Journal of Food Engineering 63 (2004) 303–324

www.elsevier.com/locate/jfoodeng

Recent advances on membrane processes for the concentration

of fruit juices: a review
B. Jiao a, A. Cassano b,*
, E. Drioli b

a
Citrus Research Institute, Chinese Academy of Agricultural Sciences, CRI-CAAS c/o Southwest Agricultural University,
Beibei, Chongqing 400712, China
b
Institute on Membrane Technology, ITM-CNR, c/o University of Calabria, via P. Bucci, cubo 17/C, Rende (CS) I-87030, Italy
Received 27 January 2003; accepted 8 August 2003

Abstract
Fruit juices have been traditionally concentrated by multi-stage vacuum evaporation, resulting in a loss of fresh juice flavors,
color degradation and a ‘‘cooked’’ taste due to the thermal effects. The promising alternative is reverse osmosis concentration.
However, it cannot reach concentrations larger than 25–30
Brix with a single-stage RO system due to high osmotic pressure limi-
tation, which is quite below the value of 45–65
Brix for standard products obtained by evaporation. Technological advances related
to the development of new membranes and improvements in process engineering have been proved to overcome this limitation. New
membrane processes, including membrane distillation and osmotic distillation, and integrated membrane processes are still being
identified and developed in concentrated fruit juice processing to improve product quality and reduce energy consumption. Recent
advances and developments of the use of membrane processes for concentrating fruit juice are reviewed and discussed in this paper.
Major attentions are focused on the application of new membrane processes and integrated membrane systems.
 2003 Elsevier Ltd. All rights reserved.

Keywords: Fruit juices; Concentration; Membranes; Reverse osmosis; Direct osmosis; Membrane distillation; Osmotic distillation; Integrated
membrane processes

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 304

2. Reverse osmosis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 304

2.1. Performance of RO membranes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 304
2.2. Effect of operating parameters on permeate flux and flavor rejection . . . . . . . . . . . . . . 305

3. Direct osmosis concentration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 307

3.1. Process fundamentals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 307
3.2. Performance of the DOC process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 307

4. Membrane distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309

4.1. Process fundamentals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309
4.2. Effect of membrane types on the permeate flux . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310
4.3. Effect of feed juice concentration on the permeate flux. . . . . . . . . . . . . . . . . . . . . . . . 310
4.4. Effect of operating temperature on the permeate flux . . . . . . . . . . . . . . . . . . . . . . . . . 310
4.5. Effect of flow rate on the permeate flux . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310
4.6. Effect of UF pretreatment on the permeate flux. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310
4.7. Effect of MD on the retention of fruit juice components . . . . . . . . . . . . . . . . . . . . . . 310

*
Corresponding author. Tel.: +39-0984-492011; fax: +39-0984-402103.
E-mail address: a.cassano@itm.cnr.it (A. Cassano).

0260-8774/$ - see front matter  2003 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2003.08.003
304 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324

5. Osmotic distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310

5.1. Process fundamentals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310
5.2. Effect of operating conditions on the OD flux . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 311
5.3. Effect of OD on the retention of fruit juice components . . . . . . . . . . . . . . . . . . . . . . . 312
5.4. OD membranes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 312
5.5. Effect of UF pretreatment on the evaporation flux. . . . . . . . . . . . . . . . . . . . . . . . . . . 314
5.6. Process design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 315

6. Integrated membrane processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 316

7. Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 321

References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 322

1. Introduction covery (Gadea, 1987; Medina & Garcia, 1988; Paulson,

To reduce the storage and shipping costs, and to
achieve longer storage, fruit juices are usually concen-
trated by multi-stage vacuum evaporation. This process
results in a loss of fresh juice flavors, color degradation
and a ‘‘cooked’’ taste due to the thermal effects. Since
consumers generally prefer the flavor, aroma, appear-
ance and mouth feel of freshly squeezed juices, scientists
and processors have tried to develop new techniques for
retaining such characteristics of freshly squeezed juice in
the concentrate and ultimately in the reconstituted juice.
The juice industry has developed complex essence re-
covery, careful process control and blending techniques
to produce a good quality concentrate that is acceptable
to consumers, but still easily distinguishable from fresh
juice. Many efforts have been devoted to develop im-
proved methods such as freeze concentration, sublima-
tion concentration and membranes (ultrafiltration and
reverse osmosis) for concentrated juice processing
(Chen, Shaw, & Parish, 1993; K€ oseoglu, Lawhon, &
Lusas, 1990). The most promising alternative is mem-
brane concentration.
Membrane processes as microfiltration (MF), ultra-
filtration (UF) and reverse osmosis (RO) have been
widely applied to the dairy, food and beverage industry
after the discovery of asymmetric membranes by Loeb
and Souriragin in the early 1960’s. The potential of de-
veloping RO process as a concentration technique to
remove water from fruit juices has been of interest to the
fruit juice industry for about 30 years. The advantages
of RO process over traditional evaporation are in lower
thermal damage to product, increase in aroma retention,
less energy consumption and lower equipment costs.
One main disadvantage of RO has its inability to reach
the concentration of standard products produced by
evaporation because of high osmotic pressure limitation.
Studies have shown that the final concentration of fruit
juices is limited by membranes and equipment to about
25–30
Brix with the most efficient flux and solute re-
Wilson, & Spatz, 1985; Pepper, 1990).
Recently, technological advances related to the de-
velopment of new membranes and improvements in
process engineering have been proved to overcome this
limitation. New membrane processes including mem-
brane and osmotic distillation and integrated membrane
processes might contribute to the improvement of con-

centrated fruit juice processing (Alvarez et al., 2000;
Calabro, Jiao, & Drioli, 1994; Cassano et al., 2003;
Cuperus, 1998; Drioli, Calabr o, & Wu, 1987; Drioli,
Jiao, & Calabr o, 1992; Girard & Fukumoto, 2000;
Hogan, Canning, Peterson, Johnson, & Michaels, 1998;
Jiao, Molinari, Calabr o, & Drioli, 1992; Petrotos &
Lazarides, 2001; Vaillant et al., 2001). This paper will
provide a review of the recent significant progress on
membrane processes for concentrating fruit juices, in-
cluding the use of reverse osmosis, direct osmosis con-
centration, membrane and osmotic distillation, and
integrated membrane processes.
2. Reverse osmosis
2.1. Performance of RO membranes
Fruit juice concentration by RO has been of interest
to the fruit processing industry for about 30 years. The
advantages of RO over traditional evaporation are in
low thermal damage to product, reduction in energy
consumption and lower capital investments (Merson,
Paredes, & Hosaka, 1980), as the process is carried out
at low temperatures and it does not involve phase
change for water removal. The retention of juice con-
stituents, especially flavors, and the permeate flux, re-
garding RO performance, are two major factors, which
are related to the type of membranes and the operating
conditions used during the process.
Early studies by Merson and Morgan (1968) found
that oil-soluble aromas of orange juice were easily re-
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
tained using cellulose acetate membrane, while there
were losses of water-soluble aromas. Membrane reten-
tion of some other juice constituents (sugars, acids,
potassium, calcium, magnesium, and phosphorus) was
shown to be excellent (Peri, Battisti, & Setti, 1973).
After that, a considerable research has been carried
out for the concentration of a variety of fruit juices,
including apple, pears, grapefruit, kiwi, pineapple, pas-
sion fruit and tomato juice (Bowden & Isaacs, 1989;
Braddock, Nikdel, & Nagy, 1988; Medina & Garcia,
1988; Palmieri, Dalla Rosa, Dall’Aglio, & Carpi, 1990;
Paulson et al., 1985; Sheu & Wiley, 1983). These works
have mainly focused on the test of different types of
membranes and the effects of operating conditions on
the permeate flux and retention of juice compounds.
It has been found that polyamide has greater retention
of flavors and other constituents as well higher fluxes
than cellulose acetate membranes (Chua, Rao, Acree, &
Cunningham, 1987; Fukutani & Ogawa, 1983a, 1983b;
Sheu & Wiley, 1983). Recovery of apple juice volatiles
during RO concentration to 20
Brix was found to be
about 80% when using a high resistance (HR) membrane
(Sheu & Wiley, 1983). Chua et al. (1987) compared a
commercial spiral wound cellulose acetate membrane
(CA-99) and an experimental polyamide membrane (PA-
99, 99% salt rejection) for concentrating apple juice using
a pilot-scale RO unit. The PA-99 membrane exhibited
higher flux and concentration rates than the CA-99
membrane. In addition, the PA-99 membrane retained
45% of the total odor-active volatiles in the feed, while
the CA-99 membrane retained 23%. Medina and Garcia
(1988) reported that the overall recovery of sugars, acids
and flavor-volatile components in orange juice was ap-
proximately 93% with a spiral wound 192 MSO2-P
polyamide membrane (Osmonics, Minnetonka, MN,
effective surface area 1.28 m2 ). Sugar recovery (>98%)
was higher than acid recovery (85%). Due to the unequal
membrane rejection of sugars and organic acids, the

Brix/acid ratio increased, making sweetness more per-
ceptible, thus improving one of the quality indicators.
Chou, Wiley, and Schlimme (1991) compared the per-
meation of apple juice volatiles by polyether-urea (TFC
SS, Fluid Systems, Allied-Signal, Inc., San Diego, CA,
surface area 1.95 m2 ) and polyamide (TFCL HP, Fluid
Systems, Allied-Signal, Inc., San Diego, CA, surface area
1.95 m2 ) thin-film composite membranes during RO.
There was two to three times less permeation of hexanal
and ethyl-2-methylbutyrate into the permeate of TFCL
HP when compared with TFC SS. Thus, apple juice
concentrated using the polyamide membrane would
demonstrate a more intense flavor than juice concen-
trated using the polyether-urea membrane. Polyamide
membranes are also known to have a longer useful life
than cellulose acetate.
Different membrane configuration may also affect the
retention of flavor compounds during apple juice con-
305
centration (Chou et al., 1991). The plate and frame
configuration had 11.5% permeation of n-hexanal
compared with 0.5% for the spiral wound. This was
probably due to greater membrane packing density and
membrane area of the spiral wound (3.90 m2 of total
membrane surface area) when compared with the plate
and frame (0.36 m2 of total membrane surface area).
The spiral wound system gave lower concentrations of
n-hexanal in the permeate because of increased rejection
and/or of increased flavor compound absorption due to
greater membrane surface. Braddock et al. (1988) re-
ported that volatile compounds except for methanol,
ethanol and traces of limonene, were not detected in
measurable quantities in the permeate, during the con-
centration of orange, grapefruit and lemon juices in the
range of 22–25
Brix at pulp contents of 7–10%, using a
composite tubular RO membrane (ZF99, Patterson
Candy International Ltd., England, 99% NaCl rejection,
surface area 0.9 m2 ). However, a 17–30% loss of volatile
peel oil (measured as limonene) was found if the mem-
brane system is not totally closed during recirculation of
the process stream to effect concentration.
2.2. Effect of operating parameters on permeate flux and
flavor rejection

