Article

pubs.acs.org/JAFC

Effects of Operating Conditions during Low-Alcohol Beer Production

by Osmotic Distillation
Giovanni De Francesco,*,† Gary Freeman,‡ Eung Lee,‡ Ombretta Marconi,§ and Giuseppe Perretti†
†
Department of Agricultural, Food and Environmental, University of Perugia, Via San Costanzo, 06126, Perugia, Italy
‡
Campden BRI, Coopers Hill Road, Nutfield, Surrey, RH1 4HY, United Kingdom
§
Italian Brewing Research Centre, University of Perugia, Via San Costanzo, 06126, Perugia, Italy

ABSTRACT: Osmotic distillation (OD) is a membrane technology most commonly used for liquid concentration, but recently
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there has been an increased interest in ethanol removal from alcoholic beverages. The aim of this paper is to investigate the effect
of the variation of some operating conditions (temperature, flow rate, type and amount of stripping solution), specifically in
regard to the effect on quality and sensory properties of the dealcoholized beers. The results indicated that temperature and flow
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rate variation showed no significant effect, whereas stripping solution variation had substantial effects mainly in terms of the
ethanol removed. A cost appraisal showed that the operating costs were high mainly because of the cost of the stripping water.
However, it is important to consider the final stripping solution, which is slightly alcoholic and enriched in flavor. For this reason,
it could be reused in the manufacture of beverages, for instance as high gravity beer dilution water.
KEYWORDS: Beer, beverages, dealcoholization, low-alcohol beer, osmotic distillation

■ INTRODUCTION
The production of low-alcoholic beverages (or low-alcohol
fermented beverages, typically defined as containing less than
1.2% v/v) is an established option for a food industry looking
for alternatives to the soft drink. Low-alcohol beer is still a small
percentage of the output of the brewing industry, but recently
there is a significant growth of this product, reflecting the global
trend for a perceived healthier lifestyle.1,2 The current
increasing demand for low-alcohol and alcohol-free beers is
attributable to various factors such as health, diet, safety, or
prohibition of alcohol consumption caused by labor protection
laws. There are also countries (such as Islamic countries) where
alcohol consumption is completely prohibited by law.2,3 Low-
alcohol and alcohol-free beers are also recommended for
specific groups of people such as pregnant women, sporting
professionals, people with cardiovascular and hepatic patholo-
gies, and medicated people.4−8
The legal definition of low-alcohol and alcohol-free beer
varies from one country to another. For instance, Italian
regulations refer to nonalcoholic beer as a product having 3−8
degrees Plato (g of extract/100 g of wort) with an alcoholic
content less than 1.2% v/v. In Europe, a nonalcoholic beer or
alcohol-free beer will usually have a final alcohol by volume
content lower than 0.5% v/v, whereas a low-alcohol beer
ethanol content is between 0.5 and 1.2% v/v.9 A large number
of factors influence beer characteristics during production of
low-alcohol or alcohol-free such as variety of barley and the
malting process, temperature and pH during mashing, sparging,
variety of hops added, and storage conditions.10 Therefore, the
main challenge in the production of low-alcohol and alcohol-
free beers is to manufacture a product that resembles as far as
possible regular beer, which is very difficult to realize. It is for
these reasons that low-alcohol and alcohol-reduced beverages
have received increased technological and economic atten-
tion.11
There are two main strategies to produce reduced alcohol
beer. First, there are physical methods such as dialysis,12 reverse
osmosis,13 vacuum rectification and evaporation, 14 or spinning
cone column distillation.15 Second, there are biological
methods such as controlled (suppressed) alcohol formation1
and use of special yeasts.16 The most common way to make
nonalcoholic beer is arrested fermentation in order to keep the
ethanol content very low.17 This method is the most simple and
uses the same resources as does a standard beer fermentation.
However, it has a drawback related to beer quality, mainly
caused by the lack of reduction in concentration of certain wort
compounds and by a poor development of important beer
flavors. Thus, the final product presents a typical worty flavor
and a thin mouthfeel that is very different from standard
alcoholic beers.18−20 The physical methods also have
advantages and disadvantages. The most important advantages
are the possibility of reaching an ethanol content of 0.05% v/v,
and some technologies employ low temperature and low
pressure during dealcoholization. The most important dis-
advantages are the high operating costs, loss of volatile
compounds, capital expenditure on the specialized process
equipment, and a risk of thermal damage to delicate
compounds. Relevant organoleptic and sensory characteristics
of the nonalcoholic beer include flavor, color, foaming
properties, body, viscosity, mouthfeel, and colloidal stability,
much the same as for normal beer.11
Beer is a complex alcoholic beverage as it contains many
organic compounds that contribute to its taste, aroma, and
mouthfeel. However, it must be pointed out that it is well
understood that the alcohol has a significant impact on the beer
Received: December 12, 2013
Revised: March 12, 2014
Accepted: March 12, 2014
Published: March 12, 2014

