考察了源于基体Ｔｂ的多原子离子质谱干扰及基体Ｔｂ对稀土杂质测定信号的影响，研究了Ｐ５０７ＨＣｌ萃取色谱体系分离高纯Ｔｂ４Ｏ７基体与痕量稀土杂质的条件，采用Ｒｅ内标补偿直接测定与分离基体后测定相结合的方式，建立了分析高纯Ｔｂ４Ｏ７中痕量稀土杂质的电感耦合等离子体质谱（ＩＣＰＭＳ）法，检出限为５～２１ｎｇ／Ｌ，加标回收率为９０％～１０９％，３次测量的相对标准偏差为１．３％～６．５％，分离周期近９ｈ。方法可用于纯度（质量分数，ｗ）为９９．９９％～９９．９９９９％的Ｔｂ４Ｏ７中痕量稀土杂质的分析。 The influence of polyatomic ion mass spectra from substrate Tb and the influence of Tb on rare earth impurities were investigated. The conditions for separation of high purity Tb4O7 matrix and trace rare earth impurities from P507-HCl extraction chromatography system were studied. Re internal standard compensation ICP-MS method was established for the analysis of trace rare earth impurities in high-purity Tb4O7 with the detection limit of 5 ~ 21ng / L and the recovery of standard addition was 90% ~ 109%. The relative standard deviations of three measurements were 1.3% ~ 6.5% and the separation period was nearly 9 hours. The method can be applied to the analysis of trace rare earth impurities in Tb4O7 with purity (mass fraction, w) of 99.99% -99.9999%.