王水水浴消解-原子荧光法测定土壤中的砷和汞
|
摘要
采用王水水浴消解-原子荧光法测定土壤样品中砷和汞,探讨消解环境、载液特性、溶液基体和还原剂硼氢化钾等因素对土壤样品中砷和汞含量测定的影响,确定了最优分析条件:土壤样品敞开消解,时间2h,期间摇动3次,用盐酸溶液(5+95)定容,混匀静置过夜,砷和汞还原剂硼氢化钾的质量分数分别为2%和0.02%,载液均为盐酸溶液(5+95)。该方法将土壤环境监测样品中砷、汞元素同步消解前处理,简化了试验步骤,节约了分析测试时间,提高了分析效率,利于处理大批量土壤样品。选取部分GSS系列标准物质进行测试试验,试验结果的精密度和准确度均可满足土壤环境监测技术规范的要求,对2种未知土壤样品进行加标回收试验,土壤样品的加标回收率:砷为94.00%～100.40%,汞为86.40%～106.80%。
This paper analyzes the factors influencing the determination of arsenic and mercury in soil samples by Aqua Regia in Water Bath-Atomic Fluorescence Spectrometry(AFS),discusses the effect of digestion environment,carrier charactevistics,solution matrix and reductant on the determination of arsenic and mercury in soil samples,and determines the optimal analytical conditions as follows:open digestion of soil samples,time 2 h,shaking 3 times during the period.Then the volume is adjusted to a constant volume with hydrochloric acid solution(5+95),mixing and staying overnight and the mass fractions of arsenic and mercury reducing agents potassium borohydride are 2% and 0.02%,respectively.The method pre-processes the arsenic and mercury elements,simplifies the test procedure,saves the analysis and test time of the environmental monitoring sample,improves the analysis efficiency,and is convenient for processing large-volume soil samples.The paper selects some GSS series standard materials for testing.The precision and accuracy of the test results can meet the requirements of soil environmental monitoring technical specifications,and then the paper spikes and recovers two kinds of unknown soil samples with the following weighted recovery rate:arsenic is 94.00%～100.40%,and mercury is 86.40%～106.80%.
This paper analyzes the factors influencing the determination of arsenic and mercury in soil samples by Aqua Regia in Water Bath-Atomic Fluorescence Spectrometry(AFS),discusses the effect of digestion environment,carrier charactevistics,solution matrix and reductant on the determination of arsenic and mercury in soil samples,and determines the optimal analytical conditions as follows:open digestion of soil samples,time 2 h,shaking 3 times during the period.Then the volume is adjusted to a constant volume with hydrochloric acid solution(5+95),mixing and staying overnight and the mass fractions of arsenic and mercury reducing agents potassium borohydride are 2% and 0.02%,respectively.The method pre-processes the arsenic and mercury elements,simplifies the test procedure,saves the analysis and test time of the environmental monitoring sample,improves the analysis efficiency,and is convenient for processing large-volume soil samples.The paper selects some GSS series standard materials for testing.The precision and accuracy of the test results can meet the requirements of soil environmental monitoring technical specifications,and then the paper spikes and recovers two kinds of unknown soil samples with the following weighted recovery rate:arsenic is 94.00%～100.40%,and mercury is 86.40%～106.80%.
引文
[1]Sánchez R D,Corns W T,Chen B,et al.Atomic Fluorescence Spectrometry:A suitable detection technique in speciation studies for arsenic,selenium,antimony and mercury[J].Journal of Analytical Atomic Spectrometry,2010,25(1):933-946.
[2]陈泽智,赵志南,何群华.王水回流消解同时测定土壤/沉积物中汞、砷和镉的方法研究[J].广东工业大学学报,2018,35(1):84-87.
[3]中国环境监测总站.土壤环境监测技术规范:HJ/T 166-2004[S].中国环境出版社,2004.
[4]祝正辉.原子荧光光谱法测定土壤中的砷和汞[J].理化检验-化学分册,2015,51(7):952-954.
[5]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.
[6]李彩虹,杨春霞,赵银宝.氢化物发生-原子荧光法测定土壤中砷、汞的方法[J].西北农业学报,2013,22(7):200-204.
[7]杨海霞,汝少国,王震宇,等.原子荧光法同时测定海产品中的砷、汞[J].环境科学与技术,2012,35(61):248-251.
[8]顾涛,赵信文,王节涛,等.某水稻田水-土-植物系统中镉、汞、砷元素的分布特征研究[J].安全与环境工程,2017,24(6):70-75.
