Turning the Heat up on Gas Chromatography - How to Successfully Perform High Temperature GC Applications without Breaking a Sweat

Importance of the Topic

High-temperature gas chromatography (HTGC) enables the analysis of high-boiling, thermally stable compounds critical to industries such as petrochemicals, polymers, food, and environmental monitoring. Extending the temperature range beyond traditional GC limits improves separation of semi-volatiles, reduces analysis time, and enhances method robustness.

Objectives and Overview

This work outlines best practices for performing HTGC up to 450 °C without compromising column integrity or instrument performance. It reviews stationary phase selection, column substrates, consumables, and leak prevention. Comparative evaluations of fused silica, stainless steel, and advanced UltiMetal columns are presented.

Methodology and Instrumentation

The study employed Agilent J&W columns including DB-5ht and DB-HT SimDis ProSteel with dimensions ranging from 5 m×0.535 mm×0.15 µm to 30 m×0.25 mm×0.10 µm. Carrier gas was helium at constant flows of 1–18 mL/min. Injection used a multimode inlet (MMI) in split and splitless modes. Detection techniques included flame ionization detection (FID), sulfur chemiluminescence detection (SCD), and GC–MS with Ultra Inert MS UI columns for mass spectrometry work. High-temperature consumables comprised graphite ferrules, BTO septa, and gas clean filters.

Main Results and Discussion

• High-temperature stationary phases (PDMS, phenyl-methyl) on polyimide-coated fused silica maintain peak shape and efficiency at 400 °C for over 100 h.
• Standard fused silica degrades above 400 °C, forming surface “potholes,” increasing bleed and retention variability.
• Deactivated stainless steel and UltiMetal columns operate reliably up to 450 °C, offering lower bleed and sustained efficiency.
• Shorter columns with thin films accelerate elution of heavy analytes, while thicker films extend column lifetime at high temperatures.
• HTGC–MS is limited by ion source and quadrupole temperature constraints; Ultra Inert MS columns deliver superior performance for mass spec analysis.

Benefits and Practical Applications

HTGC methods allow improved resolution of polymer additives, crude oil residues, sterols, waxes, and triglycerides. Proper consumable selection prevents leaks, reduces column bleed, and extends service life, yielding faster throughput and more reliable data in quality control and research laboratories.

Future Trends and Opportunities

Emerging column substrates, such as glass-infused metals, next-generation coatings, and smart gas filters, will further enhance HTGC capabilities. Integration with automated sample introduction and advanced high-temperature detectors will expand applications in environmental screening, materials science, and complex mixture analysis.

Conclusion

Successful HTGC demands an integrated approach: selecting high-temperature phases, robust column substrates, compatible consumables, and optimized operating parameters. Agilent J&W high-temp and metal columns demonstrate consistent performance at 400–450 °C, enabling reliable analysis of challenging, high-boiling compounds.

References

1. John V. Hinshaw. The Making of a Column. LCGC Europe, 19(2):93–98, 2006.
2. Agilent Technologies. Publication 5994-1013EN.
3. Agilent Technologies. Publication 5994-1385EN.
4. Agilent Technologies. Publication 5994-1384EN.