Alvarez, 
Riera, Alvarez, and Coca (1998) studied the
permeation of a model apple juice aroma solution
through a RO spiral wound aromatic polyamide mem-
brane (MSCB 2521 R99, Separem, Biella, Italy, surface
area 1.03 m2 , NaCl rejection 99.2%). Rejection was
observed to increase with transmembrane pressure
(15–35 bar) and feed flows (200–600 l/h). The major
compounds responsible for apple flavor such as ethyl-2-
methyl butanoate, ethyl butanoate and hexanol were
rejected to a degree of more than 90% under the best
operating condition (35 bar and 600 l/h). The retention
of ethyl acetate and isopentanol having a negative effect
on apple flavor was 80.2% and 98.4%.
It was observed that an increase in processing tem-
perature tends to increase the permeation rate of vola-
tiles, but this effect seems to depend on the type of
volatiles to some extent. Recoveries decreased from
41.7% to 29.2% for hexanal and from 56.6% to 50.8%
for ethyl-2-methylbutyrate during RO concentration of
apple juice using a spiral wound polyamide membrane
at 20 and 40
C, respectively (Chou et al., 1991). How-
ever, the recovery of these two flavor compounds in the
retentate increased by approximately 20% with the in-
crease of operating pressure from 35 to 50 bar. Increased
pressure can result in higher flux, reduced process time
and consequently smaller flavor compound losses at-
tributed to volatilization and adhesion to the membrane.
The permeate flux has been affected mainly by
transmembrane pressure (TMP), followed by tem-

perature and flow rate (Alvarez, 
Alvarez, Riera, &
306 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324


Alvarez, 
1997; Alvarez, Riera, Alvarez, & Coca, 2001; viscosity and density of the solution on the membrane
Fukutani & Ogawa, 1983a; Sheu & Wiley, 1983; Sheu & surface. Thus, the mass transfer coefficients of the

Wiley, 1984). Alvarez et al. (1997) reported that the aroma compounds are lower, and their concentrations
permeate flux, through a tubular polyamide RO mem- on the membrane surface as well as their permeation
brane (AFC 99, Paterson Candy International Ltd, increase. Good agreement between experimental and
England, 99% NaCl rejection, total effective surface area estimated data was observed for most aroma com-
0.9 m2 ) increased by increasing TMP (at a constant pounds and operating conditions used.
concentration). The TMP also affected the maximum In spite of the high selectivity and solute retention
concentration that can be obtained with the limit being capacity of RO membranes, this process has a signifi-
19, 23, and 27.5
Brix at 35, 45 and 55 bar, respectively. cant drawback. The high osmotic pressure of fruit juice
The high permeate flux was obtained at high feed ve- precludes its concentration to the required level of total
locities, but it considerably diminished for values higher soluble solids. Studies (Medina & Garcia, 1988; Pepper,
than 1.5–2 m/s and did not affect the maximum con- Orahard, & Merry, 1985; Sheu & Wiley, 1983) have
centration that can be obtained. It was also showed that shown that for cellulosic and non-cellulosic membranes
the permeate flux decreased as concentration increased the most efficient flux and solute recovery are at a con-
due to the increase of juice osmotic pressure and its centration lower than 30
Brix. This suggests that RO
viscosity. For apple juice concentration, the average system should be viewed as preconcentration step with
processing capacity increased about 3–4% for every 1
C other technologies like freeze concentration or evapo-
increase in operating temperature between 20 and 60
C ration combined process; it has the advantage of re-
(Sheu & Wiley, 1983). At higher temperature, the ducing energy consumption and increasing production
membrane permeability coefficient is higher, the diffu- capacity (Gadea, 1987; Sheu & Wiley, 1983).
sivity coefficient in the solution increases and the vis- Gadea (1987) described the first commercial RO plant

cosity coefficient decreases (Alvarez et al., 1998). for concentrating orange juice using AFC99 membrane
In addition, enzymatic pretreatment of orange juice as first step, before final freeze concentration. The feed
(with pectinase) increased permeate flux and did not flow rate could be varied between 4200 and 9700 l/h of
affect solute recoveries (Medina & Garcia, 1988). De- natural orange juice with a water removal rate of 2000 l/
pectinization of orange juice increased RO flux initially h. The membranes showed an excellent retention of juice
up to 15% hydraulic recovery, but flux decreased beyond constituents as illustrated in Table 1. The organoleptic
this point. Fukutani and Ogawa (1983a) found clarified characteristics, examined by specialists in taste tests
Satsuma mandarin juice had better flux than cloudy
juice (3% v/v). On the contrary, both clarified and
cloudy pineapple juice were found to have similar flux Table 1
Retention of orange juice constituents in RO concentration (Gadea,
during RO (Bowden & Isaacs, 1989). Permeate flux de- 1987)
creased as feed flow velocity decreased below 2 m/s, but
Juice strength Permeate
there was little difference between 2 and 3 m/s velocities.
Dissolved solids (
Brix) 11.2 0.0
The discrepancy may be due to different pulp charac-
Glucose (g/l) 26.6 0.1359
teristics of the two juices. Fructose (g/l) 28.4 0.1552

