Ray et al (2017) Chem Eng Sci IR.pdf (3.11 MB)

A freeze-drying microscopy study of the kinetics of sublimation in a model lactose system

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journal contribution
posted on 06.07.2017 by Purnima Ray, Chris Rielly, Andy Stapley
Freeze drying microscopy has been used to probe the lyophilisation kinetics of lactose solutions of various concentrations, at temperatures ranging from -50. °C to -30. °C and under a constant pressure of 1. Pa. Sublimation front velocities were determined by recording a sequence of video images of the sublimation and analysing the frontal progression using MATLAB. Initial experiments showed poor reproducibility. To combat this, silver iodide (AgI) was added as an ice nucleator, which raised nucleation temperatures and improved reproducibility when compared to non-AgI experiments. The lower supercooling on nucleation when AgI was used also produced larger ice crystals, which enabled the crystal microstructure of the more dilute samples to be more clearly observed. This showed long thin crystals, and the orientation of these crystals with respect to the direction of the frontal movement strongly affected frontal progression rates, which explained the earlier reproducibility problems. A twin resistance mass transfer model, comprising a fixed edge resistance and a resistance which increased with frontal depth, was able to describe the sublimation kinetics. The edge resistance first increased and then decreased with solids content. The resistance per unit depth increased exponentially with solids content, so much so that there is an optimal solids content in relation to the rate of production of dried material. Resistances were also much higher when crystals were oriented with their major axis perpendicular to the direction of frontal movement. Freeze drying rates were approximately proportional to the saturation vapour pressure of water, however the long-held belief that water vapour pressure is the main driving force for mass transfer in freeze-drying systems may be an oversimplification as this only reflects driving forces in the vapour phase (pores) rather than within the solid.

Funding

The authors would like to thank the Department of Chemical Engineering, Loughborough University, UK for funding this work.

History

School

  • Aeronautical, Automotive, Chemical and Materials Engineering

Department

  • Chemical Engineering

Published in

Chemical Engineering Science

Citation

RAY, P., RIELLY, C.D. and STAPLEY, A.G.F., 2017. A freeze-drying microscopy study of the kinetics of sublimation in a model lactose system. Chemical Engineering Science, 172, pp.731-743.

Publisher

© Elsevier

Version

AM (Accepted Manuscript)

Publisher statement

This work is made available according to the conditions of the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) licence. Full details of this licence are available at: https://creativecommons.org/licenses/by-nc-nd/4.0/

Acceptance date

26/05/2017

Publication date

2017

Notes

This paper was published in the journal Chemical Engineering Science and the definitive published version is available at http://dx.doi.org/10.1016/j.ces.2017.05.047.

ISSN

1873-4405;0009-2509

Language

en

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