J Sci Food Aqric 1994,65, 67-75

Effect of Drying on Acidity and Volatile Fatty

Acids Content of Cocoa Beans
S Jinap,* J Thien
Department of Food Science, University Pertanian, 43400 Serdang, Selangor, Malaysia

and T N Yap
Sime Darby Plantations, Ebor Research, Locked Bag # 202, Batu Tiga, 40000 Shah Alam, Malaysia
(Received 4 January 1993; revised version received 23 August 1993; accepted 9 December 1993)

Abstract: The objectives of the study were to evaluate the effect of drying on the
pH, titratable acidity and volatile fatty acids (VFA), ie acetic, propionic, butyric,
isobutyric and isovaleric acids content of cocoa beans, and on the flavour of the
resultant chocolate. Freshly harvested cocoa pods from clones of PBC 123 and
128 (1 : 1 ratio) were stored for 9 days and fermented for 5 days with a single
turning at 48 h. Four drying treatments, ie oven-drying at 6VC, air-blow drying,
shade-drying and sun-drying were carried out. Samples were taken periodically
for pH, titratable acidity, and VFA analysis. Physical characteristics were also
recorded. The resultant beans were made into dark chocolate for flavour evalu-
ation. The results showed that wet beans held in shady areas for 120 h will not
dry quickly enough to inhibit mould and yeast and other putrefactive activities;
rapid oven-drying of these still wet beans did not improve their flavour profile.
There were no significant differences ( P 3 0.05) between samples that have
undergone sun-drying and air-blow drying in the acidity and C,-C, VFA
content; both were evaluated favourably by taste panellists. Oven-dried beans
contain a high concentration of VFA and produced chocolates with a high inten-
sity of off-flavour.
Key words: Cocoa beans, drying, acidity, C,-C, fatty acids, physical appearance,
weight and loss, flavour profile, chocolate.

