Splitless inlets optimization

For semi volatile compounds, inlet optimization is very simple. Classical splitless inlet conditions, followed by an initial column temperature cool enough to refocus the analyte peaks following the desorption, work well. Thus, a typical condition would be a temperature of about 250° C, a head pressure sufficient to maintain optimum GC column flow and an initial column temperature at least 100°C below the normal boiling point of the analyte. For semivolatile analytes, a classical splitless inlet liner can be used, as the cool column will refocus these peaks. The desorption time in the inlet must be determined by experimentation, but typically, runs between 1 and 5 minutes. 

The attractive features of splitless injection techniques are that they allow the analysis of dilute samples without preconcentration (trace analysis) and the analysis of dirty samples, since the injector is easily dismantled for cleaning. Success with individual samples, however, depends on the selection of experimental variables of which the most important sample size, sample solvent, syringe position, sampling time, initial column temperature, injection temperature and carrier gas flow rate, often must be optimized by trial and error. These conditions, once established, are not necessarily transferable to another splitless injector of a different design. Also, the absolute accuracy of retention times in splitless injection is generally less than that found for split injection. For splitless injection the reproducibility of retention times depends not only on chromatographic interactions but also on the reproducibility of the sampling period and the evaporation time of the solvent in the column inlet, if solvent effects (section 3.5.6.2) are employed. The choice of solvent, volume injected and the constancy of thermal zones will all influence retention time precision beyond those for split injection. For quantitative analysis the precision of repeated sample injections is normally acceptable but the method is subject to numerous systematic errors that may... 

Minimal system requirements are a GC equipped with electronic pneumatic control (EPC), off-the-shelf capillary columns, split/splitless or on-column inlets, standard detectors optimized for capillary columns, and a fast acquisition data system. At any time, users can switch from fast GC back to the original method without major difficulties, or optimize new methods to meet new analytical demands. 

Understanding the relationships between inlet liner geometry, carrier gas flow, injection volume and solvent vapour volume is essential for optimizing splitless injections. Especially the expansion volume of the solvent used must be taken into account. The maximum liquid injection volume needs to be adjusted in the hot... 

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