Laboratory-scale distillations are almost exclusively run as batch distillations. The device used in distillation, sometimes referred to as a
still, consists at a minimum of a reboiler or
pot in which the source material is heated, a condenser in which the heated
vapor is cooled back to the liquid
state, and a receiver in which the concentrated or purified liquid, called the distillate, is collected. Several laboratory-scale techniques for distillation exist (see also ). A completely sealed distillation apparatus could experience extreme and rapidly varying internal pressure, which could cause it to burst open at the joints. Therefore, some path is usually left open (for instance, at the receiving flask) to allow the internal pressure to equalize with atmospheric pressure. Alternatively, a
vacuum pump may be used to keep the apparatus at a lower than atmospheric pressure. If the substances involved are air- or moisture-sensitive, the connection to the atmosphere can be made through one or more
drying tubes packed with materials that scavenge the undesired air components, or through
bubblers that provide a movable liquid barrier. Finally, the entry of undesired air components can be prevented by pumping a low but steady flow of suitable inert gas, like
nitrogen, into the apparatus.
Simple distillation In simple distillation, the vapor is immediately channeled into a condenser. Consequently, the distillate is not pure, but rather its composition is identical to the composition of the vapors at the given temperature and pressure. That concentration follows
Raoult's law. As a result, simple distillation is effective only when the liquid boiling points differ greatly (rule of thumb is 25 °C) or when separating liquids from non-volatile solids or oils. For these cases, the vapor pressures of the components are usually different enough that the distillate may be sufficiently pure for its intended purpose. A cutaway schematic of a simple distillation operation is shown at right. The starting liquid 15 in the boiling flask 2 is heated by a combined
hotplate and
magnetic stirrer 13 via a
silicone oil bath (orange, 14). The vapor flows through a short
Vigreux column 3, then through a
Liebig condenser 5, is cooled by water (blue) that circulates through ports 6 and 7. The condensed liquid drips into the receiving flask 8, sitting in a cooling bath (blue, 16). The adapter 10 has a connection 9 that may be fitted to a vacuum pump. The components are connected by
ground glass joints.
Fractional distillation For many cases, the boiling points of the components in the mixture will be sufficiently close that
Raoult's law must be taken into consideration. Therefore, fractional distillation must be used to separate the components by repeated vaporization-condensation cycles within a packed fractionating column. This separation, by successive distillations, is also referred to as rectification. In reality, each cycle at a given temperature does not occur at exactly the same position in the fractionating column;
theoretical plate is thus a concept rather than an accurate description. More theoretical plates lead to better separations. A
spinning band distillation system uses a spinning band of
PTFE or metal to force the rising vapors into close contact with the descending condensate, increasing the number of theoretical plates.
Steam distillation Like
vacuum distillation, steam distillation is a method for distilling compounds which are heat-sensitive.
Air-sensitive vacuum distillation Some compounds have high boiling points as well as being
air sensitive. A simple vacuum distillation system as exemplified above can be used, whereby the vacuum is replaced with an inert gas after the distillation is complete. However, this is a less satisfactory system if one desires to collect fractions under a reduced pressure. To do this a "cow" or "pig" adaptor can be added to the end of the condenser, or for better results or for very air sensitive compounds a
Perkin triangle apparatus can be used. The Perkin triangle has means via a series of glass or
Teflon taps to allows fractions to be isolated from the rest of the
still, without the main body of the distillation being removed from either the vacuum or heat source, and thus can remain in a state of
reflux. To do this, the sample is first isolated from the vacuum by means of the taps, the vacuum over the sample is then replaced with an inert gas (such as
nitrogen or
argon) and can then be stoppered and removed. A fresh collection vessel can then be added to the system, evacuated and linked back into the distillation system via the taps to collect a second fraction, and so on, until all fractions have been collected. Zone distillation is the distillation analog of zone recrystallization. Impurity distribution in the condensate is described by known equations of zone recrystallization, with the separation factor α of distillation used in place of the crystallization distribution coefficient k.
