ボロン処理鋼中の微量ボロンの態別定量

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This paper is a part of the general investigation of new metallographic analyses for steel. A simple and reliable method is described for the metallographic analysis of microamount of boron in boron treated steel, by a new electrolytic extraction method using NaCl-EDTA solution as an electrolyte. The procedure is as follows : 1. Separation of boron compound from steel. (a) Cover the steel sample with close-texture filter paper as a diaphragm, connected as an anode, is dissolved into 100 to 150 ml of 1% NaCl-5% EDTA electrolyte (pH 6∿7) at a current density of 50 mA/cm^2 for 2 to 4 hr. Remove the anode, and residue is collected into the filter paper. Transfer the paper and residue to a quartz beaker, and 20 ml of HNO_3 (1 : 2) and boil for 5 min. (b) Filter and wash with hot water. Add 12 ml of H_2SO_4 (1 : 1) and 6 ml of H_3PO_4 (1 : 1) to the filterate and evaporate to copious fumes. Dissolve the salt with 50 ml of water, cool, dilute to 250 ml, and determine boron as carbide continue in accordance with section 2. (c) Add 12 ml of H_2SO_4 (1 : 1) and 10 ml of H_2O_2 to the electrolyte and boil for 30 min, cool, dilute to 250 ml, and determine boron as solid solution continue in accordance with section 2. (d) Transfer the paper and residue (Paragraph (b)) to a quartz beaker, add 20 ml of HCl (1 : 1) and boil for 10 min. (e) Filter and wash with hot water. Add 1 ml of HNO_3 (conc.), 6 ml of H_2SO_4 (1 : 1) and 4 ml of H_3FO_4 (1 : 1) to the filterate and evaporate to copious fumes. Dissolve the salt with 10 ml of water, cool, dilute to 100 ml, and determine boron as oxide continue in accordance with section 2. (f) Transfer the paper and residue (Paragraph (e)) to a platinum crucible, and ingnite at 500℃. Add 1 g of Na_2CO_3 and heat gradually until fusion is complete. Cool, take up the melt in 6 ml of H_2SO_4 (1 : 1), and dilute to 100 ml, and determine boron as nitride continue in accordance with section 2. 2. Determination of boron compound. Transfer 25 ml of each of the solution of section 1. (b), (c), (e), and (f) to separatory funnel. Add 10 ml of water and 5 ml of HF (5%) and let stand for 1 hr. Add 20 ml of water, 2 ml of methylene blue solution (0.001 M) and 25 ml of dichlorocthane, and shake for 1 min. Let stand for 5 min to allow the layers to separate. Filter the dichlorosthane solution through a dry filter paper into a dry absorption cell. Measure the absorbance against blank solution at 660 mμ.
社団法人日本鉄鋼協会の論文
1970-05-01

ボロン処理鋼中の微量ボロンの態別定量

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