Abstract：Ferrosilicon nitride is a kind of important refractory materials. An analysis method of chromium content in ferrosilicon nitride was investigated by diphenylcarbazide spectrophotometry. The optimal analysis conditions were obtained by optimal experiments including sample decomposition method, oxidation condition, coloring condition and elimination of interference. The sample was melted in nickel crucible at 650 ℃ for 10 min with 2 g of sodium hydroxide as flux. The melt was leached with hot water. Then, silicon in the sample was removed by hydrofluoric acid and perchloric acid smoking. The salts were dissolved with sulfuric acid (1+9), and chromium in the sample solution was oxidized to chromium (VI) with 2.0 mL of 10 g/L potassium permanganate solution in sulfuric acid medium. After that, excessive 200 g/L sodium carbonate solution was added to precipitate and separate the coexisting elements such as iron and nickel. Finally, the coloring reaction of chromium with diphenylcarbazide was conducted in 0.05-0.2 mol/L sulfuric acid for the determination. The proposed method was applied to the determination of ferrosilicon nitride sample. The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). The relative standard deviation (RSD, n=11) was less than 2%. The recovery test of standard addition indicated that the recovery was 101%.
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