Advanced

Design and testing of a small-scale sublimation apparatus

Briggner, Lars-Erik; Ceolin, Rene; Giovannini, Julien; Payraudeau, Nathalie and Wadsö, Ingemar LU (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:
author
organization
publishing date
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
2009-11-24 17:12:46
date last changed
2017-01-01 05:08:43
@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},
  keyword      = {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},
  volume       = {98},
  year         = {2009},
}