低合金鋼中のモリブデンの状態分析

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This work, a part of a general program of research on the state analysis of steel, was carried out to develop a simple method for extraction and determination of molybdenum carbides [(Fe, Mo)_3C and Mo_2C] in low alloy steel. The procedure is as follows : 1. Extraction of molybdenum carbides from steel. (a) Cover the steel sample with close-texture filter paper as a diaphragm, connected as an anode, is dissolved into 100 to 130ml of 1% NaCl-5% EDTA electrolyte (H 6 to 7) at a current density of 50mA/cm^2 for 1 to 2 hr. Remove the anode and the residue is collected into an Erlenmeyer flask. To the residue add 20ml of 6N HCl and pass in a stream of argon gas for 10 min at room temperature. (b) Filter and wash with water. Add 5ml of HNO_3 and 10ml of HClO_4 to the filtrate and evaporate to dense white fumes. Cool dilute to 100ml and determine Mo as (Fe, Mo)_3C in accordance with section 2. (c) Transfer a quarter of the electrolyte to a beaker. Add 20ml of HNO_3 and 10ml of HClO_4 and evaporate to dense white fumes. Cool, dilute to 100ml and determine Mo as solid solution in accordance with section 2. (d) Transfer the paper and residue (paragraph (b)) to a beaker, and 30ml of HNO_3 and 10ml of HClO_4 and evaporate to dense white fumes. Cool, dilute to 100ml and determine Mo as Mo_2C in accordance with section 2. 2) Photometric determination of molybdenum. Transfer 10 to 20ml of each of solutions (section 1 (b), (c) and (d)) to 50ml volumetric flasks. If the iron contents is less than 40mg, add iron solution (0.02g Fe/ml) until a total of 40 to 50mg of iron. To each flask add 5ml of thiourea solution (10%), 8ml of HClO_4, 2ml of NaCNS solution (30%) and 10ml of ascorbic acid solution (5%), dilute to 50ml and let stand for 10min. Measure the absorbance of solution against water at 460mμ. A complete analysis can be carried out in 3 to 4hr.
社団法人日本鉄鋼協会の論文
1972-03-01

低合金鋼中のモリブデンの状態分析

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