INTRODUCTION small quantities of beans and the method is cheap and

Cocoa must be dried in order t o reduce its moisture
content to a safe level for storage. Drying is also a con-
tinuation of the oxidative stage of fermentation and
therefore plays a important role in reducing astringency
and bitterness. It also reduces acidity and develops fam-
iliar 'chocolate' brown colour (Cook and Meursing
1982; Wood 1983). Properly dried beans will usually
have a long shelf-life, be crisp in texture, have a plump
appearance, a well oxidised interior and a good choco-
late flavour without excessive acidity, hammy, smokey,
or other off-flavour notes (McDonald et a1 1981).
The best drying method for obtaining maximum
flavour development is sun-drying. This method is
usually practised by smallholders because it can handle
* To whom correspondence should be addressed.
67
J Sci Food Ayric 0022-5142/94/$09.00 (c) 1994 SCI. Printed in Great Britain
simple. This method, however, cannot be practised by
estates and medium-scale processors because of the
length of time involved, labour required a n d uncertain
weather conditions. At present, most estates in Malaysia
are using circular dryers equipped with stirring mecha-
nism, with a n air temperature of 60-70°C. This rapid
drying causes the beans t o have a strong acidic flavour.
Jinap and Dimick (1990a) have reported that fermented
and dried cocoa beans from the F a r East contain high
concentrations of volatile fatty acids (VFA), ie acetic,
propionic, butyric, isobutyric, isovaleric acids (C,-C,
VFA). Although further processing such as roasting and
conching can reduce the concentration of these acids
(Jinap a n d Dimick, 1990b), a high initial concentration
in the dried beans will result in a higher residual con-
centration in the final products. Lopez and Quesnel
(1973) have found that beans produced during the dry
68
season and those fermented at the corner or top layer of
the box contain significantly higher C,-C, VFA,
Duncan et a1 (1989) have developed a drying system
which was claimed to produce beans having a flavour
similar to those produced in West Africa. The beans are
subjected to slow drying using an ambient air.
This paper describes the study on the effect of differ-
ent drying treatments on acidity and VFA (C,-C,)
content of cocoa beans. Flavour profiles of the resulting
beans are also described.
MATERIALS AND METHODS
Fermentation
Fermentation parameters for this study were based on
those recommended by Duncan et a l ( l 9 8 9 ) and Biehl et
a1 (1989). Two fermentation trials were carried out
between November and December 1989 at Sime
Darby’s Devon Cocoa Estates (Malacca, Malaysia).
Commercially ripe cocoa beans (the pods had at least a
tinge of yellow in colour) of PBC 123 and 128 clones
(1 : 1 ratio) were harvested, heaped on the ground and
kept under open shade at an ambient temperature
(30°C). After 9 days, the pods were split open with a
knife, placenta discarded and the beans (approximately
1 t) were fermented in three shallow wooden boxes
(1.0 m x 1.3 m x 0.42 m) to a depth of about 0.40 m.
The fermentation was carried out for 5 days; the mass
was turned using a shovel at 48 h of fermentation.
Drying
Upon completion of fermentation, the beans were coned
and quartered to give four subsamples of approximately
40 kg each to be used for drying study.
Oven-drying
Samples (10 cm in thickness) were dried in a ventilated
oven at 60°C in order to simulate ‘conventional’ hot-air
stream drying which is currently the general Malaysian
estate practice. However, this dried sample was
expected to be better than the actual standard Malay-
sian estate beans because these beans were from a differ-
ent fermentation regime (stored pods, shorter duration,
less number of turning and reduced depth of beans).
The drying took 20 h.
Air-blow drying
The process involves agitation of the beans in a layer
10 cm thick on a rectangular flat bed dryer
(5 m x 10 m, made by Sin Heng Trading Co, Muar,
Johor) with a time-controlled paddle. Ambient air was
passed through a gas heat exchanger before being
blown through the beans at a rate of 0.5-0.7m SKI.
After 72 h the temperature of the air was increased to
about 60°C and the beans were dried for 10 h. The heat
S Jinap, J Thien, T N Y a p
was generated by a wood-fired burner. The drying tem-
perature was regulated by quenching the hot air with
ambient air.
Shade-drying
This treatment was carried out to simulate extremely
poor conditions of bean drying as a consequence of
unfavourable drying conditions such as overloading,
insufficient heat and/or air flow (rainy season), prolong-
ed breakdown of the dryer or other forms of neglect.
The beans were spread out one bean thick on bamboo
planks lined with gunny sacks and left to ‘dry’ in the
shade for 120 h before being dried in a ventilated oven
at 60°C for 10 h.
Sun-drying
Fermented beans were spread out one bean thick on
bamboo planks lined with gunny sacks which were
raised about 2 m above the ground. The beans were
dried for 120 h under the sun from 8 am to 6 pm and
turned by hand twice daily, at 12 noon and 3 pm.
The samples (2 kg for each drying method) were
obtained by coning and quartering the beans taken
from five points of each drying process. For each
method, drying was terminated when the moisture
content of the beans was about 8% DM.
Physical and chemical analysis
Immediately upon sampling, the appearance, colour,
smell, texture and other physical characteristics of the
beans were recorded. A subsample of the beans was
kept at - 10°C in order to end or reduce enzymic activ-
ities; the samples were analysed for moisture content
and VFA at the University of Agriculture (Malaysia).
Another 1 kg of sample was dried at 60°C in a venti-
lated oven, to be used for flavour evaluation. The rest of
the sample was used for analyses of rapid moisture
content and titratable acidity, on site. For the purpose
of comparison, three batches of 2-weeks old, fermented
