Semivolatile Organics Analysis Using an Agilent J&W HP-5ms Ultra Inert Capillary GC Column

Importance of the Topic

Semivolatile organic compounds (SVOCs) are widespread environmental contaminants with diverse chemical properties, including acidic, basic and nonpolar species. High-sensitivity, reliable analysis of trace-level SVOCs is essential for environmental monitoring, regulatory compliance (e.g., USEPA Method 8270), and risk assessment. However, strong adsorption of active analytes (e.g., nitrophenols) onto active sites in GC flow paths can compromise sensitivity and linearity, emphasizing the need for truly inert analytical systems.

Objectives and Study Overview

This study evaluates the analytical performance of an Agilent J&W HP-5ms Ultra Inert capillary GC column coupled to an electron impact single-quadrupole mass spectrometer for trace-level SVOC analysis. The goals were to confirm baseline inertness, assess signal-to-noise, determine linearity down to 1 ng on-column, and demonstrate improved chromatography of challenging analytes under USEPA Method 8270 conditions.

Methodology

- A “short mix” containing 18 representative SVOCs (acids, bases, PAHs, nitrosamines) and internal standards was prepared in dichloromethane at seven calibration levels (1–80 µg/mL), corresponding to 1 ng to 80 ng on-column.
- A “large mix” of 83 components was also evaluated at 5 µg/mL loading to test complex matrices.
- GC temperature program: 40 °C (1 min) to 100 °C at 15 °C/min, then to 210 °C at 10 °C/min, then to 310 °C at 5 °C/min with an 8 min hold.
- Injection: 1 µL splitless (inlet at 260 °C); helium carrier at 30 cm/s constant flow.

Used Instrumentation

• Gas chromatograph/mass spectrometer: Agilent 6890N GC with 5975B MSD (electron impact source, scan 45–450 amu).
• Autosampler: Agilent 7683B with 5 µL syringe (Agilent p/n 5181-1273).
• Column: Agilent J&W HP-5ms Ultra Inert, 30 m × 0.25 mm × 0.25 µm.
• Inlet liners: Deactivated dual-taper direct-connect (Agilent p/n G1544-80700).
• Flow-path consumables: Vials, caps, ferrules, septa selected for low activity.
• Inertness probes: 1-propionic acid, 4-picoline, trimethyl phosphate to verify column inertness.

Main Results and Discussion

The Ultra Inert column exhibited minimal active sites, yielding:

• Chromatographically sharp, symmetric peaks for highly active SVOCs (e.g., pentachlorophenol, benzidine).
• A signal-to-noise ratio of 16.9:1 for 1 ng on-column 2,4-dinitrophenol (one of the most challenging analytes).
• Excellent linearity (R2 ≥ 0.990) across 1–80 µg/mL for active phenols and nitrosamines.

Analysis of a 5 ng on-column large mix confirmed robust performance across 83 SVOCs with clear baseline resolution and no evidence of peak tailing or adsorption losses.

Benefits and Practical Applications

Implementation of the HP-5ms Ultra Inert column offers:

• Enhanced sensitivity and lower limits of quantification for trace SVOCs.
• Improved method robustness and reproducibility for QA/QC laboratories.
• Reduced analyte–surface interactions, decreasing the need for frequent maintenance or column passivation.

Future Trends and Opportunities

Advances in column inertness combined with high-performance detectors (e.g., triple-axis MS systems) will further lower detection limits and enable routine screening of emerging semivolatiles. Integration with automated sample preparation and data analytics will expand throughput and facilitate large-scale environmental monitoring.

Conclusion

The Agilent J&W HP-5ms Ultra Inert capillary column, when coupled to a 6890N/5975B GC/MSD system, delivers exceptional inertness, sensitivity and linearity for trace-level SVOC analysis under USEPA 8270 conditions. Its performance in handling chemically active probes and complex multispecies standards makes it a valuable tool for environmental chemists and regulatory laboratories.

Reference

1. US EPA Method 8270D, Revision 4, February 2007.
2. Hastings M., Vickers A.K., George C.; 54th Annual Pittcon Poster, Orlando FL, March 2003.
3. Agilent Technologies; J&W Ultra Inert GC Columns Application Note, Pub. 5989-8685EN, May 2008.
4. Szelewski M., Wilson B.; Improvements to Agilent 6890/5973 GC/MSD for EPA 8270, Pub. 5988-3072EN, Nov 2001.
5. Lynam K.; Semivolatile Analysis on Ultra Inert DB-5ms, Pub. 5989-8616EN, May 2008.
6. Lynam K., Smith D.; PAH Analysis Using Ultra Inert DB-5ms, Pub. 5989-9181EN, July 2008.
7. Lynam K., Smith D.; PBDE Analysis Using Ultra Inert DB-5ms, Pub. 5989-9571EN, Aug 2008.