Journal of Food Engineering 63 (2004) 97102

www.elsevier.com/locate/jfoodeng

Evaluation of reverse osmosis and osmotic evaporation

to concentrate camucamu juice (Myrciaria dubia)
R.B. Rodrigues a, H.C. Menezes a, L.M.C. Cabral b, M. Dornier c,*
,
G.M. Rios d, M. Reynes c
a
UNICAMP, Food Technology Department, C.P. 6041, 13083-970 Campinas, SP, Brazil
b
EMBRAPA, Food Technology Department, av. das Americas 29501, 23020-470 Rio de Janeiro, RJ, Brazil
c
CIRAD-FLHOR/ENSIA-SIARC, av. Agropolis, TA 50/PS4, 34398 Montpellier Cedex 5, France
d
IEM, Universit

e Montpellier II, C.C. 047, Place Eug
ene Bataillon, 34095 Montpellier Cedex 5, France
Received 10 March 2003; accepted 21 July 2003

Abstract
This study presents a rst evaluation of the potential of two membrane processes for the production of concentrated camucamu
juice with high vitamin C content. A claried camucamu juice at around 64 g kg 1 of total soluble solids (TSS) with an average
ascorbic acid content of 11 g kg 1 was subsequently concentrated by reverse osmosis and osmotic evaporation at low temperature
(2035 C). Reverse osmosis trials were carried out in a pilot scale equipment, using a composite lm membrane with 95% NaCl
rejection. The average permeate ux obtained were between 18 and 50 kg h 1 m 2 depending on the transmembrane pressure used.
The maximum total soluble solids content reached was 255 g kg 1 at 60 bar and the ascorbic acid losses were between 8% and 18%.
Osmotic evaporation trials were carried out using a laboratory unit with a PTFE at sheet membrane with an average pore diameter
of 0.2 lm. In that case, the juice was concentrated in two steps, the rst concentrating the juice up to 250 g kg 1 TSS, and the second
from 250 to 640 g kg 1 TSS. The dierence in temperature between the juice and the brine had a great inuence on the evaporation
rate. The higher average evaporating ux obtained was 12 kg h 1 m 2 . For all experiments, the ascorbic acid losses were about 3%
that indicated the eciency of the process in maintaining the nutritional quality of the juice regarding vitamin C content. These two
membrane concentration processes are very interesting for the concentration of camucamu juice. The low concentration level that
can be reached is the major drawback of reverse osmosis. Osmotic evaporation allows to produce a concentrate with more than 10%
of ascorbic acid.
2003 Elsevier Ltd. All rights reserved.

Keywords: Camucamu (Myrciaria dubia); Concentration; Reverse osmosis; Osmotic evaporation; Osmotic distillation; Fruit juice; Ascorbic acid

