List of cooling baths

Table[edit]
Cooling Agent Organic Solvent or Salt T (C) Notes
Dry ice p-Xylene +13
[1]

Dry ice p-Dioxane +12

Dry ice Cyclohexane +6

Dry ice Benzene +5

Dry ice Formamide +2

Ice Water 0

Ice Ammonium chloride -5 0.3 to 1 ratio of salt to ice.
Liquid N
2
Aniline -6

Ice Sodium thiosulfate pentahydrate -8 1.1 to 1 ratio of salt to ice.
Ice Calcium chloride hexahydrate -10 1 to 2.5 ratio of salt to ice.
Liquid N
2
Ethylene glycol -10

Cooling Agent Organic Solvent or Salt T (C) Notes
Liquid N
2
Cycloheptane -12

Dry ice Benzyl alcohol -15

Dry ice Ethylene glycol -15

Ice Sodium chloride -20 1 to 3 ratio of salt to ice.
Dry ice Tetrachloroethylene -22

Dry ice Carbon Tetrachloride -23

Dry ice 1,3-Dichlorobenzene -25

Dry ice o-Xylene -29

Liquid N
2
Bromobenzene -30

Dry ice m-Toluidine -32

Dry ice 3-Heptanone -38

Ice Calcium chloride hexahydrate -40 1 to 0.8 ratio of salt to ice.
Dry ice Acetonitrile -41

Dry ice Pyridine -42

Cooling Agent Organic Solvent or Salt T (C) Notes
Dry ice Cyclohexanone -46

Dry ice m-Xylene -47

Dry ice Diethyl carbitol -52

Dry ice n-Octane -56

Dry ice Isopropyl Ether -60

Dry ice Chloroform -61

Liquid N
2
Chloroform -63
[2]

Dry ice Ethanol -72

Dry ice Trichloroethylene -73

Dry ice Isopropyl alcohol -77

Liquid N
2
Butyl acetate -77

Dry ice Acetone -78

Liquid N
2
Isoamyl acetate -79

Dry ice Sulfur dioxide -82

Cooling Agent Organic Solvent or Salt T (C) Notes
Liquid N
2
Ethyl Acetate -84

Liquid N
2
n-Butanol -89

Liquid N
2
Hexane -94

Liquid N
2
Acetone -94

Liquid N
2
Toluene -95

Liquid N
2
Methanol -98

Liquid N
2
Cyclohexene -104

Liquid N
2
Isooctane -107

Liquid N
2
Ethyl iodide -109

Liquid N
2
Carbon disulfide -110

Liquid N
2
Butyl bromide -112

Liquid N
2
Ethanol -116

Liquid N
2
Ethyl bromide -119

Liquid N
2
Acetaldehyde -124

Cooling Agent Organic Solvent or Salt T (C) Notes
Liquid N
2
Methylcyclohexane -126

