FRUIT BRANDY PRODUCTION BY BATCH COLUMN ...

Blackwell Science, LtdOxford, UKJFPEJournal of Food Process Engineering0145-8876Copyright 2005 by Food & Nutrition Press, Inc., Trumbull, Connecticut.2815367Original Article FRUIT BRANDY PRODUCTION BY REFLUX DISTIL- 

LATIONM.J. CLAUS and K.A. BERGLUND 

FRUIT BRANDY PRODUCTION BY BATCH COLUMN 

DISTILLATION WITH REFLUX 

MICHAEL J. CLAUS 1,3 and KRIS A. BERGLUND 1,2,3,4,5 

Departments of 1 Biosystems & Agricultural Engineering, 2 Chemical Engineering & 

Materials Science and 3 Chemistry 

Michigan State University 

East Lansing, MI 48824 

4 Division of Biochemical and Chemical Process Engineering 

Luleå University of Technology 

SE-971 87 Luleå, Sweden 

Accepted for Publication August 12, 2004 

ABSTRACT 

The relationship between the operating parameters of batch fruit spirits 

column stills with reflux and the congener (trace compounds that provide 

flavors and aromas) concentrations in resulting fruit spirits has not been widely 

studied. Congener concentrations were determined in three different collection 

fractions, or “cuts,” during batch distillation. Acetaldehyde and ethyl acetate 

were found in higher concentrations in the head cut, first overhead fraction, 

of the distillation and have lower boiling points relative to ethanol. 1-Propanol 

and isoamyl alcohol (isopentanol) were present in higher concentrations in 

the tail cut, third or final fraction, of the distillation and have boiling points 

that are higher than ethanol. Methanol has a unique concentration profile as 

it has higher concentrations in both the head and tail cuts, but a lower 

concentration in the heart cut, the middle fraction which is the desired product 

of the distillation. Methanol was of particular interest because the distillate 

must adhere to governmental regulations that limit its concentration in the 

product. Operating-condition parameters that were studied include the number 

of trays used in the distillation as well as the use of a “catalytic converter,” 

a high surface, copper-packing material thought to catalyze formation of 

cyanide-containing compounds allowing them to be separated from the distillate. 

The effect of the number of trays used in a distillation on the concentration 

of ethanol and the congeners, methanol, acetaldehyde, ethyl acetate, 

1-propanol and isoamyl alcohol in the final distilled spirits product is presented. 

An additional result of acetaldehyde production at the copper surface 

of the catalytic converter was also discovered in the analysis of the data. 

5 Corresponding author. TEL: +46-920-493070; FAX: +46-920-491199; EMAIL: kris.berglund@ltu.se 

Journal of Food Process Engineering 28 (2005) 53–67. All Rights Reserved. 

© Copyright 2005, Blackwell Publishing 53

54 M.J. CLAUS and K.A. BERGLUND 

INTRODUCTION 

The two competing styles of fruit-brandy distillation are alambic – used 

to produce cognac, i.e., the French style and column distillation – used to 

produce fruit spirits, the German style. Alambic stills have no trays or appreciable 

reflux and require multiple distillations to achieve high-proof spirits. 

The distilled spirits are usually stored in wood for many years prior to bottling 

and sale. Column stills used to produce eau-de-vie or schnaps feature a 

batch still with a reflux column. A single pass through this type of still results 

in high proofs. These spirits are usually stored in glass and served as waterclear 

brandies. Typically fruit brandies, with the exception of Calvados 

(apple brandy) from Normandy, are produced in the German style because it 

tends to preserve the delicate fruit essences. In the United States the fruitspirits 

industry is a small but growing industry. In Michigan alone, the number 

of fruit-spirits stills has increased from zero in 1996 to seven in 2002. 

