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Other names | Rotovap |
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Uses | Solvent evaporation |
Inventor | Lyman C. Craig |
A rotary evaporator [1] (rotavap) is a device used in chemical laboratories for the efficient and gentle removal of solvents from samples by evaporation. When referenced in the chemistry research literature, description of the use of this technique and equipment may include the phrase "rotary evaporator", though use is often rather signaled by other language (e.g., "the sample was evaporated under reduced pressure").
Rotary evaporators are also used in molecular cooking for the preparation of distillates and extracts.
A simple rotary evaporator system was invented by Lyman C. Craig. [2] It was first commercialized by the Swiss company [3] in 1957. Walter Büchi developed a world first commercial rotary evaporator, which separates substances with different boiling points, and greatly simplifies work in research laboratories. In research the most common form is the 1L bench-top unit, whereas large scale (e.g., 20L-50L) versions are used in pilot plants in commercial chemical operations.[ citation needed ]
The main components of a rotary evaporator are:
The vacuum system used with rotary evaporators can be as simple as a water aspirator with a trap immersed in a cold bath (for non-toxic solvents), or as complex as a regulated mechanical vacuum pump with refrigerated trap. Glassware used in the vapor stream and condenser can be simple or complex, depending upon the goals of the evaporation, and any propensities the dissolved compounds might give to the mixture (e.g., to foam or "bump"). Commercial instruments are available that include the basic features, and various traps are manufactured to insert between the evaporation flask and the vapor duct. Modern equipment often adds features such as digital control of vacuum, digital display of temperature and rotational speed, and vapor temperature sensing.
Vacuum evaporators as a class function because lowering the pressure above a bulk liquid lowers the boiling points of the component liquids in it. Generally, the component liquids of interest in applications of rotary evaporation are research solvents that one desires to remove from a sample after an extraction, such as following a natural product isolation or a step in an organic synthesis. Liquid solvents can be removed without excessive heating of what are often complex and sensitive solvent-solute combinations.
Rotary evaporation is most often and conveniently applied to separate "low boiling" solvents such a n-hexane or ethyl acetate from compounds which are solid at room temperature and pressure. However, careful application also allows removal of a solvent from a sample containing a liquid compound if there is minimal co-evaporation (azeotropic behavior), and a sufficient difference in boiling points at the chosen temperature and reduced pressure.
Solvents with higher boiling points such as water (100 °C at standard atmospheric pressure, 760 torr or 1 bar), dimethylformamide (DMF, 153 °C at the same), or dimethyl sulfoxide (DMSO, 189 °C at the same), can also be evaporated if the unit's vacuum system is capable of sufficiently low pressure. (For instance, both DMF and DMSO will boil below 50 °C if the vacuum is reduced from 760 torr to 5 torr [from 1 bar to 6.6 mbar]) However, more recent developments are often applied in these cases (e.g., evaporation while centrifuging or vortexing at high speeds). Rotary evaporation for high boiling hydrogen bond-forming solvents such as water is often a last recourse, as other evaporation methods or freeze-drying (lyophilization) are available. This is partly due to the fact that in such solvents, the tendency to "bump" is accentuated. The modern centrifugal evaporation technologies are particularly useful when one has many samples to do in parallel, as in medium- to high-throughput synthesis now expanding in industry and academia.
Evaporation under vacuum can also, in principle, be performed using standard organic distillation glassware — i.e., without rotation of the sample. The key advantages in use of a rotary evaporator are
A key disadvantage in rotary evaporations, besides its single sample nature, is the potential of some sample types to bump, e.g. ethanol and water, which can result in loss of a portion of the material intended to be retained. Even professionals experience periodic mishaps during evaporation, especially bumping, though experienced users become aware of the propensity of some mixtures to bump or foam, and apply precautions that help to avoid most such events. In particular, bumping can often be prevented by taking homogeneous phases into the evaporation, by carefully regulating the strength of the vacuum (or the bath temperature) to provide for an even rate of evaporation, or, in rare cases, through use of added agents such as boiling chips (to make the nucleation step of evaporation more uniform). Rotary evaporators can also be equipped with further special traps and condenser arrays that are best suited to particular difficult sample types, including those with the tendency to foam or bump.
