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

采用HNO_3-HF-HClO_4消解体系,建立了全自动消解-电感耦合等离子体质谱仪测定土壤中~(75)As、~9Be、~(51)V、~(55)Mn、~(59)Co、~(60)Ni、~(63)Cu、~(66)Zn、~(98)Mo、~(111)Cd、~(138)Ba、~(205)Tl、~(208)Pb、~(107)Ag、~(52)Cr、~(121)Sb等16种元素的新方法。通过碰撞池技术和编辑干扰元素校正方程有效校正了质谱干扰,并用内标校正了土壤基体干扰。用土壤标准物质GSS-13验证该方法,其校准曲线相关系数大于0.999 9,方法检出限在0.005~0.5μg/g之间,RSD为0.22%~2.35%,加标回收率为92%~114%。采用该方法测定实际土壤样品,加标回收率为93%~123%。

Determination of sixteen elements in soil by inductively coupled plasma mass spectrometry with full-automatic digestion

With HNO₃-HF-HClO₄ digestion system,a new method of full-automatic digestion-inductively coupled plasma mass spectrometry （ICP-MS ）was established for determination of 16 elements in soil,such as ⁷⁵As,⁹Be,⁵¹V,⁵⁵Mn,⁵⁹Co,⁶⁰Ni,⁶³Cu,⁶⁶Zn,⁹⁸Mo,¹¹¹Cd,¹³⁸Ba,²⁰⁵Tl,²⁰⁸Pb,¹⁰⁷Ag,⁵²Cr,¹²¹Sb,and so on. The MS interference was corrected by collision cell technology（ CCT）and editing element correction equation,and the interference of matrix elements in soil was corrected with internal standard. The new method was confirmed using the national standard soil samples of GSS-13 with more than 0.999 9 of correlation coefficient of the calibration curve,0.005-0.5 μg/g of detection limit,0.22%-2.35% of RSD and 92%-114% of recovery rate. When actual soil sample was determined by this method,the recovery rate was 93%-123%.