高温熔融-电感耦合等离子体原子发射光谱法测定含铁尘泥中5种有害元素

准确、快速地测定含铁尘泥中有害元素,对含铁尘泥节能降废项目研究及综合利用有着重要的指导意义。实验针对含铁尘泥试样因含碳量高,导致常规酸溶解方法如果不增加除碳步骤则很难完全分解试样的问题,采用高温熔融法将试样制成熔融液后倾倒于稀酸中溶解的方法,解决了碳含量高难溶解的问题。采用四硼酸锂-碳酸锂混合熔剂在高温下将试样熔融,熔融液高温倾倒于稀酸中制成澄清溶液,由于骤冷,试样炸裂成微小玻璃珠,无迸溅,操作简单,使得后续溶解过程快速完成,从而建立了电感耦合等离子体原子发射光谱(ICP-AES)测定P、Pb、K、Na、Zn共5种有害元素的方法。按照实验方法测定含铁尘泥中P、Pb、K、Na、Zn,测定值的相对标准偏差(RSD,n=9)在1.4%～5.7%之间,加标回收率在96%～110%之间。研究结果表明方法能够满足含铁尘泥样品中5种元素的定量分析要求。

Determination of five harmful elements in iron-bearing dust by high temperature fusion-inductively coupled plasma atomic emission spectrometry

The accurate and rapid determination of harmful elements in iron-bearing dust is of great significance for the energy conservation and comprehensive utilization of iron-bearing dust. Since the content of carbon in iron-bearing dust samples is high, it is difficult to completely decompose the sample using the conventional acid dissolution method if the carbon removal procedures are not added. Aiming at this problem, the sample was melted at high temperature and then poured into a dilute acid solution. The proposed method solved the problem that the sample was hardly dissolved due to the high carbon content. In experiments, the sample was melted at high temperature using lithium tetraborate and lithium carbonate mixture as flux. The molten sample at high temperature was poured into a dilute acid solution to prepare a clear solution. Due to the rapid cooling, the sample was busted into tiny glass beads without splashing. The operation was simple,so that the subsequent dissolution process could be completed quickly. Consequently,the determination method of 5 harmful elements (including P, Pb, K, Na and Zn) in iron-bearing dust by inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The proposed method was applied to the determination of P,Pb,K,Na and Zn in iron-bearing dust. The relative standard deviations (RSD, n=9) of determination results were between 1.4% and 5.7%. The recoveries were between 96% and 110%. The experimental results indicated that the proposed method could meet the quantitative analysis requirements of 5 elements in iron-bearing dust samples.