全自动消解-电感耦合等离子体质谱法测定环境土壤中13种元素
|
摘要
建立了全自动消解-电感耦合等离子质谱法(ICP-MS)测定环境土壤中13种常见元素的新方法。确定的最佳实验条件如下:采用标准模式测定铅、镍;采用碰撞模式,以氦气流速为3.0 mL/min测定铍、锰、钴、铜、锌、钼、镉、钡、铊、铬、锑。通过内标校正土壤基体干扰,编辑干扰元素校正方程校正质谱干扰,各个元素校准曲线的线性相关系数>0.999 9,方法检出限在0.007～0.5μg/g之间,该方法用土壤标准物质GSS-13进行验证,1.05%～4.91%之间,13种元素的加标回收率89%～127%,各元素的测定值与标准值吻合。以吉林市农用地土壤为实际测定对象,加标回收率88%～134%,利用电感耦合等离子体发射光谱法(ICP-AES)进行仪器比对,结果基本一致。
A new method to determine thirteen elements contents of the soil wass established by the inductively coupled plasma mass spectrometry in this study.The optimal experimental conditions are as follows:lead and nickel were determined by the standard model.Beryllium,manganese,cobalt,copper,zinc,molybdenum,cadmium,barium,thallium,chromium,antimony were determined by the KED model,the helium flow rate was set at 3.0 mL/min.Internal standard was used to matrix correction,and the mass spectrum interference was corrected by means of editting element correction equation. The r value of all the calibration curves was higher than 0.999 9,the detection limit of the method was between 0.007 ～ 0.5 μg/g and RSD was between 1.05% ～ 4.91%,and the recovery rate was 89% ～ 127%.Using the new method to analysis the national standard soil samples of GSS-13,the determination value of each element was consistent with the standard value.The recovery rate of the 13 elements in agricultural soil of Jilin was 88% ～ 134%.It proved that the results by this method were consist with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES).
A new method to determine thirteen elements contents of the soil wass established by the inductively coupled plasma mass spectrometry in this study.The optimal experimental conditions are as follows:lead and nickel were determined by the standard model.Beryllium,manganese,cobalt,copper,zinc,molybdenum,cadmium,barium,thallium,chromium,antimony were determined by the KED model,the helium flow rate was set at 3.0 mL/min.Internal standard was used to matrix correction,and the mass spectrum interference was corrected by means of editting element correction equation. The r value of all the calibration curves was higher than 0.999 9,the detection limit of the method was between 0.007 ～ 0.5 μg/g and RSD was between 1.05% ～ 4.91%,and the recovery rate was 89% ～ 127%.Using the new method to analysis the national standard soil samples of GSS-13,the determination value of each element was consistent with the standard value.The recovery rate of the 13 elements in agricultural soil of Jilin was 88% ～ 134%.It proved that the results by this method were consist with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES).
引文
[1]Anna F S,Marzann K,Edward S.Determination of toxic metals by ICP-MS in Asiatic and European medicinal plants and dietary supplements[J].Journal of Trace Elements in Medicine and Biology,2015,30:54-58.
[2]张更宇,洪涛,薛健,等.全自动消解-电感耦合等离子体质谱法测定土壤中16种元素[J].化工环保,2018,38(2):242-247.
[3]刘静波,张更宇.全自动消解电感耦合等离子体质谱仪测定环境土壤中铍钡铊银[J].分析试验室,2018,37(2):207-211.
[4]Reidy L,Bu K,Godfrey M,et al.Elemental fingerprinting of soils using ICP-MS and multivariate statistics:A study for and by forensic chemistry majors[J].Forensic Science International,2013,233:37-44.
[5]Bora T,Aksoy C.Determination of trace elements in illicit spice samples by using ICP-MS[J].Microchemical Journal,2015,123:179-184.
[6]Pillay A E,Elkadi M,Fok S C,et al.A comparison of trace metal profiles of neem biodiesel and commercial biofuels using high performance ICP-MS[J].Fuel,2012,97:385-389.
[7]张更宇,施云芬,董湘军,等.电热消解-电感耦合等离子体质谱法测定准东煤中15种元素[J].冶金分析,2017,37(6):26-32.
[8]Catalani S,Fostinelli J,Enrica M,et al.Application of a metal free high performance liquid chromatography with inductively coupled plasma mass spectrometry(HPLC-ICP-MS)for the determination of chromium species in drinking and tap water[J].International Journal of Mass Spectrometry,2015,387:31-37.
[9]Cruz S M,Schmidt L,Dalla F M,et al.Microwave-induced combustion method for the determination of trace and ultratrace element impurities in graphite samples by ICP-OES and ICP-MS[J].Microchemical Journal,2015,123:28-32.
[10]张更宇,刘伟,崔世荣,等.分类消解-电感耦合等离子体原子发射光谱法测定环境土壤中15种金属元素含量[J].理化检验-化学分册,2018,54(4):428-432.
