Determination of Eight Heavy Metal Elements in Soil by Microwave Digestion- Inductively Coupled Plasma Atomic Emission Spectrometry
摘 要
称取经四分采样,风干并粉碎过0.149 mm孔径样筛的土壤样品0.200 0 g,置于消解罐中,加入选定的酸体系(HNO3 6 mL,HCl 2 mL及HF 2 mL)。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2~3 mL。溶液中有残留黑色不溶物,加入高氯酸3 mL,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25.0 mL。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0.3~6.6 μg·L-1范围内,其测定值的相对标准偏差(n=6)均小于2%。
Abstract
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 of 3 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 (3s) were found in the range of 0.3-6.6 μg·L-1, and RSDs (n=6) of the measured value were all less than 2%.
中图分类号 O657.3 DOI 10.11973/lhjy-hx201901011
所属栏目 工作简报
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收稿日期 2018/3/1
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备注杨叶琴,工程师,硕士,主要从事环境检测研究工作
引用该论文: YANG Yeqin,ZHAO Changping,ZHAO Jie. Determination of Eight Heavy Metal Elements in Soil by Microwave Digestion- Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(1): 63~67
杨叶琴,赵昌平,赵杰. 微波消解-电感耦合等离子体原子发射光谱法测定土壤中8种重金属元素的含量[J]. 理化检验-化学分册, 2019, 55(1): 63~67
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