快速微波消解-原子荧光光谱法测定土壤砷汞的含量
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摘要
为实现土壤样品中砷、汞元素快速准确检测,本文以国家标准物质GSS-24为实验土壤,对其中消解酸体系、消解程序、过滤方式进行了优化,建立了以HCl-HNO3体系的一套快速、用酸量少、可靠的土壤砷汞微波消解/原子荧光方法。通过对国家标准物质GSS-14、GSS-21、GSS-25土壤的元素进行验证,测定结果与参考值一致。若称样0.5000 g定容到50 ml,确定砷、汞检出限分别为0.009 mg·kg-1和0.002 mg·kg-1,相对标准偏差2.15%~9.31%,样品加标回收率在98.0%~105%。表明该方法具有良好的准确度和精密度,可为环境土样中砷、汞的测定提供了可靠的分析方法。
To achieve fast and accurate dectection of arsenic and mercury in soil,the acid system,digestion procedure and filtration mode were optimized.A fast,low acidity and reliable way is to use the HCl-HNO_3 system,which detects As and Hg in soil by microwave digestion/atomic fluorescence.The accuracy of the method was confirmed by national standard material(GSS-14,GSS-21 and GSS-25). For 0. 5000 g sample diluted to 50 m L,the detection limits of As and Hg were 0. 009 mg·kg-1 and 0. 002 mg·kg-1,respectively.The relative standard deviations were 2. 15% ~ 9. 31%,and the recoveries were 98. 0% ~ 105%. It provides a reliable method for determination of arsenic and mercury in environmental soil samples.
To achieve fast and accurate dectection of arsenic and mercury in soil,the acid system,digestion procedure and filtration mode were optimized.A fast,low acidity and reliable way is to use the HCl-HNO_3 system,which detects As and Hg in soil by microwave digestion/atomic fluorescence.The accuracy of the method was confirmed by national standard material(GSS-14,GSS-21 and GSS-25). For 0. 5000 g sample diluted to 50 m L,the detection limits of As and Hg were 0. 009 mg·kg-1 and 0. 002 mg·kg-1,respectively.The relative standard deviations were 2. 15% ~ 9. 31%,and the recoveries were 98. 0% ~ 105%. It provides a reliable method for determination of arsenic and mercury in environmental soil samples.
引文
[1]薄维平,孔肖肖,陈士新,等.水浴消解-原子荧光法测定土壤中的砷汞[J].环境监控与预警,2016,8(3):34-37.
[2]袁旭,王忻昱.王水(1+1)体系—双道原子荧光光度计同方法、同步测定土壤中的砷、汞[J].生命科学仪器,2008,6(4):45-50.
[3]周婷,张智源.热分解-冷原子吸收法测定土壤中汞[J].环境监测管理与技术,2015,27(6):48-50.
[4]陈垠勇,季晓春.冷原子吸收法测定土壤和沉积物中总汞的影响因素研究[J].资源节约与环保,2016,8:183-183.
[5]陈剑侠,柯毅龙.冷原子吸收法测定土壤中总汞[J].光谱实验室,1997,14(4):20-23.
[6]He P,Luis A C,Diana S A.Determination of total arsenic and speciation in apple juice by liquid chromatography-inductively coupled plasma mass spectrometry:an experiment for the analytical chenmistry laboratory[J].J Chem Educ,2016,93:1939-1944.
[7]田娟娟,杜慧娟,潘秋红,等.电热板消解与密闭罐消解对土壤中49种矿质元素ICP-MS法检测的影响[J].分析测试学报,2009,28(3):319-325.
[8]董贵斌,王玉兰,赵朔.王水分解-电感耦合等离子体质谱法测定土壤中砷镉[J].化学工程师,2015,3:31-33.
[9]谢蔚嵩,陈婷婷,滕明德.微波消解-电感耦合等离子体质谱法测定水系沉积物中砷的含量及其方法比对研究[J].环保科技,2016,22(5):22-25.
[10]林松.微波消解-电感耦合等离子体质谱法同时测定土壤样品中八种重金属元素[J].福建分析测试,2008,17(3):21-23.
[11]李波,崔杰华,刘东波,等.微波消解-氢化物发生原子荧光法同时测定土壤中的砷汞[J].分析试验室,2008,27(7):106-108.
[12]中华人民共和国环保部.土壤和沉积物汞、砷、硒、铋、锑的测定微波消解/原子荧光法,HJ680-2013[S].北京,中国环境科学出版社,2013
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[2]袁旭,王忻昱.王水(1+1)体系—双道原子荧光光度计同方法、同步测定土壤中的砷、汞[J].生命科学仪器,2008,6(4):45-50.
[3]周婷,张智源.热分解-冷原子吸收法测定土壤中汞[J].环境监测管理与技术,2015,27(6):48-50.
[4]陈垠勇,季晓春.冷原子吸收法测定土壤和沉积物中总汞的影响因素研究[J].资源节约与环保,2016,8:183-183.
[5]陈剑侠,柯毅龙.冷原子吸收法测定土壤中总汞[J].光谱实验室,1997,14(4):20-23.
[6]He P,Luis A C,Diana S A.Determination of total arsenic and speciation in apple juice by liquid chromatography-inductively coupled plasma mass spectrometry:an experiment for the analytical chenmistry laboratory[J].J Chem Educ,2016,93:1939-1944.
[7]田娟娟,杜慧娟,潘秋红,等.电热板消解与密闭罐消解对土壤中49种矿质元素ICP-MS法检测的影响[J].分析测试学报,2009,28(3):319-325.
[8]董贵斌,王玉兰,赵朔.王水分解-电感耦合等离子体质谱法测定土壤中砷镉[J].化学工程师,2015,3:31-33.
[9]谢蔚嵩,陈婷婷,滕明德.微波消解-电感耦合等离子体质谱法测定水系沉积物中砷的含量及其方法比对研究[J].环保科技,2016,22(5):22-25.
[10]林松.微波消解-电感耦合等离子体质谱法同时测定土壤样品中八种重金属元素[J].福建分析测试,2008,17(3):21-23.
[11]李波,崔杰华,刘东波,等.微波消解-氢化物发生原子荧光法同时测定土壤中的砷汞[J].分析试验室,2008,27(7):106-108.
[12]中华人民共和国环保部.土壤和沉积物汞、砷、硒、铋、锑的测定微波消解/原子荧光法,HJ680-2013[S].北京,中国环境科学出版社,2013
[13]中华人民共和国环保部.环境监测、分析方法标准制修订技术导则,HJ168-2010[S].北京,中国环境科学出版社,2010
[14]中华人民共和国环保部.土壤环境监测技术规范,HJ/T166-2004[S].北京,中国环境科学出版社,2004.