Design and testing of a small-scale sublimation apparatus

Research output: Contribution to journalArticle

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.

Details

Authors
  • Lars-Erik Briggner
  • Rene Ceolin
  • Julien Giovannini
  • Nathalie Payraudeau
  • Ingemar Wadsö
Organisations
Research areas and keywords

Subject classification (UKÄ) – MANDATORY

  • Physical Chemistry

Keywords

  • Single crystal, Polymorph, Drug development, Pharmaceutical industry, Sublimation
Original languageEnglish
Pages (from-to)331-335
JournalJournal of Thermal Analysis and Calorimetry
Volume98
Issue number1
Publication statusPublished - 2009
Publication categoryResearch
Peer-reviewedYes