电感耦合等离子体原子发射光谱法测定氯化烟尘中的钪铁钛

发布时间：2018-02-24 16:16

  本文关键词： 电感耦合等离子体原子发射光谱法(ICP-AES) 氯化烟尘 钪 铁 钛　出处：《冶金分析》2017年11期 　论文类型：期刊论文

【摘要】：准确测定氯化烟尘中钪、铁、钛的含量,对判断钪与铁、钪与钛的分离程度,评价钪的回收率有重要意义。实验采用电感耦合等离子体原子发射光谱法(ICP-AES)对氯化烟尘中钪、铁、钛的测定进行了研究。采用酸溶(盐酸-硝酸-磷酸)和碱熔(氢氧化钠)两种方法处理氯化烟尘,并对两种方法的钪、铁、钛测定结果进行对比,结果表明,采用酸溶法步骤简单易行,结果更准确可靠。通过共存元素干扰试验确定了钪、铁、钛的测定谱线分别为335.372nm、259.940nm和334.188nm。酸度试验表明,样品溶液中磷酸的体积分数在10%以下,对待测元素的干扰可忽略不计。方法中各元素校准曲线线性回归方程的相关系数均不小于0.999,钪、铁、钛的检出限分别为0.001 0%、0.002 8%、0.002 1%,测定下限分别为0.010 0%、0.028 0%、0.021 0%。按照实验方法测定氯化烟尘样品中的钪、铁、钛的含量与光度法的结果基本一致,相对标准偏差(RSD)在1.1%~2.7%之间,回收率在93%~107%之间。
[Abstract]:The accurate determination of scandium, iron and titanium in chlorinated smoke dust is of great significance to judge the separation degree of scandium and iron, and to evaluate the recovery rate of scandium. ICP-AESs was used to determine the content of scandium and iron in chlorinated soot dust by inductively coupled plasma atomic emission spectrometry (ICP-AESs). The determination of titanium was studied. Chlorinated soot was treated by acid solution (hydrochloric acid, nitric acid phosphoric acid) and alkali melting (sodium hydroxide). The results of scandium, iron and titanium were compared. The results are more accurate and reliable. The spectral lines of scandium, iron and titanium are 335.372nm ~ 259.940nm and 334.188nm ~ (-1), respectively. The acidity test shows that the volume fraction of phosphoric acid in the sample solution is less than 10%. The correlation coefficient of linear regression equation of calibration curve of each element in the method is not less than 0.999, scandium, iron, etc. The detection limit of titanium is 0.002 8 and the lower limit of determination is 0.010 000 and 0.028 0 and 0.021 0 respectively. The contents of scandium, iron and titanium in chlorinated smoke samples are basically consistent with the results of spectrophotometry. The relative standard deviation (RSDs) is between 1.1% and 2.7%. The recovery was between 93% and 107%.
【作者单位】： 湖南稀土金属材料研究院;
【分类号】：O657.31;X831
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