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Regulatory aspects of the pharmaceutical nanosolids and an increasing number of insoluble molecules in the developmental pipeline have encouraged scientists for conducting further pharmaceutical researches and use of nanosolids. Among various analytical techniques, DSC has been used for quantifying an amorphous or crystalline phase in nanosolids. Several methodologies based on the calorimeter type (conventional DSC or MTDSC), measured parameters, and experimental conditions are used for monitoring the behavior of pharmaceutical nanosolids. Glass transition endotherm, crystallization exotherm, and fusion endotherm are the main parameters of an amorphous or crystalline material to be assessed while using conventional DSC. Glass transition endotherm is a result of the presence of the amorphous phase, and the crystallization exotherm results from recrystallization of the amorphous content.