© 2014 American Chemical Society 3279 dx.doi.org/10.1021/jf405490x | J. Agric. Food Chem. 2014, 62, 3279−3286
Journal of Agricultural and Food Chemistry
Figure 1. Model of the dealcoholization lab unit used (feed, beer tank; P1 and P2 peristaltic pumps; MC, membrane contactor; CS, cooling system;
SS, stripping solution tank; V1−V6; manual valves; T, temperature controllers; P1−P6, pressure gauges.
flavor. Therefore, low-alcohol or alcohol-free beers produced by
the technologies applied up to now will at best reach only
approximately the high sensory quality of a “normal” beer.
Nevertheless, these beers make up distinctive, high-quality
products, which have earned significance in the market.21
The sensory quality of beer depends on the complex balance
of flavor-active components. In many cases, the dealcoholiza-
tion could negatively affect the organoleptic quality of beer,
leading in some cases to the unacceptability of the product. The
low-alcohol and alcohol-free beers are required to meet certain
quality conditions regarding their stability and sensory features,
which should be comparable to those of normal beers. It is
likely that the sensory qualities of the beer will change over the
course of the dealcoholization, where a loss of aroma, body, and
flavor can be seen.22 A reduced foaming property (especially
foam head retention) is another drawback. This issue is also
related to the lack of ethanol, which improves foamability and
foam stability in the range of 1−3.5% v/v.23 In any case, the
addition of glycerol or other sugar alcohols can reinforce the
foaming properties of beer.24,25
Principle of Osmotic Distillation. Osmotic distillation
(OD) or evaporative pertraction (EP) is a membrane process
used for removing ethanol from beverages, especially for wine
partial dealcoholization. This membrane technology has been
presented as a novel and promising technology to reduce the
ethanol content in alcoholic beverages without unacceptably
altering the organoleptic properties of the product.26,27 OD
uses hydrophobic porous membrane contactors to provide the
ethanol transfer from beer to stripping solution (usually water).
In this process water and beer flow countercurrently. The
mechanism is similar to membrane distillation,28 but in this
case, the process is carried out at ambient temperature,26 in
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Article
which the partial pressure gradient due to the high relative
volatility compared to water is the driving force for ethanol
transport. Due to this mechanism the OD has also been defined
“isothermal membrane distillation”29 and in some specific cases,
such as dealcoholization, the term evaporative pertraction is
more precise.30 OD is a form of dialysis, in which a liquid
mixture containing a volatile component is contacted with a
microporous, non-liquid-wettable membrane whose opposite
surface is exposed to a second liquid phase capable of absorbing
that component. The most important difference compared to
more common liquid−liquid contacting processes (such as
reverse osmosis) is the membrane’s composition, which is
porous and hydrophobic and typically made of PTFE or
polypropylene.31 The most important advantages of the
membrane contactors are well-defined and constant interfacial
area, high interfacial area in small volumes, small size and
weight, no dispersion between phases, no need of phase
separation downstream, no need to work with fluids of different
densities, no flooding, loading, or foaming, wide range of
operating flow-rates, flow-rates can be varied independently,
and lower operating temperatures compared to distillation
processes. The most important drawbacks are membrane
fouling, pressure drop caused by the membrane unit,
membrane lifetime, and a high stripping solution volume
requirement.32−35 The transport mechanism of ethanol by OD
process can be divided into three steps: (i) evaporation of
ethanol at the membrane pores on the feed side, (ii) diffusion
of ethanol vapor through the membrane pores, and (iii)
condensation of ethanol vapor in the stripping solution at the
membrane pore exit.36 The aim of this work was to investigate
both theoretically and experimentally the effects of the different
process parameters. The operating parameters which affect the
dx.doi.org/10.1021/jf405490x | J. Agric. Food Chem. 2014, 62, 3279−3286
Journal of Agricultural and Food Chemistry Article

