示差走査熱量計(DSC)による精密純度測定法

概要

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A study of the measurement and the data-proceeding analysis methods has been conducted in order to expand the range of the application of the differential scanning calorimeter (DSC)-based purity measurement method. Using a variety of systems that form eutectic mixtures, samples were measured by the DSC method. The heat of fusion of the melt fraction was determined including the fusion curve of the eutectic mixture. Temperature (T) versus the inverse of the melt fraction (1/F) was plotted at the inflection point on the declining side of the DSC curve at the principal component peak. The heat of fusion of the meet fraction was corrected so as to linearize the curved line of T versus 1/F. On the basis of the straightened line, the estimated values of the melting points of the pure substance (T_o) and that of the sample (T_m) were obtained and the sample purity was determined using the van't Hoff equation. A heat correction to linearize the van't Hoff plot was carried out to the negative range, because the decrease of the heat of fusion of the melt fraction with an decrease in the enthalpy of the eutectic mixture at the first heating was excluded. The purity measured by the DSC method can be determined to be fully reliable up to the purities of 95 mo1%.
社団法人日本薬学会の論文
1997-02-25