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Australian Journal of Chemistry Australian Journal of Chemistry Society
An international journal for chemical science
REVIEW

Flash (Vacuum) Pyrolysis Apparatus and Methods*

Curt Wentrup

School of Chemistry and Molecular Biosciences, The University of Queensland, Brisbane, Qld 4072, Australia. Email: wentrup@uq.edu.au




Curt Wentrup was educated at the University of Copenhagen (Cand. Scient. 1966 with K. A. Jensen; D.Sc. 1976) and the Australian National University (Ph.D. 1969 with W. D. Crow). After post-doctoral periods with Hans Dahn (Lausanne), W. M. Jones (Gainesville, FL), and Maitland Jones, Jr (Princeton), he held an assistant professorship at the Université de Lausanne, Switzerland, and a professorship at the Universität Marburg, Germany, before returning to Australia in 1985 as Professor and chair of organic chemistry and head of the organic chemistry section at the University of Queensland, where he is now Emeritus Professor. He has been the editor-in-chief of the Australian Journal of Chemistry since 2008, and chair (now immediate-past chair) of the National Committee for Chemistry of the Australian Academy of Science, of which he is a Fellow, since 2009. He has published over 300 research papers as well as over 30 reviews, chapters, and books. His interests are in the fields of both experimental and computational chemistry of reactive intermediates and unusual molecules using photochemistry, flash vacuum thermolysis, and microwave-induced chemical reactions; in particular, chemistry of nitrenes, carbenes, cumulenes, nitrile ylides, and nitrile imines, pericyclic rearrangements of cyanates, isocyanates, thio- and isothiocyanates, and nitrile oxides and sulfides, and the chemistry of extended cumulenes. He is a recipient of the 2003 Centenary Medal of the Australian Commonwealth for research in organic and physical chemistry, and the 2014 David Craig Medal of the Australian Academy of Science, and he is a JSPS Fellow in 2014.

Australian Journal of Chemistry 67(9) 1150-1165 http://dx.doi.org/10.1071/CH14096
Submitted: 25 February 2014  Accepted: 21 March 2014   Published: 30 April 2014

Abstract

The history of pyrolysis equipment, methods, and reactions is narrated in the Introduction. Detailed descriptions of flash vacuum pyrolysis (FVP) (or thermolysis, FVT) apparatus for preparative and spectroscopic (UV, IR, electron spin resonance) purposes with product isolation at 77 K or in Ar matrices at ~10 K are presented. Very low pressure pyrolysis (VLPP), laser pyrolysis, and pulsed pyrolysis (jet flash pyrolysis) are also described together with illustrations of apparatus. The solvent spray flash vacuum pyrolysis (SS-FVP) of liquids or solutions of compounds of low volatility is described together with methods for the addition of solids to a pyrolysis tube, in particular details of pipto-pyrolysis (‘falling solid pyrolysis’). Methods used for catalytic vacuum gas–solid reactions (VGSR) are also summarised.

Graphical Abstract Image


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