ethanol content, such as flow rate, system temperature, and
types of stripping solutions, were investigated. Furthermore, the
quality parameters (present gravity, pH, color, turbidity, total
soluble nitrogen, CO2) and the losses of volatile compounds of
the beer were also monitored.
Experimental Conditions. The beer feed was maintained at 10, 15,
or 20 °C in separate trials, in order to investigate the effect of
temperature changing on separation efficiency. During these trials, the
stripping water temperature was kept at 10 °C. Similarly, different
amounts of stripping solution, 3, 4, 5, or 6 L were employed in

■
separate trials, while the beer volume was 1 L for each trial.
Furthermore, the effects of types of stripping solution, i.e. normal pure
MATERIALS AND METHODS water and carbonated water, were investigated. Moreover, different
Alcoholic beers of five different commercial brands were obtained. The flow rates of stripping solution were tested, namely 500 mL min−1 and
alcoholic beers contained between 3.5% and 5% v/v. The deal- 1 L min−1. Finally, different beer brands were employed to ascertain
coholization tests were carried out by a small pilot plant equipped with the effect of variations in e.g. membrane fouling, different volatile
a polypropylene hollow fiber membrane contactor (Liqui-Cel, concentrations, etc.
MiniModule 1.7 × 5.5, Membrana GmbH, Wuppertal, Germany) Membrane Cleaning. After dealcoholization, the membrane was
(Figure 1). The typical membrane surface area was 0.54 m2, with an cleaned by flowing filtered and deionized water in tubeside and in
approximate priming volume of 78 and 53 mL, for shellside and shellside without recycling for 15 min. Subsequently, a 0.5% (w/w)
tubeside, respectively. For the first trials the membrane operating and 30 °C NaOH solution was circulated for 30 min. Finally, the
parameters were as follows: beer inlet pressure 0.3 bar gauge, beer system was rinsed with RO water without recycling for 10 min and
outlet zero pressure (atmospheric), water inlet pressure 0.3 bar gauge, then it was dried in both tube and shell side by using nitrogen gas for
water outlet zero pressure, beer flow 500 mL min−1, and water flow 20 min according to manufacturer cleaning guidelines.
500 mL min−1. These parameters were subsequently adjusted in an
experimental matrix to ascertain optimum process (below). The
ethanol content of the beers and all quality parameters were
■ RESULTS AND DISCUSSION
Different Stripping Solution Volumes. The effect of the
determined in accordance with Analytica EBC.37 different ratios of stripping solution (deaerated water) to beer
The aromatic profile of the beer and corresponding dealcoholized
beer was analyzed by gas chromatography (Perkin-Elmer, Auto System
XL, Waltham, MA). The chemical standards (acetaldehyde, n-
propanol, 2-methyl-1-butanol, 3-methyl-1-butanol, ethyl acetate,
isoamyl acetate, ethyl hexanoate, diacetyl) used for the identification
and quantification of the volatile compounds of interest were
purchased from Sigma-Aldrich (Milwaukee, WI). The internal
standard for the determination of aldehydes and vicinal diketones, 2-
chlorobenzaldehyde (Sigma-Aldrich, Milwaukee, WI), was prepared
weekly in a solution of 5% ethanol with a concentration of 10 mg L−1.
The internal standard for determination of ethanol, higher alcohols,
and esters was 1-butanol (Sigma-Aldrich, Milwaukee, WI), which was
prepared weekly in water with a concentration of 60 mg L−1. The gas
chromatograph was equipped with an electron capture detector
(ECD) for the analysis of vicinal diketones (diacetyl and 2,3- Figure 2. Percent of ethanol removed using different ratios of beer/
pentanedione) and with a flame ionization detector (FID) for the stripping solution (% of original amount) after 4 h processing. Values
analysis of the other volatile compounds.The separation column was a with different superscript letters are statistically different (P < 0.05).
CP-WAX 57CB wall coated open tubular (WCOT) fused silica
column (polyethylene glycol stationary phase, 60 m × 0.25 mm i.d.
with 0.4 μm film thickness; Chrompack, Netherlands). Ten mL of the
beer samples was added to 500 μL of internal standard 2-
chlorobenzaldehyde (10 mg L−1) and 1 mL of the internal standard
1-butanol (60 mg L−1) in a 20-mL glass vial, which was heated for 30
min at 60 °C and stirred at 250 rpm for 30 s of every minute in order
to allow the volatilization and derivatization of the compounds of
interest. The injection was performed by means of a 2.5-mL headspace
syringe at 70 °C. The syringe was placed in the sample headspace to
draw the volatile compounds and to inject them in the gas
chromatograph. The injection volume was 1 mL. The front inlet
temperature was 150 °C. The injection was in the splitless mode with
the purge valve set at 20 mL min−1. Helium was the carrier gas at a
flow rate of 1.1 mL min−1. The oven temperature program used was 34 Figure 3. Decrease in ethanol during dealcoholization using different
°C for 2 min, followed by an increase of 45 °C min−1 up to 55 °C, the ratios of beer/stripping solution. (B: beer; DW: deaerated water).
held for 8 min, then raised to 98 °C at 5 °C min−1, and finally Values with different superscript letters are statistically different (P <
increased to 150 °C at 45 °C min−1. The detector temperature was 0.05).
200 °C.
Experimental Section. A series of experiments was performed to
ascertain optimum operation of the process. The feed and stripping feed in terms of ethanol flow transfer rate (mL min−1) and in
solutions were fed into the module by peristaltic pumps. The process terms of percentage of ethanol removed (%) was measured.
temperature was controlled by a water bath fitted with temperature The different stripping solution volumes (3, 4, 5, and 6 L)
controllers. Six pressure gauges for inlet and outlet were installed for noticeably influenced the percentage ethanol removed as shown
monitoring the pressure of the feed and stripping solutions. During
processes, the beer continuously circulated from a sealed container to in Figures 2 and 3. The matrix of experiments also included
the dealcoholization apparatus while water flowed counter-currently varying the feed beer temperature. The beer temperature (10
on the other side of the membrane (Figure 1). Beer ethanol content and 20 °C) did not significantly change the ethanol transfer rate
was monitored throughout the process until the target level was and ethanol removed (Figure 3). Furthermore, Figure 3 shows
achieved. that the process was essentially finished after 2 h; hence, it was
3281 dx.doi.org/10.1021/jf405490x | J. Agric. Food Chem. 2014, 62, 3279−3286
Journal of Agricultural and Food Chemistry Article

