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Industrial trials on coadjuvants for olive oil


Article in Journal of Food Engineering March 2010

DOI: 10.1016/j.jfoodeng.2009.09.015


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Industrial trials on coadjuvants for olive oil extraction

Manuel Moya a, Francisco Espnola a, Diego G. Fernndez a, Antonia de Torres a, Javier Marcos b, Juan Vilar b,
Javier Josue c, Teodosio Snchez d, Eulogio Castro a,*
Department of Chemical, Environmental and Materials Engineering, University of Jan, 23071 Jan, Spain
Westfalia Separator Andaluca S.L., beda, Jan, Spain
Omya Clariana S.L., Esplugues de Llobregat, Barcelona, Spain
Aceites La Laguna, S.A., Baeza, Jan, Spain

a r t i c l e i n f o a b s t r a c t

Article history: Industrial scale experiments were performed in an olive oil production factory to assess the effect of dif-
Received 3 April 2009 ferent physical acting coadjuvants on oil extraction and oil quality. Up to 120,000 kg olives were pro-
Received in revised form 15 July 2009 cessed. Talc and calcium carbonate, with different particle sizes, were assayed at concentrations
Accepted 15 September 2009
ranging from 0.3% to 1% by weight. Both coadjuvant types are food grade and are recognized as food addi-
Available online 19 September 2009
tives by EU regulations (E-170 as calcium carbonate and E-553b as talc). Industrial trials were performed
at room temperature with no added water, thus avoiding volatile compound loss and hydrosoluble com-
pound content decrease. As a consequence, the obtained oils were more aromatic and their positive attri-
Olive oil
butes more intense, in comparison to other olive oils produced in different operational conditions. In
Calcium carbonate addition, energy requirements were decreased (releasing a lesser amount of carbon dioxide into the
Talc atmosphere) and water uptake was kept to a minimum.
Physical extraction Results show that the use of coadjuvants improves the oil extraction yield. The extraction efcacy,
Oil quality dened as the percentage of initial oil that is extracted, increased by 2% by using carbonate in comparison
Oil yield to experiments performed without any coadjuvant, with 91.53% of oil content in the olives being
extracted. For the same particle size, calcium carbonate was found to extract a greater oil amount than
talc. For a single coadjuvant, the extraction yield decreased as the particle size increased. The best results,
in terms of oil extraction yield, were obtained when using 0.3% calcium carbonate. Considering oil qual-
ity, no inuence by either coadjuvant was detected as oil components remained unaltered during the
extraction process. The sensorial evaluation gave the same result for all olive oils, no matter if a coadju-
vant was used or not, indicating that these compounds only act physically on the oil extraction process.
2009 Elsevier Ltd. All rights reserved.

1. Introduction In the olive oil extraction process, 1020% of oil remains inside
the unsheltered cells or is left in the colloidal system of the olive
Production of virgin olive oil is a process that may be affected by paste (microgels) and some is bound in an emulsion with the veg-
a number of factors. A deep knowledge of the extraction process is etable water. The difculty of freeing this bound oil lies mainly in
needed if oil quality is to be preserved from alterations (Salvador the fact that the droplets of dispersed or emulsied oil are sur-
et al., 2003; Jimnez et al., 1995; Di Giovacchino et al., 2002). rounded by a lipoprotein membrane (phospholipids and proteins)
The main steps in olive oil production are olive crushing, paste that keeps them in that state (Boskou, 1996; Petursson et al.,
malaxation and oil separation. Paste malaxation has been exten- 2004). This phenomenon is more pronounced in some olive varie-
sively studied because of its inuence on oil quality (Angerosa ties, like Hojiblanca or Picual, and when fruits are harvested early
et al., 2001; Ranalli et al., 2003a; Morales and Aparicio, 1999); tem- or frozen. The pastes obtained from these conditions are called
perature and mixing time are the main factors. Top quality oils are difcult pastes and usually need the use of a coadjuvant, which
obtained at low values of these variables, but extraction yields are is added at the malaxation step, to break down emulsions, allowing
also low under such conditions. It has been reported that the best most of the oil to be extracted. Spain was the rst country to reg-
option to improve extraction yields along with little oil alteration is ulate coadjuvant use (Ministerio de Sanidad y Consumo, 1986) and
increasing mixing time (Moya et al., 2006). natural talc (hydrated magnesium silicate) was the rst product al-
lowed for olive oil extraction. The coadjuvant list was modied to
* Corresponding author. Tel.: +34 953 212163; fax: +34 953 212141. include the enzyme carbohydrase from Aspergillus aculeatus (Min-
E-mail address: (E. Castro). isterio de Sanidad y Consumo, 1989). Enzyme preparations were

