Phase transitions in LiKSO<SUB>4</SUB>: low-temperature neutron diffraction results

Results of a detailed crystallographic study of the structural phase transitions in LiKSO<SUB>4</SUB>, carried out using single crystal neutron diffraction at ambient and below-ambient temperatures (300-100 K), are presented. The study indicates two clear phase transitions at 205 K (from space group P6<SUB>3</SUB> to space group P31c), at 189 K (to space group Cc) and a third transition at about 130 K in the cooling cycle. The corresponding temperatures are 250 K, 200 K and 138 K in the heating cycle. The existence of twins, mixed phases, and extremely sluggish kinetics for the various phase transitions, as well as the structural details of the various phases in this mixed salt, can explain the apparent inconsistencies in the results of several experimental investigations reported in the literature

Low-temperature phase transitions in LiKSO<SUB>4</SUB>: a neutron study

A single crystal neutron diffraction study of the low temperature structural phase transitions in LiKSO4 has been carried out. Detailed temperature dependence of the Bragg peak profiles and integrated intensities for a group of about 20 reflections has been investigated upon cooling and heating in the temperature range 300 K to 96 K. The crystal undergoes three clear phase transitions at 205 K (from sp. gr. P63 to sp. gr. P31c), at 189 K and at about 135 K on cooling. The corresponding temperatures are 250 K, 190 K and 138 K on the heating cycle. These transitions are extremely sluggish, the kinetics depending on the thermal treatment of the crystal

Using USP I and USP IV for discriminating dissolution rates of nano- and microparticle-loaded pharmaceutical strip-films.

Recent interest in the development of drug particle-laden strip-films suggests the need for establishing standard regulatory tests for their dissolution. In this work, we consider the dissolution testing of griseofulvin (GF) particles, a poorly water-soluble compound, incorporated into a strip-film dosage form. The basket apparatus (USP I) and the flow-through cell dissolution apparatus (USP IV) were employed using 0.54% sodium dodecyl sulfate as the dissolution medium as per USP standard. Different rotational speeds and dissolution volumes were tested for the basket method while different cell patterns/strip-film position and dissolution media flow rate were tested using the flow-through cell dissolution method. The USP I was not able to discriminate dissolution of GF particles with respect to particle size. On the other hand, in the USP IV, GF nanoparticles incorporated in strip-films exhibited enhancement in dissolution rates and dissolution extent compared with GF microparticles incorporated in strip-films. Within the range of patterns and flow rates used, the optimal discrimination behavior was obtained when the strip-film was layered between glass beads and a flow rate of 16 ml/min was used. These results demonstrate the superior discriminatory power of the USP IV and suggest that it could be employed as a testing device in the development of strip-films containing drug nanoparticles