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为了解决高纯仲钨酸铵中杂质元素硼的测定问题 ,采用ICP AES测定方法 ,对测定中基体效应及光谱干扰进行了研究 ,考察了酸度、蒸干程度、放置时间等因素对钨的沉淀程度及硼的回收率的影响 ;此外 ,将基体分离与干扰系数校正法相结合 ,建立了简便、快速、准确测定高纯仲钨酸铵中微量硼的新方法 .结果表明 :用该法测定硼的回收率大于 95 .8% ,测定仲钨酸铵中 0 0 0 0x%~ 0 0 0x%硼的相对标准偏差小于 3% ,其准确度及精密度均符合要求 ,能用于出口产品控制分析 .
In order to solve the problem of determination of boron in impurity element of high purity paratungstate, the matrix effect and spectral interference in the determination were studied by ICP AES method. The effects of acidity, degree of evaporation and storage time on the precipitation of boron and boron In addition, a new method for the simple, rapid and accurate determination of trace boron in high-purity ammonium paratungstate was established by combining substrate separation and interference coefficient calibration.The results showed that the recovery of boron was greater than 95 by this method. 8%. Determination of ammonium paratungstate 0 0 0 0x% ~ 0 0 0x% The relative standard deviation of boron is less than 3%, its accuracy and precision are in line with requirements, can be used for export product control analysis.