RARE Brewery & Liquor Spirits - A. Lacroix, Morez France - Watermark date 1832

£310.06 £248.05 Buy It Now or Best Offer, £14.80 Shipping, eBay Money Back Guarantee
Seller: dalebooks ✉️ (8,794) 100%, Location: Rochester, New York, US, Ships to: WORLDWIDE, Item: 304708736772 RARE Brewery & Liquor Spirits - A. Lacroix, Morez France - Watermark date 1832. To break azeotropic distillations and cross distillation boundaries, such as in the DeRosier Problem, it is necessary to increase the composition of the light key in the distillate. In continuous distillation, the source materials, vapors, and distillate are kept at a constant composition by carefully replenishing the source material and removing fractions from both vapor and liquid in the system.
SUPER RARE Old Billhead / Receipt  
 
A. Lacroix & Cie, a Morez Brewery & maker of Liquor  Watermark of Bourisson, Dated 1832

For offer - a very nice old piece of ephemera. I bought these from a friend in France. Never offered on the market until now. Vintage, Old, antique, Original - NOT a Reproduction - Guaranteed !! Superb graphic at left side edge, with "Dole, lith. de Prudont" at bottom edge. I did some research and could not locate anything about this. Seems quite rare. In fine condition. Please see photos. If you collect 19th century advertising history, design logo, French advertisement ad, drinking, etc., this is a nice one for your paper or ephemera collection. Combine shipping on multiple bid wins! 2843

A brewery or brewing company is a business that makes and sells beer. The place at which beer is commercially made is either called a brewery or a beerhouse, where distinct sets of brewing equipment are called plant.[1] The commercial brewing of beer has taken place since at least 2500 BC;[2] in ancient Mesopotamia, brewers derived social sanction and divine protection from the goddess Ninkasi.[3][4] Brewing was initially a cottage industry, with production taking place at home; by the ninth century, monasteries and farms would produce beer on a larger scale, selling the excess; and by the eleventh and twelfth centuries larger, dedicated breweries with eight to ten workers were being built.[5]

The diversity of size in breweries is matched by the diversity of processes, degrees of automation, and kinds of beer produced in breweries. A brewery is typically divided into distinct sections, with each section reserved for one part of the brewing process.

History

See also: History of beer

The Alulu beer receipt records a purchase of "best" beer from an ancient Sumerian brewery, c. 2050 BC[2]

Beer may have been known in Neolithic Europe[6] and was mainly brewed on a domestic scale.[7] In some form, it can be traced back almost 5000 years to Mesopotamian writings describing daily rations of beer and bread to workers. Before the rise of production breweries, the production of beer took place at home and was the domain of women, as baking and brewing were seen as "women's work".

Industrialization

19th century brewery installations

The machine room of the former brewery Wielemans-Ceuppens in Brussels

Breweries, as production facilities reserved for making beer, did not emerge until monasteries and other Christian institutions started producing beer not only for their own consumption but also to use as payment. This industrialization of brewing shifted the responsibility of making beer to men.

The oldest, still functional, brewery in the world is believed to be the German state-owned Weihenstephan brewery in the city of Freising, Bavaria. It can trace its history back to 1040 AD.[8] The nearby Weltenburg Abbey brewery, can trace back its beer-brewing tradition to at least 1050 AD.[9]: 30  The Žatec brewery in the Czech Republic claims it can prove that it paid a beer tax in 1004 AD.[citation needed]

Early breweries were almost always built on multiple stories, with equipment on higher floors used earlier in the production process, so that gravity could assist with the transfer of product from one stage to the next. This layout often is preserved in breweries today, but mechanical pumps allow more flexibility in brewery design. Early breweries typically used large copper vats in the brewhouse, and fermentation and packaging took place in lined wooden containers. Such breweries were common until the Industrial Revolution, when better materials became available, and scientific advances led to a better understanding of the brewing process. Today, almost all brewery equipment is made of stainless steel. During the Industrial Revolution, the production of beer moved from artisanal manufacture to industrial manufacture, and domestic manufacture ceased to be significant by the end of the 19th century.[10]

See also: brewing industry

Major technological advances

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A 16th-century brewery

A handful of major breakthroughs have led to the modern brewery and its ability to produce the same beer consistently. The steam engine, vastly improved in 1775 by James Watt, brought automatic stirring mechanisms and pumps into the brewery. It gave brewers the ability to mix liquids more reliably while heating, particularly the mash, to prevent scorching, and a quick way to transfer liquid from one container to another. Almost all breweries now use electric-powered stirring mechanisms and pumps. The steam engine also allowed the brewer to make greater quantities of beer, as human power was no longer a limiting factor in moving and stirring.

Carl von Linde, along with others, is credited with developing the refrigeration machine in 1871. Refrigeration allowed beer to be produced year-round, and always at the same temperature. Yeast is very sensitive to temperature, and, if a beer were produced during summer, the yeast would impart unpleasant flavours onto the beer. Most brewers would produce enough beer during winter to last through the summer, and store it in underground cellars, or even caves, to protect it from summer's heat.

The discovery of microbes by Louis Pasteur was instrumental in the control of fermentation. The idea that yeast was a microorganism that worked on wort to produce beer led to the isolation of a single yeast cell by Emil Christian Hansen. Pure yeast cultures allow brewers to pick out yeasts for their fermentation characteristics, including flavor profiles and fermentation ability. Some breweries in Belgium, however, still rely on "spontaneous" fermentation for their beers (see lambic). The development of hydrometers and thermometers changed brewing by allowing the brewer more control of the process, and greater knowledge of the results.

The modern brewery

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Brewery in Hurbanovo, Slovakia

Sinebrychoff Brewery in Kerava, Finland; a view from the Helsinki-Lahti Highway

Breweries today are made predominantly of stainless steel, although vessels often have a decorative copper cladding for a nostalgic look. Stainless steel has many favourable characteristics that make it a well-suited material for brewing equipment. It imparts no flavour in beer, it reacts with very few chemicals, which means almost any cleaning solution can be used on it (concentrated chlorine [bleach] being a notable exception).

Heating in the brewhouse usually is achieved through pressurized steam, although direct-fire systems are not unusual in small breweries. Likewise, cooling in other areas of the brewery is typically done by cooling jackets on tanks, which allow the brewer to control precisely the temperature on each tank individually, although whole-room cooling is also common.

Today, modern brewing plants perform myriad analyses on their beers for quality control purposes. Shipments of ingredients are analyzed to correct for variations. Samples are pulled at almost every step and tested for [oxygen] content, unwanted microbial infections, and other beer-aging compounds. A representative sample of the finished product often is stored for months for comparison, when complaints are received.

Brewing process

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Main article: Brewing

Brewing is typically divided into 9 steps: milling, malting, mashing, lautering, boiling, fermenting, conditioning, filtering, and filling.

Mashing is the process of mixing milled, usually malted, grain with water, and heating it with rests at certain temperatures to allow enzymes in the malt to break down the starches in the grain into sugars, especially maltose. Lautering is the separation of the extracts won during mashing from the spent grain to create wort. It is achieved in either a lauter tun, a wide vessel with a false bottom, or a mash filter, a plate-and-frame filter designed for this kind of separation. Lautering has two stages: first wort run-off, during which the extract is separated in an undiluted state from the spent grains, and sparging, in which extract that remains with the grains is rinsed off with hot water.

