摘要
采用高压密闭的方式,以5 mL MOS级的硝酸对植物样品进行消解,建立了氢化物发生原子荧光光谱仪测定重金属元素汞的分析方法。本方法具有酸用量少、空白值低、消解完全、污染小等显著优势。通过对Hg空心阴极灯电流、载气流量及屏蔽气流量等参数的优化,确定了最佳仪器条件。方法检出限为0.0012 mg·kg-1,线性相关系数≥0.9999。采用该方法对国家一级标准物质GBW10010、GBW10011、GBW10014、GBW10015进行测定,相对标准偏差(RSD%,n=12)为3.19%~7.57%,相对误差(n=12)为-6.25%~4.31%,方法的回收率为91%~108%。实验表明:高压密闭消解-氢化物原子荧光光谱法测定植物样品中汞的方法,具备操作简便、稳定可靠、空白值低、重现性好、分析速度快、环境友好等优势。该方法已成功应用于大批量植物样品的分析测定。
The method for the determination of heavy metal elemental mercury by hydride generation atomic fluorescence spectrometry was developed by digesting plant samples with 5 mL MOS grade nitric acid under high pressure.This method has the significant advantages of less acid consumption,lower blank value,complete digestion and less pollution.By optimizing the parameters of Hg hollow cathode lamp current,carrier gas flow and shielding gas flow,the optimum instrument conditions were determined.The detection limit of this method is 0.0012 mg·kg-1,and the linear correlation coefficient is≥0.9999.The relative standard deviation(RSD%,n=12)of GBW10010,GBW10011,GBW10014 and GBW10015 are 3.19%~7.57%,the relative error(RE%,n=12)is-6.25%~4.31%,and the recovery rate of the method is 91%~108%.The results showed that the method of determination of mercury in plant samples by high pressure closed digestion and hydride atomic fluorescence spectrometry had advantages of simple operation,good stability and reliability,low blank value,good reproducibility,fast analysis speed and environmental friendliness.The method has been successfully applied in the analysis and determination of large quantities of plant samples.
作者
李艳华
刘军
李鹏程
陈浩凤
辛涛
于亚辉
LI Yan-hua;LIU Jun;LI Peng-cheng;CHEN Hao-feng;XIN Tao;YU Ya-hui(Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Land and Resources,Henan Province Rock and Mineral Testing Center,Zhengzhou 450012,China;Henan Geological and Mineral Exploration and Development Bureau No.1 Geological Exploration Institute,Nanyang 47300,China)
出处
《当代化工》
CAS
2020年第11期2588-2591,共4页
Contemporary Chemical Industry
基金
河南省财政地质科研项目(豫国土资发[2018]98号-10)
关键词
高压密闭消解
氢化物发生
原子荧光
植物
重金属元素
汞
High pressure closed digestion
Hydride generation
Atomic fluorescence
Plant
Heavy metal element
Hg
