Metastable zone determination of lipid systems: Ultrasound velocity versus optical back-reflectance measurements



The metastable zone width (MZW) of a multi-component system as influenced by the process parameters cooling rate, agitation speed, and additive concentration was determined via ultrasound velocity measurements. The results were compared with those obtained by optical back-reflectance measurements (ORM) using coconut oil as a model substance. Increasing the cooling rate led to the shift of the nucleation point to lower temperatures. This tendency was better visualized by the ultrasonic curves while a significant disturbance of the ORM signal could be observed. Agitation led to an increase of the nucleation temperature and hence a narrower metastable zone. The influence of an additive on the MZW was found to strongly depend on its concentration. The MZW detected by the ultrasound technique was narrower compared to that obtained by the ORM method, indicating the faster response to the phase transition of the ultrasound technique. Another advantage of the ultrasound technique was the in situ evaluation of the experimental data, while ORM needed a linear fitting to estimate the saturation temperature. Furthermore, ultrasound velocity measurements are based on density determination of the medium whereas the ORM sensor is able to detect only particles that are located within the measuring zone and possess a well-defined size.

Practical applications: MZW is one of the most important parameters that determine the characteristics of crystalline products. However, a proper technique that can be used in MZW detection in fat systems has rarely been reported, due to the difficulties in dealing with natural fats. The findings of this study can greatly help those who are involved in the field of fat crystallization from both the academic and the practical point of view. This is due to the fact that new and promising techniques for the online and in situ determination of the MZW of fats, with high accuracy, and reproducibility, under most process conditions, were clarified in this work. The readers can easily follow the procedure developed in this paper. Also information about the influence of process parameters and additives on the MZW is included.