0260-8774/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
Author's personal copy

58 M. Moya et al. / Journal of Food Engineering 97 (2010) 5763

shown to increase oil extraction yields in the range 10.213.5 kg oil 2. Materials and methods
per tonne of olives, regardless of the olive variety processed
(Ranalli et al., 2003b); other reports showed that the enzyme 2.1. Raw material
treatments resulted in higher overall oil yields, the increase rang-
ing from 0.9% to 2.4% wet basis, compared to untreated pastes Olives (Olea europaea L.), Picual variety, were collected in a local
(Najaan et al., 2009). Later, the CE Norm 1513/2001 dened virgin farm and used for extraction experiments. Unwashed olives were
olive oils, excluding oils obtained by coadjuvants with a chemical milled within 6 h of picking. A visual observation revealed that
or biochemical action. Beyond this legal denition, carbohydrase- most olives were collected from the ground and just a small pro-
oils could no longer be considered as virgin olive oil, because of portion came directly from the tree.
the biochemical action causing cell wall rupture (Ranalli et al.,
2003) and talc remained as the only approved coadjuvant, since
2.2. Technological coadjuvants
its action is merely physical (Cert et al., 1996). Talc is authorized
as a food additive and coadjuvant (E553b) (CE Directive 30/
Two types of talc and three types of calcium carbonates, com-
2001). The use of talc as coadjuvant has been proved to increase
mercially available, were used as technological coadjuvants in oil
oil extraction yield with no interference on oil quality (Fernndez
extraction trials: Micro-talc FC8, Micro-talc FC CG, Calcipur 2, Cal-
et al., 2008). Nevertheless, several epidemiological studies have
cipur 5, and VP-DA. Table 1 summarizes relevant data of these
identied talc as a risk factor (Wild, 2006; Neghab et al., 2007;
products. Both talcs and carbonates are food grade and comply
Ramanakumar et al., 2008).
with requirements to be considered as food additives. Iron content
Calcium carbonate is one of the most abundant compounds on
(expressed as iron oxide III) is below 1.5% and 0.02% for talcs and
the earth. Pulverized calcium carbonate acts as adsorbent medium
carbonates, respectively, and no heavy metals other than iron are
and can make droplets of oil merge into larger drops, thus facilitat-
present in their composition.
ing oil separation. Calcium carbonate does not react with oils be-
cause of its crystalline structure and water afnity (Dentel, 1991)
and it is easily removed by centrifugation together with olive pom- 2.3. Industrial device
ace due to its high density (2.72 g/cm3) and water afnity. In addi-
tion, calcium carbonate is authorized by European Union The experiments were performed at Aceites La Laguna, an oil
regulations (Directive 2001/30/EC) and used worldwide as a hu- producing company located at Baeza, Jan (Spain). An independent
man food additive (E170). Moreover, no limits on Acceptable Daily equipment line, including reception, milling, malaxation, extrac-
Intake have been established for calcium carbonate by the Expert tion, and oil storing equipment was used. Olive fruits were cleaned
Committee on Food Additives (JEFCA) from FAO/WHO. upon reception, weighed and stored in a hopper before being fed to
Our previous work (Espnola et al., 2009) reported on the im- the extraction process. Fig. 1 shows a schematic diagram of the oil
proved extraction of virgin olive oil using calcium carbonate as extraction line (GEA Westfalia Separator Industry GmbH, Oelde,
coadjuvant extractant at laboratory scale. The present work deals Germany); all the components that may come in contact with
with industrial scale trials aimed at comparing different coadju- the raw material or the product are made of stainless steel.
vants for olive oil extraction based on improved extraction yield Olives are milled in two hammer mills, and then the paste is
and oil quality. conducted to the mixing stage. The malaxation device includes a
dosing tank for coadjuvant to be added to the olive paste and a
two-chambered mixer. The coadjuvant is added by means of an
Table 1
automatic device provided with a frequency modulator. The mixer
Basic data of the used coadjuvants.
(WS 8000 V model) is composed of two chambers with 4000 kg
Coadjuvant Medium particle Purity Density Manufacturer paste capacity each. Each chamber has three independent mixing
size (D50) (lm) (%) (g/cm3)
axes with blades which turn around at 20 rpm. Once the paste
Micro-talc 2.5 97 2.77 Mondo Minerals has been mixed, it enters the horizontal centrifugation unit (so-
FC8 (talc) OY
called decanter) through a paste injection pump, which allows
Micro-talc 8.0 97 2.77 Mondo Minerals
FC CG (talc) OY the paste ow to be regulated. The used decanter is the Westfalia
Calcipur 2 2.7 99 2.70 Omya AG Separator RCC 495-08-30 model, built in high resistant stainless
(CaCO3) steel, operating at 3000 rpm. It is provided with a cylindricalcon-
Calcipur 5 5.7 99 2.70 Omya AG ical solid-wall bowl for the continuous separation of solid and li-
VP-DA (CaCO3) 3.8 98.5 2.70 Omya AG
quid. The solid-wall bowl has a cylindrical section for efcient
separation and clarication of the liquid. Moreover, the oil stream

