电感耦合等离子体质谱法测定土壤中镉和总汞
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摘要
建立电感耦合等离子质谱法测定土壤中镉和总汞的方法。土壤样品在电热板上用盐酸和硝酸于100℃低温消解,重量法定容,取上清液上机测定。镉和总汞含量分别在0.502~10.20 ng/g,0.212~5.010 ng/g范围内线性良好,相关系数(r2)大于0.999,土壤中镉和总汞的检出限分别为0.021,0.002μg/g,测定结果的相对标准偏差分别为1.99%,5.57%(n=6),加标回收率分别为97.5%~101.1%,87.5%~92.9%。该方法样品处理简单快捷,检出限低,准确度和精密度高,适合土壤中镉和总汞含量的测定。
A method of ICP–MS was established for the determination of cadmium and total mercury in soil. The sample was dissolved at temperature of 100℃ by hydrochloric acid and nitric acid, being dissolved and dilluted to constant volume, and determined by using supernatant fluid. The linear range of cadmium and mercury was 0.502–10.20 ng/g, 0.212–5.010 ng/g, respectively, the correlation coefficients(r~2) were more than 0.999, the detection limits of cadmium and total mercury in soil were 0.021, 0.002 μg/g, respectively. The relative standard deviations of determination results were 1.99%, 5.57%(n=6), and the recoveries were 97.5%–101.1%, 87.5%–92.9% for calnium and total mercury, respectively. The method is simple and easy to process sample, with low detection limit,high accuracy and precision, and it is suitable for the determination of cadmium and total mercury content in soil.
A method of ICP–MS was established for the determination of cadmium and total mercury in soil. The sample was dissolved at temperature of 100℃ by hydrochloric acid and nitric acid, being dissolved and dilluted to constant volume, and determined by using supernatant fluid. The linear range of cadmium and mercury was 0.502–10.20 ng/g, 0.212–5.010 ng/g, respectively, the correlation coefficients(r~2) were more than 0.999, the detection limits of cadmium and total mercury in soil were 0.021, 0.002 μg/g, respectively. The relative standard deviations of determination results were 1.99%, 5.57%(n=6), and the recoveries were 97.5%–101.1%, 87.5%–92.9% for calnium and total mercury, respectively. The method is simple and easy to process sample, with low detection limit,high accuracy and precision, and it is suitable for the determination of cadmium and total mercury content in soil.
引文
[1]李龙,周海燕,张红霞.土壤中总汞元素检测方法研究[J].农村科技,2015(12):32–33.
[2]贾月存,王爱春.微博消解–石墨炉原子吸收光谱法测定土壤中镉[J].环境节约与保护,2014(1):121–121.
[3]陈保冬,赵方杰,张莘.土壤生物与土壤污染研究前沿与展望[J].生态学报,2015,35(20):6 604–6 613.
[4]曾希柏,李莲芳,梅旭荣.中国蔬菜土壤重金属含量及来源分析[J].中国农业科学,2007,40(11):2 507–2 517.
[5]李斌,赵春江.我国当前农产品产地土壤重金属污染形势及检测技术分析[J].农业资源与环境学报,2013,30(5):1–7.
[6]Gray A L,Houk R S,Jarvos K E.Handbook of inductively Coupled Plasma Mass Spectrometry[M].England:Chapman and Hall,1992.
[7]李自强,李小英,钟琦,等.电感耦合等离子体质谱法测定土壤重金属普查样品中铬铜镉铅的关键环节研究[J].矿岩测试,2016,35(1):37–41.
[8]GB/T 17141–1997土壤质量铅、镉的测定石墨炉原子吸收分光光度法[S].
[9]刘彦杰,郭永明.探讨四酸微波消解–石墨炉原子吸收光谱法测定土壤中镉的方法[J].临床医药文献电子杂志,2015,2(14):2 725–2 725.
[10]孙仓.土壤中总汞的不同测定方法对比分析研究[J].环境科学管理,2016,41(6):146–148.
[11]李龙,周海燕,张红霞.土壤中总汞元素检测方法研究[J].农村科技,2015(12):32–33.
