The dual-flow countercurrent extraction technique can be considered to be one of the true moving-bed (TMB) chromatographic methods. However, here we call it dual-flow countercurrent extraction, because the "stationary phase (bed)" is a liquid, and the principal structure of the column is to be categorized in the extractor.This method is a powerful tool for enantio-separation when 1) a suitable chiral separating agent exists, 2) recycling usage of the chiral separator is possible, and 3) a proper apparatus is procured with which continuous separation is to be performed. Although one can separate a mixture into only two fractions with this method, it is sufficient in most cases involving enantio-separations. Compared to chromatographic methods, it is advantageous because continuous separation can be performed by the technique, whereas intermittent separations are required by the chromatographic method. We planned to manufacture a proper apparatus for dual-flow countercurrent extraction for preparative use, though a countercurrent chromatograph 1 , which is not the dual-flow type, and a highspeed dual-countercurrent chromatograph 2 , which is not for the preparative use, are obtainable.We previously reported on an apparatus for dual-flow countercurrent extraction, with which the chiral separating agent can be recycled. 3 We also demonstrated that racemic β-blockers, such as propranolol and pindolol, could be extractively separated into their enantiomers in a chloroform-water two-phase system using didodecyl-L-tartrate as a chiral separator in the presence of boric acid. 4 However, with the vertical column of the previous apparatus, the efficient mixing of chloroform and water could not be attained, mainly because of a large difference in their densities. Also, the maximum flow rate of the extraction solvents was limited to about 3 ml/min with the apparatus. In order to overcome these problems, we designed an improved apparatus with a horizontal-type column. The principle of column separation is similar to that of Morris.5 Before preparing a long column, we investigated the optimal operation conditions using a short-column apparatus, because an experimental evaluation of the column becomes more difficult along with an increase in its efficiency. In this report we describe the structure of the manufactured short-column apparatus for dual-flow countercurrent distribution chromatography and a measurement of its efficiency by a simple graphical stage calculation method.
Improved Apparatus for Dual-Flow CounterCurrent ExtractionA unit cell of the improved column comprises a mixer and a settler. All of the plastic parts of the column are made of polyfluoroethylene. The structure of the column is depicted in Figs. 1a, 1b, and a view of the whole apparatus is sketched in Fig. 2. In the mixing chamber, there is a stirring wheel in which a dipole button magnet (10 mmφ×5 mm) is inserted, and on which six cogs are placed. This can be rotated magnetically.The extraction column was prepared by inserting six pairs of mixing and se...