Possible hazards include implosions resulting from use of glassware that contains flaws, such as star-cracks. Explosions may occur from concentrating unstable impurities during evaporation, for example when rotavapping an ethereal solution containing peroxides. This can also occur when taking certain unstable compounds, such as organic azides and acetylides, nitro-containing compounds, molecules with strain energy, etc. to dryness.
Users of rotary evaporation equipment must take precautions to avoid contact with rotating parts, particularly entanglement of loose clothing, hair, or necklaces. Under these circumstances, the winding action of the rotating parts can draw the users into the apparatus resulting in breakage of glassware, burns, and chemical exposure. Extra caution must also be applied to operations with air reactive materials, especially when under vacuum. A leak can draw air into the apparatus and a violent reaction can occur.
Distillation, or classical distillation, is the process of separating the components or substances from a liquid mixture by using selective boiling and condensation, usually inside an apparatus known as a still. Dry distillation is the heating of solid materials to produce gaseous products ; this may involve chemical changes such as destructive distillation or cracking. Distillation may result in essentially complete separation, or it may be a partial separation that increases the concentration of selected components; in either case, the process exploits differences in the relative volatility of the mixture's components. In industrial applications, distillation is a unit operation of practically universal importance, but is a physical separation process, not a chemical reaction. An installation used for distillation, especially of distilled beverages, is a distillery. Distillation includes the following applications:
Vapor pressure or equilibrium vapor pressure is the pressure exerted by a vapor in thermodynamic equilibrium with its condensed phases at a given temperature in a closed system. The equilibrium vapor pressure is an indication of a liquid's thermodynamic tendency to evaporate. It relates to the balance of particles escaping from the liquid in equilibrium with those in a coexisting vapor phase. A substance with a high vapor pressure at normal temperatures is often referred to as volatile. The pressure exhibited by vapor present above a liquid surface is known as vapor pressure. As the temperature of a liquid increases, the attractive interactions between liquid molecules become less significant in comparison to the entropy of those molecules in the gas phase, increasing the vapor pressure. Thus, liquids with strong intermolecular interactions are likely to have smaller vapor pressures, with the reverse true for weaker interactions.
Fractional distillation is the separation of a mixture into its component parts, or fractions. Chemical compounds are separated by heating them to a temperature at which one or more fractions of the mixture will vaporize. It uses distillation to fractionate. Generally the component parts have boiling points that differ by less than 25 °C (45 °F) from each other under a pressure of one atmosphere. If the difference in boiling points is greater than 25 °C, a simple distillation is typically used.
A fractionating column or fractional column is equipment used in the distillation of liquid mixtures to separate the mixture into its component parts, or fractions, based on their differences in volatility. Fractionating columns are used in small-scale laboratory distillations as well as large-scale industrial distillations.
A heat pipe is a heat-transfer device that employs phase transition to transfer heat between two solid interfaces.
A chiller is a machine that removes heat from a liquid coolant via a vapor-compression, adsorption refrigeration, or absorption refrigeration cycles. This liquid can then be circulated through a heat exchanger to cool equipment, or another process stream. As a necessary by-product, refrigeration creates waste heat that must be exhausted to ambience, or for greater efficiency, recovered for heating purposes. Vapor compression chillers may use any of a number of different types of compressors. Most common today are the hermetic scroll, semi-hermetic screw, or centrifugal compressors. The condensing side of the chiller can be either air or water cooled. Even when liquid cooled, the chiller is often cooled by an induced or forced draft cooling tower. Absorption and adsorption chillers require a heat source to function.
Vacuum distillation or Distillation under reduced pressure is a type of distillation performed under reduced pressure, which allows the purification of compounds not readily distilled at ambient pressures or simply to save time or energy. This technique separates compounds based on differences in their boiling points. This technique is used when the boiling point of the desired compound is difficult to achieve or will cause the compound to decompose. Reduced pressures decrease the boiling point of compounds. The reduction in boiling point can be calculated using a temperature-pressure nomograph using the Clausius–Clapeyron relation.
A cryostat is a device used to maintain low cryogenic temperatures of samples or devices mounted within the cryostat. Low temperatures may be maintained within a cryostat by using various refrigeration methods, most commonly using cryogenic fluid bath such as liquid helium. Hence it is usually assembled into a vessel, similar in construction to a vacuum flask or Dewar. Cryostats have numerous applications within science, engineering, and medicine.
