Journal of Food Engineering 17 (1992) 291-305

The Recycling of Table Olive Brine using Ultrafiltration

and Activated Carbon Adsorption
A. Garrido, P. Garcia & M. Brenes
Unidad Estructural de Investigaci6n de Biotecnologia de Alimentos. lnstituto de la
Grasa y sus Derivados, Apartado 1078.41012-Sevilla,
Spain
(Received 23 September

199 1; revised version received 28 November

accepted 1 December 1991)

199 1;

ABSTRACT

Brines from green table olive processing are a highly polluted waste water
which, at present, are discarded with the other liquid residues of the
packing factories. They are thus dificult to treat at both plant and municipal treatment facilities. Their recycling could eliminate about 80% of the
total pollution and facilitate treatment of the remaining liquid wastes.
Field tests showed that recycling of such brines after treatment with both
06% (w/v) of activated carbon and ultrafiltration through a polysulphone
membrane of IO00 daltons pore size can produce quantities of brine that,
with minor composition adjustments, can be added to the solution
employed for packing the final product. This can then be used in other
operations where brine is required. A possible design of the regeneration
process is also proposed.

INTRODUCTION
World table olive production is about 800000 t/year. Of this olive
production green table olives in brine (Sevillian or Spanish style) are the
most popular product, with production yields of 350 000 t/year, a large
proportion of which is produced in Spain (150 000 t/year).
The procedure for preparing green table olives consists of treating the
fruits with dilute NaOH solution (lye) to increase skin permeability and
partially eliminate bitterness, followed by two water washings to remove
the excess of alkali from the previous treatment. Thena 1 l-l 3% (w/v)
NaCl solution is added to the fruits, in which they undergo a lactic
291
Journal of Food Engineering 0260-8774/92/$05.00
Publishers Ltd, England. printed in Great Britain

- 0

1992

Elsevier

Science

A. Garrido, P. Garcia, A4.Brenes

292

fermentative process. They remain in this solution until they are ready
for packing or sale. Residual solutions from this process cause high
pollution levels in public watercourses and interfere in the normal work
of municipal waste water treatment plants.
Recently, the traditional method of processing has been modified and
industrial practice has incorporated technology that re-uses lye (Garrido
et al., 1979) and partially or totally eliminates wash waters (Gonzalez et
al., 1984), without any negative influence on the quality of the final
product. The reduced volume of alkaline solutions generated by this new
procedure are discarded in shallow ponds, where they undergo solar
evaporation. However, brines are still discarded when olives are packed
and, at the moment, industry has not yet adopted any measures to prevent pollution.
In Spain, 65% of the green table olive production is packed in small
containers (jars, cans, plastic bags, etc.). Thus, the packing industry
handles around 100 000 t/year, which generates about 50 000 m3 of
heavily polluted waste brines. Their principal characteristics are shown
in Table 1 (Garrido, 1990). In general, they have a high biological
oxygen demand (BOD,), lactic acid and salt content. Until now, they
have been discarded with the rest of the waste waters produced in the
factory, 6-12 litres/kg of fruit, making the whole liquid wastes untreatable at both plant and municipal treatment facilities.
A suitable solution might be the segregation of these brines, which
account for 80-85% of the final pollution but represent only 20% of the
total liquid residues. In addition, their re-use could benefit from the
value of their constituents: lactic acid and salt. Recycling possibilities are
diverse: new fermentation processes; addition to the original brines when

Main

Physico-chemical

TABLE 1
Characteristics
Brines

Characteristic
PH
NaCl (g/litre)
Free acidity, as lactic acid (g/litre)
Combined acidity (meq/litre)
Colour (&,-A
7oo)
Polyphenols, as tannic acid (g/litre)
Suspended solids (g/litre)
BOD, (g O,/litre)
COD (g O,/litre)