Fig. 1. Industrial olive oil extraction unit (GEA Westfalia Separator Industry GmbH, Oelde, Germany). 1: Olive silo; 2: hammer mill; 3: two-chambered malaxer; 4: two-phase
separating decanter; 5: vertical centrifuge; 6: storage.
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M. Moya et al. / Journal of Food Engineering 97 (2010) 5763 59

at the decanter exit is cleaned of the solids on a decantation table; The use of coadjuvants results in increased industrial extraction
afterwards, oil is directed to a vertical disk centrifugation step, yields while, at the same time, oil quality is unaltered (Espnola
where it is further water cleaned. et al., 2009).
The disk centrifuge, OSC 25-02-007 Model, operates at The experimental design is summarized in Table 2. Control
7500 rpm with automatic cleaning discharges every 15 min. The experiments, with no coadjuvant, were included at the beginning
unclaried oil is fed into rising channels and split up over a large and at the end of the experimental series for comparison purposes.
number of disk interspaces. The separated solids collect in the sol- Experiments with coadjuvants were performed on an increasing-
ids holding space where a periodically activated sliding piston dose basis, with 0.3 and 1.0% w/w coadjuvant concentration. Each
opens a gap to discharge the accumulated solids. The oil is cleaned experiment involved milling and extraction of 8000 kg of olives in
in place through a washing water stream and then goes to a central continuous operation. Feeding rate was 4000 kg/h, hence each run
discharge channel towards a centripedal pump and is discharged lasted for 2 h in the mixing device. Before using a new coadjuvant,
under pressure through the discharge line. Washing water is con- 4000 kg of olives with no coadjuvant were processed, thus guaran-
tinuously eliminated through a different discharging line. Finally, tying that each coadjuvant was in contact just with fresh olives. On
the oil goes to a clarication tank and then to store. the whole, each experiment used up to 12,000 kg olives which
were mixed for 180 min and 180 additional min for oil decanting
2.4. Analytical methods and washing. As the mixer has two chambers, decantation of the
rst 4000 kg olives overlaps with the mixing of 4000 kg milled,
Olive fruits, pastes and olive pomace were sampled throughout fresh olives, making the whole experiment last for 300 min. Taking
the process for analytical determinations. Moisture and volatile into account mass ow and device capacity, the elapsed time be-
material content were determined from weight loss at 105 C. Oil tween olives entering the mill and oil being obtained at the centri-
content assay was performed by soxhlet extraction according to fuge is about 2 h.
EEC Regulation 2568/1991. The olive maturity index was deter- The experimental installation reached its steady state by pro-
mined by a subjective evaluation of the color of the olive skin cessing 8000 kg olives before starting the trials; in addition
and esh (Uceda and Fras, 1975; Vossen, 2005). The procedure 4000 kg olives were used up at the end of the programmed exper-
consists in distributing 100 olives in eight groups, according to iments. As a whole, 120,000 kg olives were processed in a 32 h con-
the following characteristics: bright-green skin (group N = 0), tinuous operation.
green-yellowish skin (group N = 1), green skin with reddish spots The temperature of the paste was monitored during operation,
(group N = 2), reddish-brown skin (group N = 3), black skin with being almost constant (24.5 C) throughout the process.
white esh (group N = 4), black skin with <50% purple esh (group
N = 5), black skin with >50% and <100% purple esh (group N = 6),
and black skin with 100% purple esh (group N = 7). The index is 3. Results and discussion
