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:

  1. Nontoxic vapors.
  2. Low viscosity.
  3. Nonflammability.
  4. Low volatility.
  5. 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}}