of Fermentation

Range
3.60-4.30
60-90
s-15
80-120
0.20~0.60
0.18-0.30
0.20-2.00
14-18
16-26

The recycling of table olive brine

293

olives are passed, for conditioning, from the fermenters to plastic drums;
for packing the final product; etc.
The recycling of spent brines has been widely investigated. Durkee et
al. (1973) described field tests on a submerged combustion system,
which, after evaporating most of the water, removed the organic matter
and recovered the salt by incineration of the concentrated slurry. Normal
fermentation was achieved using this recycled salt (Durkee et al., 1974).
Nevertheless, further research was directed to treatment of these solutions by other physico-chemical methods with the aim of reducing the
costs involved in the recycling process. Thus, Palnitkar and McFeeters
( 1975) reported that treating spent brines from cucumber fermentations
with NaOH solutions, followed by neutralization with HCl, gave a regenerated brine that when re-used for new fermentations resulted in a
quality similar to that produced by fermentation in fresh brine. Glaros
and Geisman (1980) studied a method to speed up flocculation. A
similar process was also proposed for olives (Leoni et al., 198 1).
Field tests for reconditioning brines from the conservation step of ripe
olive processing using activated carbon adsorption demonstrated
the
effectiveness of their re-use in the following season (Ginnette, 1968).
However, experiments re-using green table olive brines at different dilutions or degrees of reconditioning for new fermentation processes have
failed until now, probably due to the presence of metabolic compounds
from the first fermentation which inhibit lactic bacteria. There are also
problems with transport of such solutions to the processing factories
which are often far away from the canning facilities. Thus, the best
solution is either their recycling for packing or their addition to the
original brines during the olive conditioning operations. Garrido (1979)
showed that this option was possible, although the high prices of the
adsorbent and the retention of a high proportion of lactic acid by the
adsorbent had prevented its industrial use. However, more recently,
Brenes and Garrido ( 1988) have discovered a special activated carbon
that adsorbs colour very selectively with the elimination of only a small
percentage of lactic acid.
Membrane technology is also applicable to the regeneration of these
solutions, in spite of the fact that early tests failed because of the substances dissolved in olive brines and the chemical composition of the
available membranes (Rose, 1982). However, ultrafiltration (UF) is
finding increasing application in the food industry, sometimes in conjunction with activated carbon - as in the system proposed by Welsh
and Zall (1984) for regenerating and re-using fishery refrigeration
brines. Regeneration of brines from cucumbers had been reported by
Buescher (1984) and Fleming et al. ( 1988). Moreover, Brenes et al.

294

A. Garrido, P. Garcia, M. Brenes

(1988) reported the successful application of ultrafiltration through

polysulphone membranes to recover green table olive brines. Later, the
influence of some operating variables on the process and the effect of the
brines on polyphenol membranes was also investigated (Brenes et al.,
1990).
As a normal continuation of the most recent developments in the
regeneration of fermentation brines by activated carbon adsorption and
ultrafiltration, the aim of this study was to carry out comparative field
tests on an industrial scale. Their performance, the influence of brine
recycling on the main quality attributes of the final products, and the
adaptability of the commercial eqdipment to the working requirements
of the packing factories were investigated. The design of the two possible
processes derived from the research is also proposed.

MATERIALS

AND METHODS

Olives and brines

Experiments were carried out on fruit of the Hojiblanca cultivar (Olea
europaea arolensis) and their fermentation brines. The characteristics of
these solutions ranged between the limits presented in Table 1. The total
previous storage period was 8 months.
Analyses
Free acidity, combined acidity, salt content and pH of the brines, as well
as the texture of the fruits, were determined as described by FernGndez et
al. (1985). The brine colour was measured, after filtration through a
0*45-pm membrane (HAWP, Millipore Corp.), as the difference in
absorbance at 440 and 700 mn (A,,,-A,,,)
(Montaiio, 1987). Olive
colour was determined as proposed by Sgnchez et al. (1985).
Treatment with activated carbon and microfiltration
A sample of 6 g/litre (0*6%, w/v) of GA type activated carbon (Industrias
Kern, Barcelona, Spain) was added to 300 litres of brine and stirred for 1
h to complete the adsorption process. The brine was then filtered
through a ceramic filter of O-2-pm pore size in a Chaconsa apparatus
(Chaconsa, S.A., Murcia, Spain).
The equipment had two modules of 19 tubular filters (4 mm diameter)
with a total filtration surface of O-2 m* each. It also had a heat exchanger