and dried Ghanaian samples which were obtained from
Cadbury (UK) were also analysed for nib moisture
content, titratable acidity, VFA, and flavour. All chemi-
cal analyses were done in triplicate.
Rapid moisture content
Two hundred beans were weighed immediately upon
sampling and was compared with weight of the beans at
the start of drying.
Nib moisture content
Moisture content of the nib was determined as
described in AOAC (1984). The samples were peeled
and the nibs ground in a Braun grinder. Ground cocoa
nibs (2.0 g) were weighed in pre-dried and cooled cruci-
bles. The samples were then dried in a ventilated oven
at 105°C until constant weight was achieved.
Efect of drying on cocoa beans
p H and titratable acidity
pH and titratable acidity (TA) of the nib were deter-
mined according to Duncan et a1 (1989). Ground nibs
(10 g) were homogenised (National MX-291N blender)
in distilled water (200 ml); the homogenate was filtered
(Whatman number 4) and pH of the supernatant was
measured (Jenway pH meter). For titratable acidity
determination, a 25 ml aliquot was titrated to pH of 8.0
with sodium hydroxide (0.01 M).
VFA
Extraction of VFA was carried out according to Jinap
and Dimick (1990a, b). Ground nibs ( 5 g) were distilled
(model Vapodest 3, Gerhardt, Germany) with sulphuric
acid (50 ml, 4 M); the distillate was collected in 2,2-
dimethylbutyric acid (5 ml, 0.01% v/v) as internal stan-
dard barium hydroxide (10 ml 0.01 M) and phenol-
phthalein (1% v/v) as indicator. The distillate (300 ml)
was evaporated to 5 ml using a rotary evaporator
(model V2000, Heidolph), transferred to a Universal
bottle, dried on a hot plate heater, taken up with 2 ml
of 1 M phosphoric acid, vortexed (30 s) and filtered
(Whatman number 4). The supernatant (0.5 pl) contain-
ing free VFA was immediately injected into a gas chro-
matograph (model 5890A, Hewlett Packard) connected
to a flame ionisation detector (FID).
The column used was 50 m x 0.32 mm x 0.3 pm
fused silica capillary column Carbowax 20 M (Hewlett
Packard) and the carrier gas was helium ( 5 ml min-').
The initial oven temperature was 110°C (2 min) with a
'
rate of 2"C, min- until final temperature of 160°C was
achieved; temperatures of the FID detector was 250°C
and the injector was 230°C.
Flavour analysis
Development of flavour was monitored according to
Duncan et a1 (1989). Samples (500 g) were roasted at
(150°C; 30 min) and cooled to ambient temperature.
After being peeled, the nibs (500 g) from each drying
treatment and the Ghanaian samples were ground for
1 min and passed through a 20 mesh screen. The
ground roasted nibs were mixed with icing sugar
(520 g), cocoa butter (160 g) in a Pascal runner mill
(45"C, 15 min), refined through a Pascal triple roll mill
to 20 pm and conched (45"C, 6 h), tempered, and
moulded into 10 x 5 cm bars. The chocolate was
wrapped in aluminium foil and maintained at 7°C until
evaluated. The chocolates were evaluated using a three-
point line-scale intensity test by 18 trained sensory
panel lists and qualitatively by two expert panel lists.
The Ghanaian sample was used as reference.
Statistical analyses
The data were subjected to the general linear models
procedure and the least significant difference test at the
5% level.
69
RESULTS AND DISCUSSION
Effect of drying on the physical appearance of the beans
The colour smell, texture and appearance of the sun-
dried and air-blown beans were similar to the fermented
and dried Ghanaian samples. The beans were noted to
have a medium rich dark brown colour and a pleasant
'roasted nut' smell. Although the beans were not wet or
sticky by the second day of drying, liquid was observed
inside the sun-dried and air-blown beans, just enough to
maintain the suppleness in the shell. The liquid which
was observed until the fourth day, diffused out of the
testa from inside the nib. The pH of the liquid was
found to be 3.2 as repoted by Duncan et al (1989) who
suggested that the free liquid contain acids and is dif-
fused from the nib. Slow drying allows the shell to be
replenished by the free liquid from the nib after mois-
ture from the shell is driven off. Therefore, shells of sun-
dried and air-blow beans were less fragile than the
oven-dried beans.
Oven-dried (60°C) beans had a lighter shade of
brown compared with that of sun-dried. The shell was
observed to be crinkly and stuck tightly to the nib; this
may be due to the high temperature used. The outer
layer of the beans (testa) which were dried at an exces-
sive rate broke the diffusion or capillarity continuum
and trapped the undesirable compounds, such as acetic
acid, within the beans. The beans have much weaker
smell compared with those of sun-dried beans.
In the case of shade-drying, from the second day
onwards the beans appeared dark and swollen; at the
same time the putrid ammonia smell was detected and
its intensity increased with time. The dark colour is due
to the presence of phlobaphenes, tannin-containing
macromolecules and quinone-amino acid adducts which
are formed during the oxidative phase of fermentation
(Ziegleder and Biehl 1988). The putrid odour was
mainly due to the production of ammonia nitrogen
through amino acid oxidase enzyme which was excreted
by aerobic microorganisms. Patches of white fungi were
observed at the fourth day of drying.
Effects of drying on moisture content and weight loss
Figure 1 shows the moisture profile of the bean samples
during drying. A consistent rate of moisture loss was
observed for sun and air-blown drying. The rate of
moisture loss was about 0.20% h -' for the first 24 h
but when the nib moisture was about 30% DM the rate
increased to 0.52% h-'. Beans dried using the air-
blown method showed a trend similar to sun-drying. In
the case of sun-drying, both heat and air movement
contribute to removal of moisture. For the air-blown
system, heat was not available for 72 h. However,
removal of moisture and acidity was achieved by air
movement, until the moisture content reached about
70 S Jinap, J Thien, T N Yap