given by (Nini)/100, where N is the group number and n is the ol-
ive number in that group. Maturity index values range from 0 to 7. 3.1. Oil extraction
Oil samples were taken in dark glass bottles and stored in a
fridge until analyzed. Before characterization, oils were paper l- Table 3 shows the composition of pastes and pomaces obtained
tered. Analytical determinations included acidity, peroxide index, from the different olive lots, together with the maturity index of
K270, K232 and DK according to CE norms 702/2007, 1989/2003 the olives. Maturity index ranged from 6.1 to 6.7, indicating that ol-
and 2568/91. Pigment composition was also measured in oil ives were in an advanced stage of maturation. The vegetation
samples following procedures proposed by Mnguez et al., 1992 water content of the olives was 43.648.6%, a relative low value
(chlorophylls and carotenoids) and by Vzquez et al., 1973 characteristic of mature fruits that should make oil extraction easy.
(polyphenols). Finally, the sensory evaluation of olive oils was Differences in oil content of olive samples are explained by differ-
performed by a taster panel (Al-Zeyt-Asociacin de Expertos en ent geographical origins.
Cata de Aceites de Oliva Vrgenes) according to EC regulations Concerning olive pomaces, obtained at the end of the trials, the
640/2008 and 2568/91. moisture content is very similar except for experiment G. Actually,
results from this experiment are anomalous, because moisture
2.5. Experimental procedure content (54.0%) was unusually low while the residual oil content
in the pomace (13.5%) was unusually high. These facts can be
All industrial experiments were performed at room tempera- attributed to mismatch operation in the horizontal centrifuge. Re-
ture with no added water. This operation procedure leads to a sults from this particular experiment were not considered for fur-
low extraction yield and improves oil quality, due to a reduced vol- ther discussion.
atile compound loss and greater polyphenol content; in addition, In an attempt to overcome differences attributable to the oil
energy requirements are kept to a low level as no heat is added. content of olives, the extraction efcacy is dened as the percent-
age of the initial oil content that is extracted in every experiment.
This variable is thus independent from the assayed olives and from
the oil content. The unextracted oil is accompanying olive pomace
Table 2
Experimental design.
from the decanter separation. The values of the extraction efcacy
for all the experiments are depicted in Fig. 2, from which it can be
Experiment Coadjuvant Dosage (% w/w)
concluded that:
A Control 0.0
B Micro-talc FC8 0.3 (a) The use of coadjuvant VP-DA at 1.0% w/w gives worse results
C Calcipur 2 0.3
D Micro-talc FC CG 0.3
in terms of extraction efcacy compared to the control
E Calcipur 2 1.0 experiment (no added coadjuvant, experiments A and I).
F Micro-talc FC CG 1.0 The same is true for Micro-talc FC CG at 1.0% concentration.
G Calcipur 5 1.0 (b) Calcipur 2 shows to be the best coadjuvant, followed by
H VP-DA 1.0
Micro-talc FC8. Compared to average extraction efcacy of
I Control 0.0
the two control experiments (A and I trials), using 0.3%
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60 M. Moya et al. / Journal of Food Engineering 97 (2010) 5763

Table 3
Olive maturity index and composition of pastes and pomaces.

Experiment Maturity Index Olive paste Olive pomace

Moisture (%) Oil content (% d.b ) Moisture(%) Oil content (% d.b*)
A 6.6 48.4 45.0 61.0 7.8
B 6.1 46.9 44.4 58.4 6.7
C 6.1 47.7 44.1 57.9 6.3
D 6.5 45.1 41.7 57.6 6.8
E 6.7 44.6 41.6 56.5 6.4
F 6.6 43.6 41.2 56.7 7.4
G 6.6 44.4 44.4 54.0 13.5
H 6.6 45.3 44.5 56.7 9.3
I 6.5 46.3 42.1 57.6 6.9

Average values of two determinations (variation coefcient < 5%).