Table 1. Representative Volatile Compounds (mg L−1) and Loss Percentage (%) of Original and Dealcoholized Beer Using
Different Ratios of Beer/Stripping Solutiona
beer brand AA EA EH IAA n-prop 2-MB 3-MB DA
lager beer brand A 4.94 ab 18.35 b 0.10 1.91 d 8.55 f 9.61 e 49.53 f 0.03 a
B (1 L, 10 °C); DW (3 L, 10 °C) 2.78 a 5.34 a 0.01 0.47 bc 1.96 b 2.24 c 12.85 d 0.01 a
loss percentage (%) 43 A 70 A 87 74 A 77 B 76 AB 74 A 27 A
lager beer brand B 10.01 d 18.31 b 0.15 1.73 d 7.38 e 6.66 d 52.22 g 0.02 a
B (1 L, 10 °C); DW (4 L, 10 °C) 2.93 a 3.64 a N.D. 0.39 ab 1.48 b 1.98 bc 10.10 c 0.02 a
loss percentage (%) 70 D 80 B 77 A 79 B 70 A 80 B
B (1 L, 20 °C); DW (4 L, 10 °C) 4.46 ab 3.44 a N.D. 0.29 ab 1.17 ab 1.40 abc 9.90 c 0.03 a
loss percentage (%) 55 C 81 B 83 AB 84 BC 79 B 81 B
B (1 L, 10 °C); DW (5 L, 10 °C) 5.34 b 3.65 a N.D. 0.25 ab 0.93 a 0.52 ab 7.75 b 0.01 a
loss percentage (%) 46 B 80 B 85 B 87 C 92 C 85 C 27 A
lager beer brand C 7.61 c 16.80 b 0.12 0.72 c 6.79 e 5.46 d 41.57 e 0.01 a
B (1 L, 10 °C); DW (6 L, 10 °C) 3.80 ab 2.67 a N.D. 0.14 a 3.74 0.34 a 5.14 a 0.07 a
loss percentage (%) 47 A 84 B 80 AB 44 A 93 C 87 C
a
Acetaldehyde (AA), ethyl acetate (EA), ethyl hexanoate (EH), isoamylacetate (IAA), n-propanol (n-prop), 2-methylbutanol (2-MB), 3-
methylbutanol (3-MB), diacetyl (DA). B: beer; DW: deaerated water. N.D.: not detectable. Statistical analysis was performed separately. Values in
the same column with different letters are statistically different (P < 0.05).

