AAN030_V1 Characterzation of frozen liquids by DMA.pdf

AAN030 Characterisation of Frozen Liquids by DMA using a Liquid Sample Holder 1 AAN030 V1 the freezing poin, forms a solid in the con- tainer. Typically samples are loaded at am- bient temperature, cooled down at a con- trolled cooling rate to a start temperature and then heated at the desired heating rate back to ambient temperature. Cross-linking reactions can be measured at elevated tem- peratures and strain induced re- crystallisation of thermoplastic materials could be investigated from the liquid to the solid state by performing cooling experi- ments from a temperature above the melt to the point of re-crystallisation. The following experimental conditions were employed for the analysis of the liquid samples. Measurement frequencies : 1 Hz Clamp pressure : 4 PSI Heating rate : 2°C/min 3°C/min Mode : 35 mm Dual cantilever. A number of samples have been investi- gated to evaluate the suitability of the liquid holder for the characterisation of the frozen state of a liquid. These sample are: ? Water to identify the melting of ice. ? A 40wt% Sucrose solution ? A commercial shower gel ? Golden Syrup Nick Hawkins, TA Instruments, Crawley, UK Keywords: DMA, Liquid holder, freezing melting point of liquids INTRODUCTION There has been considerable interest in recent years on the characterisation of the viscoelastic properties of liquids/solutions/ pastes in the frozen state. Dynamic Me- chanical Analysis testing has, until recently been a technique that has been utilised for the investigation of materials in the solid state. A novel sample container has been developed that enables liquids to be frozen in a Dynamic Mechanical Analyser and then heated to characterise the viscoelastic properties of the frozen structure. Although qualitative in nature, the technique is able to identify the glass transition and other smaller relaxation processes (such as β and γ relaxations) of frozen liquids/solutions/ pastes. Furthermore i