Boiling the wort ensures its sterility, helping to prevent contamination with undesirable microbes. During the boil, hops are added, which contribute aroma and flavour compounds to the beer, especially their characteristic bitterness. Along with the heat of the boil, they cause proteins in the wort to coagulate and the pH of the wort to fall, and they inhibit the later growth of certain bacteria. Finally, the vapours produced during the boil volatilize off-flavours, including dimethyl sulfide precursors. The boil must be conducted so that it is even and intense. The boil lasts between 60 and 120 minutes, depending on its intensity, the hop addition schedule, and volume of wort the brewer expects to evaporate.

Fermenting

Royal Brewery in Manchester, UK, with steel fermentation vessels

Fermentation begins as soon as yeast is added to the cooled wort. This is also the point at which the product is first called beer. It is during this stage that fermentable sugars won from the malt (maltose, maltotriose, glucose, fructose and sucrose) are metabolized into alcohol and carbon dioxide. Fermentation tanks come in many shapes and sizes, from enormous cylindroconical vessels that can look like storage silos, to 20-litre (5 US gal) glass carboys used by homebrewers. Most breweries today use cylindroconical vessels (CCVs), which have a conical bottom and a cylindrical top. The cone's aperture is typically around 70°, an angle that will allow the yeast to flow smoothly out through the cone's apex at the end of fermentation, but is not so steep as to take up too much vertical space. CCVs can handle both fermenting and conditioning in the same tank. At the end of fermentation, the yeast and other solids have fallen to the cone's apex can be simply flushed out through a port at the apex. Open fermentation vessels are also used, often for show in brewpubs, and in Europe in wheat beer fermentation. These vessels have no tops, making it easy to harvest top-fermenting yeasts. The open tops of the vessels increase the risk of contamination, but proper cleaning procedures help to control the risk.

Fermentation tanks are typically made of stainless steel. Simple cylindrical tanks with beveled ends are arranged vertically, and conditioning tanks are usually laid out horizontally. A very few breweries still use wooden vats for fermentation but wood is difficult to keep clean and infection-free and must be repitched often, perhaps yearly. After high kräusen, the point at which fermentation is most active and copious foam is produced, a valve known in German as the spundapparat may be put on the tanks to allow the carbon dioxide produced by the yeast to naturally carbonate the beer. This bung device can regulate the pressure to produce different types of beer; greater pressure produces a more carbonated beer.

Conditioning

When the sugars in the fermenting beer have been almost completely digested, the fermentation process slows and the yeast cells begin to die and settle at the bottom of the tank. At this stage, especially if the beer is cooled to around freezing, most of the remaining live yeast cells will quickly become dormant and settle, along with the heavier protein chains, due simply to gravity and molecular dehydration. Conditioning can occur in fermentation tanks with cooling jackets. If the whole fermentation cellar is cooled, conditioning must be done in separate tanks in a separate cellar. Some beers are conditioned only lightly, or not at all. An active yeast culture from an ongoing batch may be added to the next boil after a slight chilling in order to produce fresh and highly palatable beer in mass quantity.

Filling line, Radegast Brewery in Nošovice, Czech Republic

Filtering

Filtering the beer stabilizes flavour and gives it a polished, shiny look. It is an optional process. Many craft brewers simply remove the coagulated and settled solids and forgo active filtration. In localities where a tax assessment is collected by government pursuant to local laws, any additional filtration may be done using an active filtering system, the filtered product finally passing into a calibrated vessel for measurement just after any cold conditioning and prior to final packaging where the beer is put into the containers for shipment or sale. The container may be a bottle, can, of keg, cask or bulk tank.

Filters come in many types. Many use pre-made filtration media such as sheets or candles. Kieselguhr, a fine powder of diatomaceous earth, can be introduced into the beer and circulated through screens to form a filtration bed. Filtration ratings are divided into rough, fine, and sterile. Rough filters remove yeasts and other solids, leaving some cloudiness, while finer filters can remove body and color. Sterile filters remove almost all microorganisms.

Brewing companies

Yuengling Brewery, a regional brewery in Pottsville, Pennsylvania

Brewing companies range widely in the volume and variety of beer produced, ranging from small breweries to massive multinational conglomerates, like Molson Coors or Anheuser-Busch InBev, that produce hundreds of millions of barrels annually. There are organizations that assist the development of brewing, such as the Siebel Institute of Technology in the United States and the Institute of Brewing and Distilling in the UK. In 2012 the four largest brewing companies (Anheuser-Busch InBev, SABMiller, Heineken International, and Carlsberg Group) controlled 50% of the market[11] The biggest brewery in the world is the Belgian-Brazilian company Anheuser-Busch InBev.

In the United States, there were 69,359 people employed in breweries in 2017. This is up from 27,805 in 2001.[12]

Some commonly used descriptions of breweries are:

Microbrewery – A name used since the 1970s for a small, often independently owned brewery. In the 21st century the largely synonymous term craft brewery is also used.

Brewpub – A brewery whose beer is brewed primarily on the same site from which it is sold to the public, such as a pub or restaurant. In the United States, if the amount of beer that a brewpub distributes off-site exceeds 75% it may also be described as a craft or microbrewery.

Farm brewery – A farm brewery, or farmhouse brewery, is a brewery that primarily brews its beer on a farm. Crops and other ingredients grown on the farm, such as barley, wheat, rye, hops, herbs, spices, and fruits are used in the beers brewed. A farmhouse brewery is similar in concept to a vineyard growing grapes to make wine at the vineyard.[13]

Regional brewery – An established term for a brewery that supplies beer in a fixed geographical location.

Macrobrewery or Megabrewery – Terms for a brewery, too large or economically diversified to be a microbrewery, which sometimes carry a negative connotation.

Contract brewing

Contract brewing –When one brewery hires another brewery to produce its beer. The contracting brewer generally handles all of the beer's marketing, sales, and distribution, while leaving the brewing and packaging to the producer-brewery (which confusingly may also be referred to as a contract brewer). Often the contract brewing is performed when a small brewery can not supply enough beer to meet demands and contracts with a larger brewery to help alleviate their supply issues. Some breweries do not own a brewing facility, these contract brewers have been criticized by traditional brewing companies for avoiding the costs associated with a physical brewery.[14]

Gypsy brewing

Gypsy, or nomad, brewing usually falls under the category of contract brewing. Gypsy breweries generally do not have their own equipment or premises. They operate on a temporary or itinerant basis out of the facilities of another brewery, generally making "one-off" special occasion beers.[15] The trend of gypsy brewing spread early in Scandinavia.[16] Their beers and collaborations later spread to America and Australia.[17] Gypsy brewers typically use facilities of larger makers with excess capacity.[17]

Prominent examples include Pretty Things, Stillwater Artisanal Ales, Gunbarrel Brewing Company, Mikkeller, and Evil Twin.[18][19] For example, one of Mikkeller's founders, Mikkel Borg Bjergsø, has traveled around the world between 2006 and 2010, brewing more than 200 different beers at other breweries.[20]

Sponsorship

Breweries and football have had a symbiotic relationship since the very beginnings of the game. The English Football League was founded in 1888, and by the next decade several teams already had their own brewery sponsor. In return for their financial support, the breweries were given concessions to sell beer to spectators and advertise their products in stadiums. The most outwardly visible sign of sponsorship are the adverts printed on football team's kit. For example, Liverpool F.C. had the logo of the Denmark-based Carlsberg brewery group on the front of its shirts for nearly twenty years, from 1992 to 2010.