Dry basis.

Fig. 2. Extraction efcacy (% extracted oil) as a function of coadjuvant. Experiment conditions (% w/w coadjuvant). A: Control (0.0); B: Micro-talc FC8 (0.3); C: Calcipur 2
(0.3); D: Micro-talc FC CG (0.3); E: Calcipur 2 (1.0); F: Micro-talc FC CG (1.0); G: Calcipur 5 (1.0); H: VP-DA (1.0); I: Control (0.0).

Fig. 3. Acidity (%) and peroxide index (mEq O2/kg) of the obtained oils using different coadjuvants. A: Control (0.0); B: Micro-talc FC8 (0.3); C: Calcipur 2 (0.3); D: Micro-talc
FC CG (0.3); E: Calcipur 2 (1.0); F: Micro-talc FC CG (1.0); G: Calcipur 5 (1.0); H: VP-DA (1.0); I: Control (0.0).
Author's personal copy

M. Moya et al. / Journal of Food Engineering 97 (2010) 5763 61

Calcipur 2 (experiment C) increases results by 2%, with On the other hand, as stated in the experimental procedure sec-
91.53% of oil content in the olives being extracted. Micro- tion, the mean temperature of the paste was 24.5 C (room temper-
talc FC8 (experiment B) improves extraction efcacy by 1.4%. ature operation), while the usual malaxation temperature is
(c) Low concentrations (0.3%) are preferable to high concentra- around 30 C; although a more complete economic analysis is to
tions (1.0%) when using either Calcipur 2 or Micro-talc FC be done, a rough estimation of energy requirement savings can
CG. For example, a small improvement of 0.6% in extraction be done by taking into account the operation temperature decrease
efcacy is found for 0.3% Calcipur 2 compared to 1% dosage, in the case of carbonate addition. Considering the specic heat
thus an additional reduction cost can be obtained by using a capacity of the paste (around 0.7 cal/gC), the extra amount of fuel
lower dosage of the coadjuvant. used to warm up the paste (for example, olive stones, with a heat-
(d) Considering particle size (Table 1), extraction efcacies are ing value of 4500 kcal/kg) would be some 100 kg for the total
greater for smaller particle sizes, both in the case of talcs experimental design reported in this work. Additionally, this also
and carbonates. means a corresponding lower amount of carbon dioxide being
emitted into the atmosphere.
These results agree with those reported by Espnola et al.
(2009), based on laboratory-scale operation, and conrm that
micronized calcium carbonate offers a greater extraction efcacy 3.3. Oil quality
than micronized talc at identical particle size and dosage condi-
tions. Increasing particle size seems to have a greater negative The main quality parameters of the obtained oils, according to
inuence on oil extraction than that observed when increasing CE Norm 702/2007, are presented in Figs. 3 and 4, where the con-
coadjuvant addition. On the other hand, given the high density of tinuous upper line represents the limit above which oils cannot be
coadjuvants (Table 1), nearly three times that of olive oil, they considered as extra virgin oils.
are easily eliminated, along with olive pomace, by centrifugation The resulting oil acidity values (Fig. 3) can be considered in
in the decanter. accordance to the maturity index of the used olives. From the
It is worth mentioning that, due to industrial device availability,
this work was performed at the end of the olive harvest season, as
Table 4
can be deduced by the maturity index of the fruits (Table 3); this Pigments and polyphenols composition of the obtained oils.
means that no difcult pastes were expected from this type of ol-
ives, because that situation is more usually found at the beginning Experiment Chlorophyll Carotenoids Polyphenols
(mg/kg) (mg/kg) (mg/kg)
of the season. It is likely that the improvement in extraction ef-
cacy from early harvested olives would be greater than that found A 25.9 9.15 249
B 27.0 8.96 315
in this work, under not so favourable conditions for coadjuvants to
C 30.6 9.58 321
act. D 29.9 9.11 339
E 29.8 8.77 283
F 33.3 9.91 299
3.2. Economic considerations
G 29.8 8.77 291
H 28.4 8.39 339
Concerning economic aspects, purchase price for Calcipur 2 is I 34.0 10.1 300
currently about 250/ton, approximately one third of that corre-
sponding to Micro-talc FC8; adding 3 kg Calcipur 2 per ton olives SD* 5.7 0.67 36
ANOVA (p-value) 0.985 0.740 0.771
would increase extraction costs only by 0.75, which would be lar-
gely justied by 2% improvement in oil recovery. SD: standard deviation of the control experiments (A and I).

