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Optimized Volatiles Analysis Ensures Fast VOC Separations

Technical notes | 2011 | RestekInstrumentation
GC, GC/MSD, Purge and Trap, GC/SQ
Industries
Environmental
Manufacturer
Agilent Technologies, Restek, OI Analytical

Summary

Significance of the Topic


Volatile organic compounds are key targets in environmental monitoring regulatory compliance and industrial quality control. Fast reliable separations of a wide range of VOCs from light gases to aromatic compounds are essential to maintain high throughput reduce analysis downtime and ensure accurate quantification at low detection limits.

Objectives and Study Overview


This study aimed to develop an optimized GC/MS method for VOC analysis using a Rxi-624Sil MS column. Key goals were to synchronize purge and trap cycles with instrument runs maximize sample throughput and achieve sharp well resolved peaks across a broad volatility range.

Methodology and Instrumentation


The method was designed using computational modeling of critical analyte pairs with Pro ezGC software. The final temperature program starts at 35 C hold 5 minutes then ramps to 60 C at 11 C per minute followed by 220 C at 20 C per minute with a 2 minute hold. A 30 meter 0.25 mm id 1.4 micron Rxi-624Sil MS column was operated under constant helium flow at 1 mL per minute. Sample introduction employed an OI Analytical 4660 purge and trap system with 11 minute purge at 20 C 0.5 minute desorb at 190 C and 5 minute bake at 210 C. Detection used an Agilent 7890A GC coupled to a 5975C MSD in scan mode (36–260 amu) with a 1.5 minute solvent delay.

Key Results and Discussion


Under optimized conditions labs achieved up to 36 runs per 12-hour shift by aligning injection and purge trap cycles. The Rxi-624Sil MS column resolved critical pairs such as methyl ethyl ketone and ethyl acetate in a single analysis proving superior selectivity. Its thermal stability to 320 C and very low column bleed enhanced sensitivity and extended column lifetime compared to other 624 phases. Unique deactivation yielded symmetric peaks for active compounds like amines and alcohols minimizing tailing and improving quantification accuracy.

Benefits and Practical Applications


  • Increased instrument productivity through reduced cycle downtime.
  • Sharper peak shapes for reliable quantification of polar and active volatiles.
  • Lower baseline bleed for enhanced sensitivity and lower detection limits.
  • Extended column life lowering replacement costs.

Future Trends and Potential Applications


Further improvements may include advanced silarylene based phases for even higher stability integration of automated data analytics to streamline method development coupling with alternative detectors for comprehensive screening and miniaturized purge trap modules for field portable VOC monitoring.

Conclusion


The optimized parameters on Rxi-624Sil MS columns deliver fast high resolution VOC separations with minimal bleed and superior inertness. This approach enables laboratories to maximize sample throughput ensure accurate low level quantification and maintain reliable long term performance.

References


  • Misselwitz M Stidsen G English C Optimized Volatiles Analysis Ensures Fast VOC Separations Restek Application Note 2011

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