A Novel Long-Lifetime Ion Detector for GC-TOFMS and GCxGC-TOFMS with Sub-Femtogram Detection Limits
Posters | 2024 | LECO | ASMSInstrumentation
An efficient and long-lived ion detector is essential for high-sensitivity, high-throughput GC-TOFMS and GCxGC-TOFMS analyses. Detectors must handle intense ion flux without performance degradation to reduce maintenance, lower costs, and enable reliable trace-level measurements in complex samples.
This study presents a novel long-lifetime ion detector developed for LECO’s Pegasus BTX GC-TOFMS and GCxGC-TOFMS. The aim was to enhance sensitivity, expand linear dynamic range, ensure stable detector gain, and extend operational lifetime under high ion flux conditions. Comprehensive evaluation covered detection limits, dynamic range, robustness, and projected lifetime.
The detector accelerates ions at 8.1 keV onto a convertor plate, generating secondary electrons directed to a fast scintillator. Photons are conveyed through an L-shaped light guide into a photomultiplier tube (PMT), and signals are digitized by a 15-bit, 500 MHz acquisition system. Detector gain was optimized using perfluorotributylamine (PFTBA) infusion to set area-per-ion targets.
GC-TOFMS analyses used a 30 m×0.25 mm×0.25 µm Rxi-5MS column with 10 spectra/s acquisition; GCxGC employed an additional 2 m×0.25 mm×0.25 µm Rxi-17SilMS secondary column and 200 spectra/s.
Detection limits for octafluoronaphthalene (OFN) reached sub-2 fg on-column for GC-TOFMS and sub-femtogram for GCxGC-TOFMS based on eight replicates (IDL calculated via %RSD and t-student 99% confidence). Linear dynamic ranges spanned five orders of magnitude (5 fg–500 pg) in GC-TOFMS and four orders (2 fg–50 pg) in GCxGC. Longevity testing monitored PMT bias over accumulated charge; extrapolation indicated ~3 200 C tolerance, translating to 4–5 years of typical high-sensitivity use. Robustness trials with 900 hemp extract injections showed consistent detector bias and stable OFN peak areas, attributing resilience to both the new detector and the StayClean source.
Advancements may include integrating the detector into other mass spectrometer platforms, refining scintillator materials for further sensitivity gains, and coupling with automated sample preparation and machine-learning driven data processing. Long-term stability opens avenues for continuous monitoring applications in industrial process control and environmental surveillance.
The novel long-lifetime ion detector for GC-TOFMS and GCxGC-TOFMS delivers exceptional sensitivity, broad dynamic range, and multi-year operational life under high ion flux, while maintaining robustness in complex sample analyses.
GC/MSD, GC/TOF, GCxGC
IndustriesOther
ManufacturerLECO
Summary
Importance of the Topic
An efficient and long-lived ion detector is essential for high-sensitivity, high-throughput GC-TOFMS and GCxGC-TOFMS analyses. Detectors must handle intense ion flux without performance degradation to reduce maintenance, lower costs, and enable reliable trace-level measurements in complex samples.
Goals and Overview
This study presents a novel long-lifetime ion detector developed for LECO’s Pegasus BTX GC-TOFMS and GCxGC-TOFMS. The aim was to enhance sensitivity, expand linear dynamic range, ensure stable detector gain, and extend operational lifetime under high ion flux conditions. Comprehensive evaluation covered detection limits, dynamic range, robustness, and projected lifetime.
Methodology and Instrumentation
The detector accelerates ions at 8.1 keV onto a convertor plate, generating secondary electrons directed to a fast scintillator. Photons are conveyed through an L-shaped light guide into a photomultiplier tube (PMT), and signals are digitized by a 15-bit, 500 MHz acquisition system. Detector gain was optimized using perfluorotributylamine (PFTBA) infusion to set area-per-ion targets.
GC-TOFMS analyses used a 30 m×0.25 mm×0.25 µm Rxi-5MS column with 10 spectra/s acquisition; GCxGC employed an additional 2 m×0.25 mm×0.25 µm Rxi-17SilMS secondary column and 200 spectra/s.
Used Instrumentation
- Pegasus BTX GC-TOFMS and GCxGC-TOFMS
- Novel ion detector: convertor plate, scintillator, L-shaped light guide, PMT
- StayClean direct extraction ion source
- Columns: Rxi-5MS and Rxi-17SilMS
- Data acquisition: 15-bit, 500 MHz system
Main Results and Discussion
Detection limits for octafluoronaphthalene (OFN) reached sub-2 fg on-column for GC-TOFMS and sub-femtogram for GCxGC-TOFMS based on eight replicates (IDL calculated via %RSD and t-student 99% confidence). Linear dynamic ranges spanned five orders of magnitude (5 fg–500 pg) in GC-TOFMS and four orders (2 fg–50 pg) in GCxGC. Longevity testing monitored PMT bias over accumulated charge; extrapolation indicated ~3 200 C tolerance, translating to 4–5 years of typical high-sensitivity use. Robustness trials with 900 hemp extract injections showed consistent detector bias and stable OFN peak areas, attributing resilience to both the new detector and the StayClean source.
Benefits and Practical Applications
- Ultra-trace detection down to sub-femtogram levels for environmental, forensic, and pharmaceutical analyses
- Wide linear dynamic range reduces need for sample dilution and repeat runs
- Extended detector lifetime reduces downtime and maintenance costs
- Stable operation under heavy sample throughput enhances lab productivity
Future Trends and Opportunities
Advancements may include integrating the detector into other mass spectrometer platforms, refining scintillator materials for further sensitivity gains, and coupling with automated sample preparation and machine-learning driven data processing. Long-term stability opens avenues for continuous monitoring applications in industrial process control and environmental surveillance.
Conclusion
The novel long-lifetime ion detector for GC-TOFMS and GCxGC-TOFMS delivers exceptional sensitivity, broad dynamic range, and multi-year operational life under high ion flux, while maintaining robustness in complex sample analyses.
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