Recently, Alvarez et al. (2001) proposed the prefer- Saccharose (g/l) 35.1 0.0815
ential sorption-capillary flow model for the prediction of Citric acid anhydrous (%, w/w) 0.85 0.01
the rejection of aroma compounds and permeate flux Vitamin C (ppm) 480 6.0
Ash (%) 4.1 0.11
during the RO concentration of model solutions simu-
Sodium (ppm) 59 2
lating apple juice through the MSCB 2521 R99 spiral- Potassium (ppm) 1427 47
wound membrane (Separem, Biella, Italy, surface area Phosphorous (ppm) 200 2
1.03 m2 , NaCl rejection 99.2%). Water and aqueous Aspartic acid (mg/100 ml) 28 0.35
solutions of apple juice aroma were used to determine Asparagine (mg/100 ml) 45 1.0
Proline (mg/100 ml) 80 2.4
the parameters included in the model. Then, the model
Glycine (mg/100 ml) 1.5 Traces
was tested with aqueous solutions of glucose and aroma Alanine (mg/100 ml) 9.9 1.5
compounds. Experiments were performed at different Valine (mg/100 ml) 1.8 0.034
TMP (15–35 bar), feed flow rates (200–600 l/h), Rey- Isoleucine (mg/100 ml) 0.0 Traces
nolds numbers (51–190), temperatures (15–30
C) and Leucine (mg/100 ml) 0.5 Traces
Phenylalanine (mg/100 ml) 3 0.04
glucose concentrations (9.1–17.0
Brix). It was observed
c-Aminobutyric (mg/ml) 24 0.46
that the permeate flux and aroma rejection increased Histidine (mg/ml) 1.1 0.062
with feed flow rate and decreased with the glucose Ornitine (mg/ml) 0.8 0.32
concentration. This is due to the reduction of concen- Lysine (mg/ml) 2.9 0.14
tration polarization by increasing feed flow rate. A rise Arginine (mg/ml) 70 0.42
Total nitrogen (g/l) 1363 11
in the feed concentration involves an increase in the
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
Table 2
Advantages and disadvantages of RO applied to the concentration of fruit juices
Advantages
Technical aspects
• Broad industrial scale application
• Low temperatures
• Combination with vacuum evaporation and with systems
of vapour recompression, already commercially available
Economical aspects
• Energetically and economically convenient in comparison
with the thermal evaporation
(Leathered Food RA), as well as the physical/chemical
specification determined in the laboratory, showed no
difference between natural and the reconstituted reverse
osmosis concentrate.
Advantages and disadvantages of the RO process for
the production of concentrated juices are summarized in
Table 2.
3. Direct osmosis concentration
3.1. Process fundamentals
Direct osmosis concentration (DOC) is another
membrane process capable of concentrating fruit juice at
low temperatures and low pressures, thereby maintain-
ing original flavor and color characteristics of the fruit.
The principle uses an osmotic agent (OA) solution to
establish an osmotic pressure gradient across a semi-
permeable membrane and thus remove water from a
single strength fruit juice. An osmotic agent is generally
a solid highly soluble in water, hygroscopic, non-toxic,
inert toward the flavor, odor and color of the foodstuff,
and which does not pass through the membrane. Gen-
erally, the higher the concentration of the dissolved
solids and the lower the molecular weight of the dis-
solved solids, the higher the osmotic pressure. The most
frequently employed constituents are: sodium chloride,
sucrose or glycerol, cane molasses or corn syrup. The
OA solutions must have an osmotic pressure greater
than that of the concentrated fruit juice. For example,
the osmotic pressure of a 74
Brix high fructose corn
syrup is about 270 bar that is greater than 90 bar for
42
Brix pulpy orange juice.
3.2. Performance of the DOC process
Popper, Camirand, Nury, and Stanley (1966) first
used DOC to concentrate grape juice from 16 to
60
Brix. An average osmotic flux of about 2.5 l/m2 h was
obtained with a flat sheet cellulose acetate membrane.
307
Disadvantages
• Fouling phenomena
• High pressures
• Necessity of an inactivation enzyme pre-treatment
• Juice concentration limited at 22–23
Brix
• Loss of aroma compounds during the process
• Difficulty to concentrate solutions with high level of suspended
solids
• Membrane replacement at high cost
• High cost of working process
Stirring improved the osmotic flux by 67%. However,
the diffusion of some salt through the membranes was
observed in the grape concentrate, when using a satu-
rated brine solution as the OA solution.
OSMOTEK, Inc. of Corvallis developed the direct
osmosis technique as an efficient alternative to thermal
evaporation for concentrating food products. Beaudry
and Lampi (1990a, 1990b) reported the performance of
the Osmotek direct osmosis process for concentrating
fruit juices. They utilized new generation thin film
composite (TFC) RO membranes that were properly
modified. The overall membrane thickness was 25–85
lm, while the membrane’s top selective layer remained
similar to that of tight RO membranes (MWCO less
than 100 Da), thus impeding passage of other food in-
gredients besides water. More than 99.9% of the total
acid in orange juice and the color of red raspberry juice
were rejected by the membrane with a nominal MWCO
of 100 Da. Furthermore, a tubular membrane module
with specific design was constructed to provide housing
for the sensitive ultrathin direct osmosis membranes. It
improved turbulent flow and minimized flux resistances
rising from concentration polarization and membrane
fouling, allowing an increase in the osmotic flux. This
module configuration formulated a flow path (inside the
membrane) with a continuous change in flow direction,
providing at the same time effective support to the
membranes. A similar flat module was also developed.
These new developments were outlined in a US patent to
produce fruit juices (Herron, Beaudry, Jochums, &
Medina, 1994). Some theoretical aspects of this method
as well as its practical application concerning membrane
type, membrane configuration and suitable methods to
support the thin membrane, were discussed in the patent
document. The maximum osmotic flux of 5–6 l/m2 h was
obtained through new 100 Da membranes for several
kinds of liquid food samples including orange and
raspberry juice. In addition, no transfer of osmotic
agent through the membrane was detected. A fructose/
glucose solution (approximately 74
Brix) such as high
fructose corn syrup served as the osmotic agent that
308 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
flows countercurrent to the fruit juice. The membrane
assembly of this invention allows for rapid turbulent
flow, without excessive pressure drop, and a relatively
long region of contact with the membrane without
fouling or concentration polarization even with fluids
containing 75% or more of dissolved solutes and 35%
suspended solids. In Fig. 1 the simplified DOC flowsheet
is reported.
Unlike RO process, pressure differences across the
membrane in DOC are negligible and flux depends on
the difference in osmotic potential. The only hydraulic
pressures required are those (approximately 2 bar) nec-
essary to pump the juice and the OA solution over the
membrane surfaces (Milleville, 1990). Juices containing
large amounts of both dissolved and suspended solids
can be concentrated with minimum fouling because the
solids are not forced against the membrane. The fruit
juices can be fed to the module in a continuous, multi-
stage process. At each stage the fruit juice is recycled
through a heat exchanger (if refrigeration is desired) and
then through the DOC modules. The juice is kept under
a nitrogen or argon blanket to assist in flavor retention.
The OA solution is fed either once countercurrently
through the entire process or is recycled continuously
through an evaporation/heat recovery system. If there is
a large quantity of very concentrated solution that is
diluted at the plant, and if this solution could be used as
the OA solution, the dilution can be performed within
the juice concentration modules. This would result in
substantial cost savings for the juice concentration
process (Girard & Fukumoto, 2000). Typically, the OA
solution will be diluted and reconcentrated using evap-
oration. Therefore, the OA solution rather than the juice
is exposed to the high temperature, allowing the im-
provement of concentrate quality.
Under recirculation conditions, the flux can be
maintained at a steady rate indicating minimum fouling.
But as the juice becomes more concentrated, its osmotic
pressure increases; the flux then decreases due to the
decrease of osmotic pressure differences between the OA
solution and the juice. During a run, the flux of a de-
pectinized raspberry juice at 30
C decreased from 1.37
membrane sugar (OA)
Product
flow
concentrate
heat
exchanger
concentration
cells
Recirculation water
product loop
inlet
Fig. 1. Simplified DOC flowsheet (Herron et al., 1994).
to 0.3 l/m2 h, while the OA solution decreased from 69 to
60
Brix (Beaudry & Lampi, 1990b). The flux to make
42
Brix pulpy orange juice was similar. The time re-
quired to concentrate raspberry juice to 45
Brix ap-
proximately doubled (5 h vs. 10 h) when the processing
temperature decreased from 26 to 8
C (Wrolstad et al.,
1993).
Raspberry concentrates (45
Brix) prepared by Os-
motek’s DOC system were compared with conventional
evaporative technology (i.e., centrifugal film evaporator)
(Wrolstad et al., 1993). Concentration by either pro-
cesses resulted in small anthocyanin pigment losses,
small increases of polymerized pigment and no signifi-
cant flavor differences as compared to the single-strength
juice. Concentration of red raspberry juice using either
osmotic or evaporative processes gave juice concentrates
of good quality comparable to commercial samples.
Herron et al. (1994) also provided evidence that the
DOC can produce juice concentrate with superior
quality in comparison to that yielded by a conventional
vacuum evaporator. These studies gave an answer to
earlier claims for a negative effect of the DOC process
on the quality of the juice concentrate (Bolin & Salunke,
1971). In those days, the prolonged processing times due
to the poor process performance was probably the rea-
son for the observed quality deterioration.
Recently Petrotos, Quantick, and Petropakis (1998,
1999) studied the effect of several membranes and pro-
cess parameters on the performance of DOC during the
concentration of tomato juice. These studies suggest that
the membrane thickness and the viscosity of the osmotic
agents are of greater importance. A thinner membrane
and a low-viscosity osmosis medium (like NaCl brines)
are expected to yield a better performance. The findings
indicated that the use of viscous carbohydrate syrups as
osmotic media has to be abandoned in favour of highly
osmotic and low-viscosity salt brines. The pretreatment
of the juice by plain filtration, microfiltration or ultra-
filtration was also found to have a significant effect on
the value of the observed osmotic fluxes. The ultrafil-
tered juice gave the best performance than that of all
other filtrates with a 135% increase of the direct osmosis
flux.
Petrotos and Lazarides (2001) developed a new os-
motic apparatus with a flat configuration (Fig. 2). The
key of the system is an osmotic cell of special configu-
water ration to promote turbulence. Using the apparatus
equipped with a commercially RO membrane, with an
overall thickness of 260 lm, a tomato juice was con-
evaporator centrated from 5 to 16
Brix at low pressure and room
temperature. The obtained average flux of 4.5 kg/m2 h is
close to the values reported by Herron et al. (1994), al-
though the membrane used in this study was much
thicker than the membranes used by Herron.
Advantages and disadvantages of the DOC process
are summarized in Table 3.
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324 309

Stirrer

Brine
stock tank

Membrane
Part A
Part B
Tomato juice
stock tank

Pressure Pressure
Pressure Pressure Control valve
Control valve
meter meter

Pressure Pressure
Pressure Pressure
Control valve Osmotic Control valve
meter meter
cell
Membrane Membrane
pump pump

Fig. 2. The DOC schema for the concentration of fruit juice through flat sheet membrane module (Petrotos & Lazarides, 2001).

Table 3
Advantages and disadvantages of DOC applied to the concentration of fruit juices
Advantages Disadvantages
Technical aspects
• Low temperatures, low pressures • New technology that requires an evaluation at industrial level,
• No fouling problems, constant permeate flux in time flexibility to be evaluated
• Possibility to obtain high TSS concentration in the final • The long life of the membrane to be evaluated
product • Relatively low permeation (1.8–2.5 l/m2 h)
• Modularity, easy scale-up
• Possibility to treat solutions with high level of suspended solids
• Possibility of using modules in series, the same unit can
concentrate several different products
Economical aspects
• Low cost of membrane replacement • High investment costs
• High energy consumption