Laboratory flasks are vessels or containers that fall into the category of laboratory equipment known as glassware. In laboratory and other scientific settings, they are usually referred to simply as flasks. Flasks come in a number of shapes and a wide range of sizes, but a common distinguishing aspect in their shapes is a wider vessel "body" and one narrower tubular sections at the top called necks which have an opening at the top. Laboratory flask sizes are specified by the volume they can hold, typically in metric units such as milliliters or liters. Laboratory flasks have traditionally been made of glass, but can also be made of plastic.
A liquid-ring pump is a rotating positive-displacement gas pump, with liquid under centrifugal force acting as a seal.
The Marcusson apparatus, Dean-Stark apparatus, Dean–Stark receiver, distilling trap, or Dean–Stark Head is a piece of laboratory glassware used in synthetic chemistry to collect water from a reactor. It is used in combination with a reflux condenser and a distillation flask for the separation of water from liquids. This may be a continuous removal of the water that is produced during a chemical reaction performed at reflux temperature, such as in esterification reactions. The original setup by Julius Marcusson was refined by the American chemists Ernest Woodward Dean (1888–1959) and David Dewey Stark (1893–1979) in 1920 for determination of the water content in petroleum.
Vapour-compression refrigeration or vapor-compression refrigeration system (VCRS), in which the refrigerant undergoes phase changes, is one of the many refrigeration cycles and is the most widely used method for air conditioning of buildings and automobiles. It is also used in domestic and commercial refrigerators, large-scale warehouses for chilled or frozen storage of foods and meats, refrigerated trucks and railroad cars, and a host of other commercial and industrial services. Oil refineries, petrochemical and chemical processing plants, and natural gas processing plants are among the many types of industrial plants that often utilize large vapor-compression refrigeration systems. Cascade refrigeration systems may also be implemented using two compressors.
Round-bottom flasks are types of flasks having spherical bottoms used as laboratory glassware, mostly for chemical or biochemical work. They are typically made of glass for chemical inertness; and in modern days, they are usually made of heat-resistant borosilicate glass. There is at least one tubular section known as the neck with an opening at the tip. Two- or three-necked flasks are common as well. Round bottom flasks come in many sizes, from 5 mL to 20 L, with the sizes usually inscribed on the glass. In pilot plants even larger flasks are encountered.
A Kugelrohr is a short-path vacuum distillation apparatus typically used to distill relatively small amounts of compounds with high boiling points under greatly reduced pressure.
A centrifugal evaporator is a device used in chemical and biochemical laboratories for the efficient and gentle evaporation of solvents from many samples at the same time, and samples contained in microtitre plates. If only one sample required evaporation then a rotary evaporator is most often used. The most advanced modern centrifugal evaporators not only concentrate many samples at the same time, they eliminate solvent bumping and can handle solvents with boiling points of up to 220 °C. This is more than adequate for the modern high throughput laboratory.
An evaporator is a type of heat exchanger device that facilitates evaporation by utilizing conductive and convective heat transfer to provide the necessary thermal energy for phase transition from liquid to vapor. Within evaporators, a circulating liquid is exposed to an atmospheric or reduced pressure environment, causing it to boil at a lower temperature compared to normal atmospheric boiling.
In chemistry, a condenser is laboratory apparatus used to condense vapors – that is, turn them into liquids – by cooling them down.
Air-free techniques refer to a range of manipulations in the chemistry laboratory for the handling of compounds that are air-sensitive. These techniques prevent the compounds from reacting with components of air, usually water and oxygen; less commonly carbon dioxide and nitrogen. A common theme among these techniques is the use of a fine (100–10−3 Torr) or high (10−3–10−6 Torr) vacuum to remove air, and the use of an inert gas: preferably argon, but often nitrogen.
Reflux is a technique involving the condensation of vapors and the return of this condensate to the system from which it originated. It is used in industrial and laboratory distillations. It is also used in chemistry to supply energy to reactions over a long period of time.
An evaporating dish is a piece of laboratory glassware used for the evaporation of solutions and supernatant liquids, and sometimes to their melting point. Evaporating dishes are used to evaporate excess solvents – most commonly water – to produce a concentrated solution or a solid precipitate of the dissolved substance.