Characterizing the thermal phase behaviour of fipronil polymorphs
نویسندگان
چکیده
Abstract This manuscript reports the investigation of polymorphic behaviour fipronil using a systematic comparison thermochemical and structural properties different crystal forms obtained in this study as well those previously reported literature. The analytical techniques employed include DSC, TGA, PXRD, SCXRD hot stage microscopy. DSC proved particularly useful because it made possible to differentiate between two found as-received neat fipronil. scans revealed presence polymorphs which had melting endotherms with peak maxima at ca . 196 °C 205 °C, respectively. These were successfully separated via sublimation resulted metastable, lower polymorph sublimate thermodynamically stable, higher form residue. Clear evidence for instability was when examined under range heating rates. proportion metastable appeared increase rate increased, indicating that underwent solid–solid phase transition stable low Recrystallization from solvents yielded five forms. TGA curves all forms, except acetone-derived one, solvate pseudo-polymorphs showed solvent loss 60 100 °C. sample hemihydrate only started show mass 120 studies three have similar characteristics, while other differ notably each rest structures. Despite these differences, exhibit near-identical intra- intermolecular hydrogen bond networks.
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ژورنال
عنوان ژورنال: Journal of Thermal Analysis and Calorimetry
سال: 2023
ISSN: ['1388-6150', '1572-8943', '1588-2926']
DOI: https://doi.org/10.1007/s10973-023-12198-x