Volatile Organic Compounds Analysis in Soils and Sediments Using the Agilent 8697 Headspace Sampler

Importance of the Topic

Volatile organic compounds (VOCs) often accumulate in soils and sediments near industrial sites, posing health and environmental risks. Reliable measurement of VOC levels is critical for informed decision-making on soil remediation and regulatory compliance, particularly under frameworks such as China’s HJ 642-2013 standard.

Objectives and Study Overview

This work assessed the performance of an integrated static headspace GC/MS platform—comprising the Agilent 8697 headspace sampler, 8860 GC, and 5977B MSD—for quantifying 36 target VOCs in soils and sediments. Key metrics evaluated included repeatability, linearity, limits of detection (LOD) and quantitation (LOQ), and method recovery.

Methodology and Instrumentation

Samples were prepared by spiking quartz sand or real soil with calibration standards and internal surrogates in acidified, salt-saturated water. Calibration solutions ranged from 4 to 100 µg/L, equivalent to 10–250 µg/kg in a 2 g soil aliquot. Headspace extraction was performed at 80 °C for 50 min with vial shaking, followed by transfer of a 1 mL loop at 100 °C into the GC inlet. Separation employed a 60 m × 0.25 mm DB-624 column with a temperature program from 40 °C to 200 °C. Detection used SIM mode on the 5977B MSD.

Used Instrumentation

• Agilent 8697 Headspace Sampler with 48-vial capacity and integrated diagnostics
• Agilent 8860 Gas Chromatograph with split/splitless inlet
• Agilent 5977B Mass Selective Detector (GC/MSD) with inert extraction ion source
• Agilent J&W DB-624 column (60 m × 0.25 mm, 1.4 µm film thickness)

Results and Discussion

The system exhibited excellent repeatability, with area RSD values of 1.0–4.3% for all 38 compounds. Calibration curves demonstrated strong linearity (R² > 0.996). In a quartz sand blank, method LODs ranged from 0.51 to 1.21 µg/kg and LOQs from 1.7 to 4.1 µg/kg, meeting HJ 642-2013 requirements. Recovery studies on real soil at spike levels of 50 and 125 µg/kg yielded rates between 78.2–125.9% and 71.7–108.7%, respectively.

Benefits and Practical Applications of the Method

The described headspace-GC/MS approach offers automated diagnostic checks, high throughput sample handling, minimal carryover, and robust quantitation. It aligns with regulatory mandates for soil and sediment monitoring, supporting environmental laboratories in QA/QC and remediation assessments.

Future Trends and Potential Applications

Advances may include field-portable headspace systems, expanded compound libraries, real-time data analytics, and integration with online environmental monitoring networks. Enhanced instrument automation and machine-learning-based diagnostics will further streamline VOC analysis workflows.

Conclusion

The Agilent 8697 headspace sampler coupled with the 8860 GC and 5977B MSD delivers reliable, precise, and compliant VOC analysis in soil and sediment matrices. Performance metrics for repeatability, linearity, detection limits, and recoveries meet or exceed the HJ 642-2013 standard, demonstrating its suitability for environmental testing applications.

References

Chinese Environmental Protection Industry Standard HJ 642-2013: Soil and Sediment—Determination of Volatile Organic Compounds—Headspace-Gas Chromatography/Mass Method. Ministry of Environmental Protection of China, 21 January 2013.