标准加入法测定纯钯中的杂质元素

高纯金属纯度分析时为了克服基体效应的影响,常采用分离基体、基体匹配等方法对其中杂质元素进行分析测定,但是存在基体难分离、易造成样品污染,而且还会消耗昂贵基体等问题。以王水溶解纯钯样品,通过选择合适的谱线克服光谱干扰,采用标准加入法绘制校准曲线,在不分离基体或者不使用基体匹配的前提下消除了钯基体对杂质元素测定的基体效应影响,实现了ICP-AES对纯金属钯中30多种杂质元素的直接定量测定。将实验方法应用于纯钯样品的实际样品分析,加标回收率为92.1%～106.8%,相对标准偏差(RSD,n=7)不大于10%。

Determination of Impurity Elements in Pure Palladium by Standard Addition Method

The matrix separation or matrix matching methods are usually adopted to eliminate the influence of matrix effect of high-purity metals for determination of impurity elements, during the purity analysis of high purity metals. However, the matrix separation is difficult, the sample is easily polluted, and they consume expensive matrix. In the experiment, the pure palladium sample was digested by aqua regia. The spectral interference was overcome by selecting the appropriate spectral line, and the calibration curves were prepared by standard addition method. The influence of matrix effect of palladium for determination of impurity elements was eliminated without matrix separation or matrix matching, realizing the direct quantitative determination of more than 30 kinds of impurity elements in pure palladium by ICP-AES. The recovery of standard addition is 92.1%~106.8%, and the RSD (n = 7) is less than 10%.