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Effective Separation of N ‐benzyl‐2‐methyl‐4‐nitroaniline (BNA) Polymorphs through Antisolvent Crystallization Method
Author(s) -
Kalaivanan Raju,
Srinivasan Karuppannan
Publication year - 2018
Publication title -
crystal research and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.377
H-Index - 64
eISSN - 1521-4079
pISSN - 0232-1300
DOI - 10.1002/crat.201800052
Subject(s) - monoclinic crystal system , supersaturation , orthorhombic crystal system , solubility , crystallization , nucleation , methanol , solvent , crystallography , chemistry , materials science , analytical chemistry (journal) , chemical engineering , crystal structure , organic chemistry , engineering
Abstract The Influence of antisolvent water on the polymorphic nucleation of N ‐benzyl‐2‐methyl‐4‐nitroaniline (BNA) during its crystallization from methanol solution is revealed. The solubility of BNA in methanol‐water solvent mixtures is determined by gravimetric method and the variation in the level of supersaturation generated with respect to antisolvent concentration is assessed at different volume combinations of saturated methanol BNA solution and water. The supersaturation dependent polymorphic nucleation of orthorhombic and monoclinic forms and their growth morphologies such as platy‐like orthorhombic and needle‐like monoclinic are examined through in‐situ optical microscopy. Single crystals of the grown polymorphs are successfully separated and their structural, thermal, spectroscopic and optical transmittance properties are confirmed through PXRD, DSC, FTIR and UV‐Vis‐near IR analyses respectively.