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S R Bakalyar

Publications and source records attributed to S R Bakalyar.

3 recordsLinked to original sources

Control of column temperature in reversed-phase liquid chromatography.

When separations by reversed-phase liquid chromatography (RP-LC) are carried out at temperatures other than ambient, resulting retention times and bandwidths can depend on the equipment used. As a result, an RP-LC separation that is adequate when carried out on one LC system may prove inadequate when the separation is repeated on a second system. In the present study, various temperature-related problems which can result in a failure of method transfer for non-ambient RP-LC methods were examined. Means for correcting for such effects and thereby ensuring method transferability are described.

Chromatography, Liquid↗

Performance of experimental sample injectors for high-performance liquid chromatography microcolumns.

An experimental injector for HPLC microcolumns and a 3-nl conductivity detector connected directly to the injector outlet with a 19-nl tube were used to study injector dispersion, guide the design of improved injectors, and suggest appropriate injection techniques. With regard to the small injection volumes required when no on-column concentration technique is used, we show that in some circumstances: (i) there are two volumes to be considered, the sample volume (that which is intended to be injected) and the effective injection volume (that which contains all the sample after it has completely emerged from the injector). Due to dispersion, the latter is often many times the former. An injector performance factor is defined as the ratio of the two volumes. (ii) A smaller sample chamber volume in an injector does not necessarily produce a proportionately smaller effective injection volume, in which case there is a reduction of peak height that degrades sensitivity without a commensurate reduction in peak width that would improve resolution. (iii) Adjusting the geometry of the sample chamber and stator passage can significantly improve injector performance, as illustrated for sample volumes from 2 nl to 1 microl. (iv) In some cases, reducing the diameter of an injector passageway in an attempt to reduce dispersion actually causes performance to worsen.

Chromatography, High Pressure Liquid↗

Choosing sample volume to achieve maximum detection sensitivity and resolution with high-performance liquid chromatography columns of 1.0, 2.1 and 4.6 mm I.D.

The relationship between sample volume and the chromatographic performance factors of detection sensitivity and resolution were explored for high-performance liquid chromatography (HPLC) columns of 1.0, 2.1 and 4.6 mm I.D. Performance was evaluated for isocratic and gradient elution in systems having low, intermediate and high extracolumn dispersion. Sample volumes ranged from 0.4 microliter to 2 ml. This paper provides guideline for selecting sample injection parameters so that the performance of microbore columns is not needlessly sacrificed by using too small or too large a sample volume. The guidelines are extracted from the works of others and are modified by our own experimental results. Comments are also made on the relative merits of various injection techniques.

Chromatography, High Pressure Liquid↗