On‐column injection with split/splitless sampling onto gc capillary columns

Schomburg, G.; Husmann, H.; Schulz, Frank

doi:10.1002/jhrc.1240051011

Cited by 13 publications

(1 citation statement)

References 8 publications

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“…When either directly injecting large volumes of organic solvents into a gas chromatograph, or using on-line coupled techniques such as LC-GC [1] and SPE-GC [2], the common GC set-up of injector-column-detector has to be modified [3,4]. A retention gap, a piece of deactivated fused silica, is inserted between the injector and the column [5], in order to retain the large volume of liquid during injection/transfer and evaporation.…”

Section: Introductionmentioning

confidence: 99%

Investigations on analyte losses in systems suited for large-volume on-column injections

et al. 2001

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Use o~ a large-volume injection system with a solvent vapour exit (SVE) requires optimisation. An appropriate strategy is to determine the evaporation rate by increasing the injection time at a fixed injection speed, injection temperature and head pressure. When measuring the flow rate in the carrier gas supply line to the on-column injector, optimisation can be very rapid: some five injections of pure solvent will be sufficient.When working under pa~ially concurrent solveni evaporation conditions, loss of volatiles is often observed if no retaining precolumn is used be~een the retention gap and the SVE. To investigate the requirements (length anct stationary phase) of the retaining precolumn, C8-C18 n-alkanes in n-hexane were used. The minimum length of the retaining precolumn (0.32 mm diameter) needed to prevent substantial losses of volatiles was 2 m. Experiments with retaining precolumns with ancl without stationary phase gave identical results. This shows that there is no need to coat the capillary as it only acts as a restrictor.

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Section: Introductionmentioning

confidence: 99%

Investigations on analyte losses in systems suited for large-volume on-column injections

et al. 2001

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C Split Injection

Grob

2001

Split and Splitless Injection for Quantitative Gas Chromatography

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Injection temperature effects using On‐column and split sampling in capillary gas chromatography

Wang

Shanfield

Zlatkis

1983

J. High Resol. Chromatogr.

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SummaryThe effect of sample injection temperature on quantitation is examined for on-column and conventional split modes of sampling in capillary gas chromatography. Discrimination effects can be observed even with on-column injection if the injection temperature is too far above the boiling point of the solvent (or that of a major low boiling constituent). This is attributed to higher boiling components being left behind in the syringe needle, and a set of simulation experiments are described to illustrate this effect. Various discrimination patterns using conventional split injection were observed, depending on temperature of injection. Apart from syringe needle effects, discrimination is probably due to the preferential venting of higher boiling components as liquid sample droplets, which can havea lifetimegreaterthan thetimeof transit to thesplitter. With such a two-phase system, involving variable droplet size, the flow distribution in the splitter will be critical to uniform sampling. The use of combination on-column/split sampling, with the appropriate temperature control to provide sample uniformity to the splitter is discussed as an advantageous alternative to conventional split sampling.

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On‐column injection with split/splitless sampling onto gc capillary columns

Cited by 13 publications

References 8 publications

Investigations on analyte losses in systems suited for large-volume on-column injections

Investigations on analyte losses in systems suited for large-volume on-column injections

C Split Injection

Injection temperature effects using On‐column and split sampling in capillary gas chromatography

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