Liquid N
2
n-Propanol -127

Liquid N
2
n-Pentane -131

Liquid N
2
1,5-Hexadiene -141

Liquid N
2
Isopentane -160

Liquid N
2
(none)
-196








Cooling baths
Cooling baths are used extensively in organic chemistry for a variety of reasons. The low temperature of these baths
is determined both by the appropriate use of solvent as well as a cryogenic agent such as liquid nitrogen, dry ice
(CO2) or ice. Most of these methods require continuous monitoring to ensure the temperature remains steady. For
longer or unmonitored reactions, it may be best to invest in a cryocooler.
Temperature Mixture Composition
0 C Ice
-20 C Equal amounts of ice and NaCl. The actual temperature obtained will depend on how finely crushed and well
mixed the components are, and could be as high as -10. A dewar is recomended. Brine/ dry ice produces an
identical mixture.
-40 C Acetonitrile/dry ice. Put the acetonitrile into the Dewar with your thermocouple, slowly add dry ice until you hit
your desired temperature. Don't add too much dry ice or you'll freeze the MeCN solid.
-78 C Dry ice/acetone: Slowly adding acetone to dry ice will minimize the amount of dry ice you need to
handle. Alternatively, you must slowly add dry ice to the acetone or the large volumes of carbon dioxide
produced will cause rapid bubbling.
-98 C liquid nitrogen/methanol
-131 C liquid nitrogen/n-pentane
Temperatures between -20 and -80 can be obtained using varied mixtures of ethylene glycol and ethanol over dry
ice. A little more detailed list taken from the Hoveyda group website at Boston College.
Temperature Mixture Composition
13 C p-Xylene/ dry ice
12 C Dioxane/ dry ice
6 C Cyclohexane/ dry ice
5 C Benzene/ dry ice
2 C Formamide/ dry ice
0 C Crushed Ice
-5 -> -20 C Ice/Salt
-10.5 C Ethylene Glycol/ dry ice
-12 C Cycloheptane/ dry ice
-15 C Benzyl alcohol/ dry ice
-22 C Tetrachloroethylene/ dry ice
-22.8 C Carbon Tetrachloride/ dry ice
-25C 1,3-Dichlorobenezene/ dry ice
-29 C o-Xylene/ dry ice
-32 C m-Toluidine/ dry ice
-41 C Acetonitrile/ dry ice
-42 C Pyridine/ dry ice
-47 C m-Xylene/ dry ice
-56 C n-Octane/ dry ice
-60 C Isopropyl Ether/ dry ice
-77 C Acetone/ dry ice
-77 C Butyl Acetate/ dry ice
-83 C Propyl Amine/ dry ice
-83.6 C Ethyl Acetate/Liq N2
-89 C n-Butanol/Liq N2
-94 C Hexane/Liq N2
-94.6 C Acetone/Liq N2
-95.1 C Toluene/Liq N2
-98 C Methanol/Liq N2
-100 C Ethyl Ether/dry ice
-104 C Cyclohexane/Liq N2
-116 C Ethanol/Liq N2
-116 C Ethyl Ether/Liq N2
-131 C n-Pentane/Liq N2
-160 C Isopentane/Liq N2
-196 C Liq N2

Ethylene glycol baths (% by volume)
[1]

Cooling agent Ethylene glycol Ethanol Temp (C)
Dry ice 0% 100% 78
Dry ice 10% 90% 76
Dry ice 20% 80% 72
Dry ice 30% 70% 66
Dry ice 40% 60% 60
Dry ice 50% 50% 52
Dry ice 60% 40% 41
Dry ice 70% 30% 32
Dry ice 80% 20% 28
Dry ice 90% 10% 21
Dry ice 100% 0% 17

A cooling bath, in laboratory chemistry (often but not always organic 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 orwater ice); (2) a liquid 'carrier' (such as liquid water, ethylene glycol, acetone,
etc.), which transfers heat between the bath and the vessel; ; and (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.
Ethylene glycol baths (% by volume)
[1]

Cooling agent Ethylene glycol Ethanol Temp (C)
Dry ice 0% 100% 78
Dry ice 10% 90% 76
Dry ice 20% 80% 72
Dry ice 30% 70% 66
Dry ice 40% 60% 60
Dry ice 50% 50% 52
Dry ice 60% 40% 41
Dry ice 70% 30% 32
Dry ice 80% 20% 28
Dry ice 90% 10% 21
Dry ice 100% 0% 17
Contents
[hide]
1 Ethylene glycol and ethanol baths
2 Traditional cooling baths
o 2.1 Water and ice baths
o 2.2 Dry ice baths at 78 C
o 2.3 Dry ice baths above 77 C
o 2.4 Liquid nitrogen baths above 196 C
o 2.5 Water/ice alternatives
o 2.6 Safety Recommendations
3 See also
4 References
5 Further reading
6 External links
Ethylene glycol and ethanol baths[edit]
Temperatures between approximately 78 C and 17 C can be maintained by placing dry ice into
a mixture of ethylene glycol and ethanol.
[1]
The bath's temperature can be set by varying the relative
amounts of ethylene glycol and ethanol. Dry ice sublimes at 78 C.
If a bath is made with only ethanol, then it will maintain 78 C until all the dry ice has sublimed. The
bath will not freeze because ethanol's freezing point is 114 C.
In addition, a cooling bath can be made with both ethanol and ethylene glycol. Since ethylene glycol
freezes at 12.9 C, then the "freezing point" of this mixture will increase to above 78 C. Instead of
freezing solid, however, the solution becomes thicker and gel-like once the dry ice has performed
enough cooling. If a 60/40 mixture of ethanol/ethylene glycol is used, then a thick gel will form
around the dry ice pieces around 60 C, helping to maintain the temperature at approximately 60
C.
Relative to traditional cooling baths, ethylene glycol mixtures have the advantage of never freezing
solid. In addition, the solvents necessary are cheaper and less toxic than those used in traditional
baths.
[1]