Although fruit-brandy production is well established in Europe, there are 

challenges to the U.S. industry that differ from its European sibling. Compounds 

such as methanol and urethane (ethyl carbamate) are regulated in 

many countries, but the regulations differ (Tanner and Brunner 1982). Methanol 

is currently regulated in the United States as 0.35% v/v ethanol in fruit 

spirits (United States Code of Federal Regulations), whereas urethane is 

regulated as a possible carcinogen in Canada at 400 ppb (Zimmerli and 

Schlatter 1991). Regulations for methanol in Europe are at higher values; 

therefore, methanol control has not been as much of a concern there (Tanner 

and Brunner 1982). 

It is widely known that as more trays are used in distillation, a greater 

separation of components is possible (Tanner and Brunner 1982; Postel and 

Adam 1989; Leaute 1990; Wankat 1998). However, many of these components 

are also positive-flavor components in the fruit spirits (Postel and Adam 

1989). The concentration of congeners must meet the imposed regulatory 

limits while at the same time offering a pleasant smelling and tasting product. 

Fruit-spirits production consists of four basic steps: fruit preparation 

(mashing), fermentation, distillation and storage (Tanner and Brunner 1982). 

The fruit is crushed by mechanical means using either a rolling mill or a 

progressing cavity pump, both of which crush the pulp of the fruit while 

keeping most (~ 90%) of the pits – in the case of stone fruits – from being 

cracked. Cracked stone-fruit pits increase the amount of urethane and benzaldehyde 

in the spirits because the pits contain amygdalin, a complex of cyanide, 

benzaldehyde and glucose (Tanner and Brunner 1982). Benzaldehyde is a 

positive-flavor compound, and is commonly known as bitter-almond oil, but 

urethane is a suspect carcinogen (Zimmerli and Schlatter 1991). The resulting 

mash is transported to a fermenter, where it is stirred and cooled to a temper-

FRUIT BRANDY PRODUCTION BY REFLUX DISTILLATION 55 

ature between 15 and 20C. Yeast is dissolved in warm water and added to the 

mash to begin fermentation. The fermentation is allowed to proceed for 10– 

15 days and the brix (% soluble solids, weight basis) is measured, until the 

fermentation has reached completion. The fermented mash is distilled in a 

batch-column still with reflux in a single operation. The distillate is collected 

in volumes referred to as heads (discarded first fraction), hearts (product) and 

tails (discarded or redistilled last fraction), and the clear spirits are stored in 

glass at high (> 100) proof. The spirits can be stored for as little as 3 months 

prior to proof adjustment with water and bottling. 

MATERIALS AND METHODS 

A schematic diagram of a typical 165 L Christian-Carl column still is 

shown in Fig. 1. A volume of mash between 150 and 165 L is charged to the 

pot of the still, which is steam jacketed. A temperature sensor at the top of 

the condenser is attached to a flow regulator in the condenser which adjusts 

condenser-water flowrate in an attempt to maintain a temperature of 72C 

(Plank and Plank 1998–2001). The cooling water, which is preheated through 

Steam 

inlet 

Steam jacket 

Partial condensers 

Total condenser 

Copper packing 

Fermented mash 

To 

drain 

Stirrer 

Bottoms 

removal 

port 

Tray control 

levers 

Temperature 

sensor 

Cooling water 

control 

Water 

inlet 

To drain 

FIG. 1. SCHEMATIC OF A 165 L CHRISTIAN-CARL STILL 

Distillation vapor path 

Cooling water path 

Catalytic 

converter 

Distillate 

discharge


the condenser, then passes into one of the dephlegmators, depending on the 

valve position. The dephlegmators are partial condensers that utilize the cooling 

water from the top of the main condenser, which has been partially heated 

by the distillate through the condenser. Usually the dephlegmator at the top 

of the second column is utilized. The trays are sieve trays constructed of 

copper equipped with a bypass that consists of a manually-operated plug. The 

tray-control levers, as seen in Fig. 1 control these plugs. When closed, the 

condensate will collect on the trays and the vapor from the lower tray must 

pass through the holes and therefore through the reflux condensate, causing 

rectification and therefore more efficient separation of the different components 

(Wankat 1998). 

