高張力鋼中のニオブの態別定量

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A new, simple and reliable method has been developed for metallographic analysis of Nb in high strength steel. The procedure is as follows : 1. Separation of Nb a) Dissolve 1 g of sample in 40 ml of HCl (1 : 1) at room temperature. Filter and wash with water. b) Dilute the filterate to 250 ml with water, add 10 ml of phytin solution (1%), and boil for 10 min, and allow to stand for 5 min. Filter and wash 2 or 3 times with hot water. c) Return the paper and precipitate to the beaker, add 20 ml of HNO_3, 3 ml of HClO_4, and 2 ml of H_2SO_4 (1 : 1), and evaporate to a sirup, and determine Nb as solid solution as described in Section 2 a) to c). d) Transfer the paper and residue (Paragraph a) to the beaker, add 20 ml of HNO_3 (1 : 1) and 5 ml of H_2O_2, and boil for 5 min. Filter and wash 2 or 3 times with hot water. e) Add 2 ml of H_2SO_4 (1 : 1) to the filterate and evaporate to a sirup, and determine Nb as carbonitride as described in Section 2 a) to c). f) Transfer the paper and residue (Paragraph d) to the beaker, add 20 ml of HNO_3, 3 ml of HClO_4, and 2 ml of H_2SO_4 (1 : 1), and evaporate to a sirup, and determine Nb as oxide as described in Section 2 a) to c). 2. Photometric determination of Nb a) Dissolve each of the salt of section 1・c), e) and f) in 20 ml of tartaric acid solution (20%) and 10 ml of HOl (1 : 1) and dilute to 100 ml in a volumetric flask. b) Transfer 5 ml portion of solution to 50 ml volumetric flask, add 15 ml of water, and 2 ml of thioglycollic acid solution (10%), mix, allow to stand for 2 min, and then, add 10 ml of HCl (1 : 1), 5 ml of EDTA solution (1%), 5 ml of aceton and 2 ml of sulfochloro phenol S solution (0.05%). c) Warm to 60 to 70℃ for 5 min, cool, dilute to the mark, and mix. Measure the absorbance against water at 650 mμ.
社団法人日本鉄鋼協会の論文
1969-05-01

著者

若松茂雄
トピー工業(株)開発本部

高張力鋼中のニオブの態別定量

スポンサーリンク

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