The recycling of table olive brine

295

to control the working temperature. Every 15 min the automatic electronic control reversed the pressure on the filters, by injection of compressed air, to partially clean the membranes. Cleaning at the end of the
operation period consisted of steam injection followed by successive
rinsing with dilute NaOH and HNO, solutions, with a final water rinse to
eliminate any remaining chemicals. In general, the operation was carried
out in accordance with the manufacturers specifications (Anon., 1988).
Ultrafiltration equipment
Ultrafiltration trials were made with a Paterson Candy International
apparatus (Paterson Candy Int., Whitchurch, Hants, UK) fitted with a
module of 18 tubular polysulphone membranes of 12.5 mm internal
diameter giving a total filtration surface of 2.6 m2, and a heat exchange
module to facilitate temperature control during operation. The molecular weight cut-off of these membranes was 1000 daltons. The equipment
was used in accordance with the manufacturers specifications (Anon.,
1986). Operating pressure was 18 bars. Recycling flux was 30 litres/min,
corresponding
to a velocity of 3.9 m/s along the membranes. Postoperation cleaning consisted of water rinsing, use of a detergent solution
(Henkel P-3 141) at a temperature of 40-45C followed by further
rinsing. During the shut-down period, a 0.25% (w/v) solution of
potassium metabisulphite was introduced into the module to preserve
the membranes.
Experimental design
Active carbon adsorption and crossflowmicrofiltration
A factorial experiment was conducted with two types of regenerated
brines (one only filtered and one previously treated with 0.6% of activated carbon), two commercial olive products (plain and pitted), two can
sizes (2700 and 250 g per can) and two percentages (70 and 30%, v/v) of
recycled brine in the packing solutions. At the same time, olives were
also packed in fresh brine. The maximum proportion of re-use was
imposed by the concentrations of lactic acid and salt in the regenerated
brine which are usually higher than those required in the final product.
UltrajZtration
Three working modes were used to confirm the apparatus performance:
(i) total recycling, i.e. recycling to the feed tank both permeate and
concentrate; (ii) partial recycling, recycling concentrate to the feed tank
with removal of the permeate; (iii) partial recycling with replacement, i.e.

296

A. Garrido, P. Garcia, M. Brenes

the initial volume of brine in the feed tank was maintained by recycling
the concentrate and adding continuously to this tank the same volume of
brine as was removed as permeate. A 300-litre tank was used as a brine
reservoir.
For packing, only plain fruit and 250-g cans were used, as these gave
the highest brine colours in the carbon adsorption experiments. The
proportion of re-used brine in the final product was only 45% due to the
constraints imposed by the physico-chemical
characteristics of the
original brine and the final product. Comparisons with fruit packed in
fresh brine were also made.
Cans from all treatments were pasteurized using the normal industrial
process. Ten cans per treatment were collected and duplicates or triplicates were analysed after 3 months (to permit equilibrium). Studies were
also made at longer periods of time, although no differences between
their results and those obtained at the first sampling were noticed. Thus,
in this paper, physico-chemical analyses of brines and fruit studies correspond only to the 3-months data. Olives were also compared by the rank
method (Kramer & Twigg, 1962) to study the influence of the different
variables on the flavour.
All experiments were carried out in the factory of Agrosevilla, S.A.
Coop. (La Roda de Andalucia, Seville, Spain).

RESULTS AND DISCUSSION

Regeneration
filtration

by adsorption

with activated carbon and crossflow

No differences were found between these field tests and the data
reported previously (Brenes et al., 1988). So the main interest was to
study the equipment performance when the activated carbon slurry was
concentrated by crossflow microfiltration.
The flux changes in three different runs are shown in Fig. 1. There was
a diminution through the working day from 150-135 litres/m* per hour
at the beginning, to 110-l 15 litres/m* per hour at the end of the day.
Differences between the initial values are due to different flux recovery
rates after each cycle and indicate the remarkable influence of cleaning
on membrane permeability recovery. Maximum recovery was about
90-95% - a fairly good proportion.
The concentrated waste slurry had a high organic content, in addition
to the activated carbon. Although no treatment was attempted for its
elimination, the technical staff of the factory thought it might be burned

The recycling oftable olive brine

100

Fig. 1.