Nowadays major brewing corporations are involved in sponsorship on a number of different levels. The prevailing trend is for the leading brand not to be linked to individual teams; rather, they achieve visibility as sponsor of tournaments and leagues, so all fans can engage with them regardless of which team they support. Heineken sponsors the UEFA Champions League with its namesake lager; Carlsberg sponsors the English Premier League as well as the 2012 and 2016 UEFA European Championships. Meanwhile, the AB InBev Group supports the FA Cup and the FIFA World Cup.[21]

Head brewer/brewmaster

The head brewer (UK) or brewmaster (US) is in charge of the production of beer. The major breweries employ engineers with a chemistry/biotechnology background.

Brewmasters may have had a formal education in the subject from institutions such as the Siebel Institute of Technology, VLB Berlin, Heriot-Watt University, American Brewers Guild,[22] University of California at Davis, University of Wisconsin,[22] Olds College[23] or Niagara College.[24] They may hold membership in professional organisations such as the Brewers Association, Master Brewers Association, American Society of Brewing Chemists, the Institute of Brewing and Distilling,[25] and the Society of Independent Brewers. Depending on a brewery's size, a brewer may need anywhere from five to fifteen years of professional experience before becoming a brewmaster.[22]

See also

icon Beer portal

Drink portal

Beer and breweries by region

Breweriana—the hobby of brewery advertising collecting

List of breweries in the United States

List of microbreweries

Tower brewery

Liquor (or a spirit) is an alcoholic drink produced by distillation of grains, fruits, vegetables, or sugar, that have already gone through alcoholic fermentation. Other terms for liquor include: spirit drink, distilled beverage or hard liquor. The distillation process concentrates the liquid to increase its alcohol by volume.[1] As liquors contain significantly more alcohol (ethanol) than other alcoholic drinks, they are considered "harder" – in North America, the term hard liquor is sometimes used to distinguish distilled alcoholic drinks from non-distilled ones, whereas the term spirits is used in the UK. Examples of liquors include brandy, vodka, absinthe, gin, rum, tequila, and whisky.

Like other alcoholic drinks, liquor is typically consumed for the psychoactive effects of alcohol. Liquor may be consumed on its own (“neat”), typically in small amounts. In undiluted form, distilled beverages are often slightly sweet, bitter, and typically impart a burning mouthfeel, with a strong odor from the alcohol; the exact flavor varies between different varieties of liquor and the different impurities they impart. Liquor is also frequently enjoyed in diluted form, as flavored liquor or as part of a mixed drink; with cocktails being a common category of beverage that utilize liquor.

Acute liquor consumption causes severe alcohol intoxication, or alcohol poisoning, which can be fatal. Consistent consumption of liquor over time correlates with higher mortality and other harmful health effects, even compared to other alcoholic beverages.[2][3]

Nomenclature

The term "spirit" (singular and used without the additional term "drink") refers to liquor that should not contain added sugar[4] and usually is 35-40% alcohol by volume (ABV).[5] Fruit brandy, for example, is also known as fruit spirit.

Liquor bottled with added sugar and added flavorings, such as Grand Marnier, Frangelico, and American schnapps, are known instead as liqueurs.

Liquor generally has an alcohol concentration higher than 30%. Beer and wine, which are not distilled, are limited to a maximum alcohol content of about 20% ABV, as most yeasts cannot metabolize when the concentration of alcohol is above this level; as a consequence, fermentation ceases at that point.

Etymology

The origin of "liquor" and its close relative "liquid" was the Latin verb liquere, meaning "to be fluid". According to the Oxford English Dictionary, an early use of the word in the English language, meaning simply "a liquid", can be dated to 1225. The first use the OED mentions of its meaning "a liquid for drinking" occurred in the 14th century. Its use as a term for "an intoxicating alcoholic drink" appeared in the 16th century.

Legal definition

European Union

In accordance with the regulation (EU) 2019/787 of the European Parliament and of the Council of 17 April 2019,[6] a spirit drink is an alcoholic beverage that has been produced:

either directly by using, individually or in combination, any of the following methods:

distillation, with or without added flavorings or flavoring foodstuffs, of fermented products;

maceration or similar processing of plant materials in ethyl alcohol of agricultural origin, distillates of agricultural origin or spirit drinks or a combination thereof;

addition, individually or in combination, to ethyl alcohol of agricultural origin, distillates of agricultural origin or spirit drinks of flavorings, colors, other authorized ingredients, sweetening products, other agricultural products, foodstuffs.

or by adding, individually or in combination, to it any of the following:

other spirit drinks;

ethyl alcohol of agricultural origin;

distillates of agricultural origin;

other foodstuffs.

Spirit drinks must contain at least 15% alcohol by volume (except in the case of egg liqueur, which must contain a minimum of 14% ABV).[6][7]

Distillate of agricultural origin

Regulation makes a difference between "ethyl alcohol of agricultural origin" and "distillate of agricultural origin". Distillate of agricultural origin is defined as an alcoholic liquid which is the result of the distillation, after alcoholic fermentation, of agricultural products which does not have the properties of ethyl alcohol and which retains the aroma and taste of the raw materials used.[8]

Categories

Viru Valge, an Estonian vodka

Annex 1 to the regulation lists 44 categories of spirit drinks and their legal requirements.[9]

Some spirit drinks can fall into more than one category. Specific production requirements distinguish one category from another (London gin falls into Gin category but any gin cannot be considered as London gin).

Spirit drinks that are not produced within EU, such as Tequila or Baijiu, are not listed in the 44 categories.

Rum

Whisk(e)y

Grain spirit

Wine spirit

Brandy ou Weinbrand

Grape marc spirit or grape marc

Fruit marc spirit

Raisin spirit ou raisin brandy

Fruit spirit

Cider spirit, perry spirit and cider and perry spirit

Honey spirit

Hefebrand or lees spirit

Bierbrand, or beer spirit

Topinambur or Jerusalem artichoke spirit

Vodka

Spirit (supplemented by the name of the fruit, berries or nuts) obtained by maceration and distillation

Geist (supplemented by the name of the fruit or the raw materials used)

Gentian

Juniper-flavored spirit drink

Gin

Distilled gin

London gin

Caraway-flavored spirit drink or Kümmel

Akvavit or aquavit

Aniseed-flavored spirit drink

Pastis

Pastis de Marseille

Anis ou janeževec

Distilled anis

Bitter-tasting spirit drink or bitter

Flavored vodka

Sloe-aromatized spirit drink or pacharán

Liqueur

Crème de (supplemented by the name of a fruit or other raw material used)

Sloe gin

Sambuca

Maraschino, marrasquino or maraskino

Nocino ou orehovec

Egg liqueur or advocaat, avocat or advokat

Liqueur with egg

Mistrà

Väkevä glögi or spritglögg

Berenburg ou Beerenburg

Honey nectar or mead nectar

History of distillation

Main article: Distillation

Early history

Distillation equipment used by the 3rd century alchemist Zosimos of Panopolis,[10][11] from the Byzantine Greek manuscript Parisinus graecus 2327.[12]

Early evidence of distillation comes from Akkadian tablets dated c. 1200 BC describing perfumery operations, providing textual evidence that an early, primitive form of distillation was known to the Babylonians of ancient Mesopotamia.[13] Early evidence of distillation also comes from alchemists working in Alexandria, Roman Egypt, in the 1st century.[14] Distilled water was described in the 2nd century AD by Alexander of Aphrodisias.[15] Alchemists in Roman Egypt were using a distillation alembic or still device in the 3rd century.

