高張力鋼中のバナジウムの態別定量

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A simple and accurate method has been developed for the metallographic analysis of vanadium in high strength steel. 1. Separation of vanadium compound from steel. (a) The steel sample covered with close-texture filter paper as a diaphragm and connected as an anode, is dissolved into 100 to 130 ml of 1% NaCl-5% EDTA electrolyte (pH 6-7) with current density of 50 mA/cm^2 for 1 to 2 hr. Remove the anode, and residue is collected into the filter paper. To the residue and filter paper add 50 ml of HCl (1 : 4), and pass in a stream of air for 30min at room temperature. (b) Filter and wash with water. Add 5ml of HNO_3 and 10ml of HClO_4 to the filterate and evaporate to dense white fumes, cool, dilute to 50ml and determine vanadium as (Fe, V)_3C in accordance with section 2. (c) Add 30ml of HNO_3 and 20ml of HClO_4 to the electroyte and evaporate to dense white fumes, cool, dilute to 100ml, and determine vanadium as solid solution in accordance with section 2. (d) Transfer the paper and residue (paragraph (b)) to a beaker, add 30ml of HCl (1 : 1) and boil for 5min. (e) Filter and wash with water. Add 5ml of HNO_3 and 10ml of HClO_4 to the filterate and evaporate to dense white fumes, cool, dilute to 50ml, and determine vanadium as V_2O_3 in accordance with section 2. (f) Transfer the paper and residue (paragraph (e)) to a beaker, add 40ml of HNO_3 (1 : 3), and boil for 5min. (g) Filter and wash with water. Add 10ml of HClO_4 to the filterate and evaporate to dense white fumes, cool, dilute to 50ml, and determine vanadium as V_4C_3 in accordance with section 2. (h) Transfer the paper and residue (paragraph (g)) to a beaker, add 30ml of HNO_3 (1 : 1) and 5ml of H_2O_2 and boil for 10min. (i) Filter and wash with water. Add 10ml of HClO_4 to the filterate and evaporate to dense white fumes, cool, dilute to 50ml, and determine vanadium as VN in accordance with section 2. Discard the residue. 2. Photometric determination of vanadium. Transfer 20ml of each of solutions (section 1. (b), (c), (e), (g) and (i)) to separatory funnels, add 2ml of copper solution (0.5%) and 1 drop of KMnO_4 solution (1%), and let stand for 5min. Add 15ml of N-benzoylphenylhydroyxylamine chloroform solution (0.067%) and 10ml of HCl (2 : 1), and shake for 30 sec. Measure the absorbance of organic phase against chloroform at 530mμ.
社団法人日本鉄鋼協会の論文
1970-09-01

高張力鋼中のバナジウムの態別定量

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