Alan M.

Phipps
Boston College
Chestnut Hill, Massachusetts
General Purpose Low Temperature
and David N. Hume
Massachusetts Institute of Technoloqv
Dry-Ice Baths
Cambridge, Massachusetts 62139
- I
A great many methods have been de- is not useful since it forms a thick sludge at its melting
scribed for thc preparation and maintenance of low point ( - 2 6 T ) but mixtures of o- and m-xylene give low
temperature baths, and the field has been extensively viscosity baths with an approximately linear tempera-
reviewed recently.' Among the simpler techniques, the ture dependence on composition (see figure). Analyti-
liquid nitrogen-organic solvent slush bath has become cal grade acetonitrile gives a useful bath a t -4Z°C,
increasingly popular and a compilation of 86 such baths while temperatures between -4Z°C and -51°C are
has been published by R ~ n d e a u . ~ obtainable with acetonitrile containing 0-3% acrylo-
We have found it convenient to employ an even nitrile. Technical grade acetouitrile was found to give
simpler bath composed of solid carbon dioxide and a reproducible bath at -46'C. Some mixtures do not
organic solvents or solvent mixtures having a freezing give baths in which the temperature varies normally
point above -7S°C. Solid lumps of dry ice in a with composition. Mixtures of 3-hept,anone or cyclo-
Dewar flask containing one of several solvent systems hexanone with acetone act as if they were acetone-dry
afford a bath of rcasonahly uniform temperature and ice baths containing the solidified higher-melting ketone.
low viscosity. Such a bath is not, of course, a system a t A similar result ensues for mixtures of n-octane and
equilibrium; a layer of solid solvent appears to form iso-octane.
over the dry ice and a steady state is obtained with Because of the simplicity of the technique, the easy
slow evolution of gaseous CO1. The baths are generally availability of dry ice and its low cost, and the readiness
reproducible to + 1°C if they are agitated intermittantly with which a desired temperature may be obtained, the
and if only a small excess of dry ice is used (e.g., 2 4 cc use of dry ice baths is worth consideration even where
per 200 ml in a standard 265 ml (one pint) Dewar flask). equipment for handling liquid nitrogen is available.
Many of the solvents cited by Rondeau may be em- This work was supported in part through funds pro-
ployed, although the bath temperature is not always vided by the U.S. Atomic Energy Commission under
the melting point of the solvent. Carbon tetrachlo- Contract AT(30-1)-905.
ride (-23"C), 3-hcptanone (-3S0C), cyclohexanone
(-46°C) and chloroform (-61°C) provide reproducible
low viscosity baths at the temperature indicated.
Many solvents which have appropriate melting
points may be unsatisfactory because they solidify, or
becon~ehighly viscous at low temperatures (c.g., n-
octane, alcohols) or are noxious. Certain solvents,
however, when mixed in the right proportions provide a
considerable range of stable bath temperatures together
with low viscosity. Of especial interest to this labora-
tory has been the attainment of temperatures through-
out the liquid range of ammonia (-78' to -33"C), and
we have fonnd that most of this range can be covered
with mixtures of ovtho and nzeta-xylene. Pure o-xylene

-80
NABSLER, J., "Experimental Techniques for Low Boiling Sol- 0 0.2 0.4 0.6 0.8
vents," Academic Press, New York, N . Y . , 1966, "Vol. I.- Volume Froction of 0-rylene
The Chemistry of Non-Aqueous Solvents," (Editor: J. J. LAG-
OWSKI), p. 213.
RONDBAU, R. E., 3. Chem. and Eng. Data, 11,124 (1966). Stecldy stole temperature of dry-ice--xylene, m-xylem mixtvro~.

664 / Journal o f Chemicol Education