Coupling of large volume injection with flow modulated two-dimensional gas chromatography
Zoltán Nyiri1, Dóra Vörös-Palya1, Márton Novák1
1Joint Research and Training Laboratory on Separation Techniques, Institute of Chemistry, Eötvös Loránd University, Pázmány Péter Stny. 1/A, H-1117 Budapest, Hungary.
Large volume injection (LVI) coupled with comprehensive two-dimensional gas chromatography (GC×GC) enhances trace analysis. Optimized split-splitless LVI parameters improve peak shape and reproducibility for complex samples like diesel oil.
Area of Science:
- Analytical Chemistry
- Chromatography
Background:
- Large volume injection (LVI) coupled with comprehensive two-dimensional gas chromatography (GC×GC) offers powerful analysis of complex trace samples.
- Optimizing LVI parameters is crucial for samples with wide boiling ranges.
Purpose of the Study:
- To optimize LVI parameters for GC×GC analysis of samples with a wide boiling range.
- To evaluate injection parameters for peak shape, reproducibility, and peak volume.
Main Methods:
- Utilized a pneumatic modulator based on capillary flow technology for LVI-GC×GC coupling.
- Optimized a split-splitless LVI method using 25 microliters of a 27-compound mixture simulating diesel oil.
- Employed non-polar (Rxi-5ms) and polar (HP-INNOWax) columns for GC×GC separation.
Main Results:
- Solvent vent injection proved unsuitable due to peak splitting and loss of volatile compounds.
- The optimized split-splitless LVI method showed no peak distortion for target compounds.
- Relative peak volumes ranged from 60-120% for all compounds, with 13 compounds showing 80-120%.
Conclusions:
- A robust split-splitless LVI method was successfully developed and optimized for GC×GC.
- This optimized method is suitable for analyzing complex samples with wide boiling ranges using LVI-GC×GC.
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