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本文研究了测定钢铁及合金中痕量锌时基体元素所产生的严重干扰。其干扰主要包括二个部分,即铁的谱线重叠产生的光谱线干扰及分子吸收和光散射产生的背景吸收。提出了以不含锌的纯铁或以离子交换分离去锌的纯铁打底,准确地测定出上述的光学干扰数值从试样值中扣除,从而得到可靠的分析结果。此方法比分离试样中铁的操作简便、快速,是较为适用的分析方法。在pH4.0的HAc-NaAc缓冲溶液中,铜与紫脲酸铵(MX)反应生成橙红色显色液。本文在此显色反应基础上,依据β修正光度理论,研究了测定铜的新方法。该方法能准确扣除反应体系中剩余脲酸铵的吸光干扰,使β修正吸光度与铜浓度(x)呈良好线性关系,且分析灵敏度高。实验测得方法的相对标准偏差RSD≤2.5%,加标回收率为90.0%~109.0%,铜的最低检测浓度为0.3μg/ml。该方法适合于铜合金,铝合金及试剂级铜盐、含铜废水中铜的测定。
In this paper, the determination of trace elements in steel and alloy trace elements produced by the serious interference. The interference mainly consists of two parts: the interference of the spectral lines caused by the overlap of the lines of iron and the background absorption caused by molecular absorption and light scattering. It is proposed that pure iron with no zinc content or pure iron with zinc ion separation is used as the base to accurately measure the optical interference value deducted from the sample value so as to obtain a reliable analysis result. This method is more convenient than the separation of iron samples, fast, is a more applicable method of analysis. In pH 4.0 HAc-NaAc buffer solution, copper and ammonium urea (MX) reacts to form an orange-red color. In this paper, based on the color reaction, based on the β-corrected photometric theory, a new method for the determination of copper was studied. The method can deduct the absorption interference of the remaining ammonium nitrate in the reaction system accurately, and has a good linear relationship between the β-corrected absorbance and the copper concentration (x) and the high sensitivity of analysis. The relative standard deviations RSD≤2.5%, the spiked recoveries 90.0% ~ 109.0%, and the minimum detection concentration of copper 0.3μg / ml. The method is suitable for the determination of copper in copper alloy, aluminum alloy and reagent grade copper salt and copper-containing wastewater.