cooling bath
{{Short description|Liquid mixture used to maintain low temperatures}}
File:aldolrxnpic.jpg. Both flasks are submerged in a dry ice/acetone cooling bath (−78 °C) the temperature of which is being monitored by a thermocouple (the wire on the left).]]
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.
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|+ Mixed solvent cooling baths (% by volume){{Cite journal | last1 = Lee | first1 = Do W. | last2 = Jensen | first2 = Craig M. | year = 2000 | title = Dry-Ice Bath Based on Ethylene Glycol Mixtures | journal = J. Chem. Educ. | url = http://jchemed.chem.wisc.edu/Journal/issues/2000/May/abs629.html | volume = 77 | issue = 5 | page = 629 | doi = 10.1021/ed077p629 | bibcode = 2000JChEd..77..629J | url-access = subscription }} ! % Glycol in EtOH ! Temp (°C) ! % H2O in MeOH ! Temp (°C) |
0%
| −78 | 0% | −97.6 |
10%
| −76 | 14% | −128 |
20%
| −72 | 20% | N/A |
30%
| −66 | 30% | −72 |
40%
| −60 | 40% | −64 |
50%
| −52 | 50% | −47 |
60%
| −41 | 60% | −36 |
70%
| −32 | 70% | −20 |
80%
| −28 | 80% | −12.5 |
90%
| −21 | 90% | −5.5 |
100%
| −17 | 100% | 0 |
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.[https://chemtips.wordpress.com/2015/02/09/methanolwater-mixtures-make-great-cooling-baths/ Methanol/Water mixtures make great cooling baths]. Chemtips.wordpress.com. Retrieved on 2015-02-23.[https://chemtips.wordpress.com/2015/02/23/the-ridiculously-thorough-guide-to-making-a-meohwater-bath/ The ridiculously thorough guide to making a MeOH/Water bath]. Chemtips.wordpress.com. Retrieved on 2015-02-23. 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
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|+ Traditional cooling bath mixtures[http://chemwiki.ucdavis.edu/VV_Lab_Techniques/Cooling_baths Cooling baths – ChemWiki]. Chemwiki.ucdavis.edu. Retrieved on 2013-06-17. ! Cooling agent ! Organic solvent or salt ! Temp (°C) |
Dry ice
|p-xylene | +13 |
Dry ice
|Dioxane | +12 |
Dry ice
|Cyclohexane | +6 |
Dry ice
|Benzene | +5 |
Dry ice
|Formamide | +2 |
Ice
|Salts (see: left) | 0 to −40 |
Liquid N2
|Cycloheptane | −12 |
Dry ice
|Benzyl alcohol | −15 |
Dry ice
|Tetrachloroethylene | −22 |
Dry ice
|Carbon tetrachloride | −23 |
Dry ice
|1,3-Dichlorobenzene | −25 |
Dry ice
|o-Xylene | −29 |
Dry ice
|m-Toluidine | −32 |
Dry ice
|Acetonitrile | −41 |
Dry ice
|Pyridine | −42 |
Dry ice
|m-Xylene | −47 |
Dry ice
|n-Octane | −56 |
Dry ice
|Isopropyl ether | −60 |
Dry ice
|Acetone | −78 |
Liquid N2
|Ethyl acetate | −84 |
Liquid N2
|n-Butanol | −89 |
Liquid N2
|Hexane | −94 |
Liquid N2
|Acetone | −94 |
Liquid N2
|Toluene | −95 |
Liquid N2
|Methanol | −98 |
Liquid N2
|Cyclohexene | −104 |
Liquid N2
|Ethanol | −116 |
Liquid N2
|n-Pentane | −131 |
Liquid N2
|Isopentane | −160 |
Liquid N2
|(none) | −196 |
= 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.{{Reference needed|date=March 2018}}
= 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{{cn|date=February 2020}} 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 {{section link|#Further reading}} below).
See also
References
{{reflist}}
Further reading
- {{cite book |author1=Jonathan M. Percy |author2=Christopher J. Moody |author3=Laurence M. Harwood |title=Experimental Organic Chemistry: standard and microscale |publisher=Blackwell Publishing |year=1998 |isbn=978-0-632-04819-9 |url-access=registration |url=https://archive.org/details/experimentalorga0002harw }}
- {{cite book |author1=Wilfred Louis Florio Armarego |author2=Christina Li Lin Chai | title = Purification of Laboratory Chemicals | publisher = Butterworth-Heinemann | year = 2003 | isbn = 978-0-7506-7571-0 | edition = 5th}}
- {{cite book | author = Kenneth P. Fivizzani | title = Safety in Academic Chemistry Lab, by American Chemical Society, Volume 1: Accident Prevention for College and University Students | publisher = American Chemical Society | year = 2003 | isbn = 9780841238633 | edition = 7th}}
External links
- {{cite web | url = http://oregonstate.edu/dept/chemistry/carter/cooling-bath-table | title = Cooling Baths | author = Carter Research Group | publisher = Oregon State University}}
- {{cite web | title = 10.5.2 Different Freezing Mixtures | author = A. J. Meixner | display-authors=etal | url = http://www2.uni-siegen.de/~pci/versuche/english/v105-2.html | publisher = University of Siegen}}