The static isothermal crystallization of palm oil was studied by oscillatory rheology. The phase angle, complex modulus, storage modulus and loss modulus were followed as a function of the crystallization time. Various crystallization temperatures were applied, and the results obtained by oscillatory rheology were compared with crystallization data obtained by more classical techniques like differential scanning calorimetry (DSC) and pulsed nuclear magnetic resonance (pNMR). It was shown that oscillatory rheology is a valuable complementary method to DSC and pNMR to evaluate primary crystallization. Like DSC and pNMR, oscillatory rheology is capable of differentiating whether crystallization occurs in a two-stage or a single-stage process. In addition, oscillatory measurements also allow the evaluation of aggregation, network formation and post-hardening events like sintering and thus provide information on the crystal network and the final macroscopic properties of the crystallized sample.
The influence of shear on the crystallization of palm oil was studied at four different crystallization temperatures (18, 20, 22 and 25 degrees C). Time-resolved X-ray analyses were carried out to study the effect of continuous shear on the crystallization kinetics of the fat. Rheological measurements were used to assess the effect of a shear step on crystallization, and finally polarized light microscopy was used to follow changes in microstructure due to the applied initial shear step. It was shown that shear enhanced the primary crystallization, even when low shear rates were applied for a short period. Furthermore, a shear step prior to crystallization without shear has a marked influence on the microstructural development
To follow palm oil crystallization under shear, a new rheological method was developed. This method can be split up into two parts: In the first part, continuous shear is applied for a pre-defined period and crystallization is monitored by measuring the apparent viscosity as a function of isothermal time under shear. In the second part, shear is halted and oscillation is applied during 30 s, thus recording moduli and phase angle. These moduli and phase angle are then characteristic of a sample crystallized under shear during this pre-defined period. After repeating this procedure for increasing shearing periods in the first part, complex modulus and phase angle were plotted as a function of isothermal time under shear. The thus obtained results were compared with crystallization data obtained via time-resolved X-ray diffraction and polarized light microscopy
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