Purity Determination of Organic Compounds by a Newly Designed DTA Apparatus

概要

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An apparatus of differential thermal analysis has been designed and constructed for the purpose of determining the purity of organic compounds with as small an amount of sample as possible, within a short time and yet with an accuracy of better than ±0.001 mol%. Degussa platinum thermometers were used. They were calibrated with a precision of better than ±0.004° against a standard platinum resistance thermometer. Methods for determining the impurities in samples on the basis of irreversible thermodynamics have been developed. The results were compared with those obtained by using an adiabatic calorimeter of our laboratory and by the National Bureau of Standards. The apparatus proved to be useful in determining the purity of about 1 m<I>l</I> of samples, whose melting points lie in the temperature range −200°C–+200°C within an accuracy of ±0.004 mol% in about 1.5 hr.
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