全自动石墨消解-电感耦合等离子体质谱法测定土壤中14种重金属

Determination of 14 heavy metals in soil by automatic graphite digestion-inductively coupled plasma mass spectrometry

建立全自动石墨消解-电感耦合等离子体质谱法测定土壤中14种重金属元素的分析方法。取0.1 g左右的土壤样品于消解罐中,采用5 mL盐酸+5 mL硝酸+2 mL氢氟酸+1 mL高氯酸消解体系进行全自动消解,升温至200℃赶酸。以Rh作为内标元素,在电感耦合等离子体碰撞模式下测定土壤中铍(Be)、钒(V)、铬(Cr)、锰(Mn)、钴(Co)、镍(Ni)、铜(Cu)、锌(Zn)、钼(Mo)、镉(Cd)、锑(Sb)、铊(Tl)、铅(Pb)、铀(U)14种重金属元素。V、Cr、Mn、Co、Ni、Cu、Zn、Pb的质量浓度和Cd、Be、Tl、U、Sb、Mo的质量浓度分别在0~500、0~10μg/L范围内与信号强度具有良好的线性关系,相关系数均不小于0.9998,检出限为0.011~1.5 mg/kg。选取有证标准土壤样品进行验证,测定值的相对标准偏差为1.08%~5.72%(n=6),相对误差为0.53%~13.1%,准确度和精密度均满足分析要求。

An analysis method for the determination of 14 heavy metal elements in soil by automatic graphite digestion-inductively coupled plasma mass spectrometry(ICP-MS)was established.0.1 g of soil samples were taken and transferred into the digestion tank,and 5 mL of HCl,5 mL of HNO,2 mL of HF and 1 mL of HClOwere used as digestion system to digest soil samples automatically,the final temperature was 200℃to drive acid.14 heavy metals,including beryllium(Be),vanadium(V),chromium(Cr),manganese(Mn),cobalt(Co),nickel(Ni),copper(Cu),zinc(Zn),molybdenum(Mo),cadmium(Cd),stibonium(Sb),thallium(Tl),plumbum(Pb)and uranium(U)were analyzed andRh was selected as internal standard element.The mass concentration of V,Cr,Mn,Co,Ni,Cu,Zn,Pb and the mass concentration of Cd,Be,Tl,U,Sb,Mo had a good linear relationship with the signal intensity in the range of 0-500 and 0-10μg/L,respectively,the correlation coefficients were all not less than 0.9998,and the detection limits were 0.011-1.5 mg/kg.The certified standard soil samples were selected for verification,the relative standard deviation was 1.08%-5.72%(n=6),and the relative errors were 0.53%-13.1%.The accuracy and precision meet the analysis requirements.