高純度精製のための自動再結晶装置の試作

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タイトル別名
  • Improved automatic recrystallization apparatus for preparing highly pure crystals.
  • コウ ジュンド セイセイ ノ タメ ノ ジドウ サイケッショウ ソウチ ノ シ

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抄録

In order to generalize an automatic recrystallization method for preparing highly pure crystals, an improved apparatus was developed. The body of the extractor extremely simplified by a novel arrangement of a filter paper thimble was easy to make. A simple recrystallization flask, an effective porous glass boiling rod, and a high-heating-efficiency recrystallization heater were also easy to make and were based on the crystallization theory. A safety device for water and electricity, which was easy to construct, was useful: suspension of water supply, a burst rubber hose, or an electricity failure, which are problems that accompany unattended operations, will automatically result in shutting off both the electrical appliances and the flow of cooling water. The whole process of the recrystallization of compounds was automatically, safely, and cleanly carried out in the practically sealed system. The crystallization conditions produced in the described apparatus by using practically insoluble solvents were obviously consistent with the crystallization theory. In other words, crystals separated slowly from the dilute solutions, and these separated crystals ripened and became purified. The high-purity recrystallization purification could be performed more easily by the proposed technique than by the conventional manual technique. The quite pure phenacetins were obtained from water at extremely high recoveries(98% for each recrystallization) by the repeated automatic recrystallizations without any troublesome manual procedure required in an ordinary recrystallization. Their melting points were equal to and higher than that of acetophenetidine which was a melting point standard of National Institute of Hygienic Sciences. The transparent extraction reservoir was helpful for finding the end stage of recrystallization. The safety controlled apparatus should be quite useful for the high-purity automatic recrystallization of compounds.

収録刊行物

  • 分析化学

    分析化学 34 (9), T117-T122, 1985

    公益社団法人 日本分析化学会

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