Moisture c o n t e n t ( g per 1OOg)

50 + AIR-BLOWN

* SHADE DRY

0 10 20 30 .40 50 60 70 80 90 100 110 120

Time ( H o u r s )
Fig 1. Moisture profile during drying.

21% DM. Similar trend in weight change was noted
between these two modes of drying, despite the different
mechanism involved.
For shade-drying, heat, as well as aeration, was not
available and therefore the rate of moisture loss was
very slow. This greatly influenced the chemical and
physical stability of the beans. There was no significant
( P 3 0.05) moisture loss during the first 48 h of drying
in which the nib moisture content stayed at about 43%
DM ; significant moisture loss (0.32% h - I ) occurred
only after 48 h of drying, until the beans contained
about 22% DM moisture; thereafter the beans were
dried at 60°C. According to Wood (1983), the constant
rate stage of drying (which is the removal of water from
the testa) changes to the falling rate stage (where mois-
ture between the nib and testa, and inside the nib is
removed) occurs at a moisture content of about
40% dm. Therefore, for shade-drying, the important
stage of drying, which is the removal of moisture and
other components from the nib to the testa and from
there to the ambient air, was delayed. This promotes
numerous unfavourable changes in and around the
beans. The slow rate of moisture removal and prolifer-
ation of putrefactive organisms affected the acidity,
evolution of VFA, ammonia, and consequently flavour
and presence of off-flavours.
Effects of drying on pH and TA
Figures 2 and 3 show the pH and TA of the nib during
drying, and Table 1 shows the pH and TA of the dried
beans from each treatment, respectively. TA, which is a
better indicator of acidity than pH, showed an expected
steadily decreasing trend over time in all treatments.
The pH and TA of the sun (5.12 pH, 20.88 Meq NaOH
per 100 g) and air-blown dried beans (5.10 pH,
24.75 Meq NaOH per 100 g) respectively were not sig-
nificantly different (P 2 0.05) from that of the Ghanaian
sample (5.30 pH, 19.62 Meq per 100 g). Beans dried at
60°C in a ventilated oven were found to be highly acidic
(5.02 pH, 35.07 Meq per 100 g), confirming current

TABLE 1
pH, titrable acidity and free fatty acids of the dried cocoa beans"
_ _ _ _ _ _ _ ~ ____- ~~ ~~ -~~ ~ ______ ~~~ ~

Drying PH Titrable Acetic Propionic lsobutyric Butyric Isobutyric Total V F A

regime acidity acid acid acid acid acid
(Meq NaOH per 100 g)
mg kg-'

Sun 5.12b 20.88b 674.61~ 13.11b 20.90~ 12.49~ 29.89b 751.00~

Air-blown 5.10b 24.75b 724.98~ 13.63b 24.69~ 19.73~ 28.52b 811.55~
Oven 5.05~ 35-07a 2970.39a 42.03a 46.89a 45.21a 101.50 3206.02a
Shade 5.61a 19.69~ 1217.19b 14.88b 31.55b 29.98b 30.35b 1323.95b
Ghana 5.30b 19.62b 600.02~ 9.65~ 25.60~ 1 1.94c 46.68a 693.89~
~ ~~

Means within the same column with the same foollowing letter are not significantly different ( P > 0.05).
Effect of drying on cocoa beans 71

6
PH
S U N DRY
5.7 A I R BLOWN
0S H A D E DRY
OVEN D R Y
5.4 .~

5.1

4.8

4.5 -
0 24 48 72 96 130

Time ( H o u r s )
Fig 2. The pH profile during drying.