The distillation was initiated by adding a 150 L charge of fruit mash into 

the pot of the still. Cooling water was circulated through the entire system 

before distillation began. The number of trays to be used was fixed as well as 

if the “catalytic converter” was to be engaged (this “catalytic converter,” 

consists of a high-surface area, copper-packing material thought to catalytically 

react cyanide-containing compounds with ethanol to form urethane 

[ethyl carbmate] and improve its separation from the product cut [Postel and 

Adam 1989]). Steam in the jacket of the pot was at a gauge pressure of 

0.3–0.4 bar and kept constant for the duration of the distillation. The still was 

equipped with a stirrer to keep the fruit mash from cooking at the heat-transfer 

surfaces in the pot portion of the still, which could result in undesired flavor 

compounds in the distillate, and make cleaning more difficult. The distillate 

was collected as three 400 mL cuts, and then as 1000 mL cuts until the alcohol 

concentration was below 50% alcohol by volume (A.B.V.) by hydrometer. A 

cut of 1000 mL was then collected as a tails cut. The tails cuts were put into 

a collective tails container that is saved for later redistillation. This distilled 

tails produces a lower-quality spirits that is adequate for blending with other 

higher-quality spirits or wines, but often contains too high a concentration of 

off flavors for consumption on their own. The total volume collected varied 

from run to run due to the differences in operating conditions. 

Fruit spirits are usually marketed between 40–45% A.B.V. (United States 

Code of Federal Regulations). Results are presented as the concentration of 

the congeners as percentage (v/v) or volume of congener per volume of 

ethanol in a 40% ethanol solution. Volume calculations for the ethanol produced 

from the distillation were based on the 40% A.B.V. concentration of 

ethanol. 

Ethyl-alcohol concentrations were measured by a tralles (% alcohol as 

well as proof) hydrometer with an internal thermometer for temperature corrections 

(Tanner and Brunner 1982). A sample from each cut was analyzed 

by gas chromatography. Analyses were conducted with a Shimadzu GC-17A 

gas chromatograph equipped with flame-ionization detection and a Stabilwax


FIG. 2. SAMPLE CHROMATOGRAPH FROM A CHERRY EAU-DE-VIE DISTILLATION 

A Restek 30 m Stabilwax column with 0.25 mm i.d was used for analysis. 

The initial conditions had the column temperature at 40C, injector-port temperature at 240C and 

detector temperature of 255C. 

The analysis included a ramp from 40C to 190C at 2.5C/min. 

30 m column with an inner diameter of 0.25 mm (Restek). The initial conditions 

for the chromatographic analysis were column temperature at 40C, 

injector-port temperature of 240C and detector temperature at 255C. The 

temperature program used for the analyzes was a start-column temperature of 

40C which was ramped at 2.5C/min until a temperature of 190C was reached. 

The temperature was held at 190C for 5 min. A Shimadzu autosampler 

(AOC-20i) was used to obtain reproducibility of the 0.2 mL injection volume. 

Figure 2 is a sample chromatograph and Table 1 shows the relative retention 

times of the most common compounds in the fruit spirits, as well as their 

respective boiling points. 

RESULTS AND DISCUSSION 

Ethanol, methanol, acetaldehyde, ethyl acetate, isoamyl alcohol and 

1-propanol were chosen for monitoring because they are the compounds in 

highest concentrations as well as often studied for their flavor characteristics 

in the fruit spirits (Stinson et al. 1969a,b; Guymon 1972; Suomalainen and


TABLE 1. 

RELATIVE RETENTION TIMES FOR THE MOST COMMON COMPOUNDS IN DISTILLED 

FRUIT EAU-DE-VIES 

Chemical name Retention time (min) Boiling point (C) 

Acetaldehyde 2.5 20.8 

Acetone 3.4 56.2 

Ethyl formate 3.6 54.0 

Ethyl acetate 4.5 77.0 

Methanol 4.7 64.7 

Ethanol 5.8 78.0 

1-propanol 8.7 97.0 

Isopentanol (isoamyl alcohol) 16.3 132.0 

Benzaldehyde 33.0 179.0 

Source: Plank and Plank 1998–2001. 