Distillation was known in the ancient Indian subcontinent, evident from baked clay retorts and receivers found at Taxila and Charsadda in modern Pakistan, dating back to the early centuries of the Christian era. These "Gandhara stills" were capable of producing only very weak liquor, as there was no efficient means of collecting the vapors at low heat.[16]

Distillation in China could have begun during the Eastern Han dynasty (1st–2nd centuries), but the distillation of beverages began in the Jin (12th–13th centuries) and Southern Song (10th–13th centuries) dynasties according to archaeological evidence.[17]

Freeze distillation involves freezing the alcoholic beverage and then removing the ice. The freezing technique had limitations in geography and implementation limiting how widely this method was put to use.

Distillation of wine

An illustration of brewing and distilling industry methods in England, 1858

The inflammable nature of the exhalations of wine was already known to ancient natural philosophers such as Aristotle (384–322 BCE), Theophrastus (c. 371–287 BCE), and Pliny the Elder (23/24–79 CE).[18] This did not immediately lead to the isolation of alcohol, however, despite the development of more advanced distillation techniques in second- and third-century Roman Egypt.[19] An important recognition, first found in one of the writings attributed to Jābir ibn Ḥayyān (ninth century CE), was that by adding salt to boiling wine, which increases the wine's relative volatility, the flammability of the resulting vapors may be enhanced.[20] The distillation of wine is attested in Arabic works attributed to al-Kindī (c. 801–873 CE) and to al-Fārābī (c. 872–950), and in the 28th book of al-Zahrāwī's (Latin: Abulcasis, 936–1013) Kitāb al-Taṣrīf (later translated into Latin as Liber servatoris).[21] In the twelfth century, recipes for the production of aqua ardens ("burning water", i.e., alcohol) by distilling wine with salt started to appear in a number of Latin works, and by the end of the thirteenth century it had become a widely known substance among Western European chemists.[22] Its medicinal properties were studied by Arnald of Villanova (1240–1311 CE) and John of Rupescissa (c. 1310–1366), the latter of whom regarded it as a life-preserving substance able to prevent all diseases (the aqua vitae or "water of life", also called by John the quintessence of wine).[23]

In China, archaeological evidence indicates that the true distillation of alcohol began during the 12th century Jin or Southern Song dynasties.[17] A still has been found at an archaeological site in Qinglong, Hebei, dating to the 12th century.[17]

In India, the true distillation of alcohol was introduced from the Middle East, and was in wide use in the Delhi Sultanate by the 14th century.[16][24]

The works of Taddeo Alderotti (1223–1296) describe a method for concentrating alcohol involving repeated fractional distillation through a water-cooled still, by which an alcohol purity of 90% could be obtained.[25]

In 1437, "burned water" (brandy) was mentioned in the records of the County of Katzenelnbogen in Germany.[26]

Government regulation

Production

It is legal to distill beverage alcohol as a hobby for personal use in some countries, including New Zealand[27] and the Netherlands.[note 1]

In the United States, it is illegal to distill beverage alcohol without a license. In some parts of the U.S., it is also illegal to sell a still without a license. Nonetheless, all states allow unlicensed individuals to make their own beer, and some also allow unlicensed individuals to make their own wine (although making beer and wine is also prohibited in some local jurisdictions).

Sale

Some countries and sub-national jurisdictions limit or prohibit the sale of certain very high-percentage alcohol, commonly known as neutral spirit.

Due to its flammability (see below) alcoholic beverages with alcohol content above 70% by volume are not permitted to be transported in aircraft.[28]

Microdistilling

Microdistilling (also known as craft distilling) began to re-emerge as a trend in the United States following the microbrewing and craft beer movement in the last decades of the 20th century. In contrast, large-scale distillation facilities were never as dominant in Scotland, so the tradition of small-scale distillation was never really lost in the Scotch whisky market.

Flammability

These flaming cocktails illustrate that some liquors will readily catch fire and burn.

See also: Alcohol proof, Flash point, Fire point, and Flaming drink

Liquor that contains 40% ABV (80 US proof) will catch fire if heated to about 26 °C (79 °F) and if an ignition source is applied to it. This temperature is called its flash point.[29] The flash point of pure alcohol is 16.6 °C (61.9 °F), less than average room temperature.[30]

The flammability of liquor is applied in the cooking technique flambé.

The flash points of alcohol concentrations from 10% ABV to 96% ABV are:[31]

10% – 49 °C (120 °F) – ethanol-based water solution

12.5% – about 52 °C (126 °F) –wine[32]

15% – 42 °C (108 °F) – sake, mijiu, cheongju

20% – 36 °C (97 °F) – shōchū, fortified wine

30% – 29 °C (84 °F) – strong shōchū

40% – 26 °C (79 °F) – typical vodka, whisky or brandy

50% – 24 °C (75 °F) – typical baijiu, strong whisky, bottled in bond whisky, typical blanche absinthe

60% – 22 °C (72 °F) – strong baijiu, normal tsikoudia (called mesoraki or middle raki), barrel proof whisky, typical verte absinthe

70% – 21 °C (70 °F) – slivovitz

80% – 20 °C (68 °F) – strong absinthe

90% or more – 17 °C (63 °F) – neutral grain spirit

Serving

See also: Bartending terminology

A row of alcoholic beverages – in this case, spirits – in a bar

Liquor can be served:

Neat — at room temperature without any additional ingredient(s)[33]

Up — shaken or stirred with ice, strained, and served in a stemmed glass

Down — shaken or stirred with ice, strained, and served in a rocks glass

On the rocks — over ice cubes

Blended or frozen — blended with ice

With a simple mixer, such as club soda, tonic water, juice, or cola

As an ingredient of a cocktail

As an ingredient of a shooter

With water

With water poured over sugar (as with absinthe)

Alcohol consumption by country

Main article: List of countries by alcohol consumption

European countries grouped by preferred type of alcoholic drink, based on recorded alcohol consumption per capita (age 15+) (in litres of pure alcohol) in 2016

Map of Europe with individual countries grouped by preferred type of alcoholic drink, based on recorded alcohol consumption per capita (age 15+) (in litres of pure alcohol) in 2016.[34]

  Wine

  Beer

  Spirits

The World Health Organization measures and publishes alcohol consumption patterns in different countries. The WHO measures alcohol consumed by persons 15 years of age or older and reports it on the basis of liters of pure alcohol consumed per capita in a given year in a country.[35]

See also: Alcohol preferences in Europe

In Europe, spirits (especially vodka) are more popular towards the north and east of the continent.

Health effects

Short-term effects

Main article: Short-term effects of alcohol consumption

This section needs additional citations for verification. Please help improve this article by adding citations to reliable sources. Unsourced material may be challenged and removed.

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Distilled spirits contain ethyl alcohol, the same chemical that is present in beer and wine and as such, spirit consumption has short-term psychological and physiological effects on the user. Different concentrations of alcohol in the human body have different effects on a person. The effects of alcohol depend on the amount an individual has drunk, the percentage of alcohol in the spirits and the timespan that the consumption took place, the amount of food eaten and whether an individual has taken other prescription, over-the-counter or street drugs, among other factors.

Drinking enough to cause a blood alcohol concentration (BAC) of 0.03%-0.12% typically causes an overall improvement in mood and possible euphoria, increased self-confidence, and sociability, decreased anxiety, a flushed, red appearance in the face and impaired judgment and fine muscle coordination. A BAC of 0.09% to 0.25% causes lethargy, sedation, balance problems and blurred vision. A BAC from 0.18% to 0.30% causes profound confusion, impaired speech (e.g., slurred speech), staggering, dizziness and vomiting. A BAC from 0.25% to 0.40% causes stupor, unconsciousness, anterograde amnesia, vomiting, and respiratory depression (potentially life-threatening). Death may occur due to inhalation of vomit (pulmonary aspiration) while unconscious. A BAC from 0.35% to 0.80% causes a coma (unconsciousness), life-threatening respiratory depression and possibly fatal alcohol poisoning.

