A vapor-liquid equilibrium still suitable for small amounts of samples.
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概要
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Details are described for the apparatus and procedures for the accurate measurement of vapor–liquid equilibria by use of small amounts of samples. The new recirculation still described is a modification of the Brown's still (<I>Aust. J. Sci. Res., A,</I> <B>5</B>, 530 (1952)) and its total amount of operating charge is <I>ca.</I> 53 cm<SUP>3</SUP>, of which each 7 cm<SUP>3</SUP> is in the vapor- and liquid-sample traps and <I>ca.</I> 23 cm<SUP>3</SUP> is in the boiler. A method of determining an optimum value of the heating current of the boiler is described. Partial condensation of the vapor and entrainment of the liquid phase into the vapor were eliminated. Some results obtained for the system hexane+chlorobenzene at 338.15 K agreed with the thermodynamically consistent values of Brown, showing the reliability of this still operating with the samples having relative volatilities up to 13. The construction of a thermostatted sample vessel without vapor space for a Pulfrich refractometer is also illustrated which is suitable for small quantity of volatile or hygroscopic solution.
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