Analysis of Sulfur Compounds in High-Purity Hydrogen

Significance of the Topic

Trace sulfur impurities in high-purity hydrogen can deactivate catalysts, compromise fuel cell performance, and jeopardize product quality. Monitoring sulfur at the parts-per-billion level is therefore essential for the hydrogen supply chain and industrial applications.

Goals and Study Overview

This study evaluates a gas chromatographic method coupled with sulfur chemiluminescence detection to quantify seven sulfur species in high-purity hydrogen. The aim is to demonstrate method sensitivity, linearity, and repeatability down to low-ppb levels.

Methodology

Samples were introduced using a six-port gas sampling valve with a 2 mL loop into an inert flow path. A split ratio of 10:1 and a volatiles interface minimized peak tailing. Calibration standards from 10 to 200 ppb were generated dynamically with a mini gas blender. The oven program ramped from 40 °C (1 min) to 230 °C at 15 °C/min.

Instrumentation

• Agilent 8890 gas chromatograph
• Agilent 8355 sulfur chemiluminescence detector
• Agilent J&W DB-Sulfur SCD column (60 m×0.32 mm, 4.2 µm)
• Pneumatic control module with mini gas blender
• Six-port gas sampling valve and inert tubing
• Helium carrier gas and inert regulator

Results and Discussion

System passivation and priming stabilized adsorption of reactive sulfur species after approximately 50 injections. Chromatograms showed baseline separation of H2S, COS, CH3SH, C2H5SH, CH3SCH3, CS2, and thiophene. Repeatability RSDs were 7.4% at 15 ppb, decreasing to below 2.2% at 200 ppb. Linearity (R2 ≥ 0.9983) confirmed equimolar detector response. Practical LOD was below 10 ppb, and LOQ around 15 ppb based on S/N criteria.

Practical Benefits and Applications

This GC–SCD approach offers sensitive, interference-free quantitation of trace sulfur in hydrogen. It supports quality control, catalyst protection, regulatory compliance, and research in fuel cell development and industrial gas supply.

Future Trends and Opportunities

Advances may include inline monitoring, further miniaturization, lower detection limits, multi-impurity analysis, and integration with digital data platforms and AI algorithms for automated gas quality assessment.

Conclusion

The combination of Agilent 8890 GC and 8355 SCD delivers reliable detection of sulfur down to low-ppb levels with excellent linearity and repeatability, making it well suited for high-purity hydrogen analysis.

References

• Xu C, Xu G. Analysis Technology of Trace Impurities in Hydrogen for Hydrogen Fuel Cell Vehicles. Chemical Industry and Engineering Progress. 2021;40(2):688–702.
• Bu T. Hydrogen Impurity Analysis Using the Agilent 990 Micro GC. Agilent Technologies Application Note 5994-2138EN. 2020.
• Li W. Analysis of Trace Carbon Dioxide and Permanent Gas Impurities in Fuel Cell Hydrogen and High-Purity Hydrogen Using the Agilent 8890 GC-PDHID System. Agilent Technologies Application Note 5994-4045ZHCN. 2021.