Abstract:The ammonium metavanadate sample was dissolved with hydrochloric acid. Then, the content of ten impurity elements including aluminum, iron, silicon, phosphorus, lead, arsenic, chromium, potassium, sodium and calcium was simultaneously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Since the sample solution contained 2.18 g/L vanadium and 0.78 g/L ammonium ions, the spectral interferences such as spectral overlapping and continuous background superposition of 2.18 g/L vanadium standard solution, 0.78 g/L ammonium standard solution, their mixed standard solution, 10 mg/L testing element standard solution, water and 5% (V/V) hydrochloric acid reagent blank were focused on. Moreover, the influence of matrix effect on determination was also investigated. The results showed that the ammonium ion with this concentration had no interference with the determination. The sensitive spectral lines of some testing elements were relatively seriously interfered by spectral overlapping or sideband peaks of vanadium. The matrix effect of high content vanadium and continuous background superposition caused the increase of spectral intensity of aluminum, iron, silicon, phosphorus, lead, arsenic, chromium and calcium, leading to positive interference. Meanwhile, the matrix effect of high content vanadium also reduced the spectral intensity of potassium and sodium, leading to negative interference. Therefore, the influence of high content vanadium matrix was eliminated by matrix matching and synchronous background correction. Moreover, the analytical lines of testing elements, the background correction and detection area without spectral interference were optimized. The results indicated that the background equivalent concentration was -0.000 3%(Na)-0.000 4%(Ca). When the mass fraction of aluminum, iron, silicon, phosphorus, lead, arsenic, chromium and calcium was in range of 0.001%-0.60%, and the mass fraction of potassium and sodium was in range of 0.005%-0.60%, the mass fraction of these elements was linear to the corresponding emission intensity. The correlation coefficients of calibration curves of elements were all not less than 0.999. The detection limits of elements were between 0.000 1% and 0.000 6%. The content of aluminum, iron, potassium, sodium, silicon, phosphorus, lead, arsenic, chromium, and calcium in two ammonium metavanadate samples was determined according to the experimental method. The relative standard deviation (RSD, n=8) was less than 10%(mass fraction of 0.001%-0.010%), 7%(mass fraction of 0.010%-0.050%) and 3% (mass fraction more than 0.050%), respectively. The proposed method was applied to the determination of aluminum, iron, silicon, phosphorus, lead, arsenic, chromium, potassium, sodium and calcium in four ammonium metavanadate samples, and the results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).
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