Abstract
In the development of high-efficiency split high-temperature open-tubular liquid chromatographic systems, the study of the extra-column band broadening and the “cold-point” effect is of great importance. For a rectangular sample plug of volume V inj, σ inj 2= 0. 181 V inj 2 if the peak width at half-height is used in the column efficiency calculations. In a split system, the contribution of the connection tube between the split tee-piece and the sample valve to the observed peak variance can he calculated with the Taylor equation and the known splitting ratio. As this tube also performes as a preheating tube, a Perkin-Elmer serpentine tube is recommended from considerations of the heating efficiency and the resistance to mass transfer. In order to obtain a higher sensitivity, an external small volume Z-shaped cell was used in series with the on-column cell. The results show that a large decrease in efficiency occurs at the low-temperature column outlet outside the oven. If the Z-shaped cell is connected to the column with a very narrow-bore tube (half of the column I.D.) and the connection is made inside the column oven, higher selectivity could be obtained with little efficiency loss.
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