ANALYSIS OF SULFUR COMPOUNDS ACCORDING TO ASTM D5623

Analysis of Sulfur Compounds by GC-SCD According to ASTM D5623

Significance of the Topic

Gas chromatography with sulfur chemiluminescence detection provides critical insight into trace sulfur compounds in petrochemical streams. Elevated sulfur levels can lead to corrosion, catalyst poisoning, and environmental non-compliance. Accurate, reliable sulfur analysis supports product quality, safety, and regulatory adherence in industries handling fuels, solvents, and monomers.

Objectives and Study Overview

The study aims to evaluate the performance of the Agilent 8355 Sulfur Chemiluminescence Detector (SCD) integrated into the Agilent 7890B GC for quantifying sulfur compounds per ASTM D5623 criteria. It demonstrates detector linearity, sensitivity, and robustness through analysis of 23 sulfur standards at 1 ppm in isooctane.

Instrumentation

• Gas Chromatograph: Agilent 7890B GC
• Detector: Agilent 8355 Sulfur Chemiluminescence Detector
• Column: Agilent J&W DB-Sulfur SCD or DB-1, 30 m × 0.32 mm × 0.25 µm
• Inlet: Split mode 10:1, 1 µL injection at 275 °C
• Carrier Gas: Helium, constant flow of 2.0 mL/min
• Oven Program: 40 °C (1 min), ramp 10 °C/min to 250 °C (8 min)
• SCD Conditions:
  • Base temperature: 250 °C
  • Furnace: 800 °C
  • Air flow (oxidation): 60 mL/min
  • Ozone generator (O2): 40 mL/min
  • H2 flows: lower 38 mL/min, upper 8 mL/min

Key Results and Discussion

The chromatogram resolved 23 sulfur species including thiols, sulfides, and thiophenes with sharp, well separated peaks at 1 ppm. The detector exhibited a linear response across the tested concentration range and low limit of detection/quantitation. Baseline stability and non-quenching behavior were confirmed under the specified conditions, ensuring reliable quantification.

Benefits and Practical Applications

• High sensitivity and selectivity for trace sulfur analysis
• Non-quenching operation extends linear dynamic range
• Robust workflow suitable for walk-up laboratories
• Applicable to fuels, solvents, monomers, and natural gas fractions

Future Trends and Potential Applications

Advances may include integration with mass spectrometry for structural elucidation, miniaturized GC-SCD systems for field deployment, and automated data processing through AI-driven platforms. Expanded use in real-time process monitoring could further enhance petrochemical manufacturing efficiency.

Conclusion

The Agilent 7890B GC coupled with the 8355 Sulfur Chemiluminescence Detector meets and exceeds ASTM D5623 requirements for trace sulfur analysis, offering robust performance, ease of use, and broad applicability across the petrochemical industry.

References

1. ASTM D5623: Standard Test Method for Sulfur Compounds in Gaseous Hydrocarbons by Gas Chromatography and Sulfur Chemiluminescence Detection.
2. Agilent Technologies. 8355 Sulfur Chemiluminescence Detector Datasheet, 2015.