4. Membrane distillation The theoretical aspects and potential applications of

4.1. Process fundamentals
Membrane distillation is a relatively new membrane
process in which two aqueous solutions, at different
temperatures, are separated by a microporous hydro-
phobic membrane. In these conditions a net pure water
flux from the warm side to the cold side occurs. The
process takes place at atmospheric pressure and at
temperature that may be much lower than the boiling
point of the solutions. The driving force is the vapour
pressure difference between the two solution–membrane
interfaces due to the existing temperature gradient. The
phenomenon can be described as a three phase sequence:
(1) formation of a vapour gap at the warm solution–
membrane interface; (2) transport of the vapour phase
through the microporous system; (3) its condensation at
the cold side membrane–solution interface (Calabr
et al., 1994; Curcio, Barbieri, & Drioli, 2000; Drioli &
Wu, 1985; Jariel, Reynes, Courel, Durand, & Dornier,
1996; Jiao, Molinari et al., 1992; Jiao, Calabr
o, & Drioli,
1992).
the process have been extensively studied (Bandini,
Gostoli, & Sarti, 1991; Calabr o et al., 1994; Kimura,
Nakao, & Shimatani, 1987; Schofield, Fane, & Fell,
1987, 1990). The most suitable materials for MD
membranes include polyvinyldifluoride (PVDF), poly-
tetrafluoethylene (PTFE) and polypropylene (PP). The
size of micropores can range between 0.2 and 1.0 lm.
The porosity of the membrane will range from 60% to
80% of the volume and the overall thickness from 80–
250 lm, depending on the absence or presence of sup-
port. In general, the thinner the membrane and the
greater the porosity of the membrane, the greater the
flux rate. The membrane configurations used include flat
sheet, spiral wound and hollow fiber; the latter has re-
ceived the greatest attention.
Because MD can be carried out at the atmospheric
pressure and at a temperature which can be much lower
o than the boiling point of the solution, it can be used to
concentrate solutes sensitive to high temperature (e.g.
fruit juices), also at high osmotic pressure. Therefore
MD has received a great attention as techniques for
concentrating fruit juices.
310 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
4.2. Effect of membrane types on the permeate flux
Drioli et al. (1992) reported the concentration of or-
ange juice by MD, using a commercial plate PVDF
membrane (Millipore Corp.) with a nominal pore size of
0.22 lm and a laminated hydrophobic microporous
membrane (G0712) with a pore size of 0.2 lm manu-
factured by Gelman Science Tech. Ltd. The flux of
PVDF membrane was remarkably higher than of G0712
membrane. Curcio et al. (2000) reported that the single
strength apple juice could be concentrated to 64
Brix by
MD using a PP hollow fiber membrane module (ENKA
Microdyn MD-020-2N-CP, membrane area 0.1 m2 ,
nominal pore diameter 0.45 lm). An overall flux of 1–
1.5 kg/m2 h was obtained in this study.
4.3. Effect of feed juice concentration on the permeate flux
Permeate flux decreases with an increase of feed juice
concentration. This phenomenon can be attributed to
the reduction of the driving force due to the decrease of
the vapour pressure of the feed solution and to the ex-
ponential increase of the viscosity of the juice solution.
At high concentration ratios, fluxes are higher in the
MD process than in the RO (Drioli et al., 1992).
4.4. Effect of operating temperature on the permeate flux
The MD flux gradually increases with an increase of
the temperature difference between feed juice and the
cooling water. At lower temperature differences a de-
creasing of the permeate flux is observed due to the
lower vapour pressure difference between the two side of
the membrane (Drioli et al., 1992).
Lagan a, Barbieri, and Drioli (2000) reported that
MD was able to concentrate apple juice up to 64
Brix
with fluxes of 1 kg/m2 h. The viscosity of the juice at high
concentration induces severe polarization phenomena.
However, temperature polarization is more important
than concentration polarization and it is located mainly
on the feed side. The presence of the osmotic effects on
juice stream generates flux inversion. A small DT of 4
C
was sufficient to compensate this osmotic effect.
4.5. Effect of flow rate on the permeate flux
Studies demonstrated that the increase of flow rate
determines an increase of the permeate flux in MD
process (Drioli et al., 1992). The shearing forces gener-
ated at high flow rate cause a lower accumulation of
particulates such as pectin and cellulose on the active
membrane surface and thus reduce membrane fouling.
Besides, a lower crossflow velocity causes a lower Rey-
nolds number, thus hindering the heat transfer from the
bulk of the solution to and from the membrane surface,
and an effect of temperature polarization are more se-
vere than that of high crossflow velocity (Franken,
Mulder, & Smolders, 1990).
4.6. Effect of UF pretreatment on the permeate flux
It was found that ultrafiltration (UF) of the single
strength juice resulted in an increase in MD flux and
that the flux remained essentially constant during an
approximately two-fold concentration (Drioli et al.,
1992). The MD flux of the unfiltered juice, by contrast,
decreased steadily over the same concentration range.
The improvement in MD flux after UF was attributed to
a reduction in juice viscosity as a result of pulp and
pectin removal.
4.7. Effect of MD on the retention of fruit juice
components
The preliminary studied on the concentration of or-
ange juice by MD (Drioli et al., 1992) showed that the
PVDF membrane has very good retention of orange
juice compounds such as total soluble solids, sugars and
organic acids; the rejection of sugars and organic acids
were 100%. Vitamin C decreased by 42.1%. This de-
gradation has mainly associated with high temperature
and oxidation. As a result, the operating temperature in
MD process must be maintained as lower as possible.
Investigations have been carried out into the rela-
tionship between the structure of hydrophobic mem-
branes and the loss of volatile organic flavour/fragrance
components from liquid foods in MD process. The re-
sults have suggested that the best volatiles retention for
a given amount of water removal in membrane distil-
lation is provided by membranes having an open fibrous
structure rather than discrete pores.
5. Osmotic distillation
5.1. Process fundamentals
Osmotic distillation is a recent membrane process
(Lefebvre, 1988), also known as osmotic evaporation
(Deblay, 1995), membrane evaporation, isothermal
membrane distillation or gas membrane extraction
which has been successfully applied to the concentration
of liquid foods such as milk, fruit and vegetable juice,
instant coffee and tea and various non-food aqueous
solutions.
This technique can be used to extract selectively the
water from aqueous solutions under atmospheric pres-
sure and at room temperature, thus avoiding thermal
degradation of the solutions (Kunz, Benhabiles, & Ben-
Aim, 1996). It is therefore particularly adapted to the
concentration of heat-sensitive products like fruit juices
(Deblay, 1995; Durham & Nguyen, 1994; Gostoli, 1998;

Johnson, Valks, & Lefebvre, 1989). The process involves
the use of a microporous hydrophobic membrane to
separate two circulating aqueous solutions at different
solute concentrations: a dilute solution and an hyper-
tonic salt solution. If the operating pressure is kept
below the capillary penetration pressure of liquid into
the pores, the membrane cannot be wetted by the solu-
tions. The difference in solute concentrations, and con-
sequently in water activity of both solutions, generates,
at the vapour–liquid interface, a vapour pressure dif-
ference causing a vapour transfer from the dilute solu-
tion towards the stripping solution. The water transport
through the membrane can be summarized in three
steps: (1) evaporation of water at the dilute vapour–
liquid interface; (2) diffusional or convective vapour
transport through the membrane pore; (3) condensation
of water vapor at the membrane/brine interface (Courel,
Dornier, Herry, Rios, & Reynes, 2000; Gostoli, 1999;
Hogan et al., 1998; Lefebvre, 1992; Mengual, Zarate,
Pena, & Velazquez, 1993; Sheng, Johnson, & Lefebvre,
1991).
The typical OD process involves the use of a con-
centrated brine at the downstream side of the membrane
as the stripping solution. A number of salts such as
MgSO4 , CaCl2 , K2 HPO4 are suitable. As shown in Fig.
3, potassium salts of ortho- and pyrophosphoric acid
offer several advantages, including low equivalent
weight, high water solubility, steep positive temperature
coefficients of solubility and safe use in foods and
pharmaceuticals (Deblay, 1995; Hogan et al., 1998; Le-
febvre, 1992; Michaels, 1998).
As compared with RO and MD process, the OD
process has the potential advantage which might over-
come the drawbacks of RO and MD for concentrating
fruit juice, because RO suffers from high osmotic pres-
sure limitation, while in MD some loss of volatile
components and heat degradation may still occur due to
the heat requirement for the feed stream in order to
35
30
Vapor pressure of water, mbar
25
20
15
Sucrose
10 K2HPO4
NaCl2
5 CaCl2
0 the use of a novel helically wound hollow fibre module
0 10 20 30
Wt. % Solute
Fig. 3. The vapour pressure/concentration relationships for sugar and
salt solution at 25
C.
B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324 311
maintain the water vapour pressure gradient. OD, on
the other hand, does not suffer from any of the problems
mentioned above when operated at room temperature.
5.2. Effect of operating conditions on the OD flux
Sheng et al. (1991) studied the effect of operating
conditions (juice flow rate, juice concentration and
temperature) on the OD flux during the concentration of
apple, orange and grape juice through a PTFE mem-
brane with pore size of 0.2 lm and an overall thickness
of 100 lm. The results showed that the OD flux de-
creased with the increase of juice concentration and it
depends strongly on the osmotic pressure difference Dp
between the aqueous streams. When Dp decreased of
33%, from 416 atm (low juice concentration) to 280 atm
(high juice concentration), a five-fold decline in OD flux
was observed.
Vaillant et al. (2001) evaluated the potential of OD
for concentrating clarified passion fruit juice on an in-
dustrial scale, taking into account the relevant impact
on the overall product quality. A pilot plant containing
a 10.2 m2 of PP hollow fibres module was used to con-
centrate passion fruit juice up to a total soluble solids
(TSS) content higher than 60
Brix at 30
C. Tangential
velocity, temperature and concentration of solutions
significantly affected OD flux. An average evaporation
flux of almost 0.75 kg/m2 h was obtained with water,
0.65 kg/m2 h when juice was concentrated to 40
Brix and
0.50 kg/m2 h when it reached 60
Brix. A long-term trial,
lasting 28 h, was successfully carried out without
membrane fouling. Osmotic evaporation can also be
conducted as a multistage procedure, giving a constant
evaporation flux of around 0.62 kg/m2 h when juice was
concentrated from 14 to 60
Brix. Sensory quality and
vitamin C content were well preserved in the concen-
trated juice. It was observed that the OD flux decay was
more attributable to the reduction of the stripper con-
centration at a low TSS of the feed juice, while it mainly
depends on viscous polarization (juice viscosity) when
juice concentration reached a value higher than 40
Brix.
Cassano, Jiao, and Drioli (2002) and Cassano et al.
(2003) confirmed these observation during the concen-
tration of clarified kiwifruit juice and orange juice by
osmotic distillation. Operating factors that are expected
to enhance the performance of the OD process are the
use of higher temperature than ambient (to increase
the driving force, decrease the viscosity and to en-
hance the solute diffusivity) and improvement of the cell
hydrodynamic conditions in the OD module (Courel
et al., 2000; Hogan et al., 1998). Examples of this include
40 50 60 70 80 and a transverse flow hollow fibre module (Hogan et al.,
1998). Courel et al. (2000) summarized in detail the ef-
fect of the operating condition on the OD flux during
the concentration of sucrose solution (Table 4). The
312 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
Table 4
Summary of the relative effect of the various operating parameters
studied on the OD flux (Courel et al., 2000)
Operating parameters Effect on vapour flux
Solute content )10% Csalt )10% to )40%
+10% Csugar )8% to )95%
Fluid velocity +10% Qsalt +2% to +6%
+10% Qsugar Not quantified
Mean temperature +10% T +6% to +12%
Presence of DT DT ¼ 10
C Pure water: +75%
55–65 w/w% sucrose:
6 10%
Csalt ¼ concentration of brine solution, Csugar ¼ concentration of sugar
solution, Qsalt ¼ velocity of brine solution, Qsugar ¼ velocity of sugar
solution, T ¼ temperature.
solute content, both salt and sugar, is the most influ-
encing variable on mass transfer.
5.3. Effect of OD on the retention of fruit juice compo-
nents
Barbe, Bartley, Jacobs, and Johnson (1998) tested
nine types of hydrophobic microporous membranes for
their influence on the retention of a range of volatile
organic species when model aroma aqueous solutions
were subjected to osmotic distillation. Similar studies
were also carried out on Gordo grape juice and Valencia
orange juice. GC-MS head-space analyses of the feed
materials, coupled with SEM and image analyses of the
used membranes, indicated that lower organic volatiles
flux to water flux ratios occurred when pore sizes at the
membrane surface were relatively large. Membranes
having relatively large pore sizes at the surface have
been shown to be associated with higher organic vola-
tiles retention per unit water removal than those with
smaller surface openings. A simple model based on
differences in their resistances to organic volatiles
transport has been proposed. Accordingly, pores with
larger diameters at the membrane surface allow greater
intrusion of the liquid feed and brine streams with a
resulting increase in the thickness and hence resistance
of the boundary layer at the pore entrance. On the basis
of this study it can be concluded that the utilization of
membranes with large surface pore diameters may be
beneficial in laboratory and industrial applications of
osmotic distillation in which the retention of volatile
flavour/fragrance components is desirable for product
quality.
Shaw et al. (2001) evaluated concentrated orange and
passionfruit juices prepared by OD distillation in terms
of retention of flavors. Both juices were concentrated
three-fold to 33.5 and 43.5
Brix, respectively, in a pilot
scale osmotic evaporator containing 10.3 m2 of PP
hollow fibers. Quantitative headspace gas chromato-
graphic analysis of 20–35 volatile components showed a
loss of about 32% of volatile components in orange and
about 39% in passionfruit juices (Tables 5 and 6). As
seen from Table 5, during the OD processing of orange
juice, the sample A had two components, hexanol and
nonanal increased and the sample B had six components
(mostly alcohols) which increased. For both orange and
passionfruit, sensory evaluations using triangle differ-
ence tests showed a significant difference between the
initial juice and the reconstituted concentrate. In orange
juice, a trained taste panel was used to evaluate six
specific flavour characteristics in the two juices. The
characteristics evaluated were green, fresh orange, fru-
ity/floral, peel oil, cooked/processed and terpene. There
were no significant differences found by the panel be-
tween the juices in any characteristic, but the average
flavour score for each characteristic was slightly lower in
juice from concentrate than in the initial juice.
Transfer of three juice aroma compounds (ethyl bu-
tyrate, hexyl acetate and hexanol) in very diluted aque-
ous solution was recently evaluated during the
concentration by OD with PTFE plate membrane under
various operating conditions (Ali, Dornier, Duquenoy,
& Reynes, 2002). The results showed that the transfer of
volatiles depends on the nature of compound but also
on the operating conditions. By decreasing the circula-
tion velocity or the temperature, it is possible to slow
down the transfers significantly. Experimental kinetics
can be characterized by a global coefficient of transfer
which connects flux to the bulk concentrations. There-
fore, a more detailed approach of the phenomena which
govern the mass transfer of juice volatiles must be un-
dertaken to better optimize the process.
5.4. OD membranes
The most well-known module designed for OD is
the Hoechst-Celanese Liqui-Cel membrane contactor
00
(Liqui-Cel Extra-Flow 2.5 · 8 , effective surface area
1.4 m , effective area/volume 29.3 cm2 /cm3 , fibre potting
2
material polyethylene, maximum transmembrane dif-
ferential pressure 4.08 bar, temperature operating range
1–40
C) containing microporous polypropylene follow-
fibres of Celgard membrane. These fibres are approxi-
mately 0.3 mm in external diameter with a wall thickness
of about 0.03 mm; they have a mean pore diameter of
about 30 nm and a porosity of about 40%.
Durham and Nguyen (1994) studied the concentra-
tion of tomato juice by OD, using the Gore-tex PTFE
membrane and the Gelman 11104/2TPR (a crosslinked
acrylic fluorourethane copolymer). A fouling effect, due
to some lipid constituents of the tomato juice, was re-
ported. Furthermore, several membrane cleaning
methods were evaluated. The Gelman 11104/2TPR was
found to be suitable for the concentration of tomato
juice by OD. It would be cleaned with P3 Ultrasil 56
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324 313