Traditional cooling baths[edit]
Traditional cooling bath mixtures
[2]

Cooling agent Organic solvent or salt Temp (C)
Dry ice p-xylene +13
Dry ice Dioxane +12
Liquid N
2
Cyclohexane +6
Dry ice Benzene +5
Dry ice Formamide +2
Ice Salts (see: above) 0 to 20
Liquid N
2
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 N
2
Ethyl acetate 84
Liquid N
2
n-Butanol 89
Liquid N
2
Hexane 94
Liquid N
2
Acetone 94
Liquid N
2
Toluene 95
Liquid N
2
Methanol 98
Liquid N
2
Cyclohexene 104
Liquid N
2
Ethanol 116
Liquid N
2
n-Pentane 131
Liquid N
2
Isopentane 160
Liquid N
2
(none) 196
Water and ice baths[edit]
A bath of ice and water will maintain a temperature 0 C since the freezing 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 ratio of salt
to ice influences the temperature:
10 C can be achieved with a 1 to 2.5 ratio of calcium chloride hexahydrate to ice.
20 C can be achieved with a 1 to 3 ratio of sodium chloride to ice.
40 C can be achieved with a 1 to 0.8 ratio of calcium chloride hexahydrate to ice.
Dry ice baths at 78 C[edit]
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. Therefore, other liquids with a lower freezing point (pentane: 95 C) can also be used to
maintain the bath at 78 C.
Dry ice baths above 77 C[edit]
In order to maintain temperatures above 77 C, a solvent with a freezing point above 77 C must
be used. When dry ice is added to acetonitrile then the bath will begin cooling. Once the temperature
reaches 41 C, the acetonitrile will freeze. Therefore, dry ice must be added slowly to avoid
freezing the entire mixture. In these cases, a bath temperature of 55 C can be achieved by
choosing a solvent with a similar freezing point (n-octane freezes at 56 C).
Liquid nitrogen baths above 196 C[edit]
Liquid nitrogen baths follow the same idea as dry ice baths. A temperature of 115 C can be
maintained by slowly adding liquid nitrogen to the organic solvent (ethanol) until it begins to freeze
(ethanol freezes at 116 C).
Water/ice alternatives[edit]
In water and ice-based baths, tap water is commonly used due to ease of access and the higher
costs of using ultrapure water. However, tap water and ice derived from tap water can be a
contaminant to biological and chemical samples. This has created a host of insulated devices aimed
at creating a similar cooling or freezing effect as ice baths without the use of water or ice.
[3]

Safety Recommendations[edit]
The American Chemical Society notes that the ideal organic solvents to use in a cooling baths 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 Further Reading).

Cooling Baths
Temperature Composition
13 p-Xylene/CO2(s)
12 Dioxane/CO2(s)
6 Cyclohexane/CO2(s)
5 Benzene/CO2(s)
2 Formamide/CO2(s)
0 Crushed Ice
-5 -> -20 Ice/Salt
-10.5 Ethylene Glycol/CO2(s)
-12 Cycloheptane/CO2(s)
-15 Benzyl alcohol/CO2(s)
-22 Tetrachloroethylene/CO2(s)
-22.8 Carbon Tetrachloride/CO2(s)
-25 1,3-Dichlorobenezene/CO2(s)
-29 o-Xylene/CO2(s)
-32 m-Toluidine/CO2(s)
-41 Acetonitrile/CO2(s)
-42 Pyridine/CO2(s)
-47 m-Xylene/CO2(s)
-56 n-Octane/CO2(s)
-60 Isopropyl Ether/CO2(s)
-77 Acetone/CO2(s)
-77 Butyl Acetate/CO2(s)
-83 Propyl Amine/CO2(s)
-83.6 Ethyl Acetate/Liq N2
-89 n-Butanol/Liq N2
-94 Hexane/Liq N2
-94.6 Acetone/Liq N2
-95.1 Toluene/Liq N2
-98 Methanol/Liq N2
-100 Ethyl Ether/CO2(s)
-104 Cyclohexane/Liq N2
-116 Ethanol/Liq N2
-116 Ethyl Ether/Liq N2
-131 n-Pentane/LiqN2
-160 Isopentane/Liq N2
-196 Liq N2