Quantitative determination of nitrogen in titanium nitride involves dissolution of TiN in 10M hydrofluoric acid containing an oxidant. Released nitrogen is determined as ammonia. Best oxidizers are ferric chloride, potassium iodate, and potassium dichromate

Philipp, W. H.

Tetzlaff, J. E.

English

NASA Technical Reports Server

November 1970
	
Brief 70-10588 
NASA TECH BRIEF 
NASA Tech Briefs announce new technology derived from the U.S. space program. They are issued to encourage commercial
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application. Tech Briefs are available on a subscription basis from the Clearinghouse for Federal Scientific and Technical 
Information, Springfield, Virginia 22151. Requests for individual copies or questions relating to the TechBrief program may 
be directed to the Technology Utilization Division, NASA, Code UT, Washington, D.C. 20546. 
Determination of Nitrogen in Titanium Nitride 
A simple, reliable method has been developed for 
the quantitative determination of nitrogen in titanium 
nitride (TiN). The procedure involves dissolution of 
TiN in IOM hydrofluoric acid containing an oxidant; 
the released nitrogen is determined as ammonia. 
Interest in TiN as a refractory material has led to 
considerable investigation of its chemical and physical 
properties. Because TiN often varies widely from stoi-
chiometry, the need of a simple chemical method for 
accurate determination of its nitrogen is apparent. 
Standard techniques such as the Dumas or Kjeldajl 
method give poor results. 
This work is an extension of earlier investigations 
of the chemical reactions of nitrides. One difficulty 
encountered during the analysis of TiN is its inertness 
to many common laboratory reagents. The material is 
not readily dissolved by aqueous acids such as H 2 SO4, 
HCI, H NO 3 , and hot IOM HF, and there is little or no 
reaction with aqueous4MNaOHat 100°C. On the other 
hand a IOM HF solution containing a suitable oxi-
dizer readily dissolves TiN, converting the nitrogen 
quantitatively to NH4.
Selection of a proper oxidizing agent is of prime im-
portance to the method. In terms of accuracy and 
convenience the best oxidizers are ferric chloride, 
potassium iodate, and potassium dichromate. The re-
sultant NH 4 is determined by standard volumetric 
titration. With use of these oxidizers the results for 
titanium and for nitrogen deviate less than 0.1% from 
those for a sample known to be stoichiometric TiN. 
Note: 
Requests for further information may be directed to: 
Technology Utilization Officer 
Lewis Research Center 
21000 Brookpark Road 
Cleveland, Ohio 44135 
Reference: TSP70- 10588 
Patent status: 
No patent action is contemplated by NASA. 
Source: W. H. Philipp and J. E. Tetzlaff 
Lewis Research Center 
(LEW-1 1046) 
Category 04 
This document was prepared under the sponsorship of the National 
Aeronautics and Space Administration. Neither the United States 
Government nor any person acting on behalf of the United States
Government assumes any liability resulting from the use of the 
information contained in this document, or warrants that such use 
will be free from privately owned.rights.
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Determination of nitrogen in titanium nitride

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