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1、1989 James F.Guymon Lecture Distillation in Alambic ROBERT LEAUTI Robert Laut presented the James F.Guymon Lecture at the 40 th Annual Meeting of the American Society for Enology and Viticulture in Anaheim,California,on 30 June 1989.Leaute has been with Rmy Martin since 1973 and is currently Head Co
2、gnac Master,Research and Development Manager,and RMS Vineyards Technical Advisor.The text of his presentation has been edited for publication,but not subjected to the normal review process.History of Distillation Distillation is a very old technique which was used by the Chinese 3000 years BC,the Ea
3、st Indians 2500 years BC,the Egyptians 2000 years BC,the Greeks 1000 years BC,and the Romans 200 years BC.In the beginning,all of the above cultures produced a liquid,later called alcohol by the Arabs,which was used for medicinal purposes and to make perfumes.(Fig.1).Alambic(Hat),qP Vapors Wool Boil
4、er Cucurbit(Boiler)Fire Fig.1.Early still.Part of the vapors were condensed in the wool.The wool was changed from time to time to obtain the distillate.By the sixth century AD,the Arabs had started to invade Europe and at the same time released the tech-nique of distillation.Alchemists and monks pro
5、gres-sively improved both the technique and the distillation equipment(Fig.2).In 1250,Arnaud de Villeneuve was 1Remy Martin,16102 Cognac,Cedex,France.Some of the artwork used in this presentation was provided courtesy of R.Prulho,Cognac,France.Copyright 1990 by the American Society for Enology and V
6、iticulture.All rights reserved.90 Fig.2.Later distillation equipment.the first to distill wines in France;he called the product which resulted from this process eau-de-vie or water of life.He attributed to it the virtue of prolonging life.Origin of the alambic still:Today,the pot still used in the C
7、ognac area is known as an alambic.Ambix is a Greek word defined as a vase with a small opening.This vase was part of the distillation equip-ment.Initially,the Arabs changed the word Ambix to Ambic and called the distillation equipment A1 Ambic.Later in Europe,the word was changed to alambic.The Dutc
8、h,French,Irish,Scottish,and others started producing distilled spirits around the 15th and the 16th century.They created gin(Holland),whiskey(Scotland and Ireland),Armagnac(France),and Co-gnac(France).If the capacity of the still depended on the purpose of the distillation,then the shape was related
9、 to the country which used the distillation equipment.In the Cognac region around 1600,the Chevalier of Croix Marron perfected the eau-de-vie through double distil-lation.In France,Chaptal(1780)and Adam(1805)Am.J.Enol.Vitic.,Vol.41,No.1,1990 ALAMBIC DISTILLATION-91 dramatically improved the efficien
10、cy of distillation and gave the alambic its final design.The Cognac makers,continually seeking to obtain the best quality for their Cognac,brought both the alambic design and the double distillation methods to the peak of perfection.In North America,bourbons and whiskies were first produced around 1
11、750.In the booklet America Brandy Land,published by the California Brandy Advisory Board,the Mission San Fernando produced around 2000 barrels of brandy during the 1830s.Father Duran,the brandy maker at Mission Santa Barbara,produced brandy double distillation.Progressively during the 1950s,most of
12、brandy producers gave up distilling.Those who continued to.,.,=.I A L A M B I C C H A R E N T A I S ,.,.,distill preferred use of the column still because of its ability to produce a brandy compatible to the consumer trend.During the last decade,in California,one has no-ticed the American palate bec
