光度法同时快速测定锑冶炼炉渣中的硅、铁、钙

Rapid and Simultaneous Determination of Silicon,Iron and Calcium in Antimony Smelting Slag by Photometry

利用新型多元素分析仪,建立了光度法同时快速测定锑冶炼炉渣中的二氧化硅、铁、氧化钙,考察了样品质量、熔样温度和时间、干扰离子等因素对测定结果的影响,确定了最佳测定条件。结果表明:在优化条件下,二氧化硅、铁、氧化钙质量浓度分别在3.30~54、0.90~32和3.08~27μg/mL范围内,线性关系良好,方法检出限分别为1.00、0.27、0.95μg/mL;相对标准偏差RSD(n=6)分别为0.64%、0.79%、0.98%;样品加标回收率分别为98.96%~100.83%、98.20%~100.51%、97.81%~101.11%;炉渣用碳酸钠-氢氧化钠混合熔剂高温熔融并用盐酸溶解定容后,可不经分离直接同时测定二氧化硅、全铁、氧化钙,方法简便、快速,准确,可用于锑冶炼炉渣的生产控制分析。

Abstract.A new Photometry was developed for rapid and simultaneous determination of SiOe ,Fe,CaO in antimony smelting slag. The effects of factors such as sample amount, melting temperature and time, coexisting ions on determination were examined. The results show that under the optimized conditions,linear relations are well when SiO2 ,Fe,CaO mass concentrate are 3. 30454,0.90-32 and 3.08-27μg/mL,respectively. The detection limits are 1.00μg/mL（SiO2 ）,0.27μg/mL（Fe） and 0.95 μg/mL（CaO）. The relative standard deviation are 0. 64 G （SiO2）, 0.79 % （Fe） and 0.98 % （CaO）. The recovery rate of SiO2, Fe, CaO are 98.96 % - 100.83% for SiOz and 98. 20% - 100.51% for Fe and 97.81% -101. 11G for CaO. The sample is fused with mixture flux of Na2CO3 and NaOH then dissolved with hydrochloric acid and determined by photometry. The method is simple, rapid and sensitivity and can simultaneous determine SiO2, Fe, CaO with satisfactory results. It can be used for production control analysis of the antimony smelting slag.