123456

297

TIME fhr)

Flux change in the crossflow filtration equipment, The solution was a slurry of
green table olive brines treated with 5 g/litre of GA-type activated carbon.

in the boiler after being sun dried, as was usually done with other solid
olive residues.
Cleaning the membranes after each working day took about 2.5 h.
During this time one worker was assigned to the operation, which must
be carried out carefully to achieve a satisfactory flux recovery for further
use.
Similar behaviour was observed when brine was only filtered,
although the decline was a little slower and the final volume of solids in
the concentrate was very small.
The main physico-chemical characte~stics of some of the brines from
the factorial packing experiment with recycled brine are shown in Table
2. This shows values for 250-g cans only, as they were the containers
where the negative effects were most evident, as they had highest fruit/
brine ratio. Combined acidity and pH are higher when percentages of
recycled brine increase and the propo~ons
of activated carbon diminish. Values for packing solutions containing 70% of recycled brines are
excessively high, indicating that such conditions require a previous
partial combined acidity correction to reduce both combined acidity and
pH to the usual levels in fresh brine. However, using 35% of both types
of regenerated brines, their values were lower and could sometimes be
acceptable, although a slight correction is advisable. In any case, the
product must be preserved by pasteurization.
Brine colour was also affected. Variance analysis of the results and
Duncan multiple comparison tests (Ruiz Maya, 1977) showed no significant differences for pitted olives, between fresh brines and those containing 70% and 3St6 of recycled solution regenerated with 0.6% of
activated carbon, Brine colour of plain olives packed with fresh brine
was slightly (although significantly) worse. Using 70% and 35% of activa-

24

22

23

93
0.24

105
0.36

22

0.56

450
5.60

057

4.53
5.80

Pitted

22

22

87
0.33

0.56

4.37
5.30

Plain

24

21

22

21

110
0.45

0.58

459
5.60

Plain

Filtered

combined

24

22

101
0.48

0.52

457
5.10

Pitted

70% (v/v)

free acidity, 1 X lo-?;

66
0.22

0.53

4.27
5.40

Pitted

35% (v/v)

Percentage of recycled brine used in the packing brine (v/v).

Note:Combined standard errors: pH, 3 x lo-; NaCl, 3 X lo-;
texture, 1; fruit colour, 1.

Fruit
Texture (kgf/cm
of pitted olives)
Colour (A44,,-A700)

(% w/v)
Free acidity, as lactic
acid (%, w/v)
Combined acidity
(meqjlitre)
Cofour (A440-A70,J

Brine
L&I

Plain

70% (v/v)

Treated with 0.6% activated carbon

Recycled

Type of brine

24

22

77
0.33

052

4.32
5.50

Pitted

24

23

70
0.28

0.56

4.21
5.30

Plain

22

22

59
0.23

0.53

4.08
5.30

Pitted

acidity, 3; brine colour 1 X 10m2; fruit

22

22

93
0.46

0.56

4.42
5.30

Plain

35% (v/v)

Fresh

TABLE 2
Average Values of the Physico-chemical
Characteristics of Brines as well as Texture (kgf/cm? 100 g of Pitted Olives) and Colour
(A,,,-A ,) of Fruits of Two Replicates. Olives were Packed with Solutions Containing Different Proportions of Brines Regenerated by
Adsorption with Different Percentages of Activated Carbon in 250-g Drained Weight Cans. Analysis was Performed Three Months After
Canning

s
p

8
3
9
?J
Q
.Ii
5

299

The recycling of table olive brine

ted carbon treated brines with plain olives as well as 35% of only filtered
brine with pitted fruits, the colour was also acceptable. However, filtered
brines gave unacceptable brine colour in the rest of the cases. Figure 2
summarizes these results.
The effect on the fruit attributes is presented in Table 2 for the same
cans in which brines were studied. Variance analysis of data showed no
statistically significant difference.
Considering that fruit packed with fresh brine and fruit packed with
brine regenerated by activated carbon are the most commercially
suitable, sensory analysis was confined to such samples. Preference ranking tests carried out on both plain and pitted olives showed no significant
differences (Kramer & Twigg, 1962).
Thus, it may be concluded that brine regeneration by activated carbon
adsorption, followed by crossflow filtration could be applied successfully
for recycling brines. It gives a good concentration ratio and great flexibility in relation to the percentage of active carbon used. However, for
packing with the maximum percentage of 70% of regenerated brine in
the final volume, a proportion of about 0.6 g/litre of activated carbon is
recommended. A correction of excessive original high combined acidity
is always advisable. Lower levels of regenerated liquids in the packing
PITTRD