Heavy consumption of liquor leads to bloating, gassiness, diarrhea, painful stools, or fullness in the abdomen.[36] High quantity consumption of liquor increases cancer risk, namely head, neck, esophageal, liver, breast, and colorectal cancer.[37]

As with all alcoholic beverages, driving under the influence, operating an aircraft or heavy machinery increases the risk of an accident. As such, many countries have penalties for drunk driving.

Long-term effects

See also: Long-term effects of alcohol consumption

The main active ingredient of distilled spirits is alcohol, and therefore, the health effects of alcohol apply to spirits. Drinking more than 1-2 drinks a day increases the risk of heart disease, high blood pressure, atrial fibrillation, and stroke.[38] The risk is greater in younger people due to binge drinking, which may result in violence or accidents.[38] About 3.3 million deaths (5.9% of all deaths) are due to alcohol each year.[39] Unlike for wine and perhaps beer, there is no evidence for a J-shaped health effect for the consumption of distilled alcohol.[2]

Alcoholism, also known as "alcohol use disorder", is a broad term for any drinking of alcohol that results in problems.[40] Alcoholism reduces a person's life expectancy by around ten years[41] and alcohol use is the third-leading cause of early death in the United States.[38]

Demographics

Consumption of distilled alcohol is the most important single factor behind variation on mortality rates and life expectancy for men in Europe. For example, in heavily Islamic regions of the Caucasus (Islam forbids alcohol consumption) the life expectancy gap between women and men is five years; in nearby Christian areas it is ten years, and in the Czech Republic (where beer predominates) the chance of a man dying between the ages of 15 and 60 is less than half that of nearby Ukraine.[2][42]

Notes

 In the Netherlands, the ABV of the distilled drink must be under 15% ABV without a license.

See also

icon Liquor portal

Drink portal

Absinthe – Alcoholic drink (flavored with anise)

Aguardiente – Generic term for alcoholic beverages containing 29% to 60% alcohol by volume

Akvavit – Flavored Scandinavian spirit

Alcoholic drink

Amaro (liqueur) – Italian herbal liqueur

Arak – Middle Eastern distilled spirit

Arrack – Distilled alcoholic drink typically produced in South and Southeast Asia

Awamori – Alcoholic beverage of Okinawa

Baijiu – Chinese distilled liquor / Shōchū / Soju

Beer – Alcoholic drink made from fermented cereal grains

Borovička

Brandy – Spirit produced by distilling wine

Cachaça – Distilled beverage popular in Brazil

Eau de vie – French clear, colorless fruit brandy

Er guo tou

Fenny – Alcoholic spirit produced in Goa, India

Freeze distillation – Separating components of a mixture by their melting points

Geist – Distilled beverage

Gin – Distilled alcoholic drink flavoured with juniper (and Jenever)

Horilka – Ukrainian alcoholic beverage

Liquor store – Retail shop that sells alcohol

List of beverages

List of national drinks – Distinct beverages associated with a particlar country

Mahua

Mamajuana

Mezcal – Distilled alcoholic beverage

Moonshine – High-proof distilled spirit, generally produced illicitly

Neutral grain spirit

Orujo – Spanish pomace brandy

Padlamanggan

Pálinka – Central European alcohol

Pisco – Brandy made in Peru and Chile

Poitín – Traditional Irish distilled beverage

Rakia – Fruit brandy brand popular in the Balkans

Rakı – Sweetened, anise-flavored alcoholic drink

Rectified spirit – Highly concentrated ethanol

Rum – Distilled alcoholic beverage made from sugarcane

Rượu đế

Schnapps – Several types of flavored distilled alcoholic beverages

Slivovitz – Slavic fruit brandy

Tequila – Alcoholic beverage from Mexico

Tsikoudia – Distilled spirit from Crete

Tsipouro – Alcoholic beverage from Greece

Viche – Colombian traditional alcoholic beverage

Vodka – Clear distilled alcoholic beverage

Whisky – Distilled alcoholic beverage

Distillation, or classical distillation, is the process of separating the components or substances from a liquid mixture by using selective boiling and condensation. Dry distillation is the heating of solid materials to produce gaseous products (which may condense into liquids or solids). Dry distillation may involve chemical changes such as destructive distillation or cracking and is not discussed under this article. Distillation may result in essentially complete separation (nearly pure components), or it may be a partial separation that increases the concentration of selected components in the mixture. 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 it is a physical separation process, not a chemical reaction.

Distillation has many applications. For example:

The distillation of fermented products produces distilled beverages with a high alcohol content, or separates other fermentation products of commercial value.

Distillation is an effective and traditional method of desalination.

In the petroleum industry, oil stabilization is a form of partial distillation that reduces the vapor pressure of crude oil, thereby making it safe for storage and transport as well as reducing the atmospheric emissions of volatile hydrocarbons. In midstream operations at oil refineries, fractional distillation is a major class of operation for transforming crude oil into fuels and chemical feed stocks.[2][3][4]

Cryogenic distillation leads to the separation of air into its components – notably oxygen, nitrogen, and argon – for industrial use.

In the chemical industry, large amounts of crude liquid products of chemical synthesis are distilled to separate them, either from other products, from impurities, or from unreacted starting materials.

An installation used for distillation, especially of distilled beverages, is a distillery. The distillation equipment itself is a still.

History

See also: Distilled beverage

Distillation equipment used by the 3rd century alchemist Zosimos of Panopolis,[5][6] from the Byzantine Greek manuscript Parisinus graces.[7]

Early evidence of distillation was found on Akkadian tablets dated c. 1200 BCE describing perfumery operations. The tablets provided textual evidence that an early primitive form of distillation was known to the Babylonians of ancient Mesopotamia.[8] Early evidence of distillation was also found related to alchemists working in Alexandria in Roman Egypt in the 1st century CE.[9]: 57, 89 

Distillation was practiced in the ancient Indian subcontinent, which is evident from baked clay retorts and receivers found at Taxila, Shaikhan Dheri, Charsadda in Pakistan and Rang Mahal in India dating to the early centuries of the Common Era.[10][11][12] Allchin notes these terracotta distill tubes were "made to imitate bamboo".[13] These "Gandhara stills" were only capable of producing very weak liquor, as there was no efficient means of collecting the vapors at low heat.[14] Distilled water has been in use since at least c. 200 CE, when Alexander of Aphrodisias described the process.[15][16] Work on distilling other liquids continued in early Byzantine Egypt under Zosimus of Panopolis in the 3rd century.

Distillation in China may have begun during the Eastern Han dynasty (1st–2nd centuries CE), but the distillation of beverages began in the Jin (12th–13th centuries) and Southern Song (10th–13th centuries) dynasties, according to archaeological evidence.[17]

Medieval Muslim chemists such as Jābir ibn Ḥayyān (Latin: Geber, ninth century) and Abū Bakr al-Rāzī (Latin: Rhazes, c. 865–925) experimented extensively with the distillation of various substances.

