An investigation of glasses for capillary chromatography

An investigation was conducted of various glasses, other than soda lime or borosilicate, for use in glass capillary gas chromatography. The work has uncovered some unique chromatographic qualities in the use of potash soda lead and fused silica glasses as materials for making glass capillary columns. The fused silica proved to be an ideal material for capillary column construction, being inherently more inert than glass containing metal oxides. It has been shown that through the use of thin wall capillary tubing of high flexibility many of the mechanical problems associated with glass capillary columns, such as fragility and column straightening, can be avoided.     

The use of glass capillary columns for the analysis of polar natural products

Two published procedures for glass capillary column production are applied to produce capillaries for chromatography of polar natural compounds. Soda lime glass capillaries, after leaching with aqueous HCL, are either treated with colloidal silicic acid or with barium carbonate and coated with either Silar 7CP or SE 52. A test mixture as well as polar carbohydrate and peptide mixtures are chromatographed on the different columns and their chromatographic properties are evaluated. Combined capillary gas chromatography-electron impact and chemical ionization mass spectrometry are used for identification of the peptide sequence.     

Glass capillary gas chromatography of amino acid enantiomers

Glass capillaries coated with Chirasil-Val, a chirally functionalised polysiloxane, are capable in principle of resolving all protein amino-acid enantiomers in a single run and within a short analysis time, thus allowing for example the quantitative amino acid determination by enantiomer labelling. The elution characteristics of the individual amino acids however are also dependent upon the chemical nature of the capillary wall surface, and a surface pretreatment is found to be necessary if all protein amino acids are to be analysed. Of the various methods of pretreatment tested, etching of borosilicate glass with gaseous HCl followed by deposition of colloidal silicic acid is considered to be the most suitable.     

Gas chromatographic conditions for the linearity of the relationship between σT,t and tR in open tubes

The linearity of the relationship between σ_T,t² and (1 + k)² is studied with the view of using it for the evaluation of GC equipment. Based on appropriate analytical expressions it is concluded that in general this relationship is not linear and that practical procedures for column evaluation should be developed that take this non-linearity into account.     

Practical limitations of capillary gas chromatography

Glass capillary gas chromatography is a high resolution separation method which allows the qualitative and quantitative analysis of even complex mixtures, which may contain many components–also isomeric–in a wide range of volatilities, polarities and concentrations. The principal limitation of gas chromatographic application is given by an insufficient volatility of the species to be separated. Elevated temperatures have to be applied if the application range is to be extended and to achieve steep peak profiles, i.e. low detection limits at high resolution. The use of elevated temperatures is limited, of course, by the temperature stability of both the solvent (stationary liquid and support) and the solutes. The problems of trace analysis for low volatility compounds at high resolution and its limitational parameters regarding sampling, separation and detection are discussed. The applicability of glass capillary columns in this field is influenced by the following parameters: tailing behaviour; irreversible adsorption of polar and decomposition of unstable solutes; thermal stability of stationary liquid (including the support deactivation); separation efficiency and sample capacity (film thickness). Multidimensional gas chromatography using capillary columns coupled either with a packed or another capilllary column for preseparations may be applied with advantage in the analysis of complex mixtures.     

Analysis of nitrosamines by GC2 with a photoionization detector

The use of a photoionization detector (PID) coupled to a glass capillary gas chromatography (GC²) separation system for the detection of carcinogenic nitrosamines was investigated. The components analyzed gave a linear response with a lower detection limit of 50 to 100 pg with the 10.2 eV ionization source. No detector response was obtained with an ionization energy of 9.5 eV. Chromatography of meat extracts indicated their complex molecular composition. Simple liquid chromatographic cleaning procedures significantly decreased the complexity of these samples, but not sufficiently for the accurate quantition of nitrosamine components.     

Analysis of volatile organic compounds in polymers by dynamic headspace and gas chromatography/mass spectrometry

An experimental method for the analysis of volatile organic compounds in polymers is described. The technique involves dynamic headspace sampling, collection, and concentration of the volatiles in a cold trap, followed by capillary column gas chromatography/mass spectometry. Flow switching is carried out by the Deans switching technique. Four technical polymers used as pharmaceutical packaging materials have been analyzed in order to demonstrate the method.     

Effect of column diameter on efficiency in capillary supercritical fluid chromatography

Fused silica capillary columns with internal diameters from 100 to 25 μm were coated with SE-54 and evaluated under supercritical fluid chromatographic conditions using carbon dioxide as mobile phase. Experimental results compared well with theoretical predictions. At ten times the optimum mobile phase velocity and for a capacity factor, k of 3, efficiencies of 2300 to 5600 plates m^?1 were obtained for column diameters of 100 to 25 μm, respectively.     

Length of the flooded zone in the column inlet and evaluation of different retention gaps for capillary gas chromatography

In on-column or in splitless injection with recondensation of the solvent, the length of the flooded zone in the column inlet depends primarily on the wettability of the internal wall of the inlet. For columns with a coated inlet this explains why peak distortion due to band broadening in space by a certain sample volume is pronounced in one case and hardly observable in another. Glass or fused silica capillaries silylated with diphenyltetramethyldisilazane were found to give optimal retention gaps. They combine thorough and thermostable deactivation with good wettability and low retention power. On the other hand it is very easy to deactivate fused silica capillaries with Carbowax. The resulting retention gaps are suitable for a wide range of applications and are particularly attractive for the analysis of dirty samples which require frequent replacement of the inlet.