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 130
ml 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 20
ml of 6N HCl and pass in a stream of argon gas for 10 min at room temperature.
(b) Filter and wash with water. Add 5
ml of HNO
3 and 10
ml of HC1O
4 to the filtrate and evaporate to dense white fumes. Cool dilute to 100
ml and determine Mo as (Fe, Mo)
3C in accordance with section 2.
(c) Transfer a quarter of the electrolyte to a beaker. Add 20
ml of HNO
3 and 10
ml of HC1O
4 and evaporate to dense white fumes. Cool, dilute to 100
ml and determine Mo as solid solution in accordance with section 2.
(d) Transfer the paper and residue (paragraph (b)) to a beaker, and 30
ml of HNO
3 and 10
ml of HC1-O
4 and evaporate to dense white fumes. Cool, dilute to 100
ml and determine Mo as Mo
2C in accordance with section 2.
2) Photometric determination of molybdenum.
Transfer 10 to 20
ml of each of solutions (section 1 (b), (c) and (d)) to 50
ml volumetric flasks. If the iron contents is less than 40 mg, add iron solution (0.02g Fe/m/) until a total of40 to 50 mg of iron. To each flask add 5
ml of thiourea solution (10%), 8
ml of HC1O
4, 2
ml of NaCNS solution (30%) and 10
ml of ascorbic acid solution (5%), dilute to 50
ml and let stand for 10 min. Measure the absorbance of solution against water at 460 mu.
A complete analysis can be carried out in 3 to 4 hr.
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