ANALYSIS OF SULFUR COMPOUNDS ACCORDING TO ASTM D5504

Importance of the Topic

The detection of sulfur in natural gas and gaseous fuels is critical due to its corrosive, toxic, and odorous properties. Reliable quantification of sulfur species supports regulatory compliance, process optimization, and product quality control across upstream and downstream operations. Advanced analytical methods, such as gas chromatography combined with sulfur-selective detection, address the need for sensitive, fast, and robust measurements.

Objectives and Study Overview

This study evaluates the performance of the Agilent 8355 Sulfur Chemiluminescence Detector (SCD) coupled with gas chromatography for analyzing sulfur compounds in various gaseous matrices according to ASTM D5504. The main goals are to confirm detector linearity, sensitivity (LOD/LOQ), robustness, and operational ease for applications in natural gas, refinery fuel gases, and related streams.

Methodology and Instrumentation

Gas samples were introduced using a two-valve system with constant pressure helium carrier gas at 14.5 psi. Separation employed an Agilent DB-Sulfur column (320 µm × 60 m, 4.2 µm). Oven programming started at 30 °C (1.5 min), ramped at 15 °C/min to 250 °C (3 min). The SCD used a dual-plasma burner and reaction cell, generating chemiluminescence from the reaction of ozone with sulfur monoxide produced during combustion.
Key detector conditions:

• Detector base temperature: 250 °C
• Furnace temperature: 800 °C
• Ozone generated with O2 flow: 40 mL/min
• H2 flow: 38 mL/min (lower/oxidation), 8 mL/min (upper)
• Air flow for oxidation: 60 mL/min

Instrumentation Used

• Agilent 8355 Sulfur Chemiluminescence Detector
• Gas chromatograph equipped with an Agilent DB-Sulfur capillary column
• Ozone generator and dual-plasma burner module

Main Results and Discussion

Sensitivity tests using a 2.3 ppm sulfur standard demonstrated excellent detection limits across 15 analytes. More than half of the compounds exhibited LODs below 0.5 pg/sec. Representative detection limits include:

• Hydrogen sulfide: 0.096 pg/sec
• Carbonyl sulfide: 0.20 pg/sec
• Dimethyl sulfide: 0.20 pg/sec
• Methyl mercaptan: 0.49 pg/sec
• Thiophene: 0.21 pg/sec

Performance confirms the SCD’s capability for both qualitative and quantitative sulfur analysis in complex gaseous matrices.

Benefits and Practical Applications

• High sensitivity and selectivity for a wide range of sulfur compounds
• Robust operation with non-quenching performance and linear response
• Rapid analysis suitable for process monitoring and quality control
• Low detection limits enabling trace-level impurity detection

Applications include upstream gas quality assessment, odorant verification, environmental monitoring, and refinery gas analysis.

Future Trends and Applications

Advances in detector design and integration with automated sampling systems will further enhance throughput and reduce maintenance. Emerging needs in biogas analysis, hydrogen fuel monitoring, and stringent environmental regulations will drive adoption of sulfur-selective detectors. Coupling with data-rich platforms and AI-enabled analytics can provide real-time process insights.

Conclusion

The Agilent 8355 Sulfur Chemiluminescence Detector offers a robust, user-friendly solution for selective sulfur analysis by gas chromatography, meeting demanding sensitivity and regulatory requirements. Its performance in terms of LOD, linearity, and operational stability ensures reliable data for process optimization and compliance.

Reference

Agilent Technologies. Agilent 8355 Sulfur Chemiluminescence Detector: Analysis of Sulfur Compounds According to ASTM D5504. Application Note 5991-6552EN. January 2016.