电感耦合等离子体原子发射光谱（ICP-AES）法测定铁矿石中磷

采用盐酸-硝酸-高氯酸-氢氟酸前处理样品,电感耦合等离子体原子发射光谱法测定铁矿石中的磷。对磷元素的分析谱线、样品称样量等工作条件进行了优化,解决了非金属元素磷的分析谱线难选择、样品称样量影响测定准确度的技术难点;采用内标法,降低了样品基体效应及仪器波动产生的影响,提高了分析结果的精密度和准确度。利用所建立的方法快速分析了铁矿石中磷的含量,方法检出限为0.0036 mg/L,测定范围为0.012%~2%,测定结果与标准值和化学法测定结果相符,相对标准偏差(RSD,n=9)小于2%。拟定的方法和分光光度法进行比对实验,技术优势明显。

Determination of P in Iron ores by Inductively Coupled Plasma-Atomic Emission Spectrometry

Iron ore samples were digested with HCl-HNO3-HClO4-HF mixed acid and P in sample solutions were then directly determined by inductively coupled plasma-atomic emission spectrometry. The conditions for selection of analytical lines and the amount of sample were optimized, the matrix interference effect and the instrument fluctuation have been overcome and the precision and accuracy of the analysis were improved, using internal standard method. The method overcomes the cumbersome procedure, time consuming, heavy workload of the conventional chemical analysis methods. The established method has been applied to the rapid determination of P in iron ore samples, the determination limits of the method was 0.0036 mg/L for P and the determination content range was of 0.012%~2%, the results are in agreement with the certified values and chemical method, the precision of the method was less than 2% (RSD, n = 9). The method provides the advantages of wide dynamic linear range, high efficiency and simple operation, the analytical error meet the requirements of conventional chemical analysis, the method has been applied to the determination of P in various iron ore samples and the results are accurate and reliable.