[9]刘欢欢,徐云龙,赵杰.水浴消解和微波消解-原子荧光法测定土壤中汞和砷的研究[J].安徽农业科学,2015,43(16):90-92.
[10]杨金星,徐勇,刘永静,等.微波消解石墨炉原子吸收光谱法测定日本遗弃化学武器污染样品中总砷[J].分析试验室,2018,37(5):519-523.
[11]Long Z,Xin J,Hou X.Determination of arsenic and mercury in Chinese medicinal herbs by atomic fluorescence spectrometry with closed-vessel microwave digestion[J].Spectroscopy Letters,2004,37(5):263-274.
[12]刘凤枝,刘岩,蔡彦明,等.土壤质量总汞、总砷、总铅的测定原子荧光法第1部分:土壤中总汞的测定:GB/T 22105.1-2008[S].北京:中国标准出版社,2008.
[13]刘凤枝,刘岩,蔡彦明,等.土壤质量总汞、总砷、总铅的测定原子荧光法第2部分:土壤中总砷的测定:GB/T 22105.2-2008[S].北京:中国标准出版社,2008.
[14]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(5):106-108.
[15]袁爱萍,唐艳霞,黄玉龙,等.氢化物-原子荧光法测定锑精矿中痕量砷、汞的研究[J].光谱学与光谱分析,2006,26(8):1553-1556.
[16]李刚.HG-AFS仪双道测定铋汞时的光谱干扰及其消除[J].矿物岩石,2000,20(3):102-104.
[17]郭小伟,李立.氢化物-原子吸收和原子荧光法中的干扰及其消除[J].分析化学,1986,14(2):151-158.
[18]吕运开,孙汉文,张德强.氢化物发生-原子荧光光谱分析中的干扰机理[J].河北大学学报(自然科学版),1998,18(S1):31-36.
[2]陈泽智,赵志南,何群华.王水回流消解同时测定土壤/沉积物中汞、砷和镉的方法研究[J].广东工业大学学报,2018,35(1):84-87.
[3]中国环境监测总站.土壤环境监测技术规范:HJ/T 166-2004[S].中国环境出版社,2004.
[4]祝正辉.原子荧光光谱法测定土壤中的砷和汞[J].理化检验-化学分册,2015,51(7):952-954.
[5]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.
[6]李彩虹,杨春霞,赵银宝.氢化物发生-原子荧光法测定土壤中砷、汞的方法[J].西北农业学报,2013,22(7):200-204.
[7]杨海霞,汝少国,王震宇,等.原子荧光法同时测定海产品中的砷、汞[J].环境科学与技术,2012,35(61):248-251.
[8]顾涛,赵信文,王节涛,等.某水稻田水-土-植物系统中镉、汞、砷元素的分布特征研究[J].安全与环境工程,2017,24(6):70-75.
[9]刘欢欢,徐云龙,赵杰.水浴消解和微波消解-原子荧光法测定土壤中汞和砷的研究[J].安徽农业科学,2015,43(16):90-92.
[10]杨金星,徐勇,刘永静,等.微波消解石墨炉原子吸收光谱法测定日本遗弃化学武器污染样品中总砷[J].分析试验室,2018,37(5):519-523.
[11]Long Z,Xin J,Hou X.Determination of arsenic and mercury in Chinese medicinal herbs by atomic fluorescence spectrometry with closed-vessel microwave digestion[J].Spectroscopy Letters,2004,37(5):263-274.
[12]刘凤枝,刘岩,蔡彦明,等.土壤质量总汞、总砷、总铅的测定原子荧光法第1部分:土壤中总汞的测定:GB/T 22105.1-2008[S].北京:中国标准出版社,2008.
[13]刘凤枝,刘岩,蔡彦明,等.土壤质量总汞、总砷、总铅的测定原子荧光法第2部分:土壤中总砷的测定:GB/T 22105.2-2008[S].北京:中国标准出版社,2008.
[14]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(5):106-108.
[15]袁爱萍,唐艳霞,黄玉龙,等.氢化物-原子荧光法测定锑精矿中痕量砷、汞的研究[J].光谱学与光谱分析,2006,26(8):1553-1556.
[16]李刚.HG-AFS仪双道测定铋汞时的光谱干扰及其消除[J].矿物岩石,2000,20(3):102-104.
[17]郭小伟,李立.氢化物-原子吸收和原子荧光法中的干扰及其消除[J].分析化学,1986,14(2):151-158.
[18]吕运开,孙汉文,张德强.氢化物发生-原子荧光光谱分析中的干扰机理[J].河北大学学报(自然科学版),1998,18(S1):31-36.