Milk protein fractionation by microfiltration membranes is an established but still growing field in dairy technology. Even under cross-flow conditions, this filtration process is impaired by the formation of a deposit by the retained protein fraction, mainly casein micelles. Due to deposition formation and consequently increased overall filtration resistance, the mass flow of the smaller whey protein fraction declines within the first few minutes of filtration. Currently, there are only a handful of analytical techniques available for the direct observation of deposit formation with opaque feed media and membranes. Here, we report on the ongoing development of a non-invasive and non-destructive method based on magnetic resonance imaging (MRI), and its application to characterise deposit layer formation during milk protein fractionation in ceramic hollow fibre membranes as a function of filtration pressure and temperature, temporally and spatially resolved. In addition, the chemical composition of the deposit was analysed by reversed phase high pressure liquid chromatography (RP-HPLC). We correlate the structural information gained by in-situ MRI with the protein amount and composition of the deposit layer obtained by RP-HPLC. We show that the combination of in-situ MRI and chemical analysis by RP-HPLC has the potential to allow for a better scientific understanding of the pressure and temperature dependence of deposit layer formation.
27 December 2021 in Magnetic Resonance in Chemistry
Increasing the efficiency of disperse phase crystallization is of great interest for melt emulsion production as the fraction of solidified droplets determines product quality and stability. Nucleation events must appear within every single one of the μm‐sized droplets for solidification. Therefore, primary crystallization requires high subcooling and is, thus, time and energy consuming. Contact‐mediated nucleation is a mechanism for intensifying the crystallization process. It is defined as the successful nucleation of a subcooled liquid droplet induced by contact with an already crystallized droplet. We investigated contact‐mediated nucleation under shear flow conditions up to shear rates of 457 s−1 for a quantitative assessment of this mechanism. Rheo‐nuclear magnetic resonance was successfully used for the time‐resolved determination of the solids fraction of the dispersed phase of melt emulsions upon contact‐mediated nucleation events. The measurements were carried out in a dedicated Taylor–Couette cell. The efficiency of contact‐mediated nucleation decreased with increasing shear rate, whereas the effective second order kinetic constant increased approximately linearly at small shear rates and showed a linear decrease for shear rates higher than about 200 s−1. These findings are in accordance with coalescence theory. Thus, the nucleation rate is optimal at specific flow conditions. There are limitations for successful inoculation at a low shear rate because of rare contact events and at a high shear rate due to too short contact time.