1. Introduction tures. However it is interesting to note that a lot of new

Camucamu (Myrciaria dubia (H.B.K.) McVaugh) is
an amazonian fruit that oers a very high vitamin C
content, ranging from 9 to 50 g kg 1 (Andrade, 1991;
Ferreira, Ferreira, & Carvalho, 1987; Rodrigues,
Menezes De, Cabral, Dornier, & Reynes, 2001) for only
0.4 to 0.9 g kg 1 in orange. This fruit occurs naturally in
areas of periodic ooding, such as low lands around
river courses and lakes. These areas are considered in-
adequate for the commercial production of fruit cul-
*
Corresponding author. Fax: +33-467614433.
E-mail address: dornier@cirad.fr (M. Dornier).
0260-8774/$ - see front matter 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2003.07.009
studies are underway on this fruit. They aim at in-
creasing the quality of the fruits and the production
yield (improvements of the soil and plants, identication
of new species), at adapting the plants to rm land (thus
increasing possible plantation areas) and also at apply-
ing technological knowledge to obtain processed prod-
ucts that can be easily exported to regions where the
fruit is not cultivated (Dib Taxi, 2001; Rodrigues et al.,
2001; Silva & De Souza, 1996). Camucamu is not
consumed in natura due to its high acidity (Alvarado
Vertiz, 1969; Ferreira, 1986; Ferreyra, 1959). Because of
its particularly high vitamin C content, camucamu
juice is an excellent alternative for mixing with other
raw materials, thus increasing the vitaminic quality of
98 R.B. Rodrigues et al. / Journal of Food Engineering 63 (2004) 97102
dierent products like fruit juices, nectars, jams, ice
creams, yoghurts or isotonic beverages.
Because the production regions are far from the
consumption areas, the development of camucamu
juice can only be envisaged after some processing, of
course, to increase its shelf-life but also to reduce its
volume in order to decrease the transportation and
storage costs. During the classical processing of juices,
such as thermal pasteurization and concentration by
evaporation, losses of nutritional compounds such as
vitamin C can occur. In order to preserve better the
nutritional potential of this type of product, new pro-
cesses have to be investigated as alternatives to thermal
processing (Courel, 1999; Jariel et al., 1996; Rameteke,
Singh, Rekha, & Eipeson, 1993).
For food liquids concentration, membrane processes
are more advantageous than classical evaporation, due
to the possibility of operating under gentle conditions,
without aecting thermosensitive substances such as
vitamins. Among the dierent membrane techniques
that can be used to concentrate fruit juices, reverse
osmosis and osmotic evaporation are the two processes
that have the greatest potential (Courel, 1999; Girard &
Fukumoto, 2000; Medina & Garcia, 1988; Vaillant et al.,
2001).
The purpose of this work was to evaluate the interest
of these two membrane technologies to produce a con-
centrated camucamu juice with high nutritional qual-
ity. The processes were compared with respect to their
performance (ux and concentration factor) and to the
vitamin C content of the concentrated juice.
2. Material and methods
2.1. Raw material
Camucamu fruits were obtained from Par
a state,
Brazil. They were frozen and transported to Rio de
Janeiro where they were processed. After a classical
extraction step using a Bonina DF depulper, with a 0.6
mm diameter sieve, the juice was claried by an enzy-
matic treatment associated with microltration. The
enzyme treatment (100 mg l 1 of Pectinex Ultra SP-L,
NOVO NORDISK, incubation at 35 C for 30 min)
reduced the viscosity of the juice and improved the mi-
croltration process. Crossow microltration was car-
ried out in a Koch pilot unit, using 0.30 lm pore size
polysulphone tubular membranes with 0.05 m2 of ef-
fective area. The transmembrane pressure was main-
tained at 2 bar, the temperature at 22 C and the
crossow velocity at 2.6 m s 1 (Rodrigues, Cabral, &
Menezes De, 2000). During the process, the permeate
was continuously collected and the retentate stream re-
circulated. The claried camucamu juice was then
frozen and stored at )18 C until its use in the con-
centration processes.
2.2. Reverse osmosis
The reverse osmosis trials were carried out at 22 C
with a composite membrane (95% NaCl rejection) in a
DDS plate and frame module of 0.72 m2 of membrane
area. The experiments were realized at 20, 40 and 60 bar
in order to evaluate the inuence of the transmembrane
pressure in the permeate ux and in the quality of the
concentrated product. During the process the permeate
was continually removed and the retentate was kept
under re-circulation until the permeate ux decreased to
low values. At the same transmembrane pressure, the
dierence of average ux between two trials was below
1.5 l h 1 m 2 (evaluated at 40 and 60 bar).
2.3. Osmotic evaporation
Osmotic evaporation was conducted in a laboratory
pilot plant described by Courel, Dornier, Herry, Rios,
and Reynes (2000) with a juice circuit modied ac-
cording to Vaillant et al. (2001). The equipment con-
sisted in two independent compartments, one for the
juice, the other for the brine. The juice was concentrated
in a circulation loop continuously fed by raw juice. Two
positive pumps were used for the circulation of the so-
lutions in each membrane side. The temperature of the
process was controlled on both sides by thermostats.
The feed tank (2 l) was placed on a balance and the
evaporation ux was calculated from the loss of mass
registered by a computer. A CaCl2 solution from 4.0 to
5.2 mol l 1 was used as brine. Its big volume (5 l) al-
lowed to neglect its dilution during the trials. At the
same operating conditions the standard deviation of
average evaporation ux was 12% (three trials).
A Pall-Gelman TF200 membrane was chosen. This
plate and frame membrane are made of a thin PTFE
layer sealed on a PP supporting net. According to the
manufacturer, its average characteristics are 60% po-
rosity, 0.2 lm average pore diameter and 165 lm
thickness. The eective area of the membrane was
40 cm2 .
Some preliminary tests were done before processing
the claried camucamu juice, in order to evaluate the
eect of the temperature in an ambient range compatible
with a gentle treatment for a fruit juice. For these trials
an aqueous model solution consisting of around
60 g kg 1 of sucrose (Saint Louis Sucre, France) and of
15 g kg 1 of ascorbic acid (Sigma-Aldrich, France) was
used.
The concentration of camucamu juice was carried
out in two steps using the best operating conditions
determined by the preliminary assays. In the rst stage,
the original claried juice was concentrated up to
 R.B. Rodrigues et al. / Journal of Food Engineering 63 (2004) 97102 99

