日本金属学会誌

J. Japan Inst. Metals, Vol. 36, No. 1 (1972),
pp. 66-72

Determination of Titanium Oxide, Titanium Carbide and Titanium Nitride in Ni-Ti Alloy

Iwao Tsukahara1 and Emi Yabuki1

1Furukawa Electric Co., Ltd., Central Research Laboratory, Tokyo

Abstract:

A method for the fractional determination of titanium oxide, titanium carbide and titanium nitride in Ni-Ti alloy has been presented. For the determination of titanium oxide and carbide, 1 g of the sample is dissolved with bromine-methyl acetate (20 mL of bromine+200 mL of methyl acetate) in a decomposition flask below 20°C for 1 hr. The solution is filtered by suction through a Millipore filter (UGWP). The residue is washed with methanol and treated with 10 mL of HF (46%) on a boiling water bath for 20 min. The solution is filtered by suction through a Millipore filter (UGWP) and the amount of titanium in this solution (titanium present as oxide inclusion) is determined spectrophotometrically with 8-hydroxyquinoline. The residue undissolved with HF is treated with 25 mL of HNO3(1+1) and 5 mL of HF(46%) on a boiling water bath for 30 min. The solution is filtered and the amount of titanium in this solution (the sum of titanium present as carbide and nitride) is determined. Then, the amount of titanium present as carbide is determined by subtracting the amount of titanium present as nitride which is determined by the Kjeldahl method.
For the determination of titanium nitride, 5 g of the sample is dissolved with methanolic bromine (20 mL of bromine+200 mL of methanol) in a decomposition flask below 20°C for 1 hr. The solution is filtered by suction through a Millipore filter (UGWP). The residue is washed with methanol and treated with 7 mL of HF(46%) and H2O2(30%) on a boiling water bath for 1 hr. Ammonia in the solution obtained is determined by the Kjeldahl method and the amount of titanium present as nitride (TiN) is calculated.
The optimum conditions for extracting the titanium compounds from Ni-Ti alloy with methanolic bromine or with bromine-methyl acetate and for the fractional determination of titanium compounds have been investigated. A comparison of methanolic bromine method and bromine-methyl acetate method has been made and the structures of titanium compounds in Ni-Ti alloy are discussed.


(Received 1971/9/23)

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