25 μg/L 8260 MegaMix® Revised on Rtx®-VMS
Applications | | RestekInstrumentation
Volatile organic compounds (VOCs) are widely monitored in water and environmental matrices due to their potential toxicity and regulatory significance. The EPA Method 8260 framework is a standard approach for rapid and sensitive detection of a broad range of VOCs. The revised 8260B MegaMix® on an Rtx®-VMS column provides improved reliability by eliminating pentachloroethane artifacts and ensuring consistent quantitation at low microgram-per-liter levels.
This application study aims to demonstrate the chromatographic performance and detection capability of a 25 μg/L 8260 MegaMix® calibration standard on an Rtx®-VMS capillary column coupled to GC–MS. Key goals include:
A 5 mL aliquot of the revised 8260B MegaMix® (25 μg/L) was analyzed using a purge-and-trap concentrator. Key purge parameters included an 11 min purge at 40 mL/min followed by a 3 min dry purge, trapping on a Vocarb 3000 sorbent. Thermal desorption was performed at 260 °C with subsequent bake at the same temperature to prevent carryover. The oven program ranged from 45 °C (4.5 min hold) to 100 °C at 12 °C/min, then to 240 °C at 25 °C/min (1.32 min hold). Helium served as the carrier gas at 0.9 mL/min.
The method achieved baseline separation of 82 VOC analytes within a 14 min runtime. Extracted ion chromatograms (EIC) targeting characteristic m/z values (e.g., m/z 104 for xylenes, m/z 106 for benzene) provided selective detection and accurate peak assignment. Three compounds (isobutyl alcohol, 1,4-dioxane, 2-chloropropanol) were not observed at 25 ppb under unheated purge conditions, highlighting the importance of temperature control. Peak shapes were sharp and reproducible, and no pentachloroethane-derived tetrachloroethene artifact was detected in the revised standard.
Advances in two-dimensional GC and high-resolution MS are expected to further improve separation of coeluting VOCs and enhance sensitivity. Automated data processing with machine learning will accelerate peak identification and quantitation. Novel sorbent materials for purge-and-trap may expand the analyte range to semi-volatile compounds and polar organics.
The revised 8260B MegaMix® on an Rtx®-VMS column demonstrates reliable, interference-free analysis of 82 VOCs at 25 μg/L, meeting stringent environmental monitoring requirements. This optimized method supports rapid, accurate screening of water samples and can be adapted for regulatory compliance and research applications.
Restek Corporation. 8260B MegaMix® Revised on Rtx®-VMS Application Note. 2023.
GC/MSD, Purge and Trap, GC/SQ, GC columns, Consumables
IndustriesEnvironmental
ManufacturerAgilent Technologies, Restek, EST Analytical
Summary
Importance of the Topic
Volatile organic compounds (VOCs) are widely monitored in water and environmental matrices due to their potential toxicity and regulatory significance. The EPA Method 8260 framework is a standard approach for rapid and sensitive detection of a broad range of VOCs. The revised 8260B MegaMix® on an Rtx®-VMS column provides improved reliability by eliminating pentachloroethane artifacts and ensuring consistent quantitation at low microgram-per-liter levels.
Objectives and Study Overview
This application study aims to demonstrate the chromatographic performance and detection capability of a 25 μg/L 8260 MegaMix® calibration standard on an Rtx®-VMS capillary column coupled to GC–MS. Key goals include:
- Evaluating separation efficiency for 82 target VOCs over a 14-minute runtime.
- Verifying elimination of pentachloroethane interference in the revised mixture.
- Assessing detection sensitivity and peak resolution under purge-and-trap GC–MS conditions.
Methodology
A 5 mL aliquot of the revised 8260B MegaMix® (25 μg/L) was analyzed using a purge-and-trap concentrator. Key purge parameters included an 11 min purge at 40 mL/min followed by a 3 min dry purge, trapping on a Vocarb 3000 sorbent. Thermal desorption was performed at 260 °C with subsequent bake at the same temperature to prevent carryover. The oven program ranged from 45 °C (4.5 min hold) to 100 °C at 12 °C/min, then to 240 °C at 25 °C/min (1.32 min hold). Helium served as the carrier gas at 0.9 mL/min.
Instrumentation Used
- Gas chromatograph: Agilent 7890A GC
- Mass spectrometer: Agilent 5975C MS operated in full-scan electron ionization mode (70 eV) over 47–300 amu
- Purge-and-trap system: EST Encon with Vocarb 3000 trap and 1 mm split liner
- Column: Rtx®-VMS, 30 m × 0.25 mm ID, 1.40 μm film
Main Results and Discussion
The method achieved baseline separation of 82 VOC analytes within a 14 min runtime. Extracted ion chromatograms (EIC) targeting characteristic m/z values (e.g., m/z 104 for xylenes, m/z 106 for benzene) provided selective detection and accurate peak assignment. Three compounds (isobutyl alcohol, 1,4-dioxane, 2-chloropropanol) were not observed at 25 ppb under unheated purge conditions, highlighting the importance of temperature control. Peak shapes were sharp and reproducible, and no pentachloroethane-derived tetrachloroethene artifact was detected in the revised standard.
Benefits and Practical Applications
- Comprehensive coverage of regulatory VOC lists in a single run.
- High throughput for environmental and drinking water laboratories.
- Robust detection down to low microgram-per-liter levels with minimal artifacts.
- Suitable for QA/QC of purification processes, wastewater monitoring, and site remediation assessments.
Future Trends and Opportunities
Advances in two-dimensional GC and high-resolution MS are expected to further improve separation of coeluting VOCs and enhance sensitivity. Automated data processing with machine learning will accelerate peak identification and quantitation. Novel sorbent materials for purge-and-trap may expand the analyte range to semi-volatile compounds and polar organics.
Conclusion
The revised 8260B MegaMix® on an Rtx®-VMS column demonstrates reliable, interference-free analysis of 82 VOCs at 25 μg/L, meeting stringent environmental monitoring requirements. This optimized method supports rapid, accurate screening of water samples and can be adapted for regulatory compliance and research applications.
Reference
Restek Corporation. 8260B MegaMix® Revised on Rtx®-VMS Application Note. 2023.
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