250 g kg 1 of total soluble solids (TSS). In the second 90

Permeate flux (l h-1 m-2)

stage, a pre-concentrated juice at 250 g kg 1 was treated 80 20 bar
70 40 bar
in order to reach more than 600 g kg 1 TSS. 60 60 bar
50
40
2.4. Analyses 30
20
10
The analyses were done in duplicate (means pre- 0
sented) according to the standard AOAC methods 0 10 20 30 40 50 60 70
(AOAC, 1984, 1997). The total soluble solids con- Time (min)
tent was determined by refractometry (refractometer
Bellingham & Stanley), the pH with a Jenco pH-meter Fig. 1. Evolution of the permeate ux during the concentration of
camucamu juice by reverse osmosis at three transmembrane pres-
and the ascorbic acid content by oxido-reduction volu- sures.
metric analysis using 2,6-dichlorophenol indophenol.
The standard deviations of the results evaluated on three
dierent samples were below 7% for all the analyses
(four tests). 20 bar
300
The colour of the juices was evaluated using colo- 40 bar
rimeters Minolta CR 3000 and Suga SM-4-CH, both 60 bar

TSS (g kg-1)
using the Lab Hunter system. For the osmotic eva- 200
poration concentrates, colour analysis was done after
dilution to the feed TSS. Viscosity was determined using 100
a Contraves Rheomat 30 concentric rheometer.
0
0 10 20 30 40 50 60 70
3. Results and discussion Time (min)

3.1. Reverse osmosis concentration
The main operating conditions and the results ob-
tained during the concentration of camucamu juice
using reverse osmosis are presented in Table 1.
A drastic decline of the permeate ux with processing
time was observed for all the trials (Fig. 1). This be-
haviour, typical of pressure-driven membrane processes,
is the consequence of the membrane fouling, the increase
of the concentration polarization (mainly due to the
viscosity increase) and also of the increase of the os-
motic pressure of the juice during the concentration
(decrease of the driving force). These three phenomena
cannot be easily identied because of the continuous
changes of the retentate characteristics during the op-
eration. The higher the transmembrane pressure, the
higher the initial ux but the most important the ux
decrease. Nevertheless, the average permeate ux were
Fig. 2. Evolution of the total soluble solids content (TSS) during the
concentration of camucamu juice by reverse osmosis at three trans-
membrane pressures.
better at high pressure increasing from about
18 kg h 1 m 2 at 20 bar to 51 kg h 1 m 2 at 60 bar.
In relation with the permeate ux obtained, the total
soluble solids content (TSS) of the juice increased more
quickly when the pressure is higher (Fig. 2). The nal
TTS increased with increasing applied pressure, espe-
cially between 40 and 60 bar. These results corroborate
those of Matta (1999) and Silva (1999) obtained with the
same equipment. They are, of course, directly correlated
to the maximum osmotic pressure that can be reached
into the product depending on the transmembrane
pressure applied. However for all the transmembrane
pressures tested the values obtained were below
260 g kg 1 , that is very low for industrial applications.

