电感耦合等离子体发射光谱法测定银侧吹炉烟灰中的铋

银侧吹炉烟灰样品结构较为复杂,硝酸-酒石酸溶解样品-EDTA滴定测定其中的铋时,样品消解不完全,终点不稳定,测定结果偏低。为了准确测定银侧吹炉烟灰中的铋,试验建立了硝酸-盐酸-氢氟酸-高氯酸消解银侧吹炉烟灰,选择Bi190.234 nm为分析线,使用电感耦合等离子体发射光谱法(ICP-AES)测定银侧吹炉烟灰的铋的方法。试验讨论了溶样方法的选择,介质及加入量的选择,共存元素干扰情况对铋测定结果的影响。结果表明:采用硝酸-盐酸-氢氟酸-高氯酸消解样品能使样品消解完全,加入25mL王水后进行测定结果稳定,共存元素对铋测定结果无影响。铋在0~15μg/mL的校正曲线关系良好,相关系数为0.999998,方法检出限为0.017μg/mL。取不同银侧吹炉烟灰样品进行精密度考察,铋测定结果的相对标准偏差(RSD,n=12)在0.19%~0.58%之间,加标回收率在99.49%~100.25%之间。

Determination of Bismuth in Soot of Side Blown Furnace by ICP-AES

The structure of the soot sample from the silver side blown furnace is complex.When the bismuth is determined by EDTA titration with nitric acid tartaric acid dissolving sample,the digestion of the sample is not complete,the end point is not stable,and the determination result is low.In order to accurately determine the bismuth in the soot of side blown furnace,a method of digesting the soot of side blown furnace by nitric acid hydrochloric acid hydrofluoric acid perchloric acid was established.Bi190.234 nm was selected as the analytical line and ICP-AES was used to determine the bismuth in the soot of side blown furnace.The effects of the selection of dissolution method,the selection of medium and addition amount,the interference of coexisting elements on the determination of bismuth were discussed.The results show that the sample can be digested completely by nitric acid hydrochloric acid hydrofluoric acid perchloric acid digestion,and the results are stable after adding 25 mL nitric acid.The coexisting elements have no effect on the results of bismuth determination.The correlation coefficient is 0.999998,and the detection limit is 0.017μL/mL.The relative standard deviation(RSD,n=12)of bismuth determination results is between 0.19%and 0.58%,and the recovery is between 99.49%and 100.25%.