Table 5
Quantities (in mg/l) of 35 volatile compounds in orange juice before and after osmotic evaporationa (Shaw et al., 2001)
Compounds Sample A Sample B
b
Initial Conc. Initial Conc.b
c
Acetaldehyde 3.3 1.9 4.0 3.7
Methanolc 24 12 24 9.5
Ethanolc 429 292 535 419
Ethyl acetatec 0.20 0.12 0.25 1.05
2-Methypropanol 0.01 0.11 0.04 0.18
Butanol 0.06 0.03 0.25 0.16
Penten-3-ol 0.06 0.03 0.02 0.01
Penten-3-one 0.04 0.02 0.07 0.03
Penten-2-ol trd trd tr tr
Ethyl propinate 0.01 0.01 0.01 0.02
Methyl butanoate 0.03 0.01 0.04 0.01
3-Methylbutanol 0.06 0.05 0.29 1.04
2-Methybutanol 0.01 0.01 0.04 0.01
Pentanol tr tr tr tr
Hexanal 0.63 0.01 0.64 0.12
(E)-2-hexenal 0.62 0.62 0.62 0.61
(Z)-2-hexenale 0.26 0.15 0.18 0.12
Hexanol 0.07 0.20 0.04 0.4
Heptanal 0.05 0.01 0.0 tr
a-Pinene 1.53 1.35 0.99 1.14
Sabinene 0.18 0.16 0.09 0.09
Myrcene 8.3 7.4 6.3 7.23
Ethyl hexanoate 0.05 0.03 0.05 0.03
Octanal 0.81 0.4 0.48 0.22
a-Phellandrene 0.28 0.25 1.05 1.07
Limonene 276 247 204 240
Linalool 1.42 1.10 1.55 0.93
Nonanal 0.11 0.18 NDf NDf
Ethyl octanoate 0.36 0.14 0.25 0.10
4-Terpineol 0.21 0.17 0.33 0.24
Decanal 0.87 0.76 0.42 0.31
Carvone 0.23 0.10 0.10 0.05
Perillaldehyde 0.08 0.05 0.06 0.03
Caryophyllene 0.37 0.36 0.40 0.42
Valencene 5.6 3.4 16.7 8.7
Total oilg 420 300 250 280
a
Values determined by dynamic headspace GC unless otherwise noted.
b
Juice reconstituted to the Brix value of the initial juice prior to analysis.
c
Values, determined by static headspace GC with a polar column.
d
tr ¼ trace, too small to quantify.
e
A minor amount of (E)-2-hexenol eluted with this component.
f
ND ¼ not detected.
g
Determined by the Scott oil method.

(Henkel, UK). The OD flux was maintained and there
was no salt leakage during repeated fouling/cleaning
trials.
Some fruit juices, especially citrus juices, contain peel
oils and other highly lipophilic flavor components that
reduced their surface tension and promote wetting of
hydrophobic surfaces. Components of solutions used to
clean membrane devices often contain surface active
agents and/or residuals from these solutions, that might
also promote membrane wetting. Such liquids, in most
cases, will promote wet-out and liquid penetration into
PP membranes (Hogan et al., 1998). Development work
currently is underway to attempt to produce hollow
fiber microporous membranes from more hydrophobic
polymers such as PTFE or PVDF or to make laminate
membranes that prevent liquid intrusion without im-
peding vapour transport (Hogan et al., 1998; Mansouri
& Fane, 1998; Michaels, 1999). It was found that the
hydrophilic polymer film of adequately high intrinsic
water permeability and virtual impermeability to mac-
rosolutes and colloids, which can be fabricated in suffi-
cient thickness, is suitable for this laminate (Michaels,
1999). Such hydrophilic polymers include those com-
posed of esters and ethers of cellulose; crosslinked gel-
atin; gelatinized starch; chitin; agar; alginic acid;
crosslinked polyacrylamide; poly (hydroxyethyl) meth-
acrylate; crosslinked polyvinyl alcohol. Michaels (1999)
reported that commercially available cellophane
314 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324

Table 6 namely perfluro-2,2-dimethyl-1,3-dioxole (PDD), can be

Quantities (in mg/l) of 22 volatile compounds in passionfruit juice formed into non-porous gas membranes, which provide
before and after osmotic evaporationa (Shaw et al., 2001)
acceptable transmission rates for OD. Osmotic distilla-
Compounds Initial Conc.b tion utilizing such high free volume, non-porous gas
c
Acetaldehyde 2.5 2.1 membranes, as a thin layer on the feed side of com-
Methanolc 16 12
mercial microporous membranes, can concentrate pulpy
Ethanolc 307 57
Ethyl acetatec 0.31 0.11 fruit juices and especially, limonene-containing juices,
2-Methypropanol 0.06 0.03 such as orange juice. The process can be operated at
Butanol 0.06 0.05 high flux for long durations between membrane clea-
2-Methybutanol 0.38 0.22 nings. Additionally, less contamination of the strip so-
Methyl butanoate 0.007 0.003
lution into the feed juice occurs to provide a high quality
Hexanald 0.06 0.02
Hexanol 0.14 0.09 concentrate (Bowser, 2001).
a-Pinene 0.27 0.23 Surface morphology changes of hydrophobic Celgard
Benzaldehyde 0.004 0.002 2500 and Accurel 1E-PP membranes during initial
Sabinenee 2.23 1.54 contact with water were examined using scanning elec-
Myrcene 0.69 0.58
tron microscopy (SEM) and image analysis (Barbe et al.,
Ethyl hexanoate 0.13 0.08
Octanal 0.032 0.008 1998). The surfaces of both membranes showed
Hexyl acetate 0.017 0.010 increases in several of the following morphology pa-
Limonene 25 21 rameters after 72 h of contact: porosity, pore area, pore
c-Terpinene 1.37 1.14 length, pore breadth, pore equivalent diameter and pore
(E)-linalool oxide 2.2 1.2
spread factor. This was attributed to non-wetting in-
Linalool 0.29 0.19
4-Terpineol 0.04 0.03 trusion of the water meniscus into some pores with a
Total oilf 30 20 resulting enlargement of pore entrances. The results also
a
Values determined by dynamic headspace GC unless otherwise suggested that the larger pores became larger and the
noted. smaller pores became smaller. A model based on more
b
Juice reconstituted to the Brix value of the initial juice prior to effective intrusion of liquid water into the larger pores
analysis. and a resulting lateral displacement of the fibrils that
c
Values determined by static headspace GC with a polar column.
d formed the boundaries with neighbouring, smaller pores
Ethyl butanoate also present.
e
b-Pinene also present. was invoked to explain the latter observation. Celgard
f
Determined by the Scott oil method (Scott & Veldhuis, 1966). 2500 membrane was also subjected to contact with 30%
w/w CaCl2 solution but no significant morphology
change was observed in this medium after 72 h. The
membranes, as thin as 12.5 lm, would probably be absence of a morphology change was attributed to a
suitable for this purpose. The hydrogel-film-side of the lower degree of intrusion of the CaCl2 solution relative
laminate should be in contact with the feed liquid or to that of water due to the higher surface tension of the
solution to be concentrated. former.
Mansouri and Fane (1999) developed modified hy-
drophobic membranes that are tolerant to oil feeds (e.g. 5.5. Effect of UF pretreatment on the evaporation flux
limonene solution) by coating the feed side of the
commercial membranes (including the Celgard 2500, UF of single strength Gordo grape juice using
Millipore GVSP and the UPVP) with a thin layer of membranes with nominal pore diameters of 0.1 lm or
polyvinylalcohol (PVA). The tolerance of laminates was less (Osmonics Sepra CF flatsheet unit, membrane area
evaluated against oil containing feeds in short and long 0.0155 m2 ) result in appreciable osmotic distillation flux
term experiments. For concentrations up to 1 wt.% increases over that observed for juice not subjected to
limonene solution laminate membranes remained un- the UF (Bailey, Barbe, Hogan, Johnson, & Sheng,
changed when the experiment continued for up to 24 h. 2000). This has been attributed to a reduction in the
In contrast, membranes without the hydrogel coating viscosity of the concentrated juice-membrane boundary
were wetted out very rapidly by the oily feed. Due to layer where the solute concentration is highest and the
their high water content and the small thickness of the effect of protein removal is expected to be most pro-
hydrogel, the water permeabilities for laminate mem- nounced. In addition to the advantage of a higher OD
branes in most cases were not significantly lower than flux in permeate concentration, the fermentable sugars
the ones for uncoated substrate. This means that lami- content of standard 68
Brix concentrate can be achieved
nates with comparable permeability and superior resis- at a significantly lower Brix value, thereby providing a
tance to organic solutions should be fabricated. possible means of reducing the handling of highly vis-
Recently, it has been found that an amorphous co- cous streams. UF pretreatment results in a small in-
polymer of a certain perfluorinated dioxole monomer, crease in juice surface tension with a consequent
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324 315

reduction in the tendency for membrane wet-out to

occur.

