微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定土壤中11种金属元素

称取0.25 g样品加入5ml硝酸和2ml氢氟酸，用微波消解技术对样品进行前处理。以Re作为As、Pb、Tl的内标，Rh作为Cd、Co、Cr、Ni的内标，Bi作为Be、Cu、Zn的内标，Tb作为V的内标，建立了KED模式下可同时测定土壤中Be、As、Cd、Co、Cr、Cu、Ni、Pb、Tl、V、Zn 11种金属元素的微波消解ICP-MS方法。该方法线性关系良好，线性相关系数均在0.9990以上，检出限为0.002mg/kg-0.054 mg/kg。检测土壤标准物质GSS-17、GSS-18验证方法准确性，结果显示测定值均在标准差允许范围内，相对标准偏差在0.29%-5.33%，是一种快速、可靠的土壤多种金属元素检测方法。

Simultaneous Determination of Eleven Kinds of Metal Elements in Soil by Microwave Digestion and ICP-MS

Weighed 0.25 g samples, then added 5 ml nitric acid and 2 ml hydrofluoric acid. The samples were decomposed by microwave digestion technique. Using rhenium as internal standard of arsenic, plumbum and thallium, rhodium as internal standard of cadmium, cobalt, chromium and nickel, bismuth as internal standard of beryllium, cuprum and zinc, terbium as internal standard of vanadium, the method of microwave digestion and ICP-MS in KED mode was established which could conduct the simultaneous determination of eleven kinds of metal elements of beryllium, arsenic, cadmium, cobalt, chromium, cuprum, nickel, plumbum, thallium, vanadium and zinc in soil. The method had good linear relationship and the linear correlation coefficients of eleven metal elements were all over 0.9990. The detection limit was between 0.002mg/kg and 0.054 mg/kg. The accuracy of this method was validated by determining and analyzing the soil reference materials GSS-17 and GSS-18. The results showed that the determination results of the soil reference materials were within the scope of the standard value, and the relative standard deviation was between 0.29% and 5.33%.This method was rapid and reliable for the simultaneous determination of multiple metal elements of soil.