石墨消解-原子荧光法同时测定水中砷汞硒
Simultaneous determination of arsenic,mercury and selenium in water by graphite digestion and atomic fluorescence method
林锦忠 1张鑫 1丁友明 1任智宏 2黄婵3
作者信息
- 1. 德阳市旌阳区疾病预防控制中心检验科,四川德阳 618000
- 2. 德阳市疾病预防控制中心检验科,四川德阳 618000
- 3. 成都大学基础医学院,四川成都 610106
- 折叠
摘要
目的 建立石墨消解-三通道原子荧光一次样品消解一次进样同时测定水中砷、汞、硒的方法.方法 以K2Cr2O7-HNO3-HClO4为消解液,石墨消解仪消解水样,三通道原子荧光同时测定水中砷、汞、硒,标准曲线法定量,测定结果与国标方法进行比较.结果 本方法检测水中砷、硒浓度为1.0～20.0 μg/L,汞为0.10～2.00 μg/L,曲线相关系数均＞0.999 0;检出限分别为砷0.064 μg/L、汞0.030 μg/L、硒0.051 μg/L,相对标准偏差分别为砷2.95％、汞1.13％、硒1.34％,质控样品测定均值与标准值的相对偏差分别为砷3.37％、汞2.93％、硒-3.39％,加标实验平均回收率分别为砷97.3％、汞99.9％、硒103.3％;配对t检验对2种方法的样品测定结果进行比较,差异均无统计学意义(均P＞0.05).结论 所建立的方法能较好的提高工作效率,减少化学试剂用量.方法 的曲线线性、检出限、精密度、准确度、样品测定结果均能满足国标方法要求,具有一定的实用价值.
Abstract
Objective To establish a method for simultaneous determination of arsenic,mercury and selenium in water by graphite digestion and three channel atomic fluorescence spectrometry.Methods K2Cr2O7-HNO3-HClO4 was used as the digestion solution,and the water sample was digested by graphite digester.Arsenic,mercury and selenium were simultaneously determined in water by three-channel atomic fluorescence method,quantified by standard curve method and the results were compared with the national standard method.Results In this method,arsenic and selenium were in the range of 1.0-20.0 μg/L,mercury was in the range of 0.10-2.00 μg/L,the correlation coefficients of standard curve were all greater than 0.999 0.The detection limits were 0.064 μg/L for arsenic,0.030 g/L for mercury and 0.051 μg/L for selenium.The relative standard deviations were 2.95％for arsenic,1.13％for mercury,and 1.34％for selenium.The relative deviations between the mean value of quality control samples and the standard value were 3.37％for arsenic,2.93％for mercury,and-3.39％for selenium.The average recoveries in the spiking experiment were 97.3％for arsenic,99.9％for mercury,and 103.3％for selenium.Paired t-test was used to compare the sample determination results of the two methods,and there was no statistical significance(all P＞0.05).Conclusions The method can improve the working efficiency and reduce the amount of chemical reagents.The curve linearity,detection limit,precision,accuracy and sample determination results of the method all meet the requirements of the national standard method,and having certain practical value.
关键词
砷汞硒/同时测定/原子荧光法/石墨消解/水质Key words
Arsenic,mercury and selenium/Simultaneous determination/Atomic fluorescence/Graphite digestion/Water quality引用本文复制引用
出版年
2024
NETL
NSTL
万方数据