5.6. Process design

The most important design parameters of an OD

process for concentration of an aqueous feed are: (1) the
required plant capacity in daily volume of feed to be
concentrated; (2) the solute concentrations in the feed
and final concentrate; (3) the water vapour pressure/
concentration relationship for the feed stream; (4) the
water vapour pressure/concentration relationship for the
strip solution and (5) the intrinsic water vapour per-
meability of the OD membrane (Hogan et al., 1998). A
schematic for a simple juice-concentration unit is shown
in Fig. 4.
The process employs partial batch recycle on the feed
side and continuous countercurrent recycle plus evapo-
rative reconcentration of the brine strip. The contactors
can be arranged in a series, parallel, or series-parallel
array.
Recently, Nii, Jebson, and Cussler (2002) have built
and tested a flat-sheet membrane evaporator, made of
flat sheet of thin, non-porous membranes (supplied by
GKSS, Max-Plank Strasse, D-21502 Geesthact, Ger-
many) for removing water from dilute feed streams like
milk and orange juice. In the membrane evaporator, Fig. 5. Schematic diagram of (a) the membrane evaporator and (b) the
shown schematically in Fig. 5a, the membrane is flow channel (Nii et al., 2002).
mounted between two 0.2 cm gaskets which form flow
channels for liquid and vapour. Each 0.2 cm gasket
other forms of ‘‘membrane distillation’’. Such a mem-
defines a flow channel. In some cases, the flow channel
brane evaporator may offer advantages to conventional
was straight; in others, it had the tortuous shape shown
evaporator, including larger surface area per volume
in Fig. 5b. The top of the vapour channel is solid; the
and high selectivity. The membrane evaporator retains
bottom of the liquid channel is a piece of metal foil.
flavors effectively. Because it has an overall vapor phase
Steam condensing on the other side of the metal foil
mass transfer coefficient of about 1 cm/s, it is only 68%
supplies energy to evaporate water through the mem-
efficient: only about 0.68 kg water is evaporated per kg
brane. This vapour flows out of the apparatus; if de-
steam condensed. This efficiency should be over 95% for
sired, its flow may be enhanced with an inert gaseous
a membrane which is 10 times more permeable. This
sweep stream. Therefore, the energy for the water’s
efficiency must be improved for this system to be prac-
evaporation comes from steam channels next to the feed
tical. It seems possible by using a thinner, water selective
channels, so that the operation differs sharply from
membrane (Nii et al., 2002).
Although OD has been studied mainly in the labo-
single strength
ratory at present, concentration of fruit juices by OD
juice diluted brine have been successfully demonstrated at pilot facilities in
reconcentrated condenser Melbourne and Mildura, Australia. The Melbourne
osmotic distillation
membrane array
brine plant contains two 19.2 m2 Liqui-Cel modules and it can
concentrate 50 l/h of juice to 65–70
Brix. The Mildura
condensate
to waste plant, designed by Vineland Concentrates (a subsidiary
of the Wingara Wine Group) and Celgard LLC, con-
evaporator
tains 22 4 in. · 28 in. Liqui-Cel modules (total interfacial
area 425 m2 ). It operates at 30–35
C and 2 atm. Color,
flavor and aroma retention are good, but module
cleaning is an issue (Hogan et al., 1998).
juice concentrate
The potential and suitability of OD for concentrating
Fig. 4. Typical OD system for juice concentration (Hogan et al., 1998). fruit juices have been well proved. The flux losses
316 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
Table 7
Advantages and disadvantages of MD and OD applied to the concentration of fruit juices
Advantages
Technical aspects
• Techniques suitable for heat-sensitive products
• A 60% of dry matter can be reached in the concentrated product
• Modularity, easy scale-up
• Possibility to treat solutions with high level of suspended solids
• Possibility of using modules in series, the same unit can
concentrate several different products
• Low temperatures
• Low operating pressures
• No fouling problems, constant permeate flux in time
• New technologies based on the use of conventional
well-tested materials
Economical aspects
• Low investment cost
attributable to viscous polarization are sufficiently low
to render the OD process both technically and eco-
nomically feasible for industrial production of high de-
gree Brix juice concentrate. A serious problem
associated with commercial application of OD in con-
centrated fruit juice processing is the management of the
diluted brine strip. It is essential to re-use the brine
several times before it is removed from the process.
Corrosion and scaling makes expensive the regeneration
of exhausted brines that can be hardly accomplished by
conventional evaporators. In addition to heat evapora-
tion, the effective methods need to be developed for the
concentration of the osmotic brine. Thompson (1991)
reported solar ponding or even reverse osmosis and
pervaporation could be used to re-concentrate the di-
luted stripper. Petrotos and Lazarides (2001) suggested
the use of electrodialysis as the most suitable way to the
regeneration of the NaCl brine.
Table 7 summarizes the advantages and the disad-
vantages of the MD and OD applications in fruit juices
production.
6. Integrated membrane processes
The potential for concentrating fruit juice by inte-
grated membrane processes, particularly for industrial
production of high quality concentrated juices, appears
today very attractive. Because fruit juices such as orange
juice have high solids and pectin content, they create a
very viscous stream when directly submitted to con-
centration by RO or OD, which results in a lower per-
meate flux. Also, using a single-stage RO system it
cannot reach concentrations larger than 25–30
Brix due
to higher osmotic pressure limitation. If RO combines
MF or UF being used for separating the suspended
solids and pectins from juices, the viscosity decreases
and the flux increases. Volatiles (alcohols, aldehydes,
Disadvantages
• New technology that requires an evaluation at industrial level,
flexibility to be evaluated
• Low evaporative capacity (3 l/m2 h) with a long time of treatment
• Necessity of an inactivation enzyme pre-treatment
• Production costs higher than the thermal evaporation
• High cost of membrane replacement
esters) in fruit juices may have lower retentions in the
retentate as they tend to be associated with the serum
(Rao, Acree, Cooley, & Ennis, 1987). Therefore, the
benefits including high quality product and lower energy
consumption could be achieved with integrated mem-
brane processes.
Lawhon and Lusas (1987) described the use of UF to
separate juice into the pulp and serum prior to heat
treatment and help to minimize flavor loss and deteri-
oration. The serum containing almost all the flavor and
aroma components is concentrated by RO to levels
above 42
Brix. The retentate containing all the sus-
pended solids, pectins and the spoilage microorganisms
is quickly heated to inactivate the spoilage microor-
ganisms, and then recombined with RO concentrate.
The reconstituted juice is claimed to have a quality close
of fresh juice. Based on the Lawhon and Lusas patent
(1987), Cross (1989) described a commercial design of
UF–RO process for membrane concentration of orange
juice. After, it has been reported (Walker, 1990) that
Separasystems LP, a joint venture between FMC and
Du Pont, has developed a combined membrane process,
which is called FreshNote system, that could concen-
trate orange juice to 60
Brix while almost retaining the
fresh juice flavors. The process involves a plurality of
two-stage RO system after MF or UF process, the first
stage employing high-rejection membranes and the sec-
ond employing low-rejection membranes (Fig. 6). The
orange juice is initially clarified using MF (i.e., 0.2 lm)
and/or UF (i.e., 20 kDa). The permeate is fed to a high-
rejection RO stage (i.e., three units in series, 10.2–13.5
MPa, 10
C) equipped with polyamide hollow fiber
membranes having 98.5% salt rejection. The retentate
leaving the final high-rejection RO unit is fed to low-
rejection RO. For example, there can be two low-rejec-
tion units in series, the first membrane having a 93% and
the second with a 97% salt rejection. The retentate of the
first having a sugar concentration of 50
Brix is the feed
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
UF HR RO LR RO
juice
Pasteurizer Concentrate
Fig. 6. Schematic diagram of the combined high-retention (HR)–low-
retention (LR) RO process for juice concentration (Walker, 1990).
of the second unit. The permeate from the first, having a
sugar concentration of 18
Brix, and that of the second,
with a sugar concentration of 40
Brix, can be combined
to form a 31
Brix permeate which is recycled to the feed
of the first high-rejection unit. The retentate from the
second low-rejection unit having a sugar concentration
of 63
Brix is mixed with the pasteurized UF retentate to
make a blended 54
Brix product. Finisher pulp, peel oil
and/or essence can be added to produce a concentrated
product tailored to particular market needs. The re-
constituted juice consistently scored higher in flavor
than any thermally concentrated product, and is nearly
indistinguishable from the freeze-concentrated and the
feed juice. Although production costs are higher for the
product compared with the current blended concen-
trates, this process is significantly cheaper than freeze
concentration (Cross, 1989). Also, this system has been
installed and operated in Japan in 1989 (Walker, 1990;
Walker & Ferguson, 1990). This plant is designed to
process 7.5 m3 /h of single strength Satsuma mandarin
juice, yielding about 2 m3 /h of concentrate.
This concept has also been implemented commer-
cially for apple juice concentrate (Mans, 1992). Apple
juice is first submitted to centrifuges and then to tubular
polymeric membrane (0.2 lm) for complete clarification.
The system contained 51 RO hollow fiber modules
(4-foot-long) piped in up to eight stages comprising
high-rejection and low-rejection units. The 58–60
Brix
concentrate is pumped through a scraped surface heat
exchanger where it is cooled from 21 to 2
C followed by
bulk cold storage and a final aseptic packaging opera-
tion. Nabetani (1996) developed an integrated RO–NF
membrane system for highly concentrated fruit juice.
The feed juice is firstly concentrated to 30
Brix with RO
membranes and the RO retentate is then concentrated to
above 45
Brix using NF membranes. The NF permeate
is recycled to the feed of RO unit. This system is shown
to be suitable for concentrating various fruit juices, with
advantages of not only retaining the fresh juice flavor,
but also of minimizing energy consumption. For ex-
ample, using this system to concentrate fruit juice from
10 to 45
Brix, energy savings of 1/8 and 1/5 by this
317
system can be obtained when compared with evapora-
tion and freeze concentration, respectively.
The theoretical basis for these processes mentioned
above relies on the understanding that the effective os-
motic pressure to overcome is not equal to the osmotic
pressure of the retentate, but is rather determined by the
concentration difference existing across the membrane
(Girard & Fukumoto, 2000). The use of low-retention
membranes allows to reach high retentate concentration
values because part of the solute passes the membrane,
thus reducing the effective osmotic pressure difference.
Low retention means that a large amount of solute is
lost in the permeate. The solute recovery can be ac-
complished by recycling the permeate stream to a high-
retention module, which also acts as a feed preconcen-
trator. The key variable is the membrane retention, re-
lated to the solute/solvent permeability ratio. Hollow
fibers are better suited than spiral wound modules for
this process. Hollow fibers have lower concentration
polarization effects and lower fluxes are counterbalanced
by larger packing density (Walker, 1990). Recovery ra-
tios as large as 15–20% can be achieved for product
concentration of 55–60
Brix. The membrane area nee-
ded to concentrate juices to 60
Brix with a hollow fiber
system is about twice the area needed to concentrate up
to 20
Brix with a conventional RO system, while the
energy requirement is approximately three times larger
(Gostoli, Bandini, Di Franscesca, & Zardi, 1995).
However, an accompanying disadvantage is the loss of
important components of the juice. To overcome this
problem, a fairly complex processing scheme must be
adopted (Watanabe, Nabetani, & Nakajima, 1990).
A combined membrane-evaporation process was ap-
plied to develop an improved method for concentrating
orange juice (Johnson, 1993). An UF membrane was
used to separate the juice into pulpy suspended solids
(retentate) and clarified juice (permeate). The mem-
brane-clarified clear juice was then concentrated by a
conventional evaporative method using a TASTE
(thermally accelerated short time evaporator) evapora-
tor. The pulpy retentate may be pasteurized by a heat
exchanger. The clear juice concentrate from the com-
bined membrane-evaporation technique can reach a
higher degree Brix (>80
Brix) than traditional whole
juice concentrate processed in a TASTE evaporator
under similar conditions (Hernandez, Chen, Johnson, &
Carter, 1995). Higher degree Brix orange juice concen-
trates offer significant energy savings during storage and
distribution due to reduced volume and increased mi-
crobial stability at higher temperatures (Crandall &
Graumlich, 1982). The resulting clear juice concentrated
can also be further utilized to formulate new fruit bev-
erage juice blends. For example, it is ready to pour to
yield six-fold concentrate at freezer temperatures about
)15
C. In contrast, the traditional three-fold frozen
juice concentrate becomes frozen at common domestic
318 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
freezer temperatures of )5 to 15
C and it is inconve-
nient to pour and to mix with water (Chen, 1998).
Because clear orange juice concentrate produced by
the combined membrane-evaporation technique is a new
type of product and this highly concentrated (>80
Brix)
clear orange juice resembles honey or sugar syrups,
which are usually stored and marketed at room tem-
perature, it is desired to evaluate the storage stability of
this product at temperatures above freezing. This could
feasibly replace conventional frozen storage of orange
juice concentrates. A preliminary study (Lee, Johnson,
Barros, & Chen, 1994) with this high-density clear or-
ange juice concentrate of 80
Brix indicated that major
changes in clear orange juice concentrate during storage
were due to chemical reactions rather than microbial
deterioration. Recently, first-order rate constants for
non-enzymic browning and ascorbic acid loss of mem-
brane-clarified clear juice during conventional evapora-
tive processes at 70.3–97.6
C have been presented
(Johnson, Braddock, & Chen, 1995). Lee and Chen
(1998) studied rates of vitamin C loss and discoloration
in clear orange juice concentrate (80.2
Brix) produced
by the combined membrane-evaporation technique at
storage temperatures of 4, 14, and 24
C for 19 weeks.
Absorption at 420 nm and CIE L , a , b color para-
meters were determined to evaluate color changes due to
non-enzymic browning during storage. Calculated val-
ues of reaction rate constants indicated that vitamin C
degradation occurred slowly in clear orange juice con-
centrate at 4
C. Rates of vitamin C degradation ranged
from 4.79 · 104 to 3.13 · 102 mg/100 ml per week. The
activation energy for vitamin C degradation was on the
order of 34.3 kcal/g mol. Main color changes in stored
clear orange juice concentrate in amber glass vials were
due to increases in b value and chroma.
The coupling of UF and evaporation for concen-
trating passionfruit juice has also been tested by Yu and
Chiang (1986). Pretreatment of the juice prior to UF
with pectinase, centrifugation, and pasteurization could
improve the UF flux of 50%. Permeate of passionfruit
juice from UF had a higher evaporation rate than juice
with solid due to improved heat transfer. The evapo-
rated concentrate could be reblended with UF retentate
to form a final concentrated product. Although the
process resulted in 20% flavor losses, the reconstituted
juice and the fresh juice were not significantly different in
overall acceptance.
An integrated membrane process for producing apple
juice and apple juice aroma concentrates has been pro-