Table 2. Representative Parameters of Original and Dealcoholized Beer Using Different Ratios of Beer/Stripping Solutiona
beer brand OG (°P) RE (°P) AE (°P) EtOH (% v/v) pH color (EBC) TU (EBC) TN (mg L−1) CO2 (g L−1)
lager beer (brand A) 10.73 b 2.94 a 1.93 a 4.53 e 4.17 a 6.24 a 0.85 a 492 ab 5.32 cd
B (1 L, 10 °C); DW (3 L, 10 °C) 3.86 a 2.37 a 2.11 ab 1.06 d 4.15 a 6.88 b 2.54 b 518 ab 0.3 b
lager beer (brand B) 11.25 b 2.36 a 1.86 a 5.00 g 4.27 a 7.13 b 0.71 a 521 b 5.57 d
B (1 L, 10 °C); DW (4 L, 10 °C) 3.81 a 2.30 a 2.01 a 0.88 bc 4.17 a 7.49 b 1.78 ab 546 bc 0.19 ab
B (1 L, 20 °C); DW (4 L, 10 °C) 4.21 a 2.54 a 2.22 ab 0.93 c 4.24 a 7.77 b 1.07 a 535 bc 0.13 ab
B (1 L, 10 °C); DW (5 L, 10 °C) 3.89 a 2.77 a 2.55 b 0.79 b 4.27 ab 7.64 b 0.91 a 534 bc 0.44 b
lager beer (brand C) 10.94 b 3.50 a 1.90 a 4.81 f 4.42 b 7.57 b 0.65 a 549 c 5.23 d
B (1 L, 10 °C); DW (6 L, 10 °C) 3.22 a 2.40 a 2.30 ab 0.51 a 4.30 ab 7.78 b 0.92 a 569 c 0.36 ab
a
Original gravity (OG), real extract (RE), apparent extract (AE), turbidity (TU), total nitrogen (TN). Beer (B); deaerated water (DW). Statistical
analysis was performed separately. Values in the same column with different letters are statistically different (P < 0.05).

Figure 5. Decrease in ethanol during dealcoholization using different

Figure 4. Percent of ethanol removed using different stripping stripping solutions (B: beer; DW: deaerated water, CW: carbonated
solutions. Values with different superscript letters are statistically water). Values with different superscript letters are statistically different
different (P < 0.05). (P < 0.05).

not necessary to run it for 4 h. As well as the ethanol, the
increase of the stripping solution quantity caused a diminution
of volatile compounds concentration at the end of treatment
(Table 1). The quality parameters monitored did not change
significantly (Table 2), except for carbon dioxide, which was
decreased considerably, and turbidity, which was increased
slightly after dealcoholization.
Different Stripping Solution. The effect of different kinds
of stripping solution was studied in this part of the work.
Carbonated water (CW) was compared with normal deaerated
water (DW) in order to reduce the loss of carbon dioxide by
3282
the end of the process. If possible, the stripping solution was
pure water, which had been previously deoxygenated by boiling
and/or flushing with a gas, usually nitrogen. In other words, if
the stripping solution is similar to beer from a compositional
point of view (especially in the case of carbon dioxide and low
oxygen content), the pressure gradient between carbon dioxide
in the beer and in the stripping solution would be minimal,
preventing its diffusion across the membrane.28 The amount of
alcohol removed was the same with both strip solutions (Figure
4). On the contrary, the carbonation initially appeared to
restrict ethanol transfer as shown in Figure 5 (mechanism
dx.doi.org/10.1021/jf405490x | J. Agric. Food Chem. 2014, 62, 3279−3286
Journal of Agricultural and Food Chemistry Article

