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Development of a single droplet freezing apparatus for studying crystallisation in cocoa butter droplets

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Talhat, AM 
Lister, VY 
Moggridge, GD 
Rasburn, JR 
Ian Wilson, D 


The single droplet freezing apparatus described by Pore et al. (J. Am. Oil. Chem. Soc., 86, 215-225), which allows crystallisation to be monitored in situ by X-ray diffraction, was modified to allow rapid switching of coolant gas and monitoring by video microscopy. The apparatus was used to study drops of cocoa butter undergoing simulated spray freezing at high cooling rates, e.g. 130 K/min. The transformation of an Ivory Coast cocoa butter to the Form V polymorph was significantly faster in drops (~40 h) than in static bulk samples (10 days) crystallised under isothermal conditions. Phase transformation was observed from Forms I/II → III → IV → melt → V, with Form V crystallising directly from the melt at 28.6°C. Numerical simulations of the temperature evolution within the droplet established that the drops are not isothermal, explaining why nucleation was initially observed in the lower (upstream) part of the droplet.



Cocoa butter, Polymorphism, Crystallisation, Simulation, Heat transfer

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Journal of Food Engineering

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Elsevier BV
The provision of an EPSRC studentship for AMT and project support from Nestlé PTC York is gratefully acknowledged. The apparatus was constructed by Lee Pratt, Gary Chapman, Kevin Swan and Wei-Yao Ma. Assistance with the DSC testing from Zlatko Saraçevic, video microscopy from Dr Simon Butler, and general X-ray analysis from Dr Joanna Stasiak are all gratefully acknowledged.