化学法稀土复合钇锆陶瓷粉中14种痕量金属杂质的测定

Determination of 14 trace metal impurities in tombarthite composite yttrium zirconium ceramic powder by chemical anlaysis method

采用HNO 3-HF混合酸对样品进行前处理,选择合适的同位素,采用KED模式和干扰系数校正法消除质谱干扰,以103 Rh为内标测定Na、Mg、Al、K、Ti、Cr、Mn、Fe、Ni、Cu、Zn、Cd和Ba,以185 Re为内标测定Pb,建立了电感耦合等离子体质谱法对化学法制得的稀土复合钇锆陶瓷粉中14种痕量杂质元素的测定方法。实验发现,样品前处理选择6 mL HNO 3+2 mL HF,可以完全消解样品,也能避免环境因素导致的流程空白显著增加;基体主成分Y 2 O 3和ZrO 2在质量标准范围内的变化,对各元素的测定结果影响不大,以Rh和Re做内标,可以克服基体效应并校正仪器产生的信号漂移。通过绘制校准曲线及测定流程空白,各元素校准曲线的相关系数均在0.9996以上,方法检出限为0.001~0.255μg/g,方法定量限为0.003~0.765μg/g。对化学法稀土复合钇锆陶瓷粉实际样品进行测定,各待测元素的相对标准偏差(RSD,n=11)在1.45%~7.31%之间,加标回收率为88.9%~112.1%。

The anlaysis samples are pretreated with nitric acid and hydrofluoric acid digestion system.Mass Spectrum interference is eliminated by selecting sui Table isotopes and KED mode and interference coefficient correction.103 Rh is used as the internal standard of Na,Mg,Al,K,Ti,Cr,Mn,Fe,Ni,Cu,Zn,Cd and Ba.185 Re is used as the internal standard of Pb.The chemical analysis method to determine 14 trace impurity elements in the tombarthite composite yttrium zirconium ceramic powder is established by Inductively Coupled Plasma Mass Spectrometry(ICP-MS).It is found that sample pretreatment with 6 mL HNO 3+2 mL HF could completely solve the sample and avoid significant increase of process blank caused by environmental factors.The variation of Y 2 O 3 and ZrO 2 in the range of quality standard has little effect on the determination results of each element.Rh and Re are used as internal standards to overcome matrix effect and to correct instrument drift.The correlation coefficient of calibration curve of each element is above 0.9996,the method detection limit is 0.001-0.255μg/g,and the quantitative limit of the method is 0.003-0.765μg/g.The practical samples of yttrium zirconium ceramic powder are analyzed with the chemical method.The relative standard deviations(RSD,n=11)are in the range of 1.45%-7.31%,and the recovery ratios are from 88.9%to 112.1%.