.微波消解ICP-MS法同时测定大气颗粒物中多种痕量元素[J].环境监测管理与技术,2012,24(4):52-55.
CAO L,RENG Y B,YAO Y.Simultaneous determination of trace elemtents in atmospheric particulates by ICP-MS with microwave digestion[J].The Administration and Technique of Environmental Monitoring,2012,24(4):52-55.
[18] 朱奕,葛飞,徐雄飞.微波消解ICP-OES法同时测定总悬浮颗粒物中多种重金属[J].环境科学导刊,2013,32(2):112-115.
ZHU Y,GE F,XU X F.Determination of heavy metals in total suspended particulate by microwave-assisted digestion coupled with plasma spectroscopy(ICP-OES)[J]. Environmental Science Survey,2013,32(2):112-115.
[19] 邓继,陈国海,郑晓红,等.密闭微波消解ICP-AES法测定大气颗粒物中金属元素[J].环境监测管理与技术,2009,21(1):28-30.
DENG J,CHEN G H,ZHENG X H,et al.Determination of metals in atmospheric particles by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].The Administration and Technique of Environmental Monitoring,2009,21(1):28-30.
[20] 杏艳,王舒婷,田渭花,等.大气颗粒物重金属元素消解方法的响应面优化[J].环境保护科学,2019,45(4):114-120.
XING Y,WANG S T,TING W H,et al.Optimization of digestion parameters for heavy metal in atomspheric particles using response surface methodology[J].Environmental Protection Science,2019,45(4):114-120.
[21] 金钦汉.微波化学[M].北京:科学出版社,1999:151-166.