Table 1
Main operating conditions used, permeate ux and ascorbic acid losses obtained during concentration of camucamu juice by reverse osmosis
1
Trans- Tempera- Duration Total soluble solids Permeate ux (kg h m 2) Ascorbic acid content Ascorbic
membrane ture (C) (min) (g kg 1 ) (g kg 1 ) acid losses
pressure (%)
Feed Concen- Initial Final Average Feed Concen-
(bar)
trate trate
20 21 60 61 148 41.8 4.0 18.2 11.0 21.7 18.4
40 24 60 64 224 54.8 2.9 24.8 11.6 33.4 17.3
60 22 36 64 255 76.7 6.8 50.6 11.0 40.4 7.6
100 R.B. Rodrigues et al. / Journal of Food Engineering 63 (2004) 97102
Table 2
Main characteristics of camucamu juice before and after concentration by reverse osmosis
Operating pressure (bar)
20
Feed Concentrate
1
Total soluble solids (g kg ) 61 148
pH 2.7 2.6
Titrable acidity (eq l 1 ) 0.35 0.85
Viscosity (mPa s) 0.9 1.4
Colour (Hunter)
L 81.3 55.8
a 3.3 31.8
b 43.5 37.9
The losses of ascorbic acid ranged between 8% and
18%. Theses losses seemed to depend on the trans-
membrane pressure: the lower the pressure used, the
higher the ascorbic acid losses. A signicant variation of
the ascorbic acid retention by the membrane cannot
only explain these results. So, losses of ascorbic acid are
mainly due to oxidation during the treatment that is
longer for the low transmembrane pressures (60 min at
20 or 40 bar and only 36 min at 60 bar).
The other characteristics of the products are pre-
sented in Table 2. During the concentration, the titrat-
able acidity increased in the same way than the TSS. The
pH decreased only a little because of the high buer
power of the solution. The juice and the dierent con-
centrates obtained had a newtonian behaviour. The
viscosity of the concentrates were very close to 1 mPa s
and not very dierent of the viscosity of the initial juice.
The luminosity (L) of the concentrates decreased as
compared to the original claried juice. This decrease
became greater as the applied pressure increased because
of the higher TSS reached. With respect to the other
colour parameters, an increase in TSS resulted in an
increase in red colour (a) and a decrease in yellow colour
(b) for all the pressures tested.
In the best operating conditions, reverse osmosis al-
lowed to produce a concentrated juice at 255 g kg 1 of
TSS containing 4% of ascorbic acid with an average
permeate ux of about 50 kg h 1 m 2 .
3.2. Osmotic evaporation concentration
The main operating conditions and results obtained
during the concentration of the model solution and the
camucamu juice using osmotic evaporation are pre-
sented in Table 3. During all the trials, the evaporation
ux decreased vs. time. This decrease is mainly due to
the increase in TSS because the fouling of the membrane
is very low in osmotic evaporation as previously men-
tioned by Vaillant et al. (2001).
According to the results obtained with the model
solution, we showed the temperature had a great inu-
40 60
Feed Concentrate Feed Concentrate
64 224 64 255
2.7 2.5 2.7 2.5
0.39 1.38 0.36 1.48
0.9 1.8 0.7 2.2
77.7 47.9 78.1 37.2
10.3 40.8 9.7 36.4
44.9 33.0 44.8 25.6
ence on the process performance. The increase in the
temperature dierence between juice and brine sides
(DT ) improved the evaporation ux considerably. These
results corroborated those obtained by Courel et al.
(2000). As previously described, the application of a
temperature gradient between the juice and the brine
contributes to the driving force together with the con-
centration dierence. The highest ux (around
13 kg h 1 m 2 ) was obtained using a DT of +15 C.
Considering the ascorbic acid content, losses were very
low, between 2% and 4%. The concentration of the juice
in the closed circulation loop limited the oxidation of the
solute. It explained the best results obtained compared
with reverse osmosis even if the duration of the trials
was much more longer (from 5 to 9 h). In that range of
temperatures, it is then possible to increase the evapo-
rating ux without damaging the vitamin content by
increasing the temperature of the juice.
The concentration of the claried camucamu juice
was carried out in two stages using the best operating
conditions obtained with the model solution. In the rst
stage (66247 g kg 1 TSS), the evaporating ux de-
creased of 16% and its average value was 12 kg h 1 m 2
(Fig. 3). On the contrary, the ux decreased of 53%
when the TSS increased from 247 to 634 g kg 1 in
the second stage but the average ux was kept at
9 kg h 1 m 2 . In osmotic evaporation, the ux decrease
during the process is mainly due to the increase of the
concentration polarization phenomena. Compared to
the reverse osmosis, the ux are lower but less aected
by the TSS. The nal TSS is not so limited like for
reverse osmosis.
In the two stages, the ascorbic acid losses were about
3% like for the model solutions. These results con-
rmed the interest of the process in maintaining the
quality of the juice. As in the reverse osmosis process,
the pH decreased due to the increase in titrable acidity,
as the TSS content increased (Table 4). In the two
stages, there was no signicant dierence in the colour
of the concentrated juice compared to the claried juice
(L, a and b).
 R.B. Rodrigues et al. / Journal of Food Engineering 63 (2004) 97102 101

acid losses
16

Ascorbic

Evaporation flux (kg h-1 m-2)

