过氧化钠熔融-电感耦合等离子体发射光谱法快速测定稀散元素矿石中高含量钨

Rapid determination of tungstenin scattered elements mineral by ICP-AES with sodium peroxide alkali fusion

建立了电感耦合等离子体发射光谱快速测定稀散元素矿石中高含量钨的方法。稀散元素矿石经Na2O2熔融,水提取,上清液经HNO3(3+97,V/V)(含0. 067 mol/L的酒石酸)酸化稀释,溶液中的钨离子与酒石酸络合形成稳定的络合物抑制酸性介质中钨酸析出,直接进行测定,方法检出限为114μg/g,RSD为1. 2%,样品平均加标回收率为96. 4%。经实际测定国家一级标准物质与推荐值相符;能力验证样品测定结果与KSCN-TiCl3光度法相符,同时反馈回的能力验证结果为满意结果(|z︱≤2)。

A method of ICP-AES for the determination of high content tungsten in scattered elements mineral was proposed. The samples were decomposed by sodium peroxide alkali fusion, and then extracted with water. The supernatant liquor was diluted with nitric aeid （3 ＋ 97, V/V） including 0. 067 mol/L tartaric acid, which could form stable complex with the tungsten ions in solution to prevent the precipitate of tungstic acid. The detection limit was 114 μg/g, RSD was 1.2% , and the average recovery was 96.4%. The proposed method was applied to the analysis of the reference materials and the results were consistent with the certified values. The results of the proficiency testing sample by ICP-AES coincided well with the traditional spectrophotometry, and the result feed back was satisfactory（ ｜ z｜ ≤2）.