Malaysian cocoa industry problems of high acidity in
beans. The shade-dried samples were observed to have
less acidity (5.61 pH, 17.69 Meq per 100 g) than the
Ghanaian sample due to putrefactive activities
occurring in the nibs. These activities were induced by
the prolonged high nib moisture of the beans. There-
fore, TA alone is not a good criterion for comparison of
total bean quality but must be used judiciously with
flavour evaluation. The results from these experiments
suggested that reduced acidity can be achieved when
rate of evaporation of liquid from the testa is balanced
with its rate of diffusion from the nib. Thus, rapid
drying will cause the testa to become hardened and
impermeable to the free liquid carrying the acetic acid
to the nib, allowing only water to escape and trapping
the acid molecules. In the case of shade-drying, the
acetic acid accumulated in the nibs during fermentation
was neutralised by the alkaline compounds derived
during putrefactive activities.
Effect of drying on the concentration of VFA
The progressive changes of the mean concentration of
each of the acids during different drying regimes are
shown in Figs 4-8. The VFA concentration of the dried
beans from each drying treatment are shown in Table 1.
Inspection of data available confirmed the observed
trends of dissipation of VFA and titratable acidity in
the various drying methods. Oven-dried samples had

Meq N a O H p e r lOOg dr! weight

I

SUN DRY
A I R BLOWN

0SHADE DRY
OVEN DRY

35

25

15
0 21 48 72 96 120

Time ( H o u r s )
Fig 3. Titratable acidity profile during drying.
72 S Jinap, J Thien, T N Yap

g per kg dry weight

8

-
m S U N DRY
AIR BLOWN
0 SHADE DRl
OVEN DR'L-

0 24 48 72 96 I20
Time (Hours)
Fig 4. Acetic acid profile during drying.

the highest total VFA content (3206.02 mg kg-') while
sun (751.00 mg kg-' and air-blown (811.55 mg kg-')
dried beans were not significantly different (P 2 0.05)
from the Ghanaian (693.89 mg kg-') in total VFA
content.
Concentration of acetic acid was observed to follow a
decreasing trend in all the treatments (Fig 4). The low
acetic acid content in the shade-dried beans should not
be interpreted as a sign of improvement of flavour. On
the contrary, the low acidity could well indicate neutral-
isation of acids with the alkaline compounds derived
during purefactive activities in the nibs. Residual
amounts of these compounds can cause off-flavours.
Oven-dried beans were found to have the highest con-
centration of acetic acid. In the case to propionic acid, a
downward trend was observed for all the drying treat-
ments (Fig 5). A sharp decrease in the acid content
occurred during the first and second day of drying, after
which the content of propionic acid declined at a slower
rate.
In the case of butyric acid, plots showing the develop-
ment of butyric acid profile over time (Fig 6) agree well
with the expected trend. The two more efficient drying
systems showed an increase in concentration of butyric
acid within 25-45 h but this was later dissipated with
increased removal of water. The shade-dried beans
showed a high increase in butyric acid but due to the
slower water loss, this butyric acid remained. The iso-
butyric acid development and dissipation trend (Fig 7)
was not as clear as that observed for butyric acid.

mg per kg dry weight

120
100
7 AIR BLOWN
0 SHADE DRY
80

60

40

20

0
0 24 48 72 96 120

Time (Hours)
Fig 5. Propionic acid profile during drying.
Efect of drying on cocoa beans 73

m g p e r kg d r y weight
70

S U N DRY
60 AIR BLOWN
0 SHADE DRY
OVEN DRY
50

40

30

20
0 24 48 72 96 120

Time (Hours)
Fig 6. Isobutyric acid profile during drying.

