直读光谱仪铜、铅和铋工作曲线的扩展

Extension of the Working Curves of Copper,Lead and Bismuth in Direct-Reading Spectrometer

使用直读光谱仪分析高含量铜、铅和铋(w(Cu)≥0.60%,w(Pb)≥1.20%,w(Bi)≥0.11%)时,其元素含量已超出了校准曲线的线性范围,导致分析值偏低。以随原机带来的铜、铅和铋元素的原始工作曲线为基础,实验通过增加高含量标准样品,扩展铜、铅和铋的工作曲线,完成共存元素的干扰校正,拓宽了铜、铅和铋元素的分析范围,铜质量分数上限由0.60%扩展至1.75%,线性相关系数0.98844;铅质量分数上限由1.20%扩展至2.30%,线性相关系数0.98118;铋质量分数上限由0.11%扩展至0.30%,线性相关系数0.99734。校准曲线扩展后重新选择标准化样品进行漂移校正。对扩展含量段的样品w(Cu)≥0.60%,w(Pb)≥1.20%,w(Bi)≥0.11%进行精密度考察,结果相对标准偏差(RSD,n=11)为1.17%,0.40%和4.97%;对比了不同铜、铅和铋含量的样品,发现扩展后校准曲线的铜、铅和铋的测定值与化学法测定结果相符。因此,扩展曲线用于锡锭前处理样品锅中样铜铅铋元素的分析,并将分析结果与化学法分析结果进行比较,结果一致,能满足企业生产的需要。

When the content of copper,lead and bismuth(w(Cu)≥0.60%,w(Pb)≥1.20%,w(Bi)≥0.11%)was analyzed by direct-reading spectrometer,the element content of the samples exceeded the linear range of calibration curve,resulting in lower analytical value.Based on the original working curves of copper,lead and bismuth,the interference correction of coexisting elements was accomplished by adding high content standard samples and expanding the working curves of copper,lead and bismuth,the analytical range of copper,lead and bismuth was widened,the upper limit of copper content was extended from 0.60% to 1.75%,and the linear correlation coefficient was 0.98844.The upper limit of lead content was extended from 1.20% to 2.30%,and the linear correlation coefficient was 0.98118.The upper limit of bismuth mass fraction was extended from 0.11%to 0.30%,and the linear correlation coefficient was 0.99734.After the calibration curve expanded,the standardized sample was selected again for drift correction.The relative standard deviations(RSD,n=11)were 1.17%,0.40% and 4.97% for w(Cu)≥0.60%,w(Pb)≥1.20%,w(Bi)≥0.11%,respectively.It was found that the measured values of copper,lead and bismuth in the expanded calibration curve were in good agreement with those of the chemical method.Therefore,the extended curve is applied to the analysis of copper,lead and bismuth in the pot of Tin Ingot pretreatment sample,and the analysis results are in agreement with those of chemical method.