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Cooling bath

Cooling bath

A cooling bath or ice bath, in laboratory chemistry practice, is a liquid mixture which is used to maintain low temperatures, typically between 13 °C and −196 °C. These low temperatures are used to collect liquids after distillation, to remove solvents using a rotary evaporator, or to perform a chemical reaction below room temperature (see Kinetic control). Cooling baths are generally one of two types: (a) a cold fluid (particularly liquid nitrogen, water, or even air) — but most commonly the term refers to (b) a mixture of 3 components: (1) a cooling agent (such as dry ice or ice); (2) a liquid "carrier" (such as liquid water, ethylene glycol, acetone, etc.), which transfers heat between the bath and the vessel; (3) an additive to depress the melting point of the solid/liquid system. A familiar example of this is the use of an ice/rock-salt mixture to freeze ice cream. Adding salt lowers the freezing temperature of water, lowering the minimum temperature attainable with only ice.

Mixed-solvent cooling baths Mixing solvents creates cooling baths with variable freezing points. Temperatures between approximately −78 °C and −17 °C can be maintained by placing coolant into a mixture of ethylene glycol and ethanol, while mixtures of methanol and water span the −128 °C to 0 °C temperature range. Dry ice sublimes at −78 °C, while liquid nitrogen is used for colder baths. As water or ethylene glycol freeze out of the mixture, the concentration of ethanol/methanol increases. This leads to a new, lower freezing point. With dry ice, these baths will never freeze solid, as pure methanol and ethanol both freeze below −78 °C (−98 °C and −114 °C respectively). Relative to traditional cooling baths, solvent mixtures are adaptable for a wide temperature range. In addition, the solvents necessary are cheaper and less toxic than those used in traditional baths.

Traditional cooling baths

Water and ice baths A bath of ice and water will maintain a temperature 0 °C, since the melting point of water is 0 °C. However, adding a salt such as sodium chloride will lower the temperature through the property of freezing-point depression. Although the exact temperature can be hard to control, the weight ratio of salt to ice influences the temperature:

−10 °C can be achieved with a 1:2.5 mass ratio of calcium chloride hemihydrate to ice. −20 °C can be achieved with a 1:3 mass ratio of sodium chloride to ice.

Dry ice baths at −78 °C Since dry ice will sublime at −78 °C, a mixture such as acetone/dry ice will maintain −78 °C. Also, the solution will not freeze because acetone requires a temperature of about −93 °C to begin freezing.

Safety recommendations The American Chemical Society notes that the ideal organic solvents to use in a cooling bath have the following characteristics:

Nontoxic vapors. Low viscosity. Nonflammability. Low volatility. Suitable freezing point. In some cases, a simple substitution can give nearly identical results while lowering risks. For example, using dry ice in 2-propanol rather than acetone yields a nearly identical temperature but avoids the volatility of acetone (see § Further reading below).

See also List of cooling baths Pumpable ice technology

References

Further reading Jonathan M. Percy; Christopher J. Moody; Laurence M. Harwood (1998). Experimental Organic Chemistry: standard and microscale. Blackwell Publishing. ISBN 978-0-632-04819-9. Wilfred Louis Florio Armarego; Christina Li Lin Chai (2003). Purification of Laboratory Chemicals (5th ed.). Butterworth-Heinemann. ISBN 978-0-7506-7571-0. Kenneth P. Fivizzani (2003). Safety in Academic Chemistry Lab, by American Chemical Society, Volume 1: Accident Prevention for College and University Students (7th ed.). American Chemical Society. ISBN 9780841238633.

External links Carter Research Group. "Cooling Baths". Oregon State University. A. J. Meixner; et al. "10.5.2 Different Freezing Mixtures". University of Siegen.

Tags

  • Cooling technology
  • Cryogenics
  • Laboratory techniques