The distillation of wine is attested in Arabic works attributed to al-Kindī (c. 801–873 CE) and to al-Fārābī (c. 872–950), and in the 28th book of al-Zahrāwī's (Latin: Abulcasis, 936–1013) Kitāb al-Taṣrīf (later translated into Latin as Liber servatoris).[18] In the twelfth century, recipes for the production of aqua ardens ("burning water", i.e., ethanol) by distilling wine with salt started to appear in a number of Latin works, and by the end of the thirteenth century it had become a widely known substance among Western European chemists.[19] The works of Taddeo Alderotti (1223–1296) describe a method for concentrating alcohol involving repeated distillation through a water-cooled still, by which an alcohol purity of 90% could be obtained.[20]

The fractional distillation of organic substances plays an important role in the works attributed to Jābir ibn Ḥayyān, such as in the Kitāb al-Sabʿīn ('The Book of Seventy'), translated into Latin by Gerard of Cremona (c. 1114–1187) under the title Liber de septuaginta.[21] The Jabirian experiments with fractional distillation of animal and vegetable substances, and to a lesser degree also of mineral substances, is the main topic of the De anima in arte alkimiae, an originally Arabic work falsely attributed to Avicenna that was translated into Latin and would go on to form the most important alchemical source for Roger Bacon (c. 1220–1292).[22]

A still was found in an archaeological site in Qinglong, Hebei province, in China, dating back to the 12th century. Distilled beverages were common during the Yuan dynasty (13th–14th centuries).[17]

In 1500, German alchemist Hieronymus Braunschweig published Liber de arte destillandi (The Book of the Art of Distillation),[23] the first book solely dedicated to the subject of distillation, followed in 1512 by a much expanded version. In 1651, John French published The Art of Distillation,[24] the first major English compendium on the practice, but it has been claimed[25] that much of it derives from Braunschweig's work. This includes diagrams with people in them showing the industrial rather than bench scale of the operation.

Hieronymus Brunschwig's Liber de arte Distillandi de Compositis (Strassburg, 1512) Science History Institute

A retort

Distillation

Old Ukrainian vodka still

Simple liqueur distillation in East Timor

As alchemy evolved into the science of chemistry, vessels called retorts became used for distillations. Both alembics and retorts are forms of glassware with long necks pointing to the side at a downward angle to act as air-cooled condensers to condense the distillate and let it drip downward for collection. Later, copper alembics were invented. Riveted joints were often kept tight by using various mixtures, for instance a dough made of rye flour.[26] These alembics often featured a cooling system around the beak, using cold water, for instance, which made the condensation of alcohol more efficient. These were called pot stills. Today, the retorts and pot stills have been largely supplanted by more efficient distillation methods in most industrial processes. However, the pot still is still widely used for the elaboration of some fine alcohols, such as cognac, Scotch whisky, Irish whiskey, tequila, rum, cachaça, and some vodkas. Pot stills made of various materials (wood, clay, stainless steel) are also used by bootleggers in various countries. Small pot stills are also sold for use in the domestic production[27] of flower water or essential oils.

Early forms of distillation involved batch processes using one vaporization and one condensation. Purity was improved by further distillation of the condensate. Greater volumes were processed by simply repeating the distillation. Chemists reportedly carried out as many as 500 to 600 distillations in order to obtain a pure compound.[28]

In the early 19th century, the basics of modern techniques, including pre-heating and reflux, were developed.[28] In 1822, Anthony Perrier developed one of the first continuous stills, and then, in 1826, Robert Stein improved that design to make his patent still. In 1830, Aeneas Coffey got a patent for improving the design even further.[29] Coffey's continuous still may be regarded as the archetype of modern petrochemical units. The French engineer Armand Savalle developed his steam regulator around 1846.[9]: 323  In 1877, Ernest Solvay was granted a U.S. Patent for a tray column for ammonia distillation,[30] and the same and subsequent years saw developments in this theme for oils and spirits.

With the emergence of chemical engineering as a discipline at the end of the 19th century, scientific rather than empirical methods could be applied. The developing petroleum industry in the early 20th century provided the impetus for the development of accurate design methods, such as the McCabe–Thiele method by Ernest Thiele and the Fenske equation. The first industrial plant in the United States to use distillation as a means of ocean desalination opened in Freeport, Texas in 1961 with the hope of bringing water security to the region.[31] The availability of powerful computers has allowed direct computer simulations of distillation columns.

Applications

The application of distillation can roughly be divided into four groups: laboratory scale, industrial distillation, distillation of herbs for perfumery and medicinals (herbal distillate), and food processing. The latter two are distinctively different from the former two in that distillation is not used as a true purification method but more to transfer all volatiles from the source materials to the distillate in the processing of beverages and herbs.

The main difference between laboratory scale distillation and industrial distillation are that laboratory scale distillation is often performed on a batch basis, whereas industrial distillation often occurs continuously. In batch distillation, the composition of the source material, the vapors of the distilling compounds, and the distillate change during the distillation. In batch distillation, a still is charged (supplied) with a batch of feed mixture, which is then separated into its component fractions, which are collected sequentially from most volatile to less volatile, with the bottoms – remaining least or non-volatile fraction – removed at the end. The still can then be recharged and the process repeated.

In continuous distillation, the source materials, vapors, and distillate are kept at a constant composition by carefully replenishing the source material and removing fractions from both vapor and liquid in the system. This results in a more detailed control of the separation process.

Idealized model

The boiling point of a liquid is the temperature at which the vapor pressure of the liquid equals the pressure around the liquid, enabling bubbles to form without being crushed. A special case is the normal boiling point, where the vapor pressure of the liquid equals the ambient atmospheric pressure.

It is a misconception that in a liquid mixture at a given pressure, each component boils at the boiling point corresponding to the given pressure, allowing the vapors of each component to collect separately and purely. However, this does not occur, even in an idealized system. Idealized models of distillation are essentially governed by Raoult's law and Dalton's law and assume that vapor–liquid equilibria are attained.

Raoult's law states that the vapor pressure of a solution is dependent on 1) the vapor pressure of each chemical component in the solution and 2) the fraction of solution each component makes up, a.k.a. the mole fraction. This law applies to ideal solutions, or solutions that have different components but whose molecular interactions are the same as or very similar to pure solutions.

Dalton's law states that the total pressure is the sum of the partial pressures of each individual component in the mixture. When a multi-component liquid is heated, the vapor pressure of each component will rise, thus causing the total vapor pressure to rise. When the total vapor pressure reaches the pressure surrounding the liquid, boiling occurs and liquid turns to gas throughout the bulk of the liquid. A mixture with a given composition has one boiling point at a given pressure when the components are mutually soluble. A mixture of constant composition does not have multiple boiling points.

An implication of one boiling point is that lighter components never cleanly "boil first". At boiling point, all volatile components boil, but for a component, its percentage in the vapor is the same as its percentage of the total vapor pressure. Lighter components have a higher partial pressure and, thus, are concentrated in the vapor, but heavier volatile components also have a (smaller) partial pressure and necessarily vaporize also, albeit at a lower concentration in the vapor. Indeed, batch distillation and fractionation succeed by varying the composition of the mixture. In batch distillation, the batch vaporizes, which changes its composition; in fractionation, liquid higher in the fractionation column contains more lights and boils at lower temperatures. Therefore, starting from a given mixture, it appears to have a boiling range instead of a boiling point, although this is because its composition changes: each intermediate mixture has its own, singular boiling point.

The idealized model is accurate in the case of chemically similar liquids, such as benzene and toluene. In other cases, severe deviations from Raoult's law and Dalton's law are observed, most famously in the mixture of ethanol and water. These compounds, when heated together, form an azeotrope, which is when the vapor phase and liquid phase contain the same composition. Although there are computational methods that can be used to estimate the behavior of a mixture of arbitrary components, the only way to obtain accurate vapor–liquid equilibrium data is by measurement.