13、oming more and more educated and ready for sophisticated products.At the same time,many wines and sparkling wines have reached a very high level of quality and are recognized as world class products.In the 1980s,well-established and new brandy producers decided the time had come to develop a more co
14、mplex California brandy.Today,if one produces a brandy using an alambic and the Cognac distillation method,the brandy can be called alambic brandy.Cognac Type of Still-Alambic l i:-ill,.,.CONDENSER PREHEA TER BO I LER.-.:.-.-ff-i I,.-.t.i_ L I=._.T,.t .!.ffT-,.i .?.I,)-.-.,.i .,:-=Fig.3.Diagram of t
15、he Cognac still-alambic:A standard alambic is 2500 liters(660 gal)capacity.(A)copper boiler(chaudiere);(B)hat(chapeau,chapiteau);(C)swans neck(col de cygne);(D)preheater(chauffe-vin);(E)coil(serpentin);(F)condenser(condenseur,pipe);(G)hydrometer port(porte-alcoometre);(H)heads tank(cuvon de tetes);(
16、I)gas burner(bruleur).(Courtesy of R.Prulho,Cognac.)The most famous alambic manu-facturers(Binaud,Chalvignac,Mareste,R.Prulho)are based in the Cognac area.Raw materials to manufac-ture alambics:An alambic is made of copper and bronze.Some of the alambic parts not important to the quality of the Cogn
17、ac or the brandy can be made of stainless steel for practical reasons(e.g.,valves,fit-tings,condenser tank).Hovever,copper remains the most efficient metal to build alambics.Copper of-fers the following advantages:it is malleable;it is a good conductor of heat;it resists corrosion from fire and from
18、 wine;it reacts with wine components such as sulfur compo-nents and fatty acids(this property is always favorable for the Cognac or brandy quality);and it is a catalyst for favorable reactions between wine components.Copper boiler(A):When the boiler is filled with 660 gallons of wine,the head space
19、above is around 130 gallons.The boiler is the main part of the alambic,and it is specially built for to withstand continuous direct flame of approximately 1500F and for ease of cleaning.The inside of the boiler is well polished so that the copper presents a smooth surface for easy cleaning.The boile
20、r is in constant contact with the direct flame fueled by natural gas,pro-pane,or butane.Boiler equipment includes the pipe to fill the boiler,the vent,the side glass,the sprinkler to clean boiler,and the valve to empty the boiler(Fig.4).Hat(chapiteau,chapeau)(B):Am.J.Enol.Vitic.,Vol.41,No.1,1990 92-
21、ALAMBIC DISTILLATION SPRINKLER I v 16 IN-I W INEP I PE VENT 71 IN#D i,/I 0 ,I SI DE GLASS A_ I!I Fig.4.(A)Copper boiler(chaudiere).(Courtesy of R.Prulho,Cognac.)6.30 IN SPRI VALVE W A T E R /IF=:I I t t I!Z Fig.5.(B)Hat(chapeau,chapiteau).(Courtesy of R.Prulho,Cognac.)This part of the alambic is loc
22、ated directly above the boiler.The volume of the hat is approximately 10%to 12%of the capacity of the boiler,depending on the specifications required by the distiller.The shape and the volume of the chapiteau deter-mine the concentration,selection,and separation of the Z 6.3 IN Fig.6.(C)Swans neck(c
23、ol de cygne).(Courtesy of R.Prulho,Cognac.)different volatile components.This selection process occurs when volatile compounds condense in the chap-iteau and fall back down into the boiler,where they must be re-distilled upward.This phenomenon is called the reflux process(Fig.5).Swans neck(col de cy
24、gne)(C):This part of the alambic is curved like the neck of a swan and directs the vapor into the coil.The height and the curve of the swans neck are extremely important to the reflux process(Fig.6).Preheater(chauffe-vin)(D):This is a cost effective part of the alambic.The swans neck pipe runs throu
25、gh the preheater and around its back.During the first hours of distillation,one refills the preheater for the next batch of distillation.By directing the hot vapors of Am.J.Enol.Vitic.,Vol.41,No.1,1990 ALAMBIC DISTILLATION-93 665 USG.:-=-:-T_-_-_-=-t I I Fig.7.(19)Preheater(chauffe-vin).(Courtesy of
