微波消解-电感耦合等离子体质谱法测定赤泥中稀土总量及分量

Microwave Dissolving-inductively Coupled Plasma Mass Spectrometric Determination of Total and Individual REE in Red Mud

针对赤泥内有价稀土元素,建立了一种微波消解溶样-电感耦合等离子体质谱法测定稀土元素总量及分量的方法,并对河南某铝厂赤泥样品内稀土元素进行了测定。通过选择合适的同位素、控制基体质量浓度和选择185Re为内标元素,避免了元素测定中的质谱干扰和非质谱干扰。实验结果表明,在选定条件下0~100 ng/mL稀土元素的质量浓度与其质谱强度呈良好的线性关系,校准曲线线性相关系数为0.9991~0.9999,方法的检出限为0.0001 ng/mL^0.0074 ng/mL。将该方法应用于河南某铝厂产生的赤泥样品内稀土元素总量及分量的测定,7次平行测定结果的相对标准偏差在1.5%~4.7%之间,测定结果的加标回收率在96.2%~107%之间,在国家地质矿产行业标准DZ/T0130-2006第3部分规定的回收率允许限范围内。该方法实现了赤泥内10×10^-9~0.1%含量范围内稀土元素的准确测定。

A microwave dissolving-ICP-MS method for the determination of total and individual REE in red mud was established. By selecting suitable isotopes, controlling matrix concentration and using 185 Re as internal standard element, mass spectral interference and non-mass spectral interference were avoided.The results showed that the mass concentrations of rare earth elements in range of 0~ 100 ng/ mL had good linear relationship with its' corresp on ding mass spectrometric intensity under the optimized experimental conditions. The correlation coefficients of calibration curves were between 0. 9991 ~0. 9999 and the detection limits of this method were between 0. 0001 ng/mL .0. 0074 ng/mL.The method was used in the determination of total and individual REE in red mud samples in a factory in Henan province, the recovery rates of the measured results were between 96. 2~ 107% and the relative standard deviations of seven parallel determination were between 1. 8~4. 7%.The determination results satisfied the requirement of DZ/T 0130-2006. This method achieved the accurate determination of rare earth elements in red mud ranged from 10× 10 ^-9 to 0.1%.