Table 3. Representative Volatile Compounds (mg L−1) and Loss Percentage (%) of Original and Dealcoholized Beer Using
Different Stripping Solutionsa
beer brand AA EA EH IAA n-prop 2-MB 3-MB DA
lager beer brand B 10.01 c 18.31 c 0.16 1.74 c 7.38 c 6.66 c 52.23 c 0.02 ab
B (1 L, 10 °C); DW (5 L, 10 °C) B in tubeside 3.86 ab 4.43 bc 0.02 0.15 a 4.28 b 0.47 a 0.22 a 0.01 a
loss percentage (%) 61 B 75 A 91 B 41 A 92 A 88 A 32 A
lager beer brand D 4.97 b 13.88 b 0.05 0.76 b 11.44 a 7.28 c 61.19 d 0.07 c
B (1 L, 10 °C); DW (5 L, 10 °C) B in shellside 2.48 a 3.06 a N.D. 0.22 a 1.26 a 0.56 b 9.12 b 0.03 ab
loss percentage (%) 50 A 77 A 71 A 88 B 92 A 85 A 61 A
B (1 L, 10 °C); CW (5 L, 10 °C) B in shellside 2.82 a 3.79 a N.D. 0.15 a 1.35 a 0.60 b 8.11 b 0.04 b
loss percentage (%) 43 A 72 A 80 A 88 B 91 A 86 A 46 A
a
N.D.: not detectable. Statistical analysis was performed separately. Values in the same column with different letters are statistically different (P <
0.05).

Table 4. Representative Parameters of Original and Dealcoholized Beer Using Different Stripping Solutionsa
OG RE EtOH (% v/ color TU TN CO2 (g
beer brand (°P) (°P) AE (°P) v) pH (EBC) (EBC) (mgL−1) L−1)
lager beer (brand B) 11.25 b 2.36 a 1.86 a 5.00 c 4.27 ab 7.13 a 0.71 a 521 b 5.57 d
B (1 L, 10 °C); DW (5 L, 10 °C) B in tubeside 3.89 a 2.77 a 2.55 ab 0.79 a 4.27 ab 7.64 a 0.91 ab 534 b 0.44 a
lager beer (brand D) 10.92 b 3.70 a 1.88 a 4.71 b 4.02 a 7.80 a 0.71 a 354 a 4.84 c
B (1 L, 10 °C); DW (5 L, 10 °C) B in shellside 4.80 a 3.54 a 3.19 b 0.84 a 4.17 ab 7.34 a 1.11 b 342 a 0.38 a
B (1 L, 10 °C); CW (5 L, 10 °C) B in shellside 5.00 a 3.76 a 3.45 b 0.79 a 4.39 b 7.55 a 1.21 b 346 a 1.98 b
a
Carbonated water (CW). Statistical analysis was performed separately. Values in the same column with different letters are statistically different (P <
0.05).

