Dynamic-mechanical thermoanalysis test: a rapid alternative for accelerated freeze-thaw stability evaluation of W/O emulsions.

The aim of this study was to develop a new dynamic-mechanical thermoanalysis (DMTA) test and evaluate its performance as rapid rheological alternative to routinely used freeze-thaw test for accelerated stability testing of water-in-oil (W/O) emulsions. Due to inherent emulsion instability and versatilities of storage and use conditions, stability assessment of emulsion products still remains complex and challenging task. Recommended stability evaluation protocols are time-consuming, imposing need for alternate test procedures, especially in the early stage of product development, as well as in the quality assurance setting, including quality control. Five model W/O emulsions were prepared, comprehensively rheologically characterized (continual and oscillatory tests), and subjected to stability evaluation through freeze-thaw test in stability chamber and DMTA tests using an air-bearing rheometer. Analyzed emulsions displayed desired shear-thinning flow behavior with yield point. The storage modulus dominated over the loss modulus in the linear viscoelastic regions of amplitude sweeps, as was the case in frequency sweeps over entire frequency range. Statistical comparison showed good agreement between freeze-thaw test, as a method available and used in daily routine work for accelerated evaluation of the physical stability, and DMTA test, as a rheological simulation of the said routine method. Duration of DMTA test was significantly shorter compared to routine but lengthy freeze-thaw test (3.5 h versus 12 days).: According to our results, DMTA test could be a rapid alternative for accelerated freeze-thaw stability evaluation of W/O emulsions, thus enabling high formulating turnover and decision making in R&D and QC departments.