微波消解-电感耦合等离子体质谱法测定镍精矿中Ga、Ge、Se、Cd、In、Te、La和Tl

Determination of Ga, Ge, Se, Cd, In, Te, La and Tl in Nickel Concentrates by ICP-MS Combined with Microwave Digestion

摘要: 样品经硝酸-盐酸-氢氟酸-过氧化氢（3+1+1+1）混合液微波消解后，加入硝酸（1+1）溶液溶解盐类，定容后供电感耦合等离子体质谱分析。以¹⁰³Rh和²³²Th为内标，采用校正方程消除质谱干扰。Se的线性范围为0.500~500.0 μg·L^-1，其他7种元素的线性范围均为0.050~100.0 μg·L^-1，8种元素的检出限（3s）在0.01~0.8 mg·kg^-1之间。加标回收率在90.9%~113%之间，测定值的相对标准偏差（n=4）在0.90%~7.7%之间。方法用于测定镍精矿标准物质中Cd，测定值与认定值相符。

Abstract: The sample was digested by microwave with the mixed solution of HNO₃、HCl、HF and H₂O₂ (3+1+1+1), then HNO₃ (1+1) solution was added to dissolve the salt and the solution was diluted for ICP-MS analysis with ¹⁰³Rh and ²³²Th as internal standard. The calibration equation was used to eliminate mass spectral interference. The linearity range of Se and the other 7 elements were 0.500-500.0, 0.050-100.0 μg·L^-1, respectively. The detection limits (3s) of 8 elements were in the range of 0.01-0.8 mg·kg^-1. Recovery rates obtained by standard addition method were in the range of 90.9%-113%, and RSDs (n=4) were in the range of 0.90%-7.7%. The proposed method was applied to the determination of Cd in nickel concentrate standard substances, giving results in agreement with the certified values.