HNO_3-HClO_4消解-电感耦合等离子体质谱法测定粪肥中27种元素

Simultaneous determination of 27 trace elements in manure by HNO_3-HClO_4 digestion-inductively coupled plasma mass spectrometry method

建立了电感耦合等离子体质谱仪(ICP-MS)测定粪肥中微量元素的分析方法。采用HNO_3-HClO_4[V(HNO_3)∶V(HClO_4)=3∶1]体系消解样品,利用普通/ORS混合模式-电感耦合等离子体质谱仪(ICP-MS)测定粪肥中Li、Be、Al、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Se、Sr、Mo、Ag、Cd、Sn、Sb、Te、Ba、Tm、Tl、Pb、U等27种微量元素。经标准物质和加标样品检测验证表明,测定结果与推荐值(或加标值)基本相符,回收率为80. 2%～112. 5%,相对标准偏差RSD<10%。27种元素的检测限(LOD)为0. 1～48. 3 mg/kg。该方法适用于实验室开展粪肥中27种微量元素的同步检测。

This paper describes a validation process for the simultaneous determination of 27 elements including Li,Be,Al,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,As,Se,Sr,Mo,Ag,Cd,Sn,Sb,Te,Ba,Tm,Tl,Pb and U in manure samples by inductively coupled plasma mass spectrometry( ICP-MS) with octopole reaction system( ORS).Several criteria such as sample digestion condition,method linearity and limits of detection( LOD) are evaluated. A standard reference material and some spiked test samples are analyzed,and the recovery varies from 80. 2% to 112. 5%. Relative standard deviations RSD for this method are less than 10%.Limits of detection for 27 elements are obtained within the range of 0. 1 mg·kg-1( V,etc) to 48. 3 mg·kg-1( Fe).Results indicate that this method can be used in the laboratory for the routine determination of these 27 essential and nonessential elements in manure fertilizers.