摘要
称取经四分采样,风干并粉碎过0.149mm孔径样筛的土壤样品0.200 0g,置于消解罐中,加入选定的酸体系(HNO36mL,HCl 2mL及HF 2mL)。将消解罐置于微波消解仪中按程序升温模式进行消解。将消解罐移至赶酸仪中,于170℃使溶液蒸缩至2～3mL。溶液中有残留黑色不溶物,加入高氯酸3mL,于180℃继续加热消解至样品溶解完全,将溶液蒸缩至黏稠状,冷却后,将溶液用硝酸(1+99)溶液洗涤并定容至25.0mL。按仪器工作条件采用电感耦合等离子体原子发射光谱法在所选定的分析谱线处测定其中8种重金属元素(Co、Cr、Cu、Ni、Mn、Pb、V及Zn)的含量。8种元素的质量浓度在一定范围内与其信号强度值呈线性关系,测得8种元素的检出限(3s)在0.3～6.6μg·L^(-1)范围内,其测定值的相对标准偏差(n=6)均小于2%。
Soil was sampled by quartering,air-dried and pulverized to pass through sample sieve with bore diameter of 0.149 mm.A portion(0.200 0 g)of the soil sample was taken and digested in a microwave digester with a selected acid mixture of 6 mL of HNO3 and 2 mL each of HCl and HF,under programmed temperature elevation.The digested solution was removed to an acid expeller and evaporated to 2-3 mL at 170 ℃.There are some black residues remaind insoluble in the solution,the evaporation should repeated by heating at 180℃ with an addition of3 mL of HClO4 to have the sample dissolved completely.The solution was concentrated to a syrupy consistency and after cooling,its volume was made up to 25.0 mL with HNO3(1+99)solution.The solution was mixed thoroughly and use for ICP-AES determination of 8 heavy metal elements,i.e.,Co,Cr,Cu,Ni,Mn,Pb,V and Zn.Linear relationships between values of mass concentrations of the 8 elements and their signal intensities were found in definite ranges.Values of detection limits(3 s)were found in the range of 0.3-6.6μg·L^-1,and RSDs(n=6)of the measured value were all less than 2%.
作者
杨叶琴
赵昌平
赵杰
YANG Yeqin;ZHAO Changping;ZHAO Jie(Suzhou Guohuan Environmental Inspection Co.,Ltd.,Suzhou 215129,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第1期63-67,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
