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Temperature and Heat Transfer Control During Freeze Drying. Effect of Vial Holders and Influence of Pressure

Palmkron, Shuai Bai ; Gustavsson, Linnea ; Wahlgren, Marie LU orcid ; Bergensthål, Björn LU and Fureby, Anna Millqvist (2022) In Pharmaceutical Research 39(10). p.2597-2606
Abstract

Objective: A common issue of freeze drying is the inhomogeneity between samples, both in regards to water content and structure. The purpose of this study is to address this issue, and try to understand the cause of inhomogeneity in the heat transfer and sample temperature. Methods: The temperature and the heat transfer was measured using different setups, both with and without vial holders at various positions at different shelf temperature and chamber pressures. By comparing sublimation rate measurements (water sample) with temperature equilibrium measurements with a non-evaporating liquid (oil sample), the heat transfer contribution from radiation and conduction could be separated and investigated individually. Results: The oil... (More)

Objective: A common issue of freeze drying is the inhomogeneity between samples, both in regards to water content and structure. The purpose of this study is to address this issue, and try to understand the cause of inhomogeneity in the heat transfer and sample temperature. Methods: The temperature and the heat transfer was measured using different setups, both with and without vial holders at various positions at different shelf temperature and chamber pressures. By comparing sublimation rate measurements (water sample) with temperature equilibrium measurements with a non-evaporating liquid (oil sample), the heat transfer contribution from radiation and conduction could be separated and investigated individually. Results: The oil sample temperature increases each time the pressure is decreased; the increase is highest at lower shelf temperatures. Using vial holder reduces the deviation between the samples but have limited effect on the temperature increase. The sublimation rate for water sample is pressure dependent and samples close to the walls have a higher sublimation rate than vials in the center. The sublimation rate increases slightly when using a vial holder but the deviation between vials becomes more random. Conclusions: The heat transfer consists of conduction through rectified vapor and radiation from surrounding walls, about 65–75% of the heat is transferred by conduction and 25–35% by radiation under normal operational conditions. As the vial holder is also influenced by the radiation, the vial inside the holder is indirectly affected by the surrounding radiation.

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Please use this url to cite or link to this publication:
author
; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
freeze-frying, heat transfer, radiation, sublimation rate, vial holder
in
Pharmaceutical Research
volume
39
issue
10
pages
2597 - 2606
publisher
Springer
external identifiers
  • pmid:35925479
  • scopus:85135560525
ISSN
0724-8741
DOI
10.1007/s11095-022-03353-4
language
English
LU publication?
yes
id
5201dd1a-48c2-4d1e-ac03-56a7597e7c0b
date added to LUP
2022-09-20 15:28:03
date last changed
2024-07-11 23:31:11
@article{5201dd1a-48c2-4d1e-ac03-56a7597e7c0b,
  abstract     = {{<p>Objective: A common issue of freeze drying is the inhomogeneity between samples, both in regards to water content and structure. The purpose of this study is to address this issue, and try to understand the cause of inhomogeneity in the heat transfer and sample temperature. Methods: The temperature and the heat transfer was measured using different setups, both with and without vial holders at various positions at different shelf temperature and chamber pressures. By comparing sublimation rate measurements (water sample) with temperature equilibrium measurements with a non-evaporating liquid (oil sample), the heat transfer contribution from radiation and conduction could be separated and investigated individually. Results: The oil sample temperature increases each time the pressure is decreased; the increase is highest at lower shelf temperatures. Using vial holder reduces the deviation between the samples but have limited effect on the temperature increase. The sublimation rate for water sample is pressure dependent and samples close to the walls have a higher sublimation rate than vials in the center. The sublimation rate increases slightly when using a vial holder but the deviation between vials becomes more random. Conclusions: The heat transfer consists of conduction through rectified vapor and radiation from surrounding walls, about 65–75% of the heat is transferred by conduction and 25–35% by radiation under normal operational conditions. As the vial holder is also influenced by the radiation, the vial inside the holder is indirectly affected by the surrounding radiation.</p>}},
  author       = {{Palmkron, Shuai Bai and Gustavsson, Linnea and Wahlgren, Marie and Bergensthål, Björn and Fureby, Anna Millqvist}},
  issn         = {{0724-8741}},
  keywords     = {{freeze-frying; heat transfer; radiation; sublimation rate; vial holder}},
  language     = {{eng}},
  number       = {{10}},
  pages        = {{2597--2606}},
  publisher    = {{Springer}},
  series       = {{Pharmaceutical Research}},
  title        = {{Temperature and Heat Transfer Control During Freeze Drying. Effect of Vial Holders and Influence of Pressure}},
  url          = {{http://dx.doi.org/10.1007/s11095-022-03353-4}},
  doi          = {{10.1007/s11095-022-03353-4}},
  volume       = {{39}},
  year         = {{2022}},
}