26、 R.Prulho,Cognac.)L:220 FT VENT i.4,-t Fig.8.(E)Coil(sepentin).(Courtesy of R.Prulho,Cognac.)the currently distilling pot still through the preheater,the wine can be preheated for the next distillation.The alternative pipe running around the outside of the preheater is used when the temperature of t
27、he contents in the preheater is correct;this will avoid over-heating the contents of the preheater(Fig.7).Coil(serpentin)(E):The coil pipe is also made of copper.During the condensation,the copper reacts with components of the distillates(sulfur components and fatty acids)to give insoluble combinati
28、ons.These com-binations are removed from the distillate by filtration when they reach the hydrometer port.The coil has two i TO THE :._._ C O I L J I 1 rh I 300 USG i COLD WATER l,l i,l,!,II ij,iJi,Fig.9.(F)Condenser(condenseur).(Courtesy of R.Prulho,Cognac.)i lilll HIIIlillli II 11 HYDROMETER PORT
29、d J Fig.10.(G)Hydrometer port(porte-alcoolmetre).(Courtesy of R.Prulho,Cognac.)functions:to condense the vapors and to cool the distil-late to proper temperature for filtration.At the begin-ning of the coil,to facilitate the condensation,the coil has a larger diameter.Progressively,the coil diameter
30、 becomes smaller until it reaches the hydrometer port(Fig.8).Condenser(condenseur)(F):This is a cylindrical tank made of copper or stainless steel which contains the copper coil pipe.Its capacity is around 1300 gallons.The condenser is filled with water during distillation.Cold water enters the cond
31、enser at the bottom,while the hot water,heated during the condensing process,exits off at the top of the condenser.(Fig.9).Hydrometer port(porte-alcoomtre)(G):The hy-drometer port is also made of copper and has several purposes:to filter the distillate,to monitor the tempera-ture,to monitor the alco
32、hol content of the future Cognac or brandy,to offer an access point for the distiller,and to check the progress of the distillation(Fig.10).Heads tank(H):This is a small stainless tank(15 gal capacity)used to collect the first part of the distillate,Am.J.Enol.Vitic.,Vol.41,No.1,1990 94-ALAMBIC DISTI
33、LLATION called the heads.Gas burner(I):The gas burner is equipped with a pilot light and a reliable security system.The most commonly used fuels are propane,butane,and natural gas.The gas panel to monitor the burner is located at the front of the alambic.Under the boiler,the temperature reaches 1400
34、F to 1600F.This high temperature is essential to heat and cook the wine to create aromas during thedistillation process.(Fuel usage:450 pounds of liquid propane is required to produce 100 gallons pure alcohol of Cognac or brandy).Processing Aspects Theory of distillation in the case of batch distill
35、ation:Distillation is the technique used to sepa-rate and select,by use of heat,specific volatile compo-nents from a liquid mixture(e.g.,wine).Laboratory still:The mixture(e.g.,wine)is loaded into the boiler and heated by a gas burner for partial vaporization.The vapor is condensed and then collecte
36、d into one or a series of fractions.All of these fractions are called distillate(Fig.11).Vapors/Fig.11.Laboratory still.173.3F(78.5C)PART PART,A B(_.i(-!i i i i i i i C2H50H(100%)96%C O G N A C DISTILLATION 212F ioooc)H20(100%1 _J Fig.12.Vapor-liquid equilibrium diagram of water/alcohol mixture.DI S
37、TI LLATI ON DI STI LLATI ON MIXTURE A MIXTURE B 10%ALC./VOL.2 8%ALC./VOL.MIXTURE C 7 0%ALC./VOL.r Fig.1 Hot water ndenser.f-Colcl water.(i)O 3.Double distillation technique eog,!,t,l i i,I|I C2H50H WI Distillate 96%60%(10%1 FIRST FRACTION OF THE DISTILLATE 212F(I00C)Fig.14.First distillation diagram