water is a viable option to reduce the carbon dioxide loss,

Figure 6. Percent of ethanol removed using different stripping solution
flow rate (mL min−1). Values with different superscript letters are
statistically different (P < 0.05).
Figure 7. Decreasing ethanol during dealcoholization using different
stripping solution flow rate. Values with different superscript letters are
statistically different (P < 0.05).
unknown), but at the end of the process no difference was
found. This would be explained by the equilibrium being
reached between the beer and stripping solution. In other
words, the ethanol concentration became the same in both beer
and stripping solution. As expected, low-alcohol beer obtained
using CW showed about 2 g L−1 of carbon dioxide, whereas the
process with normal deaerated water resulted in about 0.4 g L−1
in each trial. The results showed that the use of carbonated
3283
allowing a low-alcohol beer with an acceptable carbon dioxide
concentration. In these experiments the final carbon dioxide
level, even when carbonated water was employed as stripping
solution, was low compared to a typical specification for beer,
and it would have been necessary to add more before packaging
in a commercial process. On the other hand, the employment
of stripping solutions with higher concentrations of carbon
dioxide may have resolved the problem. Concerning the most
important volatile compounds, no significant difference was
found when using CW or DW (i.e., similar losses) (Tables 3
and 4).
Effect of Stripping Solution Flow Rate. The effects of
the stripping solution flow rate on the ethanol decrease are
shown in Figure 6. In this case two different flow rates were
employed: first 500 mL min−1 for feed and stripping solution,
second 500 mL min−1 of feed solution and 1000 mL min−1 of
stripping solution. A similar study was performed by Liguori et
al. 38 That work showed that when increasing the stripping flow
rate from 1.2 to 2.4 mL min−1, a more rapid decrease in ethanol
content was observed. In this case no significant effect was
observed as shown in Figures 6 and 7. Figure 7 was in
agreement with Diban,30 confirming that flow rate has little
influence on mass transfer resistance because the trans-
membrane resistance was the limiting stage in this transport
mechanism. The volatile compounds and quality parameters
did not change significantly when different stripping solution
flow rates were employed (Tables 5 and 6).
Feed Solution and Stripping Solution Inversion. In the
trials above, the stripping solution flowed in the shellside so
that the beer flowed tubeside. In the following trials these
operating conditions were inverted so that the beer flowed
shellside and stripping solution flowed tubeside. In this
dealcoholization trial 83% of ethanol was removed instead of
79% when it was used with beer tubeside (Figures 8 and 9).
Thus, the beer shellside and water tubeside could be a better
option. More significantly, the ethanol results after 30, 60 and
dx.doi.org/10.1021/jf405490x | J. Agric. Food Chem. 2014, 62, 3279−3286
Journal of Agricultural and Food Chemistry Article

Table 5. Representative Volatile Compounds (mg L−1) and Loss Percentage (%) of Original and Dealcoholized Beer Using
Different Flow Ratesa
beer brand AA EA EH IAA n-prop 2-MB 3-MB DA
lager beer (brand B) 10.01 b 18.31 b 0.16 1.74 b 7.38 b 6.66 b 52.23 b 0.02 a
flow rate 500 mL min−1 4.46 a 3.44 a N.D. 0.30 a 1.17 a 1.41 a 9.90 a 0.03 a
loss percentage (%) 55 A 81 A 83 A 84 A 79 A 81 A
flow rate 1000 mL min−1 4.56 a 3.79 a N.D. 0.27 a 1.01 a 0.55 a 9.20 a 0.03 a
loss percentage (%) 54 A 79 A 84 A 86 A 91 B 82 A
a
N.D.: not detectable. Statistical analysis was performed separately. Values on the same column with different letters are statistically different (P <
0.05).

Table 6. Representative Parameters of Original and Dealcoholized Beer Using Different Flow Ratesa
beer brand OG (°P) RE (°P) AE (°P) EtOH (% v/v) pH color (EBC) TU (EBC) TN (mg L−1) CO2 (g L−1)
lager beer brand B 11.25 b 2.36 a 1.86 q 5.00 b 4.27 a 7.13 a 0.71 a 521 a 5.57 b
flow rate 500 mL min−1 4.21 a 2.54 a 2.22 ab 0.93 a 4.24 a 7.77 a 1.07 b 535 b 0.13 a
flow rate 1000 mL min−1 4.14 a 2.68 a 2.42 b 0.94 a 4.31 a 7.29 a 1.00 b 529 b 0.24 a
a
Statistical analysis was performed separately. Values on the same column with different letters are statistically different (P < 0.05).

