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image/svg+xml Jakob Voss, based on art designer at PLoS, modified by Wikipedia users Nina and Beao Closed Access logo, derived from PLoS Open Access logo. This version with transparent background. http://commons.wikimedia.org/wiki/File:Closed_Access_logo_transparent.svg Jakob Voss, based on art designer at PLoS, modified by Wikipedia users Nina and Beao Journal of Pharmaceu...arrow_drop_down
image/svg+xml Jakob Voss, based on art designer at PLoS, modified by Wikipedia users Nina and Beao Closed Access logo, derived from PLoS Open Access logo. This version with transparent background. http://commons.wikimedia.org/wiki/File:Closed_Access_logo_transparent.svg Jakob Voss, based on art designer at PLoS, modified by Wikipedia users Nina and Beao
Journal of Pharmaceutical Sciences
Article . 2002 . Peer-reviewed
License: Elsevier TDM
Data sources: Crossref
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Freeze‐drying using vacuum‐induced surface freezing

Authors: Martin, Kramer; Bernd, Sennhenn; Geoffrey, Lee;

Freeze‐drying using vacuum‐induced surface freezing

Abstract

A method of freezing during freeze-drying, which avoids undercooling of a solution and allows growth of large, dendritic ice crystals, was investigated. Aqueous solutions of mannitol, sucrose, or glycine were placed under a chamber vacuum of approximately 1 mbar at a shelf temperature of +10 degrees C. Under these conditions, the solutions exhibit surface freezing to form an ice layer of approximately 1-3 mm thickness. On releasing the vacuum and lowering the shelf temperature to below the freezing point of the ice in the solution, crystal growth occurs to yield large, chimney-like ice crystals. The duration of primary drying of a frozen cake--as measured by using inverse comparative pressure measurement--was up to 20% shorter than when using a "moderate" freezing procedure (2 K shelf temperature per min). With mannitol, however, the residual moisture content of the final dried product was higher than with moderate freezing, and with sucrose and glycine there was no difference. These findings are related to the structures of the dried cakes formed during freezing, as examined by light microscopy and wide-angle X-ray diffraction. The introduction of an annealing step (4 h at a shelf temperature slightly above the onset melting point of the ice in the frozen cake) combined with the vacuum-induced surface freezing procedure maintains the rapid primary drying and produces a low residual moisture (0.2%) for the freeze-dried mannitol solution.

Related Organizations
Keywords

Microscopy, Vacuum, Surface Properties, Ice, Glycine, Temperature, Solutions, Freeze Drying, Mannitol, Crystallization

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Powered by OpenAIRE graph
Found an issue? Give us feedback
selected citations
These citations are derived from selected sources.
This is an alternative to the "Influence" indicator, which also reflects the overall/total impact of an article in the research community at large, based on the underlying citation network (diachronically).
BIP!Citations provided by BIP!
popularity
This indicator reflects the "current" impact/attention (the "hype") of an article in the research community at large, based on the underlying citation network.
BIP!Popularity provided by BIP!
influence
This indicator reflects the overall/total impact of an article in the research community at large, based on the underlying citation network (diachronically).
BIP!Influence provided by BIP!
impulse
This indicator reflects the initial momentum of an article directly after its publication, based on the underlying citation network.
BIP!Impulse provided by BIP!
71
Top 10%
Top 10%
Average
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