Flesh
brine

up to 70% of
recycled brine
treated with
recycled brine
0.6% of activated carbon

same

<

35% of recycled
filtered brine

colour

colour

acceptable

brine

<

Fig. 2.

acceptable

colour

70% of recycled
filtered brine

-m

increase

FRUITS

up to 70% of recycled
brine treated with
0.6 % of activated
carbon

colour
*

<

unacceptable
colour

colour

PLAIN

Fresh

PRUITR

<

up to 70% of recycled
filtered brine

increase
unacceptable

colour

Summary of the influence of recycling proportion of different regenerated

brines on the colour of packing brines (250-g drained weight cans).

A. Garrido, I? Garcia, M. Brenes

300

solutions would need a lower proportionof adsorbent and combined

acidity reduction.
The only equipment problems noticed were related to the filters. The
length of the cleaning process was excessive and their small internal
diameter may lead to blockages if the velocity of the circulating slurry
decreases unexpectedly. So, a greater diameter of filter would be desirable. However, no problem was detected during this test.
Ultrafiltration
Permeate flux changes in the threedifferent operation modes are shown
in Fig. 3. In general, they declined throughout the working time. There
was a flux diminution of about 8 lure/m2 per hour from the beginning of
the work to the end of the 7-8 h of daily operation, except in the total
recycling mode in which it was around half of this amount. Partial recycling mode with replacement of the permeate had the lowest flux.
However, differences were small between the two possible working
modes, recycling of permeate with and without replacement. If the
operating period is less than 7-8 h, simple recycling is better. With
longer periods, performance was very similar. Thus, the working mode
does not have a significant influence on the equipment effectiveness; as
Fig. 4 shows for an experiment in which both modes were used
successively.
Usually, experiments
were carried out at room temperature
(1518C) but higher temperatures and previous flocculation of brines

TOTAL
PARTIAL

123456

Fig. 3.

RECYCLING

MODE

RECYCLING

MODE

PAriTIAL
RECYCLING
REPLACEMENT

MODE

WITH

TIME (hr)

Flux change of permeate during ultrafiltration of brines in different operation

modes (temperature = 1SOC).

The recycling of table olive brine

301

30
28

,
.
.

\.

26

=
x
3

24

lL

t;

. Partial
recy - I*
cling
mode

with replace
- I
22 - ment of per - I
_ meate
-

\
%

20

I Partial
t

recycling

Fig. 4.

1.

TIME (hrl

Flux change of permeate during ultrafiltration of brines in partial recycling and

partial recycling with replacement modes (temperature = 1ST)

with 2 g/litre of bentonite (from a 2%, w/v solution) increased the flux
and maintained it better than treating brines directly. The joint effect can
achieve an increase of about 30% in the flux. The industrial use of these
favourable influences will depend on the balance between the treatment
costs and the investment reduction (less filtering surface) that may be
achieved.
In all cases, the cleaning operation took about 1.5 h. An operator was
required only at the beginning and end of the process. After this operation, flux recovery was measured by using water as the ultrafiltration
liquid. Considerable fluctuations were observed between the initial flux
on the different working days, showing that the correct application of
cleaning had a determining influence on this parameter and, consequently, must be carried out carefully. No flux diminution
with
membrane utilization time was noticed during the period of the experiments (about 90 h).
The physico-chemical
characteristics of brines from olives packed
with solutions containing 45% of regenerated brine, together with those
of brine from olives packed with fresh brine are shown in Table 3. Data
are for plain fruit and 250-g cans, which was the treatment that showed
the most unfavourable effects of recycling. There were clear differences
in pH and combined acidity values in the equilibrium between both
forms of packing. This was similar to regeneration by adsorption,
although the pH values reached in the case of recycled brine by ultrafiltration were lower than those obtained in the adsorption experiment and
were appropriate for packing when pasteurization was used to assure the
product preservation. With respect to brine colour there were no statistical differences and in all cases it was the normal colour that might be

