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
Distillation, also classical distillation, is the process of separating the component substances of a liquid mixture of two or more chemically discrete substances; the separation process is realized by way of the selective boiling of the mixt ...
, to remove solvents using a
rotary evaporator, or to perform a
chemical reaction
A chemical reaction is a process that leads to the chemistry, chemical transformation of one set of chemical substances to another. When chemical reactions occur, the atoms are rearranged and the reaction is accompanied by an Gibbs free energy, ...
below room temperature (see
Kinetic control).
Cooling baths are generally one of two types: (a) a cold fluid (particularly
liquid nitrogen
Liquid nitrogen (LN2) is nitrogen in a liquid state at cryogenics, low temperature. Liquid nitrogen has a boiling point of about . It is produced industrially by fractional distillation of liquid air. It is a colorless, mobile liquid whose vis ...
,
water
Water is an inorganic compound with the chemical formula . It is a transparent, tasteless, odorless, and Color of water, nearly colorless chemical substance. It is the main constituent of Earth's hydrosphere and the fluids of all known liv ...
, or even
air
An atmosphere () is a layer of gases that envelop an astronomical object, held in place by the gravity of the object. A planet retains an atmosphere when the gravity is great and the temperature of the atmosphere is low. A stellar atmosph ...
) — but most commonly the term refers to (b) a mixture of 3 components: (1) a cooling agent (such as
dry ice
Dry ice is the solid form of carbon dioxide. It is commonly used for temporary refrigeration as CO2 does not have a liquid state at normal atmospheric pressure and Sublimation (phase transition), sublimes directly from the solid state to the gas ...
or
ice
Ice is water that is frozen into a solid state, typically forming at or below temperatures of 0 ° C, 32 ° F, or 273.15 K. It occurs naturally on Earth, on other planets, in Oort cloud objects, and as interstellar ice. As a naturally oc ...
); (2) a liquid "carrier" (such as liquid water,
ethylene glycol
Ethylene glycol ( IUPAC name: ethane-1,2-diol) is an organic compound (a vicinal diol) with the formula . It is mainly used for two purposes: as a raw material in the manufacture of polyester fibers and for antifreeze formulations. It is an odo ...
,
acetone
Acetone (2-propanone or dimethyl ketone) is an organic compound with the chemical formula, formula . It is the simplest and smallest ketone (). It is a colorless, highly Volatile organic compound, volatile, and flammable liquid with a charact ...
, 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
Ethylene glycol ( IUPAC name: ethane-1,2-diol) is an organic compound (a vicinal diol) with the formula . It is mainly used for two purposes: as a raw material in the manufacture of polyester fibers and for antifreeze formulations. It is an odo ...
and
ethanol
Ethanol (also called ethyl alcohol, grain alcohol, drinking alcohol, or simply alcohol) is an organic compound with the chemical formula . It is an Alcohol (chemistry), alcohol, with its formula also written as , or EtOH, where Et is the ps ...
,
while mixtures of
methanol
Methanol (also called methyl alcohol and wood spirit, amongst other names) is an organic chemical compound and the simplest aliphatic Alcohol (chemistry), alcohol, with the chemical formula (a methyl group linked to a hydroxyl group, often ab ...
and
water
Water is an inorganic compound with the chemical formula . It is a transparent, tasteless, odorless, and Color of water, nearly colorless chemical substance. It is the main constituent of Earth's hydrosphere and the fluids of all known liv ...
span the −128 °C to 0 °C temperature range.
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
Liquid nitrogen (LN2) is nitrogen in a liquid state at cryogenics, low temperature. Liquid nitrogen has a boiling point of about . It is produced industrially by fractional distillation of liquid air. It is a colorless, mobile liquid whose vis ...
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
The melting point (or, rarely, liquefaction point) of a substance is the temperature at which it changes state of matter, state from solid to liquid. At the melting point the solid and liquid phase (matter), phase exist in Thermodynamic equilib ...
of water is 0 °C. However, adding a salt such as sodium chloride
Sodium chloride , commonly known as Salt#Edible salt, edible salt, is an ionic compound with the chemical formula NaCl, representing a 1:1 ratio of sodium and chloride ions. It is transparent or translucent, brittle, hygroscopic, and occurs a ...
will lower the temperature through the property of freezing-point depression
Freezing-point depression is a drop in the maximum temperature at which a substance freezing, freezes, caused when a smaller amount of another, non-Volatility (chemistry), volatile substance is added. Examples include adding salt into water (u ...
. 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
The American Chemical Society (ACS) is a scientific society based in the United States that supports scientific inquiry in the field of chemistry. Founded in 1876 at New York University, the ACS currently has more than 155,000 members at all ...
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
Isopropyl alcohol (IUPAC name propan-2-ol and also called isopropanol or 2-propanol) is a colorless, flammable, organic compound with a pungent alcoholic odor.
Isopropyl alcohol, an organic polar molecule, is miscible in water, ethanol, an ...
rather than acetone yields a nearly identical temperature but avoids the volatility of acetone (see below).
See also
* List of cooling baths
* Pumpable ice technology
Pumpable ice technology (PIT) uses thin liquids, with the cooling capacity of ice. Pumpable ice is typically a slurry of ice crystals or particles ranging from 5 micrometers to 1 cm in diameter and transported in brine, seawater, food liquid ...
References
Further reading
*
*
*
External links
*
* {{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
Laboratory techniques
Cryogenics
Cooling technology