V Andronis1, G Zografi. 1. School of Pharmacy, University of Wisconsin-Madison 53706, USA.
Abstract
PURPOSE: To determine the viscosity and the frequency-dependent shear modulus of supercooled indomethacin as a function of temperature near and above its glass transition temperature and from these data to obtain a quantitative measure of its molecular mobility in the amorphous state. METHODS: Viscoelastic measurements were carried with a controlled strain rheometer in the frequency domain, at 9 temperatures from 44 degrees to 90 degrees C. RESULTS: The viscosity of supercooled indomethacin shows a strong non-Arrhenius temperature dependence over the temperature range studied, indicative of a fragile amorphous material. Application of the viscosity data to the VTF equation indicates a viscosity of 4.5 x 10(10) Pa.s at the calorimetric Tg of 41 degrees C. and a T0 of -17 degrees C. From the complex shear modulus and the Cole-Davidson equation the shear relaxation behaviour is found to be non-exponential, and the shear relaxation time at Tg is found to be approximately 100 sec. CONCLUSIONS: Supercooled indomethacin near and above its Tg exhibits significant molecular mobility, with relaxation times similar to the timescales covered in the handling and storage of pharmaceutical products.
PURPOSE: To determine the viscosity and the frequency-dependent shear modulus of supercooled indomethacin as a function of temperature near and above its glass transition temperature and from these data to obtain a quantitative measure of its molecular mobility in the amorphous state. METHODS: Viscoelastic measurements were carried with a controlled strain rheometer in the frequency domain, at 9 temperatures from 44 degrees to 90 degrees C. RESULTS: The viscosity of supercooled indomethacin shows a strong non-Arrhenius temperature dependence over the temperature range studied, indicative of a fragile amorphous material. Application of the viscosity data to the VTF equation indicates a viscosity of 4.5 x 10(10) Pa.s at the calorimetric Tg of 41 degrees C. and a T0 of -17 degrees C. From the complex shear modulus and the Cole-Davidson equation the shear relaxation behaviour is found to be non-exponential, and the shear relaxation time at Tg is found to be approximately 100 sec. CONCLUSIONS: Supercooled indomethacin near and above its Tg exhibits significant molecular mobility, with relaxation times similar to the timescales covered in the handling and storage of pharmaceutical products.