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Preparation and evaluation of polar stabilized phase open tubular (SPOT) columns

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  • Chemistry
  • Design
  • Ecology
  • Geography
  • Medicine


Preparation and evaluation of polar stabilized phase open tubular (SPOT) columns Preparation and Evaluation of Polar Stabilized Phase Open Tubular (SPOT) Columns C. A. Cramers / E. A. Vermeer / J. J. Franken Department of Instrumental Analysis, Eindhoven University of Technology, Eindhoven, The Netherlands Summary A method is described for the routine preparation of high resolution stabilized phase open tubular (SPO 7-) columns. A finely dispersed siliceous material (Cab-O-Sil) is treated with benzyltripheny/phosphoniumchloride and dynamically coated onto the inside wall of glass capillary columns. Additional dynamic coating with a polar stationary phase yields thermostable columns of high efficiency. The columns show favourable adsorption properties and good long term stability. The mechanical stability of the stationary phase film is explained in terms of the rheological behaviour of concentrated dispersions. The designation PL 0 T columns appears inapplicable, and these columns will be referred to as SPOT columns. A theoretical model, describing band spreading in SPOT columns, is proposed and compared with the experimental results. Some applications in routine use and in ultra trace analysis are presented. Introduction Glass open tubular colunms offer the best prospects in the analysis of complex biochemical and environmental mix- tures. Much progress has been made in the development of these columns, especially for apolar stationary liquids. One of the main problems met with in the preparation of polar columns is the poor wettability of the glass wall. Polar coatings, deposited uniformly on untreated glass surfaces, usually soon break up and form microdrops when at higher temperatures. The result is a rapid loss of column efficiency and a useful life of hours to days at best. Of the numerous possible methods of overcoming the problem, that of surface roughening has found the widest application. Surface roughening is based either on the dep

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