[12]高小青,漆晓旭.直接测汞仪测定土壤中总汞的方法研究[J].甘肃科技,2012,28(11):41–43.
[13]HJ 680–2013土壤和沉积物汞、砷、硒、铋、锑的测定微波消解/原子荧光法[S].
[14]GB/T 22105.1–2008土壤质量总汞、总砷、总铅的测定原子荧光法第一部分:土壤中总汞的测定[S].
[15]冯艳红,王国庆,应蓉蓉.土壤中总汞测定的预处理方法探讨[J].环境科学与技术,2014(9):87–91.
[16]王瑞芬,赵智勇,高簌玲.土壤中镉的测定[J].微量元素与健康研究,2014,5(3):76–77.
[17]李百灵,周健,申治国,等.ICP–AES和ICP–MS法测定大米中的微量元素[J].光谱实验室,2002,19(3):420–422.
[18]黄丽娟,林文业,黄一帆,等.ICP–MS等离子体质谱法测定土壤中铬镍铜锌砷镉铅元素含量[J].大众科技,2011,5(1):102–103.
[19]樊欢,张飞,朱欢.热分解汞齐化原子吸收法快速测定土壤中总汞的探讨[J].环境与发展,2013(7):130–133.
[2]贾月存,王爱春.微博消解–石墨炉原子吸收光谱法测定土壤中镉[J].环境节约与保护,2014(1):121–121.
[3]陈保冬,赵方杰,张莘.土壤生物与土壤污染研究前沿与展望[J].生态学报,2015,35(20):6 604–6 613.
[4]曾希柏,李莲芳,梅旭荣.中国蔬菜土壤重金属含量及来源分析[J].中国农业科学,2007,40(11):2 507–2 517.
[5]李斌,赵春江.我国当前农产品产地土壤重金属污染形势及检测技术分析[J].农业资源与环境学报,2013,30(5):1–7.
[6]Gray A L,Houk R S,Jarvos K E.Handbook of inductively Coupled Plasma Mass Spectrometry[M].England:Chapman and Hall,1992.
[7]李自强,李小英,钟琦,等.电感耦合等离子体质谱法测定土壤重金属普查样品中铬铜镉铅的关键环节研究[J].矿岩测试,2016,35(1):37–41.
[8]GB/T 17141–1997土壤质量铅、镉的测定石墨炉原子吸收分光光度法[S].
[9]刘彦杰,郭永明.探讨四酸微波消解–石墨炉原子吸收光谱法测定土壤中镉的方法[J].临床医药文献电子杂志,2015,2(14):2 725–2 725.
[10]孙仓.土壤中总汞的不同测定方法对比分析研究[J].环境科学管理,2016,41(6):146–148.
[11]李龙,周海燕,张红霞.土壤中总汞元素检测方法研究[J].农村科技,2015(12):32–33.
[12]高小青,漆晓旭.直接测汞仪测定土壤中总汞的方法研究[J].甘肃科技,2012,28(11):41–43.
[13]HJ 680–2013土壤和沉积物汞、砷、硒、铋、锑的测定微波消解/原子荧光法[S].
[14]GB/T 22105.1–2008土壤质量总汞、总砷、总铅的测定原子荧光法第一部分:土壤中总汞的测定[S].
[15]冯艳红,王国庆,应蓉蓉.土壤中总汞测定的预处理方法探讨[J].环境科学与技术,2014(9):87–91.
[16]王瑞芬,赵智勇,高簌玲.土壤中镉的测定[J].微量元素与健康研究,2014,5(3):76–77.
[17]李百灵,周健,申治国,等.ICP–AES和ICP–MS法测定大米中的微量元素[J].光谱实验室,2002,19(3):420–422.
[18]黄丽娟,林文业,黄一帆,等.ICP–MS等离子体质谱法测定土壤中铬镍铜锌砷镉铅元素含量[J].大众科技,2011,5(1):102–103.
[19]樊欢,张飞,朱欢.热分解汞齐化原子吸收法快速测定土壤中总汞的探讨[J].环境与发展,2013(7):130–133.