微波消解ICP-AES法测定铁矿石中痕量砷、锑、铋

用微波消解仪预处理样品,高氯酸冒烟驱除硝酸、氢氟酸等,用抗坏血酸-硫脲作为还原剂,溶样酸及还原剂用量均以10mL为宜,用硼氢化钾产生砷、锑、铋的氢化物,以ICP-AES法测定,采用基体高纯铁或砷锑铋含量低的钢铁标样消除基体效应,对铁矿石样品的测定表明,方法检出限低,简单、快捷、准确,RSD分别为As3.06%、Sb3.33%、Bi3.33%。

Determination of Trace As, Sb and Bi in Iron Ore by Microwave Digestion and ICP-AES Method

Sample pretreatment was made with microwave digestion instrument, the nitric acid and hydrofluoric acid etc were lustrated by smoking of perchloric acid, with ascorbic acid-thiourea as a reducing agent, and 10 mL are suitable amount of reducing agent and solvent acid, the hydrides of arsenic, antimony and bismuth produced by potassium boiohydride were made a measurement with ICP-AES. Using the matrix of high purity iron or iron and steel standard samples with low As, Sb and Bi contents eliminated the matrix effect. The determination of iron ore samples showed that the method had low detection limits and was simple, fast and exact. The RSD was as follows： As 3.06%, Sb 3.33% and Bi 3.33%.