Design and testing of a small-scale sublimation apparatus
(2009) In Journal of Thermal Analysis and Calorimetry 98(1). p.331-335- Abstract
- In many areas of scientific research and development, for example in the pharmaceutical industry, it is important to prepare and to characterize crystals of pure organic compounds which are thermodynamically stable. The formation of crystals from the gas phase is technically less straightforward than crystallisation from solution, but sublimation techniques can have several important features. In the present paper we report the design and testing of a novel apparatus for small scale sublimation and fractional deposition of crystals. The instrument has been developed with special reference to the needs in the pharmaceutical industry. A few mg of the samples are enclosed, under reduced pressure, in thin-walled glass tubes, along which a well... (More)
- In many areas of scientific research and development, for example in the pharmaceutical industry, it is important to prepare and to characterize crystals of pure organic compounds which are thermodynamically stable. The formation of crystals from the gas phase is technically less straightforward than crystallisation from solution, but sublimation techniques can have several important features. In the present paper we report the design and testing of a novel apparatus for small scale sublimation and fractional deposition of crystals. The instrument has been developed with special reference to the needs in the pharmaceutical industry. A few mg of the samples are enclosed, under reduced pressure, in thin-walled glass tubes, along which a well defined temperature gradient can be formed. During an experiment the substance will sublime from the hot end of the glass tube and crystals will be deposited along the temperature gradient. The applicability of the instrument has been verified by experiments with several test compounds. Results from experiments with carbamazepine, are reported in some detail. Carbamazepine single crystals of high quality were obtained and the transition temperature between the triclinic (Form I) and the monoclinic (Form III) crystal modifications agreed with literature values. (Less)
Please use this url to cite or link to this publication:
https://lup.lub.lu.se/record/1504993
- author
- Briggner, Lars-Erik ; Ceolin, Rene ; Giovannini, Julien ; Payraudeau, Nathalie and Wadsö, Ingemar LU
- organization
- publishing date
- 2009
- type
- Contribution to journal
- publication status
- published
- subject
- keywords
- Single crystal, Polymorph, Drug development, Pharmaceutical industry, Sublimation
- in
- Journal of Thermal Analysis and Calorimetry
- volume
- 98
- issue
- 1
- pages
- 331 - 335
- publisher
- Akademiai Kiado
- external identifiers
-
- wos:000271282000044
- scopus:70350767358
- ISSN
- 1588-2926
- DOI
- 10.1007/s10973-009-0114-4
- language
- English
- LU publication?
- yes
- id
- 2cef7fcd-70b9-47e5-be44-9b8ff2c659da (old id 1504993)
- date added to LUP
- 2016-04-01 12:26:23
- date last changed
- 2022-01-27 03:44:06
@article{2cef7fcd-70b9-47e5-be44-9b8ff2c659da,
abstract = {{In many areas of scientific research and development, for example in the pharmaceutical industry, it is important to prepare and to characterize crystals of pure organic compounds which are thermodynamically stable. The formation of crystals from the gas phase is technically less straightforward than crystallisation from solution, but sublimation techniques can have several important features. In the present paper we report the design and testing of a novel apparatus for small scale sublimation and fractional deposition of crystals. The instrument has been developed with special reference to the needs in the pharmaceutical industry. A few mg of the samples are enclosed, under reduced pressure, in thin-walled glass tubes, along which a well defined temperature gradient can be formed. During an experiment the substance will sublime from the hot end of the glass tube and crystals will be deposited along the temperature gradient. The applicability of the instrument has been verified by experiments with several test compounds. Results from experiments with carbamazepine, are reported in some detail. Carbamazepine single crystals of high quality were obtained and the transition temperature between the triclinic (Form I) and the monoclinic (Form III) crystal modifications agreed with literature values.}},
author = {{Briggner, Lars-Erik and Ceolin, Rene and Giovannini, Julien and Payraudeau, Nathalie and Wadsö, Ingemar}},
issn = {{1588-2926}},
keywords = {{Single crystal; Polymorph; Drug development; Pharmaceutical industry; Sublimation}},
language = {{eng}},
number = {{1}},
pages = {{331--335}},
publisher = {{Akademiai Kiado}},
series = {{Journal of Thermal Analysis and Calorimetry}},
title = {{Design and testing of a small-scale sublimation apparatus}},
url = {{http://dx.doi.org/10.1007/s10973-009-0114-4}},
doi = {{10.1007/s10973-009-0114-4}},
volume = {{98}},
year = {{2009}},
}