However, as shown in Table 8, for all dealcoholization

Figure 8. Percent of ethanol removed using different flowsides. Values
with different superscript letters are statistically different (P < 0.05).
Figure 9. Decreasing ethanol during dealcoholization using different
flowsides (B: beer; DW: deaerated water, CW: carbonated water).
Values with different superscript letters are statistically different (P <
0.05).
90 min suggested that the ethanol was being removed more
quickly with the beer shellside. Equilibrium may be achieved
more quickly, making the process more efficient and cost-
effective. With regard to the volatile compounds a larger
amount of isoamyl and ethyl acetate was lost with beer in
tubeside, while other compounds exhibited no significant
differences (Table 7). These findings appeared to be similar to
the performance of reverse osmosis when applied to deal-
coholization in terms of ethanol, n-propanol, and esters removal
(Table 8). Osmotic distillation appeared to compare favorably
with vacuum distillation, which is a commonly employed
dealcoholization technique and also the process with the
highest ethanol and volatile compounds removal.
3284
techniques surveyed substantial losses of volatile compounds
occurred, which would have had a significant effect on the
flavor. However, OD compared favorably with alternative
techniques such as dialysis, vacuum distillation, falling film
evaporation, and reverse osmosis (Table 8).
Operating Cost Examination. A cost examination was
performed in order to appraise OD as an economically viable
technique. It was assumed an annual production of 100 000 hL
of a low-alcohol beer with the initial ethanol content of 4.5 and
a final one of 0.5% v/v. The finished plant cost (pumps, pipes,
valves) emerged directly from a request for a quotation by a
manufacturer, which is approximately 340 000 €, Thus,
considering the plant amortization over 10 years, the annual
plant cost is 34 000 €, with a cost of 0.0034 € L−1 of produced
beer. The membrane replacement cost, assuming a membrane
life of 2 years, is approximately 25 000 € per year. Membrane
cost information was obtained from a private company
specializing in membrane production. Finally, assuming United
Kingdom industrial energy unit cost of 0.09895 € kW h−1, the
estimated energy cost was about 0.00021 € L−1 (www.energy.
eu). Regarding water cost, supposing a unit water cost in
United Kingdom of 1.9 € m−3, the value produced is
approximately 0.0114 € L−1, including water required for
processing and cleaning. Regarding manpower, this is always an
estimate because of a wide variability across the European
Member States, where the average labor cost is 23.50 € h−1
(Eurostat, 2013). Although membrane plants have a low
requirement for supervision compared to many processes, it is
important to take into account membrane maintenance,
cleaning, and controlling. It could be right to consider one
person per day, in this case the manpower cost would be about
50 000 € year −1. Operating costs, investment, and membrane
replacement costs could be problems that inhibit the
commercialization. Improved profitability could be reached
with a few process improvements such as employing sparkling
and flavored water as stripping solution, thereby generating
another valuable product stream.
The process settings and control was relatively simple, as well
as membrane and plant cleaning. A membrane unit setup with
the beer on the shellside resulted in the most efficient ethanol
removal (Tables 7 and 8, Figures 8 and 9), whereas employing
different temperatures and different stripping solution flow
dx.doi.org/10.1021/jf405490x | J. Agric. Food Chem. 2014, 62, 3279−3286
Journal of Agricultural and Food Chemistry Article

Table 7. Representative Volatile Compounds (mg L−1) and Loss Percentage (%) of Original and Dealcoholized Beer Using
Different Flowsidesa
beer brand AA EA EH IAA n-prop 2-MB 3-MB DA
lager beer brand B 10.01 b 18.31 c 0.16 1.74 c 7.38 bc 6.66 c 52.23 c 0.02 a
beer in tubeside 4.51 a 3.99 a N.D. 0.21 a 2.60 ab 0.51 a 7.02 a 0.02 a
loss percentage (%) 54 A 78 B 88 B 64 B 92 A 86 A 12 A
lager beer brand D 4.97 a 13.88 b 0.05 0.76 b 11.44 c 7.28 c 61.19 d 0.07 b
beer in shellside 3.49 a 3.06 a N.D. 0.22 a 1.26 a 0.56 a 9.12 a 0.03 a
loss percentage (%) 50 A 77 B 71 A 88 C 92 A 85 A 61 B
lager beer brand E 7.61 ab 16.88 c 0.13 0.73 b 6.80 b 5.46 b 41.57 b 0.02 a
beer in shellside 3.78 a 4.39 a N.D. 0.15 a 4.23 ab 0.46 a 6.20 a 0.02 a
loss percentage (%) 50 A 73 A 79 A 37 A 91 A 85 A
a
N.D.: not detectable. Statistical analysis was performed separately. Values on the same column with different letters are statistically different (P <
0.05).

Table 8. Aroma Compounds Loss Percentage (%) before

and after Dealcoholization by Means of Falling Film
■ ACKNOWLEDGMENTS
We gratefully acknowledge the financial support of the Italian
Evaporation (FFE),39 Dialysis,40 Vacuum Distillation
Minister of Agriculture and the Ministry of Education,
(VD),41 and Reverse Osmosis (RO)42a
University and Research.

■
volatile compound dialysis FFE VD RO OD
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