Simple distillation

In simple distillation, all the hot vapors produced are immediately channeled into a condenser that cools and condenses the vapors. Therefore, the distillate will not be pure - its composition will be identical to the composition of the vapors at the given temperature and pressure, and can be computed from Raoult's law. As a result, simple distillation is usually used only to separate liquids whose boiling points differ greatly [13] (rule of thumb is 25 C), or to separate liquids from involatile solids or oils. For these cases, the vapor pressures of the components are usually sufficiently different that Raoult's law may be neglected due to the insignificant contribution of the less volatile component. In this case, the distillate may be sufficiently pure for its intended purpose

Fractional distillation
Main article: 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 in order to separate the components well by repeated vaporization-condensation cycles within a packed fractionating column. [14] This separation, by successive distillations, is also referred to as rectification. As the solution to be purified is heated, its vapors rise to the fractionating column. As it rises, it cools, condensing on the condenser walls and the surfaces of the packing material. Here, the condensate continues to be heated by the rising hot vapors; it vaporizes once more. However, the composition of the fresh vapors is determined once again by Raoult's law. Each vaporization-condensation cycle (called [15] atheoretical plate) will yield a purer solution of the more volatile component. 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 Teflon or metal to force the rising vapors into close contact with the descending condensate, [16] increasing the number of theoretical plates.

Steam distillation
Main article: Steam distillation Like vacuum distillation, steam distillation is a method for distilling compounds which are heat[17] sensitive. The temperature of the steam is easier to control than the surface of a heating element, and allows a high rate of heat transfer without heating at a very high temperature. This process involves bubbling steam through a heated mixture of the raw material. By Raoult's law, some of the target compound will vaporize (in accordance with its partial pressure). The vapor mixture is cooled and condensed, usually yielding a layer of oil and a layer of water.

Steam distillation of various aromatic herbs and flowers can result in two products; an essential oil as well as a watery herbal distillate. Theessential oils are often used in perfumery and aromatherapy while the watery distillates have many applications in aromatherapy, food processing and skin care.

Dimethyl sulfoxide usually boils at 189 C. Under a vacuum, it distills off into the receiver at only 70 C.

Perkin triangle distillation setup 1: Stirrer bar/anti-bumping granules 2: Still pot3: Fractionating column 4:Thermometer/Boiling point temperature 5:Teflon tap 1 6: Cold finger 7: Cooling water out 8: Cooling water in 9: Teflon tap 2 10:Vacuum/gas inlet 11: Teflon tap 3 12: Still receiver

[edit]Vacuum

distillation

Main article: Vacuum distillation Some compounds have very high boiling points. To boil such compounds, it is often better to lower the pressure at which such compounds are boiled instead of increasing the temperature. Once the pressure is lowered to the vapor pressure of the compound (at the given temperature), boiling and the rest of the distillation process can commence. This technique is referred to asvacuum distillation and it is commonly found in the laboratory in the form of the rotary evaporator. This technique is also very useful for compounds which boil beyond their decomposition temperature at atmospheric pressure and which would therefore be decomposed by any attempt to boil them under atmospheric pressure. Molecular distillation is vacuum distillation below the pressure of 0.01 torr. 0.01 torr is one order of magnitude above high vacuum, where fluids are in the free molecular flow regime, i.e. the mean free path of molecules is comparable to the size of the equipment. The gaseous phase no longer exerts significant pressure on the substance to be evaporated, and consequently, rate of evaporation no longer depends on pressure. That is, because the continuum assumptions of fluid dynamics no longer apply, mass transport is governed by molecular dynamics rather than fluid dynamics. Thus, a short path between the hot surface and the cold surface is necessary, typically by suspending a hot plate covered with a film of feed next to a cold plate with a line of sight in between. Molecular distillation is used industrially for purification of oils.
[18]

Fractional Distillation
The various components of crude oil have different sizes, weights and boiling temperatures; so, the first step is to separate these components. Because they have different boiling temperatures, they can be separated easily by a process called fractional distillation. The steps of fractional distillation are as follows: 1. You heat the mixture of two or more substances (liquids) with different boiling points to a high temperature. Heating is usually done with high pressure steam to temperatures of about 1112 degrees Fahrenheit / 600 degrees Celsius. 2. The mixture boils, forming vapor (gases); most substances go into the vapor phase. 3. The vapor enters the bottom of a long column (fractional distillation column) that is filled with trays or plates. The trays have many holes or bubble caps (like a loosened cap on a soda bottle) in them to allow the vapor to pass through. They increase the contact time between the vapor and the liquids in the column and help to collect liquids that form at various heights in the column. There is a temperature difference across the column (hot at the bottom, cool at the top). 4. The vapor rises in the column. 5. As the vapor rises through the trays in the column, it cools. 6. When a substance in the vapor reaches a height where the temperature of the column is equal to that substance's boiling point, it will condense to form a liquid. (The substance with the lowest boiling point

will condense at the highest point in the column; substances with higher boiling points will condense lower in the column.). 7. The trays collect the various liquid fractions. 8. The collected liquid fractions may pass to condensers, which cool them further, and then go to storage tanks, or they may go to other areas for further chemical processing Fractional distillation is useful for separating a mixture of substances with narrow differences in boiling points, and is the most important step in the refining process.

Gas Liquid Chromatography

Gas-liquid chromatography (GC) was in

invented by James and Martin and is a chromatography separation technique in which the mobile phase is a gas (usually helium or nitrogen) and the stationary phase is a liquid. In the original columns used by James and Martin, the liquid stationary phase was adsorbed on the surface of an inert support such as Celite (a diatomateous earth) or calcined Celite (a form of brick dust). The support was usually deactivated before use by acid treatment and subsequent reaction with hexamethyldisilazane. The technique was extensively used for the separation of a wide range of volatile substances. The packed column, however, had high flow impedance, which limited the column length that could be used, and, consequently, the column efficiency and the resolution that could be obtained. The packed columns were eventually replaced by the capillary columns in which the mobile phase was coated on the walls of an open tube. The tubes could be 50-500 micron ID and from 10 m to several 100 m long. Thus, very fast or very efficient columns could be employed. Gas liquid chromatography is now a very popular technique and used by almost every analytical laboratory.