Abstract:The sample was decomposed with anhydrous sodium carbonate-boric acid mixed flux. The phosphates in other forms were oxidized to orthophosphates with potassium permanganate in nitric acid medium. Then, the excessive potassium permanganate was reduced by sodium nitrite. At the acidity of about 0.80mol/L, phosphorus could react with ammonium molybdate and ammonium vanadate to form soluble phosphorus-vanadium-molybdenum yellow complex, thus realizing the determination of phosphorus in sample by phosphorus vanadium molybdenum yellow spectrophotometry. Under the selected experimental conditions, Beer′s law was obeyed when the mass of phosphorus in coloring solution was in range of 0.023-0.278mg. The correlation coefficient of calibration curve was 0.9998. The detection limit of method was 0.20% (mass fraction), and the lower determination limit was 0.60% (mass fraction). The interference of vanadium, chromium and other coexisting elements in vanadium-phosphorus-iron ore with the determination was investigated. The results showed that the interference of these coexisting elements could be ignored. Six vanadium-phosphorus-iron ore samples were selected and determined by proposed method and national standard method (GB/T 1871.1-1995, including quinoline phosphomolybdate gravimetric method and titration method) for comparison analysis. It was found that the determination results were basically consistent. The vanadium-phosphorus-iron ore was determined for eight parallel times according to the proposed method. The relative standard deviation (RSD, n=8) was less than 4%. The standard solution of phosphorus was added into sample for recovery test, and the recoveries were between 98% and 101%.
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