Determination of iron, phosphorus and titanium in vanadium carbide by inductively coupled plasma atomic emission spectrometry
ZHANG Gao-qing1, WANG Lu-feng1, YAN Yue-e1, LI Guo-wei2, TIAN Cong-xue1
1. Vanadium and Titanium College, Panzhihua University, Panzhihua 617000, China; 2. National Quality Supervision and Testing Center of Vanadium and Titanium Products, Panzhihua 617000, China
Abstract：The accurate and rapid determination of impurity elements such as iron, phosphorus and titanium in vanadium carbide has great significance to judge the quality of vanadium carbide products. The sample was dissolved in experiments by acid dissolution-alkali fusion of slag. In other words, the sample was first dissolved with aqua regia. After filtration, the filter residue and filter paper were ashed and then fused with mixed flux (sodium carbonate-boric acid). The calibration curve was prepared by matrix matching method to eliminate the interference of matrix effect. The content of iron, phosphorus and titanium were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The linear correlation coefficients of calibrations curves for iron, phosphorus and titanium were all higher than 0.999. The limit of detection was 0.00036%, 0.00082% and 0.0012%, respectively. The experimental method was applied for the determination of iron, phosphorus and titanium in three actual samples of vanadium carbide. The relative standard deviations (RSD, n=7) were less than 0.90%, and the spiked recoveries were between 96% and 103%. The found results were consistent with those obtained by other methods (Fe: flame atomic absorption spectrometry in GB/T 20255.2-2006; P: bismuth-phosphorus-molybdenum blue spectrophotometry in YB/T 4566.6-2016; Ti: flame atomic absorption spectrometry in GB/T 20255.3-2006). The proposed method effectively solved the difficulty in simultaneous determination of low-content iron, phosphorus and titanium in vanadium carbide samples, and it was applicable for the determination of vanadium carbide samples with iron, phosphorus and titanium content in the range of 0.015%-0.113%, 0.016%-0.046% and 0.015%-0.088%, respectively.
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