posed by Alvarez et al. (2000). The process scheme is
shown in Fig. 7. It involves the following operations: an
integrated enzyme membrane reactor to clarify the raw
juice; reverse osmosis (RO) to preconcentrate the juice
up to 25
Brix; pervaporation (PV) to recover and con-
centrate aroma compounds; a final evaporation step to
concentrate apple juice up to 72
Brix. These operations
Fresh juice
Retentate and
20˚C Enzyme recirculation
EMR
Clarified juice
water 20-25˚C
RO Preconcentrated
Juice, 25˚Brix
PV
20˚C
Dearomatized juice
Aroma
Evaporation compounds
60-80˚C
Concentrated Juice
(70-72˚ Brix)
Aroma enriched
concentrated juice
Fig. 7. Integrated membrane process for the production of clarified

apple juice concentrate and apple juice aroma (Alvarez et al., 2000).
EMR ¼ enzymatic membrane reactor; RO ¼ reverse osmosis;
PV ¼ pervaporation.
were tested in laboratory and pilot plant units. Pro-
mising results were obtained with the membrane oper-
ations involved. It has been shown that a membrane
reactor could be used for the production of clarified
apple juice with lower enzyme cost. The use of immo-
bilized enzyme resulted in better performance with
respect to fouling and cleaning. Permeate flow of 75–110
l/h and concentration value of 25.5–26.6
Brix were ob-
tained in RO unit. The flux and NaCl rejection did not
decrease significantly after three weeks of continuous
operation with apple juice. Rejection of aroma com-
pounds exceeded 90% for most compounds considered.
High overall enrichment factors in the range 100–1000
and overall mass transfer coefficients in the range 5–500
kg/m2 h were achieved in PV process using POMS-PEI,
POMS-PVDF and PDMS-PT1100 membranes. Fouling
did not give rise to any detectable problems and cleaning
did not significantly affect the performance of the
membranes. Organoleptic evaluation of the clarified and
RO concentrate was excellent in terms of odour and
flavor. The final products were more clear and brilliant
than apple juice produced by conventional methods.
In order to have an economic process assessment, the
pilot plant units were assembled into an integrated unit
and operated with raw apple juice. Process design basis
was to produce 2500 kg of apple juice per hour. Taking
into account the periods when apples are available, 3500
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324 319

Table 8

Capital investment and manufacturing costs for the conventional and integrated membrane process (Alvarez et al., 2000)
Item Cost (EURO)
Conventional process Membrane process
Investment
Apple storage 1.7 · 105 1.7 · 105
Washing and inspecting apples 0.1 · 105 0.1 · 105
Milling apples 0.4 · 105 0.1 · 105
Clarification 6.4 · 105 3.9 · 105
Preconcentration (RO) 1.3 · 105
Aroma compounds recovery and apple juice concentration 4.2 · 105 5.1 · 105
Total 13.73 · 105 12.48 · 105
Total capital investment 47.72 · 105 43.38 · 105
Operating costs
Raw material (apples) 810.0 EURO/ton conc. 810.0 EURO/ton conc.
Membranes 19.7 EURO/ton conc.
Others 99.9 EURO/ton conc. 50.2 EURO/ton conc.
Total variable cost 909.9 EURO/ton conc. 839.9 EURO/ton conc.
Labor, maintenance and other fixed costs 151.9 EURO/ton conc. 145.0 EURO/ton conc.
Total manufacturing costs 1068.8 EURO/ton conc. 984.9 EURO/ton conc.

tons of apple juice concentrate would be produced an- scheme is shown in Fig. 8. By allowing brine to flow
nually in the plant. As seen from Table 8, the total through the permeate side of the membrane in a
capital investment of the new integrated membrane counter-current mode to feed, the corresponding os-
process accounts for 14% less than that of the conven- motic pressure difference can be minimized or even re-
tional process. As compared with the conventional versed. High concentration of the feed could be achieved
process, apple consumption decreased by 5% when using at moderate operating pressures that keep high enough
the integrated membrane process, due to the corre- transmembrane permeate fluxes. Membrane areas to be
sponding increases in process yield. Total manufactur- required for high solute concentration could be reduced
ing costs decreased by 8%, mainly because less energy is
required to concentrate the juice. The profitability
analysis for the conventional and integrated membrane
Concentrated Concentrated
process was shown in Table 9. The integrated membrane
sugar out salt in
process also seemed to be more advantageous on the
basis of economics than the conventional one.
Coupling RO and osmotic dehydration process for
concentrating sucrose solution has recently been pro- Enricher
posed by Karode, Kulkarni, and Ghorapade (2000), in
which the feasibility of such a technique was investi-
(a) Lean sugar in Lean salt out
gated with both theory and experiments. The process

