希薄水溶液の冷凍濃縮 : 基礎的検討

概要

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A procedure of several 100-fold freeze concentration was investigated for a dilutc aqueous solution of potassium permanganate, cupric sulfate, or Methylene Blue in 3 to 51. The sample solution was carefully frozen under stirring in a polycthylene bottle cooled at -20 to -23℃. Ice forms slowly from the side and the bottom. The concentrated solution in a conical hole on the top of ice was taken out of the hole, and both concentration and recovery were determined spectrophotometrically. To make a transparent ice required for the best recovery, stirring under the experimentally settled conditions was an essential part of the procedure. In order to achieve both high recovery and high concentration rate, it was essential to cool the concentrate in the conical hole enough at a low temperature. It was possible to concentrate 51 of the sample solution to 15.5ml in 6 to 7hrs with 85% recovery at -23℃ and 66% at -20℃. In all 154 runs, recoveries decreased with an increase of r_V(r_v : initial vol./final vol.). The plots of log r_C (r_C : final concn./initial concn.) vs. log r_V were linear. The initial concentration of sample can be calculated from the final concentration based on this linear relationship. The errors calculated for the 154 runs were within ±20%.
社団法人日本分析化学会の論文
1977-02-10