A. Garrido, P. Garcia, M. Brenes

302

TABLE 3
Average Values of the Physico-chemical Characteristics of the Brines of Green Table
Olives Packed with 45% of Recycled and Fresh Brines. Plain Fruit and 250-g Drained
Weight Cans were used U
Type of brine
Recycledb
4.05
4.60
0.70
104.0
0.109

PH
NaCl (%, w/v)
Free acidity, as lactic acid (%, w/v)
Combined acidity (meq/litre)
Colour (A,,,,-A 7oo)

Fresh
3.66
4.80
0.76
65.0
0.100

The values are the averages of three replicates. Analysis was performed 3 months after
canning.
Combined standard errors: pH, 1 X lo- l; NaCl, 9X lo-*; free acidity, 2x lo-*;
combined acidity, 2.3; colour, 6 x 10 - j.
hOf the packing brine, 45% had been recycled.

BRINE

INLE.1

TANK

FILTER

02

PUMP

HEAT

Fig. 5.

GROUP
EXCHANGER

Possible scheme for an industrial process.

expected in these green table olive solutions from jars or cans. No effect
on texture, colour or sensorial preferences was detected.
Thus, the experiment showed that using the correct initial combined
acidity and proportion of recycled brine, good physico-chemical conditions could be achieved in the final packing solution.
Possible schematic

design of the regeneration

processes

The whole process for the two treatments can be designed as shown in
Fig. 5. In both cases, a tank with a capacity depending on the daily

The recyclingof rubleoZivebrine

303

production would be required. It might be used for the activated carbon

treatment, the ~occulation with bentonite or just as a brine reservoir if
brine is ultrafiltered directly. This container must be provided with a
stirrer and a device in the bottom to remove the decanted solids as well
as with accessories to add the carbon or any other additive. The
decanted treated solution would pass from the container to the crossflow
or ultrafiltration equipment, as appropriate.

CONCLUSIONS
From the above results it can be deduced that the two treatments used to
regenerate green table olive fermentation brines could be used to recycle
such solutions. Their re-use can be diverse: addition to the solutions
used for packing; making up of brine requirements when olives are put in
plastic drums for conditioning; and employment for new fermentative
processes, although in this case proportions should be low and it is the
least recommended mode of reutilization at present.
In any case, re-use in adequate proportions to prepare packing solutions might be a reasonable alte~ative. The main influence on the final
product depends on the physico-chemical characteristics of the solutions. An increase in pH and combined acidity is always observed. This
increase in buffer capacity might be a serious drawback if fruit is to be
preserved only by its pH and salt concentrations. In this case, a correction in the combined acidity by addition of a strong acid is required.
Otherwise, final pH will not reach a value low enough for product stability. However, if the product is pasteurized, as is becoming standard
practice in the industry, there is always the possibility of selecting the
appropriate
proportion
of regenerated brine for the required final
characteristics. This percentage will vary from case to case and will
depend on the constraints imposed by the product conditions - in
particular, combined acidity, acid and salt contents in the fermentation
brine as well as type of packing containers (jars, cans, plastic bags, etc.).
With the Hojibl~ca cultivar it has been shown that 45% of ultraf~tered
and up to 70% of carbon regenerated brines treated with 06% of activated carbon (with a slight acidity correction) can be added to the packing
solutions.
No serious economic conclusions can be deduced from these experiments. However, an approximate study was made by the technical staff
of the firm where the experiment was carried out. They considered the
prices of the lactic acid and salt, and the reduction in pollution taxes. The
results showed that returns would more than pay for the investment and
running costs of any of the regeneration systems studied.

304

A. Garrido, P. Garcia, M. Brenes

ACKNOWLEDGEMENTS
The authors wish to thank Agrosevilla, S.A. Coop. (La Roda de
Andalucia, Sevilla, Spain) where field tests were carried out, TFB
(Madrid, Spain) and Chaconsa, S.A. (Murcia, Spain) for the use of the
ultrafiltration and crossflow microfiltration equipment, respectively, and
Drs Rejano and Sanchez for advising on the sensory analysis.
The authors also express their sincere gratitude to Consejo Superior
de Investigaciones Cientificas (Madrid, Spain) for providing special
support for this research and CICYT under whose project ALI88-0151CO2-0 1 this work was done.

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