Fast Volatile Organic Compound Analysis of Drinking Water Using the Agilent 8697 Headspace Sampler in Tandem with Intuvo 9000 GC and 5977B GC/MSD

Significance of the Topic

Volatile organic compounds (VOCs) in drinking water pose health and regulatory concerns due to their widespread use and potential to leach into water supplies. Rapid, sensitive analysis of VOCs is essential for compliance testing, contamination monitoring, and ensuring safe drinking water quality.

Objectives and Study Overview

This application note evaluates a fast method for VOC determination in drinking water using an Agilent 8697 headspace sampler coupled with an Agilent Intuvo 9000 GC and 5977B GC/MSD. The study aimed to optimize headspace conditions, assess system performance (repeatability, linearity, limits of quantitation, and recovery), and demonstrate improved sample throughput.

Methodology and Instrumentation

The protocol uses 10 mL water samples spiked with VOC standards and sodium chloride to enhance headspace partitioning. Key parameters include:

• Sample incubation: 80 °C, 20 min with shaking
• Headspace injection: 1 mL loop, N₂ transfer gas
• GC column: 20 m × 0.18 mm DB-624 Ultra Inert, 1 µm film
• Carrier gas: H₂ for scan mode; He for SIM mode
• Oven program: Fast ramp to 200 °C and 230 °C for separation in ~6 min, plus 2.5 min conditioning
• Mass spectrometer: 5977B MSD with high-efficiency ion source, SIM and scan data acquisition

Main Results and Discussion

Performance metrics for 64 VOCs included:

• Repeatability: average area RSD 1.7% (SIM) and 2.0% (scan)
• Linearity: coefficients of determination (R²) >0.994 (SIM) and >0.995 (scan)
• Limits of quantitation: 0.033–1.51 µg/L (SIM); 0.24–11.9 µg/L (scan with He); 0.50–38.2 µg/L (scan with H₂)
• Recovery: 72–116% across tested levels, with most compounds 85–110%
• Analysis speed: <13 min per sample; overlapping headspace runs increase throughput

Benefits and Practical Applications

This method enables rapid, high-throughput VOC analysis with reliable quantitation for regulatory compliance and routine monitoring of drinking water. The combination of fast GC separation and sensitive MSD detection allows identification and quantitation of coeluting compounds.

Future Trends and Potential Applications

Future developments may include further reduction of dwell times, exploration of alternative carrier gases, and hardware refinements (e.g., larger drawout plates) to improve linearity and sensitivity. Expanded application to complex environmental and industrial water matrices can leverage high-efficiency sources and automated sample overlaps for higher throughput.

Conclusion

The Agilent 8697 headspace sampler combined with Intuvo 9000 GC and 5977B GC/MSD provides a fast, robust VOC analysis workflow for drinking water. Optimized headspace conditions, rapid oven programs, and dual acquisition modes yield excellent repeatability, linearity, and sensitivity, enhancing laboratory productivity and regulatory compliance.

References

1. Rothweiler B. Analysis of Volatile Organic Compounds in Environmental Waters Using the Agilent 7697A Headspace and 7890B/5977A GC/MS. Agilent Technologies Application Note, 2014.
2. Gautschi P., Prest H. Improved Volatiles Analysis Using Static Headspace, the Agilent 5977B GC/MSD, and a High-Efficiency Source. Agilent Technologies Application Note, 2016.