Fig. 4. K270 and K232 index of the obtained oils using different coadjuvants. A: Control (0.0); B: Micro-talc FC8 (0.3); C: Calcipur 2 (0.3); D: Micro-talc FC CG (0.3); E: Calcipur
2 (1.0); F: Micro-talc FC CG (1.0); G: Calcipur 5 (1.0); H: VP-DA (1.0); I: Control (0.0).
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62 M. Moya et al. / Journal of Food Engineering 97 (2010) 5763

Table 5
Organoleptic parameters of oils*.

Experiment Musty Earthy Winey Fruity Bitter Pungent

A 2.5 0.21 2.5 0.38 2.0 0.10 0.5 0.14 0.8 0.21 0.8 0.24
B 2.4 0.24 3.0 0.24 1.2 0.42 0.4 0.03 0.6 0.21 0.8 0.24
C 2.5 0.70 2.2 0.07 1.5 0.03 2.2 0.03 1.2 0.03 1.1 0.14
D 2.6 0.59 3.0 0.84 2.0 0.17 1.4 0.07 1.4 0.45 0.0
E 2.0 0.03 3.5 0.80 2.5 0.21 1.3 0.07 1.3 0.10 1.5 0.10
F 3.0 0.03 2.0 0.07 2.0 0.17 1.4 0.24 1.4 0.45 1.3 0.24
G 3.0 0.28 3.6 0.28 3.0 0.28 2.2 0.63 1.1 0.07 1.6 0.10
H 2.5 0.42 2.0 0.24 2.0 0.21 1.0 0.03 1.5 0.21 1.2 0.24
I 2.5 0.10 2.9 0.10 3.0 0.14 1.5 0.10 2.0 0.07 1.4 0.28
ANOVA (p-value) 0.162 0.325 0.726 0.706 0.977 0.566
Median solid standard deviation.

ANOVA analysis of the values it can be deduced that the use of All the assayed coadjuvants exert a physical action in the olive
coadjuvants does not modify the oil composition in free fatty acids oil extraction process, increasing the industrial yield without mod-
(p-value = 0.694), and hence there is no neutralizing action. ifying neither quality parameters nor sensorial assessment. Acidity
The same is also true concerning peroxide index, K270 and K232 index, peroxide index, K270 and K232 of the resulting oils can be
(Fig. 4) with p-values 0.107, 0.659 and 0.820, respectively. Values considered in accordance to the maturity index of the used olives,
for DK are all negative and remain below the maximum allowed as well as the organoleptic evaluation. In addition, pigments and
(0.01) for an oil to be considered as extra virgin. It can thus be con- polyphenol contents are greater than those from control experi-
cluded that none of the assayed coadjuvants exert any alteration ments oil.
on quality parameters and they show just a physical action on Increasing coadjuvant addition from 0.3% to 1.0% results in an
the extraction process. extraction yield decrease. In the same sense, the extraction efcacy
On the other hand, the composition of photosynthesis pigments decreases as the particle size is increased, as a consequence of a
and polyphenols of oils decreases as the maturity increases (Mn- comparative lower specic surface.
guez et al., 1992; Gimeno et al., 2002). Nevertheless, the obtained The use of coadjuvants, together with no added water and room
oils in this work show a composition of these compounds (Table 4) temperature operation enables olive oils to be obtained at the
greater than those corresponding to the maturity index of the used same or higher extraction yields than when using different condi-
fruits; this fact can be attributed to the absence of added water in tions; on the other hand, oil quality is higher, and water uptake, ol-
the extraction process. Thus, the use of this operational procedure ive pomace production and fuel requirements are reduced.
allows oils with high polyphenols content to be obtained. The sta-
tistical analysis (ANOVA) on parameters from Table 4 yielded p-
values >0.05, so the use of coadjuvants does not produce any sig-
nicant variation on the amount of photosynthetic pigments and References
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