火花源原子发射光谱法测定热镀铝锑锌合金中主次成分

建立了利用火花源原子发射光谱法同时测定热镀铝锑锌合金中的合金元素铝、锑及杂质元素铜、镉、铁、铅的分析方法。考察了光源参数、分析线参数、共存元素干扰等因素对测定的影响。在选定的最佳光源激发参数(冲洗时间为2 s, 预燃时间为4 s, 总的火花积分时间为14 s)条件下, 采用自制校准样品, 对选定的铝、锑、镉、铜、铁、铅元素分析线绘制了最佳校准曲线。其中, 合金元素铝分析范围从0.000 2%～15.0%, 在考虑了共存元素干扰校正后, 3条铝元素分析线线性相关系数均达到0.999以上;而锑元素分析范围从0.000 3%～0.30%, 线性相关系数达到0.99以上;其他杂质元素的线性相关系数也均在0.99以上。通过对实际生产样品的分析, 待测元素的相对标准偏差(RSD, n=8)在0.48%～8.3%之间, 随机抽取的几个样品的测定结果与电感耦合等离子体原子发射光谱法(ICP-AES)基本吻合。

Determination of major and minor components in hot dip aluminized-antimony-zinc alloy by spark source atomic emission spectrometry

A method for simultaneously determination of aluminum and antimony, as well as impurity cadmium, copper, iron and lead in hot dip aluminized-antimony-zinc alloy was developed by spark source atomic emission spectrometry. The influence factors including light source parameters, the analysis line parameters and the co-existing element interference were investigated. The result indicated self-made calibration samples was used to draw optimum calibration curve for aluminum, antimony, cadmium, copper, iron and lead under the condition of optimum light source excitation parameter with washing time of 2 s, pre-burning time of 4 s and the total integration time of 14 s. Among them, the linear range for aluminium was 0.000 2%-15.0%. After taking the interference correction of coexistent elements into account, the linear correlation coefficient of three aluminum analysis lines were all higher than 0.999. The linear range for antimony was 0.000 3%-0.30%, and the linear correlation coefficient was above 0.99. The linear correlation coefficient of other impurity elements was also above 0.99. The relative standard deviations (RSD, n=8) of test elements were in the range of 0.48%-8.3% through the analysis of actual production samples, and the determination results of the random samples were consistent with those obtained by coupled plasma atomic emission spectrometry (ICP-AES).