Table 9 Concentrated
Profitability analysis for the conventional and integrated membrane sugar out

processes (Alvarez et al., 2000)
Conventional Membrane Enricher
process
(1) Revenue (EURO/year) 5.469 · 106 5.469 · 106
Lean sugar in Concentrated
(2) Annual manufacture cost 3.716 · 106 3.432 · 106 Lean salt salt
(EURO/year) Water
(3) Gross profit (a–b) (EURO/ 1.753 · 106 2.037 · 106
year)
(4) Taxes (33%) (EURO/year) 0.758 · 106 0.672 · 106 Stripper
(5) Net profit (EURO/year) 1.175 · 106 1.365 · 106
(6) Gross margin (c/a) 0.32 0.37
(7) Return on investmenta (%) 24.6 33 (b)
(8) Payback timeb (years) 4.1 3.0
Fig. 8. Osmotic dehydration coupled reverse osmosis concentration
a
Means net profit/total investment  102 . process for concentrating fruit juice (a) enricher alone and (b) enricher-
b
Means total investment/net profit  102 . stripper configuration (Karode, Kulkarni, & Ghorapade, 2001).
320 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
by the process. They concluded that the process would
be limited by permeate-side concentration polarization
and that to reduce contamination of the sucrose solution
being concentrated, a very high rejection RO membrane
would be required. The same authors further investi-
gated the concentration of sucrose solutions from 5 to
60
Brix by coupled RO and osmotic dehydration with a
hydrophobic high-rejection RO membrane in the en-
richer and a high-rejection, thin-film composite RO
membrane in the stripper. A grapher method for esti-
mating operating pressure limits in the enricher and the
stripper was discussed. The results showed that the type
of membrane used in the enricher, the operating pres-
sure of the enricher and the stripper, the ratio of the
salt-solution elution, and the flow rate of the sucrose
solution into the enricher affect the optimum salt con-
centration that should be fed into the enricher to mini-
mize the total membrane area. For a specific set of
operating pressures, the optimum salt concentration
reduced as the ratio of flow rates increases. A configu-
ration has proposed that would enable the concentra-
tion of a sucrose solution from 5% to 60% using a
natural source of brine (seawater, 3.5% salt) under a
limited maximum operating pressure of 54.4 bar (800
psi). The proposed configuration may reduce operating
and installation costs due to the management of flow
rate and pressure requirements. The seawater can be
eventually discharged back to the sea. Therefore, the
integrated RO and osmotic dehydration system can be
used to concentrate fruit juices.
The coupling of UF to MD has also examined for
concentration of kiwifruit and orange juice (Jiao, Ca-
labro et al., 1992). More recently, Cassano et al. (2002,
2003) proposed an integrated membrane processes for
the production of high quality fruit juice concentrate
such as blood orange and kiwifruit juice. As shown in
Fig. 9, UF process firstly separates fruit juices into the
serum and the pulp. The clarified juices are pre-con-
pulp pasteurizer
fruit
juice
UF RO
(10-11 ˚Brix)
evaporator
preconcentrated diluted
juice
(25-26 ˚Brix)
brine
OD
Fig. 9. Integrated membrane process for the production of concen-
trated fruit juices (Cassano et al., 2003).
centrated to 20–25
Brix by RO, and the RO retentates
are concentrated to above 60
Brix by OD using the
Liqui-Cel Extra-Flow module and Celgard micropor-
ous PP hollow fibers. The proposed process employs
continuous countercurrent recycle plus evaporative
reconcentration of the brine. The UF retentate could be
submitted to a pasteurization process and then added to
the final OD concentrate.
The stability of the antioxidant activity (TAA) during
juice processing is of interest since they play an impor-
tant role in reducing the risk of free radical related ox-
idative damage associated with a number of diseases.
Changes in ascorbic acid, phenolics and total antioxi-
dant activity during integrated membrane processing of
blood orange juice were evaluated (Galaverna et al.,
2002). The results showed that the content of these an-
tioxidant compounds besides anthocyanins and Vitamin
C remained almost the same of the feed juice during the
proposed integrated membrane process (Table 10). As
compared with the fresh blood orange juice, the contents
of anthocyanins and Vitamin C decreased by 15–20% in
the concentrate. Only 15% reduction of TAA was found
in the blood orange juice concentrate. The concentrate
retains its bright red color and its pleasant flavor.
Successful application of integrated membrane oper-
ations in fruit juice concentration has been developed by
the Australian company (Wingara Wine Group, Mel-
bourne). A hybrid pilot plant where UF/RO and OD are
integrated has been realized. It consists of UF and RO
pretreatment stages, an OD unit and a single-stage brine
evaporator. A first-stage UF treatment for removal of
suspended solids and colloids is also desirable to mini-
mize possible fouling of either RO or OD units. This
plant concentrates fresh juices up to 65–70
Brix and has
a capacity of 50 l/h. Being athermal, OD allows con-
centrating without product deterioration or loss of fla-
vors (Hogan et al., 1998).
Hogan et al. (1998) reported a total process cost of
OD concentration on the order of $1.00/l of concentrate.
From one liter of fresh juice, it is possible to achieve
about 200 ml of 70
Brix concentrate. The value of this
concentrate is between $2.50 and $7.50/l. From these
data, the economical benefits of the integrated mem-
water brane process seem evident.
Table 11 summarizes the main advantages and dis-
advantages of membrane concentration techniques dis-
concentrated
cussed with respect to the evaporation process. The low
brine (CaCl2 ) relatively permeation fluxes attainable with direct os-
mosis, OD and MD (when operating at low tempera-
tures) with respect to those achievable with the RO
process would appear to make these processes eco-
nomically uncompetitive. When, however, the product
concentrated
juice to be concentrated is a solution containing macrosolutes
(63-65 ˚Brix)
or colloids sensitive to shear or thermal degradation
there are serious limitations to the degree of concen-
tration achievable via RO without significant product
 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324 321

Table 10
Contents of ascorbic acid, flavonoids, hydroxycinnamic acids and TAA in blood orange juice as affected by membrane processes (Galaverna et al.,
2002)
Samples Total Ascorbic Total Hesperi- Narirutin Sinapic Caffeic Ferulic p-coumaric TAA
soluble acid (mg/l) anthocya- din (mg/l) (mg/l) acid (mg/l) acid (mg/l) acid (mg/l) acid (mg/l) (mMtrolox)
solids nins (mg/l)
(
Brix)
Fresh juice 12.6 701.0 ± 2.3 56.3 ± 0.2 45.1 ± 0.1 50.7 ± 0.1 6.6 ± 0.1 6.8 ± 0.1 51.3 ± 0.1 33.5 ± 0.1 8.65
UF 12.4 636.5 ± 3.1 55.0 ± 0.2 45.5 ± 0.1 50.8 ± 0.1 6.6 ± 0.1 6.8 ± 0.1 51.7 ± 0.1 34.9 ± 0.1 8.21
permeate
UF 13.0 624.9 ± 2.5 55.3 ± 0.2 42.1 ± 0.1 49.9 ± 0.1 6.1 ± 0.1 7.0 ± 0.1 53.9 ± 0.1 33.9 ± 0.1 8.29
retentate
RO 21.4 610.6 ± 2.0 44.7 ± 0.2 46.6 ± 0.1 50.2 ± 0.1 6.0 ± 0.1 7.4 ± 0.1 51.1 ± 0.1 34.3 ± 0.1 7.47
concentrate
OD 60.6 594.2 ± 3.1 43.3 ± 0.2 46.3 ± 0.1 48.7 ± 0.1 5.6 ± 0.1 7.6 ± 0.1 51.0 ± 0.1 33.5 ± 0.1 7.33
concentrate

Table 11
Key factors of conventional evaporation and membrane concentration techniques
Process Maximum Product Evaporation Possibility of Operating Capital Energy Maturity of
achievable quality rate or flux treating different cost investment consumption technology
concentration products with
(
Brix) the same
installation
Evaporation 80 Very poor 200–300 l/h No Moderate Moderate Very high Developed
Reverse 25–30 Very good 5–10 l/m2 h No High High High Developed
osmosis
Direct 50 Good 1–5 l/m2 h Yes High High Low Developing
osmosis
Membrane 60–70 Good 1–10 l/m2 h Yes High Moderate Low Developing
distillation
Osmotic 60–70 Very good 1–3 l/m2 h Yes High Moderate Low Developing
distillation

deterioration or costly process equipment. For these 7. Conclusions

applications OD has important advantages.
OD is inherently more costly for concentration of
aqueous mixtures than such conventional process as
evaporation or RO. However its capacity to remove
selectively water from other low molecular weight sol-
utes and, thus, to yield concentrates of superior quality
is an additional advantage of the OD process. On the
other hand, RO, where it can be carried out at relatively
low pressure, is the cheapest system for water removal
for feeds of low solute concentration. Losses in volatile
and non-volatile flavours, fragrances and other essential
microsolutes can be minimized by limiting the fraction
of water removed. Acceptable concentrates can be pro-
duced economically in this manner. Therefore, an inte-
grated process involving preconcentration of the feed by
RO followed by further concentration by OD or MD
should yield a high-solids product concentrate of quality
comparable to that achieved by OD alone but at sig-
nificant reduction in processing cost (Hogan et al.,
1998). Direct osmosis hydrophilic membranes are
cheaper than MD and OD membranes; they have a
longer life cycle if compared with hydrophobic mem-
branes used in MD and OD.
The potential advantages of membrane concentration
techniques over conventional evaporation for concen-
trating fruit juice have been successfully demonstrated,
including improved product quality, easily scaled up and
lower energy consumption, but they are generally limited
by the fouling and lack of longer durability of mem-
branes. Although today fruit juice concentration by
membranes may be more expensive than evaporation,
with the enlargement of the world’s fruit juice market
and the request of product quality, commercial appli-
cations of membrane processes in concentrated fruit
juice processing, especially integrated membrane system,
will expand in the near future. However, in order to gain
a foothold in the juice industry, studies on developments
of new membranes which are both highly selective and
permeable, or robust and stable in long-term application
for juice processing, and improvements of process engi-
neering including module design and process design and
optimization need to be carried out in detail. It can be
anticipated that the use of membrane processes will bring
great changes in the juice industry in the future, with the
development of membrane science and technology.
322 B. Jiao et al. / Journal of Food Engineering 63 (2004) 303–324
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