A novel powder sample holder for the determination of glass transition temperatures by DMA

The use of a new sample holder for dynamic mechanical analysis (DMA) as a means to characterise the Tg of powdered hydroxypropyl methyl cellulose (HPMC) has been investigated. A sample holder was constructed consisting of a rectangular stainless steel container and a lid engineered to fit exactly within the walls of the container when clamped within a TA instruments Q800 DMA in dual cantilever configuration. Physical mixtures of HPMC (E4M) and aluminium oxide powders were placed in the holder and subjected to oscillating strains (1 Hz, 10 Hz and 100 Hz) whilst heated at 3 °C/min. The storage and loss modulus signals showed a large reduction in the mechanical strength above 150 °C which was attributed to a glass transition. Optimal experimental parameters were determined using a design of experiment procedure and by analysing the frequency dependence of Tg in Arrhenius plots. The parameters were a clamping pressure of 62 kPa, a mass ratio of 0.2 HPMC in aluminium oxide, and a loading mass of either 120 mg or 180 mg. At 1 Hz, a Tg of 177 ± 1.2 °C (n = 6) for powdered HPMC was obtained. In conclusion, the new powder holder was capable of measuring the Tg of pharmaceutical powders and a simple optimization protocol was established, useful in further applications of the DMA powder holder.