38、.INE H 2 0(100%)ALC./VOL.)Binary distillation.Wateralcohol equilibrium:Wines can be considered roughly as a mixture which contains mainly water and alcohol.The boiling points at atmospheric pressure(760 mm)of water and alcohol are:water,212F(100C);alcohol 173.3F(78.5C).This mixture is homogeneous be
39、cause only one liquid phase is present.In addition,it is a binary azeotrope with a minimum boiling(Fig.12).During the Cognac distillation,the alcohol content of the distillate always stays below 96%alcohol by volume(max.80%(alc/vol).The Cognac distillation only takes place in the part(B)of the diagr
40、am.In this case,the vapor-liquid equilibrium diagram is like a single-phase binary mixture.Double distillation technique:The first mixture,A,IIkPOR,I I C2H!O H 96%I I I,I I I I I!o BROUILLIS 78%(28%ALC./VOL.)FIRST FRACTION OF THE DISTILLATE Fig.15.Second distillation diagram.212F 100C)120 100%Am.J.E
41、nol.Vitic.,Vol.41,No.1,1990 ALAMBIC DISTILLATION-95 is distilled to produce a second mixture B.When mix-ture B is sufficient in volume,mixture B is then distilled to produce mixture C.This is known as the double distillation technique(Fig.13,14,15).The double distillation.Variations of the alco-hol
42、content:Example:wine at 10%(alc/vol).First distillation:The distillate is cut into three HEART TAILS 6O HEADS 5 0 STARTING UP i I I I I!I!i!H I;(BROu I-LL IS),TAILS I I-,;TIME 8(HOURS)END _/Y DISTILLATE Fig.16.First distillation(wine).%ALC.78 75 6O!HEART I b-,.(COGNAC),HEADS ,I _ L 0 STARTING UP I I
43、 I I i I I I I I HEART 2 I I(SECONDES)I I TAI I I p,.T I ME 3(HOURS)END/%ALC.DISTILLATE Fig.17.Second distillation(brouillis).CONCENTRATION ,I I!I i I I I I i :,i I I,i t.;,.,TA I LS TIME Fig.18.Distillation curve(Type 1).Examples:acetaldehyde,ethyl acetate.CONCENTRATI ON I I i TIME Fig.19.Distillat
44、ion curve(Type 2).Examples:ethyl caproate,isoamyl acetate,ethyl caprylate,ethyl caprate,ethyl laurate.CONCENTRATION I,HEADS:1 i I I I i i I i i TAI LS TIME Fig.20.Distillation curve(Type 3).Examples:methanol,isobutanol,methyl-2-butanol and methyl-3-butanol.CONCENTRATION I i!HEADS I I I!i/j-ART:TAILS
45、 I TIME Fig.21.Distillation curve(Type 4).Examples acetic acid,2-phenyl ethanol,ethyl lactate,diethyl succinate.CONCENTRATION!HEADS I HEART I I t i I I/i TAILS/;Fig.22.Distillation curve(Type 5).Example furfural.v TIME Am.J.Enol.Vitic.,Vol.41,No.1,1990 96 mALAMBIC DISTILLATION fractions:heads,heart
46、or brouillis,and tails.The alco-hol content of the distillate is around 60%(alc/vol)in the first fraction and reaches 0%(alc/vol)at the end of the first distillation(Fig.16).Second distillation:The distillate is cut into four fractions:heads;heart 1,or Cognac(or brandy);heart 2 or secondes;and tails
47、.The alcohol content of the distil-late is around 80%(alc/vol)in the first fraction and reaches 0%(alc/vol)at the end of the second distillation(Fig.17).Distillation of volatile compounds of wines:The wines contain approximately 300 volatile com-pounds,and except for water and alcohol,it is very com
48、plex to calculate the volatility coefficient K for each of them.How the volatile compounds distill:Each volatile component will distill following three criteria:boiling point,relationship with alcohol or water,and the vari-ation of alcohol content in the vapor during the distilla-tion.With respect t
49、o the relationships with alcohol or water,there are several possibilities:(1)the component is completely or partly soluble in alcohol and will distill when the vapor is rich in alcohol;(2)the component is soluble in water and will distill when the vapor is low in alcohol;(3)the component is soluble
50、in both alcohol and water and will distill throughout the entire distillation;or(4)the component is not soluble in water,but the water vapor will carry over this component(hydrodistil-lation).Classification of volatile compounds(in the case of the first distillation):Type 1 components(which distill