It is not possible to completely purify a mixture of components by distillation, as this would require each component in the mixture to have a zero partial pressure. If ultra-pure products are the goal, then further chemical separation must be applied. When a binary mixture is vaporized and the other component, e.g., a salt, has zero partial pressure for practical purposes, the process is simpler.

Batch or differential distillation

A batch still showing the separation of A and B.

Heating an ideal mixture of two volatile substances, A and B, with A having the higher volatility, or lower boiling point, in a batch distillation setup (such as in an apparatus depicted in the opening figure) until the mixture is boiling results in a vapor above the liquid that contains a mixture of A and B. The ratio between A and B in the vapor will be different from the ratio in the liquid. The ratio in the liquid will be determined by how the original mixture was prepared, while the ratio in the vapor will be enriched in the more volatile compound, A (due to Raoult's Law, see above). The vapor goes through the condenser and is removed from the system. This, in turn, means that the ratio of compounds in the remaining liquid is now different from the initial ratio (i.e., more enriched in B than in the starting liquid).

The result is that the ratio in the liquid mixture is changing, becoming richer in component B. This causes the boiling point of the mixture to rise, which results in a rise in the temperature in the vapor, which results in a changing ratio of A : B in the gas phase (as distillation continues, there is an increasing proportion of B in the gas phase). This results in a slowly changing ratio of A : B in the distillate.

If the difference in vapour pressure between the two components A and B is large – generally expressed as the difference in boiling points – the mixture in the beginning of the distillation is highly enriched in component A, and when component A has distilled off, the boiling liquid is enriched in component B.

Continuous distillation

Main article: Continuous distillation

Continuous distillation is an ongoing distillation in which a liquid mixture is continuously (without interruption) fed into the process and separated fractions are removed continuously as output streams occur over time during the operation. Continuous distillation produces a minimum of two output fractions, including at least one volatile distillate fraction, which has boiled and been separately captured as a vapor and then condensed to a liquid. There is always a bottoms (or residue) fraction, which is the least volatile residue that has not been separately captured as a condensed vapor.

Continuous distillation differs from batch distillation in the respect that concentrations should not change over time. Continuous distillation can be run at a steady state for an arbitrary amount of time. For any source material of specific composition, the main variables that affect the purity of products in continuous distillation are the reflux ratio and the number of theoretical equilibrium stages, in practice determined by the number of trays or the height of packing. Reflux is a flow from the condenser back to the column, which generates a recycle that allows a better separation with a given number of trays. Equilibrium stages are ideal steps where compositions achieve vapor–liquid equilibrium, repeating the separation process and allowing better separation given a reflux ratio. A column with a high reflux ratio may have fewer stages, but it refluxes a large amount of liquid, giving a wide column with a large holdup. Conversely, a column with a low reflux ratio must have a large number of stages, thus requiring a taller column.

General improvements

Both batch and continuous distillations can be improved by making use of a fractionating column on top of the distillation flask. The column improves separation by providing a larger surface area for the vapor and condensate to come into contact. This helps it remain at equilibrium for as long as possible. The column can even consist of small subsystems ('trays' or 'dishes') which all contain an enriched, boiling liquid mixture, all with their own vapor–liquid equilibrium.

There are differences between laboratory-scale and industrial-scale fractionating columns, but the principles are the same. Examples of laboratory-scale fractionating columns (in increasing efficiency) include

Air condenser

Vigreux column (usually laboratory scale only)

Packed column (packed with glass beads, metal pieces, or other chemically inert material)

Spinning band distillation system.

Laboratory procedures

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 distillation types).

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

Schematic of a simple distillation setup.

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)[32] 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

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 by repeated vaporization-condensation cycles within a packed fractionating column. This separation, by successive distillations, is also referred to as rectification.[33]

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 are determined once again by Raoult's law. Each vaporization-condensation cycle (called a theoretical plate) will yield a purer solution of the more volatile component.[34] 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, increasing the number of theoretical plates.[35]

Steam distillation

Main article: Steam distillation

Like vacuum distillation, steam distillation is a method for distilling compounds which are heat-sensitive.[1]: 151–153  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. The essential 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

Stirrer bar/anti-bumping granulesStill potFractionating columnThermometer/Boiling point temperatureTeflon tap 1Cold fingerCooling water outCooling water inTeflon tap 2Vacuum/gas inletTeflon tap 3Still receiver

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 as vacuum 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.

Short path and molecular distillation

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.

Short path vacuum distillation apparatus with vertical condenser (cold finger), to minimize the distillation path; Still pot with stirrer bar/anti-bumping granulesCold finger – bent to direct condensateCooling water outcooling water inVacuum/gas inletDistillate flask/distillate.

Short path distillation is a distillation technique that involves the distillate travelling a short distance, often only a few centimeters, and is normally done at reduced pressure.[1]: 150  A classic example would be a distillation involving the distillate travelling from one glass bulb to another, without the need for a condenser separating the two chambers. This technique is often used for compounds which are unstable at high temperatures or to purify small amounts of compound. The advantage is that the heating temperature can be considerably lower (at reduced pressure) than the boiling point of the liquid at standard pressure, and the distillate only has to travel a short distance before condensing. A short path ensures that little compound is lost on the sides of the apparatus. The Kugelrohr apparatus is a kind of short path distillation method which often contains multiple chambers to collect distillate fractions.

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

Zone distillation is a distillation process in a long container with partial melting of refined matter in moving liquid zone and condensation of vapor in the solid phase at condensate pulling in cold area. The process is worked in theory. When zone heater is moving from the top to the bottom of the container then solid condensate with irregular impurity distribution is forming. Then most pure part of the condensate may be extracted as product. The process may be iterated many times by moving (without turnover) the received condensate to the bottom part of the container on the place of refined matter. The irregular impurity distribution in the condensate (that is efficiency of purification) increases with the number of iterations. Zone distillation is the distillation analog of zone recrystallization. Impurity distribution in the condensate is described by known equations of zone recrystallization – with the replacement of the distribution co-efficient k of crystallization - for the separation factor α of distillation.[36][37][38]

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.[39][40]

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 distallation 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

Main article: Azeotropic distillation

Interactions between the components of the solution create properties unique to the solution, as most processes entail non-ideal mixtures, where Raoult's law does not hold. Such interactions can result in a constant-boiling azeotrope which behaves as if it were a pure compound (i.e., boils at a single temperature instead of a range). At an azeotrope, the solution contains the given component in the same proportion as the vapor, so that evaporation does not change the purity, and distillation does not effect separation. For example, ethyl alcohol and water form an azeotrope of 95.6% at 78.1 °C.

If the azeotrope is not considered sufficiently pure for use, there exist some techniques to break the azeotrope to give a pure distillate. This set of techniques are known as azeotropic distillation. Some techniques achieve this by "jumping" over the azeotropic composition (by adding another component to create a new azeotrope, or by varying the pressure). Others work by chemically or physically removing or sequestering the impurity. For example, to purify ethanol beyond 95%, a drying agent (or desiccant, such as potassium carbonate) can be added to convert the soluble water into insoluble water of crystallization. Molecular sieves are often used for this purpose as well.

Immiscible liquids, such as water and toluene, easily form azeotropes. Commonly, these azeotropes are referred to as a low boiling azeotrope because the boiling point of the azeotrope is lower than the boiling point of either pure component. The temperature and composition of the azeotrope is easily predicted from the vapor pressure of the pure components, without use of Raoult's law. The azeotrope is easily broken in a distillation set-up by using a liquid–liquid separator (a decanter) to separate the two liquid layers that are condensed overhead. Only one of the two liquid layers is refluxed to the distillation set-up.