Lehtonen 1979; Postel and Adam 1989). The first set of experiments explored 

the effect of the number of trays on the ethanol concentration in the resulting 

product. The second set of experiments explored how the number of trays 

affected the concentration of congeners in the product. Sampling of the spirits 

occurred at the time of distillation and the samples were run on the GC-FID 

within 36 h of collection. 

Two fermentations of Stanley plums, which were frozen for six months 

and thawed prior to fermentation, were studied for the effects of ethanol 

concentration as the number of trays were changed. Also the effect of the 

catalytic converter was studied for its effect on the ethanol concentration. 

These spirits are usually bottled in 375-mL bottles and the results are presented 

in total volume of 40% ethanol as well as number of 375-mL bottles 

of 40% ethanol. Each distillation contained the same volume of mash from 

the fermentation. Overhead product was collected with 1200 mL of heads (in 

three 400 mL volumes) and volumes of 1000 mL of hearts until a concentration 

of

Ethanol conc. (% v/v) 

90 

80 

70 

60 

50 


0 2000 4000 6000 8000 

Cumulative distillate volume (mL) 

1 2 3 4 

FIG. 3. THE AVERAGE CONCENTRATION OF ETHANOL (% V/V) WITH VARYING 

DISTILLATION CONDITIONS 

(1) All three trays used and catalytic converter engaged. (2) All three trays used with no catalytic 

converter. (3) Two trays used with catalytic converter engaged and (4) Two trays used with no catalytic 

converter. A single fermentation of plum mash was divided into four distillations for these results. 

Operating conditions 

0 5 10 15 20 25 30 

Number of 40% A.B.V. bottles 

1 2 3 4 

FIG. 4. TRANSLATION OF THE DATA IN FIG. 3 INTO BOTTLES OF 40% ETHANOL, PLUM 

BRANDY AT THE FOUR DIFFERENT OPERATING CONDITIONS 


converter. (3) Two trays used with catalytic converter engaged and (4) Two trays used with no 

catalytic converter.


Acetaldehyde concn. 

(% v/v) 

0.9 

0.6 

0.3 

0 

0 2100 4200 6300 


1 2 3 4 

FIG. 5. ACETALDEHYDE PROFILE: CONCENTRATION OF ACETALDEHYDE IN CHERRY 

DISTILLATES AS A FUNCTION OF CUMULATIVE VOLUME OF DISTILLATE AT FOUR 

DIFFERENT OPERATING CONDITIONS 



converter. A single cherry fermentation divided into four distillations to obtain these results. 

harvest and thawed prior to mashing and fermentation were used. The congeners 

studied were acetaldehyde and ethyl acetate (low-boilers); methanol 

because of its regulation; and 1-propanol and isoamyl alcohol (high-boilers). 

These components are the five congeners present in the highest concentration. 

Acetaldehyde is the main component emerging before methanol in the 

distillation of cherry spirits. It has a distinctive aroma characteristic, which 

can cause an eau-de-vie to have a poor aromatic characteristic when present 

in too high concentration (Stinson et al. 1969a). As acetaldehyde has a low 

boiling point, its largest concentration is distilled into the heads portion of the 

distillate. However, when fewer trays are used, a larger concentration proceeds 

into the hearts portion of the distillate. Acetaldehyde is completely soluble in 

both water and ethanol; therefore, it is not easily separated from the spirits. 

A plot of the acetaldehyde profile can be found in Fig. 5. After acetaldehyde, 

ethyl acetate is the most abundant of the minor components of cherry distillates 

boiling before methanol (Stinson et al. 1969a). Ethyl acetate has a similar 

profile to that of acetaldehyde, as can be seen in Fig. 6. 

