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

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0.0010%、0.0028%、0.0021%,测定下限分别为0.0100%、0.0280%、0.0210%。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。

Determination of scandium,iron and titanium in chlorination dust by inductively coupled plasma atomic emission spectrometry

The accurate determination of scandium, iron and titanium in chlorination dust has important significance to judge the separation degree of scandium/iron and scandium/ titanium and to evaluate the recovery of scandium. The determination of scandium, iron and titanium in chlorination dust by inductively coupled plasma atomic emission spectrometry (ICP-AES) was investigated. The chlorination dust was treated using two methods, i.e., acid dissolution (hydrochloric acid-nitric acid-phosphoric acid) and alkali fusion (sodium hydroxide). The determination results of scandium, iron and titanium in two sample preparation methods were compared. It was found that the acid dissolution method was simple and easily conducted. Furthermore, the determination results were more accurate and reliable. The spectral lines of 335.372, 259.940 and 334.188nm were selected as the analytical lines for scandium, iron and titanium through the interference test of coexisting elements. The acidity test indicated that the interference to testing elements could be ignored when the concentration of phosphoric acid in sample solution was less than 10% (volume fraction). In this method, the correlation coefficients of linear regression equations of calibrations curves for elements were all higher than 0.999. The detection limit for scandium, iron and titanium was 0.0010%, 0.0028% and 0.0021%, respectively. The lower determination limit was 0.0100%, 0.0280% and 0.0210% respectively. The determination results of scandium, iron and titanium in chlorination dust according to experimental method were consistent with those obtained by spectrophotometry. The relative standard deviations (RSD) were between 1.1% and 2.7%. The recoveries were between 93% and 107%.