High boiling azeotropes, such as a 20 percent by weight mixture of hydrochloric acid in water, also exist. As implied by the name, the boiling point of the azeotrope is greater than the boiling point of either pure component.

To break azeotropic distillations and cross distillation boundaries, such as in the DeRosier Problem, it is necessary to increase the composition of the light key in the distillate.

Breaking an azeotrope with unidirectional pressure manipulation

The boiling points of components in an azeotrope overlap to form a band. By exposing an azeotrope to a vacuum or positive pressure, it's possible to bias the boiling point of one component away from the other by exploiting the differing vapor pressure curves of each; the curves may overlap at the azeotropic point, but are unlikely to remain identical further along the pressure axis to either side of the azeotropic point. When the bias is great enough, the two boiling points no longer overlap and so the azeotropic band disappears.

This method can remove the need to add other chemicals to a distillation, but it has two potential drawbacks.

Under negative pressure, power for a vacuum source is needed and the reduced boiling points of the distillates requires that the condenser be run cooler to prevent distillate vapors being lost to the vacuum source. Increased cooling demands will often require additional energy and possibly new equipment or a change of coolant.

Alternatively, if positive pressures are required, standard glassware can not be used, energy must be used for pressurization and there is a higher chance of side reactions occurring in the distillation, such as decomposition, due to the higher temperatures required to effect boiling.

A unidirectional distillation will rely on a pressure change in one direction, either positive or negative.

Pressure-swing distillation

Further information: Azeotrope § Pressure swing distillation

Pressure-swing distillation is essentially the same as the unidirectional distillation used to break azeotropic mixtures, but here both positive and negative pressures may be employed.

This improves the selectivity of the distillation and allows a chemist to optimize distillation by avoiding extremes of pressure and temperature that waste energy. This is particularly important in commercial applications.

One example of the application of pressure-swing distillation is during the industrial purification of ethyl acetate after its catalytic synthesis from ethanol.

Industrial process

Typical industrial distillation towers

Main article: Continuous distillation

Large scale industrial distillation applications include both batch and continuous fractional, vacuum, azeotropic, extractive, and steam distillation. The most widely used industrial applications of continuous, steady-state fractional distillation are in petroleum refineries, petrochemical and chemical plants and natural gas processing plants.

To control and optimize such industrial distillation, a standardized laboratory method, ASTM D86, is established. This test method extends to the atmospheric distillation of petroleum products using a laboratory batch distillation unit to quantitatively determine the boiling range characteristics of petroleum products.

Industrial distillation[33][41] is typically performed in large, vertical cylindrical columns known as distillation towers or distillation columns with diameters ranging from about 0.65 to 16 metres (2 ft 2 in to 52 ft 6 in) and heights ranging from about 6 to 90 metres (20 to 295 ft) or more. When the process feed has a diverse composition, as in distilling crude oil, liquid outlets at intervals up the column allow for the withdrawal of different fractions or products having different boiling points or boiling ranges. The "lightest" products (those with the lowest boiling point) exit from the top of the columns and the "heaviest" products (those with the highest boiling point) exit from the bottom of the column and are often called the bottoms.

Diagram of a typical industrial distillation tower

Industrial towers use reflux to achieve a more complete separation of products. Reflux refers to the portion of the condensed overhead liquid product from a distillation or fractionation tower that is returned to the upper part of the tower as shown in the schematic diagram of a typical, large-scale industrial distillation tower. Inside the tower, the downflowing reflux liquid provides cooling and condensation of the upflowing vapors thereby increasing the efficiency of the distillation tower. The more reflux that is provided for a given number of theoretical plates, the better the tower's separation of lower boiling materials from higher boiling materials. Alternatively, the more reflux that is provided for a given desired separation, the fewer the number of theoretical plates required. Chemical engineers must choose what combination of reflux rate and number of plates is both economically and physically feasible for the products purified in the distillation column.

Such industrial fractionating towers are also used in cryogenic air separation, producing liquid oxygen, liquid nitrogen, and high purity argon. Distillation of chlorosilanes also enables the production of high-purity silicon for use as a semiconductor.

Section of an industrial distillation tower showing detail of trays with bubble caps

Design and operation of a distillation tower depends on the feed and desired products. Given a simple, binary component feed, analytical methods such as the McCabe–Thiele method[33][42] or the Fenske equation[33] can be used. For a multi-component feed, simulation models are used both for design and operation. Moreover, the efficiencies of the vapor–liquid contact devices (referred to as "plates" or "trays") used in distillation towers are typically lower than that of a theoretical 100% efficient equilibrium stage. Hence, a distillation tower needs more trays than the number of theoretical vapor–liquid equilibrium stages. A variety of models have been postulated to estimate tray efficiencies.

In modern industrial uses, a packing material is used in the column instead of trays when low pressure drops across the column are required. Other factors that favor packing are: vacuum systems, smaller diameter columns, corrosive systems, systems prone to foaming, systems requiring low liquid holdup, and batch distillation. Conversely, factors that favor plate columns are: presence of solids in feed, high liquid rates, large column diameters, complex columns, columns with wide feed composition variation, columns with a chemical reaction, absorption columns, columns limited by foundation weight tolerance, low liquid rate, large turn-down ratio and those processes subject to process surges.

Large-scale, industrial vacuum distillation column[43]

This packing material can either be random dumped packing (25–76 millimetres (1–3 in) wide) such as Raschig rings or structured sheet metal. Liquids tend to wet the surface of the packing and the vapors pass across this wetted surface, where mass transfer takes place. Unlike conventional tray distillation in which every tray represents a separate point of vapor–liquid equilibrium, the vapor–liquid equilibrium curve in a packed column is continuous. However, when modeling packed columns, it is useful to compute a number of "theoretical stages" to denote the separation efficiency of the packed column with respect to more traditional trays. Differently shaped packings have different surface areas and void space between packings. Both of these factors affect packing performance.

Another factor in addition to the packing shape and surface area that affects the performance of random or structured packing is the liquid and vapor distribution entering the packed bed. The number of theoretical stages required to make a given separation is calculated using a specific vapor to liquid ratio. If the liquid and vapor are not evenly distributed across the superficial tower area as it enters the packed bed, the liquid to vapor ratio will not be correct in the packed bed and the required separation will not be achieved. The packing will appear to not be working properly. The height equivalent to a theoretical plate (HETP) will be greater than expected. The problem is not the packing itself but the mal-distribution of the fluids entering the packed bed. Liquid mal-distribution is more frequently the problem than vapor. The design of the liquid distributors used to introduce the feed and reflux to a packed bed is critical to making the packing perform to it maximum efficiency. Methods of evaluating the effectiveness of a liquid distributor to evenly distribute the liquid entering a packed bed can be found in references.[44][45] Considerable work has been done on this topic by Fractionation Research, Inc. (commonly known as FRI).[46]

Multi-effect distillation

The goal of multi-effect distillation is to increase the energy efficiency of the process, for use in desalination, or in some cases one stage in the production of ultrapure water. The number of effects is inversely proportional to the kW·h/m3 of water recovered figure, and refers to the volume of water recovered per unit of energy compared with single-effect distillation. One effect is roughly 636 kW·h/m3.

Multi-stage flash distillation can achieve more than 20 effects with thermal energy input, as mentioned in the article.

Vapor compression evaporation – Commercial large-scale units can achieve around 72 effects with electrical energy input, according to manufacturers.

There are many other types of multi-effect distillation processes, including one referred to as simply multi-effect distillation (MED), in which multiple chambers, with intervening heat exchangers, are employed.

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