14

(%)

4.4
3.1
2.1

2.5

3.1
12
10
Ascorbic acid content

Concen- 8

108.1
19.4
34.7
51.0

41.7
trate 6
Operating conditions used, evaporating ux and ascorbic acid losses obtained during concentration of the model solution and of camucamu juice by osmotic evaporation

TSS from 66 to 247 g kg-1

4 TSS from 247 to 634 g kg-1
(g kg 1 )

2
Feed

14.2
13.5
13.5

11.4

43.5
0
0 100 200 300 400 500 600
Time (min)
Average
m 2)

12.9

12.0
5.1
8.2

9.0 Fig. 3. Evolution of evaporation ux during the concentration of

camucamu juice by osmotic evaporation.
1
Evaporating ux (kg h

Final

11.4

11.1
4.1
7.4

5.8

Table 4
Main characteristics of camucamu juice before and after concentra-
tion by osmotic evaporation
Initial

7.4
12.7
14.7

13.3

12.4

First stage Second stage

Feed Concentrate Feed Concentrate
Concen-

Total soluble 66 247 247 634

Total soluble solids

solids (g kg 1 )
trate

100
167
247

247

634

pH 2.6 2.2 2.4 2.1

Titrable acidity 0.33 1.33 1.45 3.47
(eq l 1 )
(g kg 1 )

Colour (Hunter)a
Feed

247
70
63
64

66

L 29.5 29.5 27.1 27.4

a 1.8 1.8 1.4 0.9
Duration

b 4.2 3.4 0.3 0.7

a
Measured on the concentrate after dilution to the total soluble
(h)

solids content of the feed.

5
8
9

8
in the two
Average

In the best operating conditions, osmotic evaporation

pressure

circuitsa

allowed to produce a concentrated juice at 634 g kg 1 of

(bar)
2.8
2.5
2.1

2.3

2.3

TSS containing more than 10% of ascorbic acid with an

average permeate ux of about 10 kg h 1 m 2 .
DT (C)

0
+10
+15

+15

+15

4. Conclusion

Reverse osmosis allowed to reach a maximum TSS

Temperature (C)

Brine

content of 255 g kg 1 using a transmembrane pressure of

30
20
20

20

20

60 bar at 22 C: The average permeate ux was

50 kg h 1 m 2 and the ascorbic acid losses was 8%. By
Transmembrane pressure <0.1 bar.
Juice

using this rst membrane process a juice with high nutri-

30
30
35

35

35

tional quality was obtained, in spite of the limitation of the

concentration factor. Thus it can be considered as a pre-
Brine con-
centration

4.0 (0.1)
5.2 (0.2)
5.2 (0.2)

5.2 (0.2)

5.2 (0.2)
(mol l 1 )

concentration step for the classical evaporation process.

Osmotic evaporation process allowed to concentrate
Camucamu juice

camucamu juice up to the same TSS content as that

obtained with thermal evaporation (up to 600 g kg 1 ).
The product obtained presented nutritional quality very
Second
solution
Product

stage

stage
First
treated

similar to that of the original juice regarding vitamin C

Model
Table 3

content (losses below 5%). The average evaporation ux

a

was close to 10 kg h 1 m 2 .
102 R.B. Rodrigues et al. / Journal of Food Engineering 63 (2004) 97102
These two membrane processes are very interesting to
concentrate camucamu juice without damaging the
nutritional potential of the raw material. Reverse os-
mosis has the advantage of being well developed at the
industrial scale. Osmotic evaporation has the advantage
of reaching higher concentration levels. Nevertheless, in
order to envisage any industrial application, the two
processes have to be compared on an economical point
of view.
Acknowledgements
The present work was supported by Fundac~ao de
Amparo 
a Pesquisa do Estado de S~
ao Paulo (FAPESP).
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