摘要:
样品经过氧化钠碱熔,溶解后的上层清液直接酸化,用电感耦合等离子体发射光谱测定钛铁矿中铬、磷、钒的含量。确定了钛铁矿石中Cr、P、V的分析谱线、光谱级次;为了消除钠盐基体的影响,确定稀释因子为1000,标准曲线基体与样品基体保持一致;为避免过氧化钠熔矿后溶液碱性较大对进样系统造成腐蚀,加入2.00 mL盐酸对溶液进行酸化。方法检出限为4.46~23.55 μg/g,采用国家一级标准物质进行验证,方法准确度小于10%,精密度为0.68%~9.90%。本法与分光光度法单一元素测定相比较,具有测量范围宽、结果准确、操作简便、省时省力、适合大批量样品测定等突出的优点。
Abstract:
An analytical method for the determination of trace elements of Cr, P and V in ilmenite with sodium peroxide by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) is proposed. The sample was digested by sodium peroxide fusion following which, the clear top solution was acidized to measure Cr, P and V by ICP-AES. The optimum instrumental conditions and selection of spectral lines for the elemental analysis were studied. The large dilution of 1000 and calibration standard solution by adding sodium as the matrix were conducted to eliminate the matrix effect. 2 mL HCl was loaded to acidize the sample solution in order to avoid eroding the machine's sampling system by the strong basicity of the solution by sodium peroxide fusion. The detection limit of this method was 4.46-23.55 μg/g. According to the validation by national standard materials, the accuracy of the method (relative error) was less than 10%, and precision (RSD, n=12) was 0.68% to 9.90%. Compared with the spectrophotometer method for single element determination, this method showed many advantages, such as a low detection limit, high sensitivity, a wide measuring range, convenient operation, and was suitable for batch samples.
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