Closed-system vacuum distillation (cryovap) Non-condensable gas can be expelled from the apparatus by the vapor of relatively volatile co-solvent, which spontaneously evaporates during initial pumping, and this can be achieved with regular oil or diaphragm pump.
Other types • The process of
reactive distillation involves using the reaction vessel as the still. In this process, the product is usually significantly lower boiling than its reactants. As the product is formed from the reactants, it is vaporized and removed from the reaction mixture. This technique is an example of a continuous vs. a batch process; advantages include less downtime to charge the reaction vessel with starting material, and less workup. Distillation "over a reactant" could be classified as a reactive distillation. It is typically used to remove volatile impurity from the distillation feed. For example, a little
lime may be added to remove carbon dioxide from water followed by a second distillation with a little
sulfuric acid added to remove traces of ammonia. •
Catalytic distillation is the process by which the reactants are catalyzed while being distilled to continuously separate the products from the reactants. This method is used to assist equilibrium reactions in reaching completion. •
Pervaporation is a method for the separation of mixtures of liquids by partial vaporization through a non-porous
membrane. •
Extractive distillation is defined as distillation in the presence of a miscible, high boiling, relatively non-volatile component, the solvent, that forms no
azeotrope with the other components in the mixture. •
Flash evaporation (or partial evaporation) is the partial
vaporization that occurs when a saturated liquid stream undergoes a reduction in pressure by passing through a throttling
valve or other throttling device. This process is one of the simplest unit operations, being equivalent to a distillation with only one equilibrium stage. • Codistillation is distillation which is performed on mixtures in which the two compounds are not miscible. In the laboratory, the
Dean-Stark apparatus is used for this purpose to remove water from synthesis products. The Bleidner apparatus is another example with two refluxing solvents. • Membrane distillation is a type of distillation in which vapors of a mixture to be separated are passed through a membrane, which selectively permeates one component of mixture. Vapor pressure difference is the driving force. It has potential applications in seawater desalination and in removal of organic and inorganic components. The unit process of
evaporation may also be called "distillation": • In
rotary evaporation a vacuum distillation apparatus is used to remove bulk
solvents from a sample. Typically the vacuum is generated by a
water aspirator or a
membrane pump. • In a
Kugelrohr apparatus a short-path distillation apparatus is typically used (generally in combination with a (high) vacuum) to distill high boiling (> 300 °C) compounds. The apparatus consists of an oven in which the compound to be distilled is placed, a receiving portion which is outside of the oven, and a means of rotating the sample. The vacuum is normally generated by using a high vacuum pump. Other uses: •
Dry distillation or
destructive distillation, despite the name, is not truly distillation, but rather a
chemical reaction known as
pyrolysis in which solid substances are heated in an inert or
reducing atmosphere and any volatile fractions, containing high-boiling liquids and products of pyrolysis, are collected. The destructive distillation of
wood to give
methanol is the root of its common name –
wood alcohol. •
Freeze distillation is an analogous method of purification using
freezing instead of evaporation. It is not truly distillation, but a
recrystallization where the product is the
mother liquor, and does not produce products equivalent to distillation. This process is used in the production of
ice beer and
ice wine to increase ethanol and
sugar content, respectively. It is also used to produce
applejack. Unlike distillation, freeze distillation concentrates poisonous congeners rather than removing them; As a result, many countries prohibit such applejack as a health measure. Also, distillation by evaporation can separate these since they have different boiling points. • Distillation by filtration: In early alchemy and chemistry, otherwise known as natural philosophy, a form of "distillation" by capillary filtration was known as a form of distillation at the time. In this, a series of cups or bowls were set upon a stepped support with a "wick" of cotton or felt-like material, which had been wetted with water or a clear liquid with each step dripping down through the wetted cloth through capillary action in succeeding steps, creating a "purification" of the liquid, leaving solid materials behind in the upper bowls and purifying the succeeding product through capillary action through the moistened cloth. This was called "distillatio" by filtration by those using the method. ==Azeotropic process==