Higher concentrations of this VFA was again noted in
the shade-dried beans, while sun-dried and air-blown
processed beans showed similar concentrations of iso-
butyric acid as the Ghanaian sample. Again, it was
noted that a high concentration of the acid has accumu-
lated in the oven-dried beans. The trend of development
and dissipation of isovaleric acid (Fig 8) was not as
clear as butyric acid.
Effects of drying on flavour
Table 2 shows the flavour intensity of six attributes for
each drying treatment. These flavour scores represent
the perceived difference from the standard reference
chocolate. The chocolate attribute is expected to be zero
at best, which will mean that the sample is as good as
the standard reference chocolate. It should be noted
that the chocolate score can be adversely affected by
excessive acidity and/or off-flavour.
There was no significant difference (P 2 0.05)
between the acidity score for air-blown and sun-dried
beans. The similar trend was found with the ‘citrus
fruits’ score although the range was narrower. The
expert panellists gave favourable comments of ‘no off-
flavour’ for air-blown dried sample, and ‘clean flavour’,
‘well-developed chocolate flavour’ and ‘fruity’ flavour
for sun-dried samples.
The shade-dried beans have the lowest acidity flavour
score (- 0.57); this was due to putrefaction and neutral-
isation of acid during the later stage of fermentation.
The shade-dried beans were also shown to have signifi-
cantly (P < 0.05) high intensity of ‘off-flavour’ score

100 ,m g per kg d r y weight

=
80 1 &IN DRI-
$IR BLOWN
a SHADE D R I
O \ E N DR’I

0 24 48 72 96 120

Time (Hours)
Fig 7. Butyric acid profile during drying.
74 S Jinap, J Thien, T N Yap

mg per kg dry weight

80 I

S U N DRY
AIR BLOWN

0SHADE DRY
OVEN DRY

0 24 48 72 96 120

Time (Hours)
Fig 8. Isovaleric acid profile during drying.

(1.67) compared to other three treatments. This obser-
vation demonstrates that shade-drying, which prolong-
ed the termination of microbial action produces higher
total VFA which could be relate to organoleptically
detectable off-flavours. The two expert panellists
described these off-flavours as ‘musty’, ‘stale’, ‘cheese-
rind’, ‘unpleasant’ and ‘hammy’.
Oven-dried beans has the poorest flavour score (2.75)
in acidity which could be due to undissipated acids
during drying. In addition to being highly acidic, the
oven-dried samples were also found to be significantly
sour (P < 0.05) compared to the other treatments. The
samples were noted to be low in chocolate flavour by
the expert panellists.
CONCLUSIONS
Occurrence of over-fermentation was noted clearly in
the shade-dried beans. These beans were dark in colour,
infested by mould and yeast and putrid in smell; the
resultant chocolates had a low intensity of chocolate
flavour but high in off-flavour. An increase in VFA and
pH, and a decrease in titratable acidity suggests
putrefactive activities in the beans due to the high reten-
tion of moisture. The results have shown that over-
fermentation will occur when inadequate heat and air
movement is available to facilitate the removal of mois-
ture and other undesirable water-soluble components of
the beans; thus promoting various unfavourable
changes in the beans. Oven-dried (at 60°C) beans were
found to be acidic and high in their C,-C, VFA
content; thus causing the resultant chocolate to be
evaluated below the standard in the major attributes.
There was no significant difference between the air-
blown dried and sun-dried beans in acidity, C,-C,
VFA, physical appearance and flavour quality. There-
fore the air-blown drying should be practised when sun-
drying is not possible. The drying method achieved 80%
of the required drying capacity with ambient air and
thus at much reduced energy cost compared with high
temperature drying usually practiced by the estates. The
shells did not strongly dehydrate, hence they did not

TABLE 2
Flavour score of the resultant chocolates“

Drying Flavour projileb

regime
1 2 3 4 5 6

Sun -0.llb 0.85b 0.llb 0.53b 0.69b 0.32b

Air-blown -0.34b 0.74b O.llb 0.43b 0.66b 0.41b
Oven - 1.55a 2.75a 0.39a 1.48a 1.73a 0.38b
Shade -1.30a -0.57~ -0.19~ 1.32a 1.55a 1.67a

Mean values with a common following letter within the same column are not
significantly difference ( P 0.05).
1, Chocolate; 2, acid; 3, citrus fruits; 4, bitter; 5, astringent; 6, off-flavour.
Effect of drying on cocoa beans
become brittle as easily; therefore the shells became less
vulnerable to mechanical damage during drying and
further handling of the beans.
The study has confirmed that the flavour character-
istics of Malaysian cocoa, and its quality as perceived
by the manufacturers, can be improved through the pod
storage, and proper fermentation and drying regimes.
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