Oxygen and Hydrogen Determination in Copper and Copper Alloys

Significance of the Topic

Accurate measurement of oxygen and hydrogen content in copper and its alloys is essential for ensuring optimal electrical conductivity, mechanical strength and corrosion resistance. Trace levels of these interstitial elements can significantly affect the performance of copper-based components in electronics, power transmission and industrial applications.

Objectives and Study Overview

This application note demonstrates a reliable procedure for semi-automated determination of oxygen and hydrogen using the ROH600 and TCH600 inert-gas fusion analyzers. The study outlines sample preparation, calibration, analysis parameters and variant loading methods, with the goal of achieving precise, reproducible results across solid, powder and chip forms of copper materials.

Methodology and Instrumentation

Samples are first abraded, cleaned with methanol and dried. Analysis is performed on ROH600/TCH600 instruments equipped with:

• 782-720S crucibles, 761-739 tin pellets
• 501-059 or 502-040 tin capsules and 617-997 funnel for manual top loading
• Calibration standards such as LECO and NIST copper reference materials

Key parameters include three outgas cycles, defined analysis delays, current-controlled furnace power (650–850 amps) and element-specific integration delays. Calibration and drift correction are carried out by repeated runs of known reference materials following blank determinations.

Main Results and Discussion

Typical solid copper samples yielded oxygen levels around 5.8 ppm (s=0.38 ppm) and hydrogen around 1.30 ppm (s=0.087 ppm). Oxygen-free high-conductivity (OFHC) copper showed lower oxygen (3.8 ppm, s=0.49 ppm) and similar hydrogen (0.78 ppm, s=0.056 ppm). Tin-capsule and chip methods produced oxygen near 311 ppm and hydrogen near 0.33 ppm (s=0.03 ppm). Manual top load of chip samples achieved oxygen at 309 ppm (s=4 ppm) and hydrogen at 0.25 ppm (s=0.05 ppm). Variations reflect sample form and loading technique, highlighting the importance of blank control and consistent handling.

Benefits and Practical Applications

The described method delivers high sensitivity and precision for trace O and H analysis in copper alloys. Its semi-automated workflow reduces operator variability, making it suitable for QA/QC in metallurgy, electronic materials manufacturing and research laboratories.

Future Trends and Potential Uses

Advancements may include full automation of sample loading, integration of smaller-volume crucibles for micro-samples, direct powder analysis without capsules and the incorporation of data analytics or machine learning to optimize calibration and drift correction.

Conclusion

The ROH600/TCH600 inert-gas fusion method offers a robust, reproducible approach for determining oxygen and hydrogen in diverse copper sample types. Careful sample preparation, calibration and method tuning ensure reliable trace analysis for industrial and research applications.

References

LECO Corporation Form No. 203-821-276 Application Note, 2005