チタン処理鋼中のチタンの態別定量

Abstract

A simple accurate method for the metallographic analysis of titanium in titanium treated steel is devised. The procedure is as follows:1. Separation of titanium:(a) Dissolve 1 g of sample in 30 ml of HCl (1: 2). Filter and wash with hot HCl (1: 9).(b) Dilute the filtrate to 50 ml in a volumetric flask, and determine titanium as solid solution continue in accordance with section 2 (a) to (c).(c) Transfer the paper and residue (Paragraph (a)) to the beaker, add 30 ml of HNO3 (1: 1) and boil for 5 min. Filter and wash with hot water.(d) Add 2 ml of H2SO4 to the filtrate and evaporate to a sirup. Dissolve salt with 40 ml of HC1 (1: 1), cool, dilute to 100 ml or 200 ml in a volumetric flask, and determine titanium as carbide continue in acordance with section 2 (a) to (c).(e) Transfer the paper and residue (Paragaph (c)) to the beaker, add 20 ml of HNO3 (1: 1) and 5 ml of H202, and boil for 10 min. Filter and wash with hot water.(f) Add 2 ml of H2SO4 to the filtrate and evaporate to a sirup. Disslove salt with 10 ml of HCl (1: 1), cool, dilute to 50 ml in a volumetric flask, and determine titanium as nitride continue in accordance with section 2 (a) to (c).(g) Transfer the paper and residue (Paragraph (e)) to the beaker, add 40 ml of HNO3, 3 ml of HClO4, and 2 ml of H2SO4, and evaporate to a sirup. Dissolve salt with 10 ml of HCl (1: 1), cool, dilute to 50 ml in a volumetric frask, and determine titanium as oxide continue in accordance with section 2 (a) to (c).2. Photometric determination of titanium:(a) Sample solution-Transfer 10 ml aliquot of solution Section (b), (d), (f) and (g) to 50 ml volumetric flask, add 5 ml of H2O and 8 ml of ascorbic acid solution (10%) to reduce iron, and then add 5 ml of HCl (1: 1) and 20 ml of diantipyrylmethane solution (1.5%), dilute to the mark.(b) Reference solution-Carry through all the steps of the procedure as directed in paragraph (a). However, no add diantipyrylmethane solution.(c) After 20 min, measure the absorbance against reference solution at 385 μ