电感耦合等离子体发射光谱法测定钛铁矿中主、微量元素

Determination of Main and Trace Elements in Ilmenite by Using Inductively Coupled Plasma Atomic Emission Spectrometry Method

摘要:

采用氢氟酸-盐酸-硝酸-硫酸四酸溶矿，建立了电感耦合等离子体发射光谱仪法（ICP-AES）同时测定钒钛磁铁矿、钛铁矿中铝、钙、镁、钾、钠、锰、钛、铬、锶、锌和钒11种元素的方法。对最佳仪器条件及分析谱线进行了优化筛选，并探讨了4种消解方法及酸度对测定的影响。实验结果表明： ICP-AES法测定钒钛磁铁矿、钛铁矿中铝、钙、镁、钾、钠等元素，与原子吸收光谱法、分光光度法、滴定法、重量法等单一元素测定方法相比较，具有检出限低、灵敏度高、测量范围宽、操作简便，适合大批量样品测定等突出优点。方法准确度（RE）小于10%，元素精密度（RSD，n=12）为0.68％～5％。采用国家一级标准物质进行了方法验证，取得了令人满意的结果。

Abstract:

After using hydrofluoric acid-hydrochloric acid-nitric acid-sulfuric acid to dissolve ores, the method for determing aluminum, calcium, magnesium, potassium, sodium, manganese, titanium, chromium, strontium, zinc and vanadium in vanadium-titanium magnetite and ilmenite at the same time by using inductively coupled plasma-optical emission spectrometry (ICP-AES) has been established. The optimal instrument conditions and analytical lines have been optimized for screening, and four digestion methods and the effect of acidity on the determination have been studied. As showed by the experimental results, comparing with atomic absorption spectrometry, spectrophotometry, titration and gravimetry methods for determing single element, ICP-AES method has outstanding advantages for determing aluminum, calcium, magnesium, potassium, sodium and other elements in vanadium-titanium magnetite and ilmenite, such as low detection limit, high sensitivity, wide measuring range, simple operation, and suitability for large-scale sample measurement. The accuracy of the method (RE) is less than 10%, and the element precision (RSD, n=12) is 0.68%~5%. Method validation has been carried out by using national-level reference materials. It is proved that the result is satisfied.