Oxygen and Hydrogen Determination in Titanium Hydride

Importance of the Topic

Titanium hydride serves as a cost-effective alternative to titanium powder, offering comparable mechanical properties and simplified processing. Its inherent hydrogen content (~4.04 wt %) makes it valuable for applications such as metal foaming, gettering of impurities, powder metallurgy additives and advanced research in hydrogen storage. Accurate determination of oxygen and hydrogen levels is vital for predicting material performance and ensuring consistent quality control in industrial and research settings.

Objectives and Study Overview

This application note presents a validated procedure for simultaneous measurement of hydrogen and oxygen in titanium hydride samples using LECO’s ONH836 inert gas fusion analyzer. The protocol covers sample preparation, instrument blanking, calibration and drift correction, through to final analysis, highlighting the low-temperature hydrogen determination followed by high-temperature oxygen evaluation.

Instrumentation Used

• ONH836 Series inert gas fusion analyzer
• Graphite crucibles (part 782-720)
• Nickel capsules (part 502-822)
• Lower electrode tips: 782-721 (manual) or 618-376 (automated)

Methodology and Instrumentation

Samples of uniform titanium hydride powder or chips are weighed (≈0.10 g) into open nickel capsules using clean tweezers and a five-place balance. The instrument blank is established with at least three replicates, followed by calibration using reagent grade TiH2 for hydrogen and copper pin standards for oxygen. Key analysis parameters include:

• Hydrogen determination at low temperature with 10 s integration delay and 210 s integration time
• Oxygen determination at high temperature with 5 s integration delay and 210 s integration time
• Furnace settings: initial outgas cycles, constant and ramped power modes up to 4800 W
• Helium carrier gas; argon use requires adjusted power and extended integration times

Key Results and Discussion

Reagent grade TiH2 calibrant yielded a mean hydrogen content of 4.02 % (s = 0.01 %) and oxygen of 0.54 % (s = 0.01 %). Copper pin standards confirmed oxygen performance at 0.054 % (s = 0.0002 %). A test TiH2 sample showed 3.99 % hydrogen (s = 0.01 %) and 0.67 % oxygen (s = 0.01 %). The method demonstrated excellent precision, linear calibration forced through the origin and reliable blank correction.

Benefits and Practical Applications

• Simultaneous determination of hydrogen and oxygen in a single run increases throughput
• High reproducibility supports stringent quality control in powder metallurgy and materials research
• Automatable workflow and rapid analysis cycles enable integration into production laboratories

Future Trends and Opportunities

With the growing demand for advanced hydride materials and hydrogen storage, this method can be extended to other metal hydrides and fine powders. Automation enhancements and integration with real-time data analytics will further streamline quality assurance. Adapting carrier gases and refining furnace power profiles will expand the technique’s versatility for diverse sample matrices.

Conclusion

The described inert gas fusion procedure on the ONH836 analyzer offers a robust, precise and efficient approach for quantifying oxygen and hydrogen in titanium hydride. It underpins critical quality metrics for industrial production and advanced research, ensuring consistent material performance.

Reference

No external literature references were provided in the original application note.