[11]张更宇,吴超,邓宇杰.电感耦合等离子体质谱(ICP-MS)联用技术的应用及展望[J].中国无机分析化学,2016,6(3):19-26.
[12]赵小学,赵宗生,王玲玲,等.微波ICP-MS联用快速测定小麦中砷、镉和铅[J].中国测试,2014,40(6):42-44.
[13]吴俊斌,廖建波,吴超飞,等.带ORS的ICP-MS测定沉积物中重金属总量及形态含量方法的优化[J].中国测试,2016,42(5):50-55.
[14]Yong L,Gui L P,Qiang H,et al.Dispersive liquid-liquid microextraction based on the solidification of floating organic drop followed by ICP-MS for the simultaneous determination of heavy metals in wastewaters[J].Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2015,140:156-161.
[15]Donovan A R,Adams C D,Ma Y,et al.Single particle ICP-MS characterization of titanium dioxide,silver,and gold nanoparticles during drinking water treatment[J].Chemosphere,2016,144:148-153.
[16]HJ 168-2010,环境监测分析方法标准制修订技术导则[S].
[17]陈秋生,张强,刘烨潼,等.电感耦合等离子体质谱法同时测定土壤中多种元素含量的研究[J].中国土壤与肥料,2013,(4):97-101.
[18]乐淑葵,段永梅.电感耦合等离子体质谱法(ICP-MS)测定土壤中的重金属元素[J].中国无机分析化学,2015,5(3):16-19.
[19]HJ/T 166-2004,土壤环境监测技术规范[S].
[2]张更宇,洪涛,薛健,等.全自动消解-电感耦合等离子体质谱法测定土壤中16种元素[J].化工环保,2018,38(2):242-247.
[3]刘静波,张更宇.全自动消解电感耦合等离子体质谱仪测定环境土壤中铍钡铊银[J].分析试验室,2018,37(2):207-211.
[4]Reidy L,Bu K,Godfrey M,et al.Elemental fingerprinting of soils using ICP-MS and multivariate statistics:A study for and by forensic chemistry majors[J].Forensic Science International,2013,233:37-44.
[5]Bora T,Aksoy C.Determination of trace elements in illicit spice samples by using ICP-MS[J].Microchemical Journal,2015,123:179-184.
[6]Pillay A E,Elkadi M,Fok S C,et al.A comparison of trace metal profiles of neem biodiesel and commercial biofuels using high performance ICP-MS[J].Fuel,2012,97:385-389.
[7]张更宇,施云芬,董湘军,等.电热消解-电感耦合等离子体质谱法测定准东煤中15种元素[J].冶金分析,2017,37(6):26-32.
[8]Catalani S,Fostinelli J,Enrica M,et al.Application of a metal free high performance liquid chromatography with inductively coupled plasma mass spectrometry(HPLC-ICP-MS)for the determination of chromium species in drinking and tap water[J].International Journal of Mass Spectrometry,2015,387:31-37.
[9]Cruz S M,Schmidt L,Dalla F M,et al.Microwave-induced combustion method for the determination of trace and ultratrace element impurities in graphite samples by ICP-OES and ICP-MS[J].Microchemical Journal,2015,123:28-32.
[10]张更宇,刘伟,崔世荣,等.分类消解-电感耦合等离子体原子发射光谱法测定环境土壤中15种金属元素含量[J].理化检验-化学分册,2018,54(4):428-432.
[11]张更宇,吴超,邓宇杰.电感耦合等离子体质谱(ICP-MS)联用技术的应用及展望[J].中国无机分析化学,2016,6(3):19-26.
[12]赵小学,赵宗生,王玲玲,等.微波ICP-MS联用快速测定小麦中砷、镉和铅[J].中国测试,2014,40(6):42-44.
[13]吴俊斌,廖建波,吴超飞,等.带ORS的ICP-MS测定沉积物中重金属总量及形态含量方法的优化[J].中国测试,2016,42(5):50-55.
[14]Yong L,Gui L P,Qiang H,et al.Dispersive liquid-liquid microextraction based on the solidification of floating organic drop followed by ICP-MS for the simultaneous determination of heavy metals in wastewaters[J].Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2015,140:156-161.
[15]Donovan A R,Adams C D,Ma Y,et al.Single particle ICP-MS characterization of titanium dioxide,silver,and gold nanoparticles during drinking water treatment[J].Chemosphere,2016,144:148-153.
[16]HJ 168-2010,环境监测分析方法标准制修订技术导则[S].
[17]陈秋生,张强,刘烨潼,等.电感耦合等离子体质谱法同时测定土壤中多种元素含量的研究[J].中国土壤与肥料,2013,(4):97-101.
[18]乐淑葵,段永梅.电感耦合等离子体质谱法(ICP-MS)测定土壤中的重金属元素[J].中国无机分析化学,2015,5(3):16-19.
[19]HJ/T 166-2004,土壤环境监测技术规范[S].