GC
IndustriesEnergy & Chemicals
ManufacturerAgilent Technologies
Importance of the Topic
Monocyclic aromatic hydrocarbons such as benzene, toluene, ethylbenzene, p-xylene, and styrene are widely used in polymer, additive, and specialty chemical production. Accurate and rapid purity assessment of these solvents is critical for quality control in petrochemical and manufacturing laboratories. The ASTM D7504 method provides a streamlined, reliable procedure to quantify trace impurities and overall purity without complex sample preparation.
Objectives and Study Overview
This work evaluates a dual-channel Agilent 8890 GC system configured with two J&W DB-HeavyWAX columns for analysis of monocyclic aromatics per ASTM D7504. Key goals were to:
- Double sample throughput via dual-simultaneous injections
- Implement retention time locking (RTL) to achieve consistent retention times across channels
- Verify separation performance and quantitative range from 0.0004 to >99.9 wt %
- Demonstrate compliance with ASTM repeatability requirements for multiple solvents
Used Instrumentation
- Agilent 8890 Gas Chromatograph with dual split/splitless inlets
- Dual Agilent 7693A Automatic Liquid Samplers
- Two J&W DB-HeavyWAX capillary columns (60 m × 0.32 mm, 0.25 µm film)
- Dual Flame Ionization Detectors (FIDs)
- Agilent OpenLab ChemStation software
Methodology
Sample introduction and GC conditions were set according to ASTM D7504:
- Injection volume: 0.6 µL, split ratio 100:1
- Carrier gas: helium, constant flow at 1.2 mL/min
- Oven program: 60 °C (10 min) → 150 °C at 5 °C/min (2 min hold)
- Inlet and detector temperatures: 270 °C and 300 °C
- Detector flows: air 400 mL/min, hydrogen 30 mL/min, nitrogen makeup 25 mL/min
- Retention time locking (RTL) calibrated using o-xylene target peak to align both channels within <0.01 min
Main Results and Discussion
Dual-channel analysis achieved a 100 % increase in throughput without loss of precision. Baseline separation was obtained for most target compounds; known coelutions (e.g., 3- and 4-ethyltoluene) are consistent with method allowances. RTL reduced inter-channel retention time differences from ~0.1 min to <0.01 min, simplifying peak identification and calibration. Purity assessments for benzene, toluene, ethylbenzene, p-xylene, and styrene met or exceeded ASTM repeatability criteria, detecting impurities down to 0.0004 wt %.
Practical Benefits and Applications
• Eliminates sample preparation and external calibration through Effective Carbon Number (ECN) responses
• Ensures comparable data across instruments and laboratories via RTL
• Provides a broad dynamic range from trace level to >99 wt % for impurity profiling
• Doubles lab productivity without sacrificing analytical performance
Future Trends and Opportunities
Advances may include coupling with mass spectrometric detectors for enhanced specificity, expansion to polycyclic aromatic analysis, integration with laboratory information management systems, and application of chemometric or machine-learning approaches to further automate impurity detection and trending.
Conclusion
The dual-channel Agilent 8890 GC system with RTL and ECN-based calibration effectively implements ASTM D7504 for monocyclic aromatic hydrocarbon purity analysis. This approach delivers high throughput, reliable retention time alignment, and compliance with stringent repeatability requirements, making it ideal for modern QA/QC environments.
References
- ASTM D7504-18, Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and Effective Carbon Number, ASTM International, 2018.
- Giarrocco V.; Quimby B. D.; Klee M. S. Retention Time Locking: Concepts and Applications, Agilent Technologies Application Note 228-392, 1997.
- McCurry J. D. A Unified Gas Chromatographic Method for Aromatic Solvent Analysis, Agilent Technologies Application Note 5988-3741EN, 2001.
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