Large volume splitless injection with concurrent solvent recondensation: Keeping the sample in place in the hot vaporizing chamber
- 6 October 2004
- journal article
- research article
- Published by Wiley in Journal of Separation Science
- Vol. 27 (14) , 1157-1165
- https://doi.org/10.1002/jssc.200401847
Abstract
An injector liner packed with a plug of glass wool is compared with a laminar and a mini laminar liner for large volume (20–50 μL) splitless injection with concurrent solvent recondensation (CSR‐LV splitless injection). Videos from experiments with perylene solutions injected into imitation injectors show that glass wool perfectly arrested the sample liquid and kept it in place until the solvent had evaporated. The sample must be transferred from the needle to the glass wool as a band, avoiding ‘thermospraying’ by partial solvent evaporation inside the needle. The liquid contacted the liner wall when the band was directed towards it, but from there it was largely diverted to the glass wool. In the laminar liners, part of the liquid remained and evaporated at the entrance of the obstacle, while the other proceeded to the center cavity. Vapors formed in the center cavity drove liquid from the entrance of the obstacle upwards, but the importance of such problems could not be verified in the real injector. Some liquid split into small droplets broke through the obstacle and entered the column. Breakthrough through the laminar liners was confirmed by a chromatographic experiment. An improved design of a laminar liner for large volume injection is discussed as a promising alternative if glass wool causes problems originating from insufficient inertness.Keywords
This publication has 22 references indexed in Scilit:
- Inability of Unpacked Gooseneck Liners To Stop the Sample Liquid after Injection with Band Formation (Fast Autosampler) into Hot GC InjectorsAnalytical Chemistry, 2004
- Concurrent solvent recondensation large sample volume splitless injectionJournal of Separation Science, 2003
- Large volume injection in capillary GC using PTV injectors: Comparison of inertness of packing materialsJournal of High Resolution Chromatography, 1995
- Procedure for testing inertness of inserts and insert packing materials for GC injectorsJournal of High Resolution Chromatography, 1993
- Explanation of the matrix-induced chromatographic response enhancement of organophosphorus pesticides during open tubular column gas chromatography with splitless or hot on-column injection and flame photometric detectionJournal of Chromatography A, 1993
- Sample evaporation in conventional split/splitless GC injectors: Part 2: Use of perylene for visual observation of three different scenarios in empty injector insertsJournal of High Resolution Chromatography, 1992
- Pesticide residue analysis in food with CGC — study of long‐term stability by the use of different injection techniquesJournal of High Resolution Chromatography, 1990
- Accuracy and reproducibility in splitless, and packed and open tubular cool on‐column injectionsJournal of High Resolution Chromatography, 1982
- Splitless injection and the solvent effectJournal of High Resolution Chromatography, 1978
- Isothermal analysis on capillary columns without stream splittingJournal of Chromatography A, 1974