Methanol is a health hazard that is regulated in the U.S.A. at 0.35% 

(v/v) in distilled spirits (United States Code of Federal Regulations). The 

amount of methanol produced in the hearts was just above this level. The 

methanol profile exists such that the methanol concentration is higher in

Ethyl acetate concn. (% v/v) 

0.5 

0.4 

0.3 

0.2 

0.1 

0 


0 2100 4200 6300 


1 2 3 4 

FIG. 6. ETHYL ACETATE PROFILE: THE CONCENTRATION OF ETHYL ACETATE IN 

CHERRY DISTILLATES AS A FUNCTION OF CUMULATIVE VOLUME OF DISTILLATE 

UNDER FOUR DIFFERENT OPERATING CONDITIONS 




the heads, drops in the hearts to a lower concentration, and then increases 

again in the tails. Of the compounds examined, methanol has a unique distillation 

profile. Figure 7 shows the methanol-concentration curves per cumulative 

distillation volume for the operating conditions used. The distillation 

profile of methanol in this type of multistage-batch distillation is different 

than it would be for an alambic-style distillation (Suomalainen and Lehtonen 

1979). It is important to test each cut to minimize the methanol concentration 

in the hearts cut. Methanol is considered by many to be a positive-flavor 

constituent in distilled spirits. It is difficult to separate the methanol from the 

ethanol-water mixture further without loss of many of the other flavor components 

from the distillate. The concentration must be below 0.35% (v/v) but 

it is desirable to have the concentration close to regulatory limit, as it is a 

positive-flavor component. 

Fusel alcohols compose the largest group of aroma compounds in alcoholic 

beverages (Stinson et al. 1969b). Isoamyl alcohol (3-methyl-1-butanol) 

is the main fusel alcohol synthesized during fermentation by yeast. 1-Propanol 

is considered as another important fusel alcohol, as it is the simplest alcohol 

larger than ethanol (Stinson et al. 1969b; Suomalainen and Lehtonen 1979).


Methanol concn. (% v/v) 

0.55 

0.45 

0.35 

0.25 

0 2100 4200 6300 


1 2 3 4 

FIG. 7. THE CONCENTRATION OF METHANOL IN CHERRY DISTILLATES AS 

A FUNCTION OF CUMULATIVE VOLUME OF DISTILLATE UNDER DIFFERENT 





However, these two compounds distill earlier than most of the other fusel 

alcohols and therefore they are considered to be early indicators of the balance 

of the remaining fusel alcohols. The fusel alcohols produce a “damp cloth” 

aroma that is undesirable in the production of spirits. 1-Propanol and isoamyl 

alcohol are present in the hearts in small quantities, and increase in concentration 

at the end of the hearts cut and begin to decrease in the tails. Most 

fusel alcohols will be present in greater concentrations in the tails than in the 

hearts. Measuring the presence of 1-propanol or isoamyl alcohol on line would 

allow for an easier determination of where to make the hearts/tails cut. A plot 

of the concentration of isoamyl alcohol and 1-propanol per distillation volume 

can be seen in Figs. 8 and 9, respectively. 

Figure 10 shows the concentration of acetaldehyde, ethyl acetate, methanol, 

1-propanol and isoamyl alcohol as they would exist when the distillate 

was diluted to 40% ethanol. A higher number of trays produced a lower 

concentration of acetaldehyde in the distillate, although the catalytic converter 

seemed to increase the amount of acetaldehyde in the hearts of the distillate. 

The isoamyl alcohol shows the effect of the trays on the congeners with 

boiling points greater than ethanol. The more trays that were used resulted in 

a reduced concentration of congener. This is useful for controlling the fusel 

alcohols as they have an undesired aroma characteristic.

Isoamyl alcohol concn. 

(% v/v) 

0.24 

0.16 

0.08 


0 

0 2100 4200 6300 


1 2 3 4 

FIG. 8. ISOAMYL ALCOHOL CONCENTRATION IN CHERRY DISTILLATES AS A 

FUNCTION OF CUMULATIVE VOLUME OF DISTILLATE UNDER FOUR DIFFERENT 





1-Propanol concn. (% v/v) 

0.35 

0.25 

0.15 

0.05 

0 2100 4200 6300 


1 2 3 4 

FIG. 9. 1-PROPANOL CONCENTRATION IN CHERRY DISTILLATES AS A FUNCTION OF 

CUMULATIVE VOLUME OF DISTILLATE WITH DIFFERENT OPERATING CONDITION 



converter. A single cherry fermentation divided into four distillations to obtain these results.


Congener concn. (% v/v) 

0.4 

0.3 

0.2 

0.1 

0 

Acetaldehyde Ethyl acetate Methanol 1-propanol Isoamyl alcohol 

Congener 

1 2 3 4 

FIG. 10. CONGENER CONCENTRATION IN DRINKING STRENGTH EAU-DE-VEUX (40% 

ETHANOL v/v) PRODUCED BY BLENDING AND DILUTION OF HEART CUTS 




Overall most compounds with a higher boiling point (than ethanol) will 

have a profile that contains smaller concentrations of congener in the heads 

and early hearts and then the concentration will increase in the latter hearts 

and tails. The compounds that have lower boiling points (than ethanol) tend 

to have higher concentrations in the heads and early hearts and the concentration 

steadily decreases throughout the distillation process. Methanol has a 

distillation profile different from most of the other congeners. Methanol tends 

to have a higher concentration in the heads and tails than it does in the hearts. 

Because in these fruit spirits the concentration of methanol is so close to the 

regulatory limit of 0.35% v/v one must be careful as to where to take one’s 

cuts. 

The presence of the catalytic converter affected the amount of the congeners 

in the distillate. One explanation for the concentration differences in 

runs with this device from those without it is that the device acts as an 

additional tray. However, upon inspection, the copper packing in the device 

was visibly corroded after three of four distillations. The corroding material 

is probably a mixture of congeners that have condensed on the copper surface 

and adhered to the copper surface over time. The surface can be cleaned with 

a dilute citric acid solution, but the effectiveness of the device will need to be 

further studied.


TABLE 2. 

ACETALDEHYDE CONCENTRATIONS PRESENT IN A DISTILLATION OF 5% ETHANOL 

UNDER TWO DIFFERENT DISTILLATION CONDITIONS, WITH CATALYTIC CONVERTER 

AND WITH THE CATALYTIC CONVERTER BYPASSED 

Cumulative volume (mL) Acetaldehyde concentration (% v/v) 

No catalytic converter Catalytic converter used 

500 None detected None detected 

1000 None detected 0.00287 







A further look at the acetaldehyde profile in Fig. 5 reveals a slight 

increase in acetaldehyde concentration in the latter parts of the distillation 

when the catalytic converter was engaged. The formation of acetaldehyde on 

the copper surface as a dehydrogenation product from ethanol was postulated. 

Dai and Gellman have demonstrated the formation of acetaldehyde on copper 

surfaces during the heating of alcohols (Dai and Gellman 1993). A distillation 

of a pure 5% ethanol solution with both the catalytic converter engaged, and 

bypassed, was conducted to see if the acetaldehyde were being produced from 

the ethanol, or another source in the fermentation. The chromatography of the 

cuts taken resulted in peaks for ethanol and acetaldehyde when the catalytic 

converter was engaged, and only a peak for ethanol when the catalytic converter 

was bypassed. The acetaldehyde concentrations can be seen in Table 2, 

with the resulting distillate volume for each cut taken. 

CONCLUSION 

The concentration profiles for ethanol, methanol, acetaldehyde, ethyl 

acetate, 1-propanol and isoamyl alcohol were measured for different operating 

conditions in fruit-spirits distillation. Methanol was shown to have a unique 

distillation profile that did not simply track boiling point as is generally the 

case for other congeners. Use of all the trays increased the concentration of 

the ethanol while decreasing the concentration of the congeners in the product. 

The catalytic converter was shown to act as an additional tray for the


distillation process; however, the catalytic converter promoted formation of 

acetaldehyde during the distillation procedure. 

ACKNOWLEDGMENTS 

The authors wish to thank the financial support of Project Generating 

Research and Extension to meet Environmental and Economic Needs 

(GREEEN) from the Michigan Department of Agriculture and the Michigan 

Agricultural Experiment Station. In addition, the United States Department of 

Agriculture, the Cherry Marketing Institute and Michigan Horticultural 

Society are thanked for their support. 

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