Moisture sorption isotherms and heat of sorption of instant

(soluble) green tea powder and green tea granules

V.R. Sinija
*
, H.N. Mishra
Post Harvest Technology Centre, Agricultural and Food Engineering Department, Indian Institute of Technology, Kharagpur 721 302, West Bengal, India
Received 19 August 2007; received in revised form 29 October 2007; accepted 30 October 2007
Available online 4 November 2007
Abstract
Moisture adsorption isotherms of green instant tea powder and green tea granules were determined at 20, 30, 40 and 50 C. A gravi-
metric static method was used under 0.110.90 water activity ranges for the determination of sorption isotherms that were found to be
typical type II sigmoid. Experimental data were tted to various mathematical models and found that Peleg model suits best in describing
equilibrium moisture contentequilibrium relative humidity (EMCERH) relationships for instant green tea samples as well as green tea
granules, over the entire range of temperatures. The net isosteric heat of sorption was determined from the equilibrium data at dierent
temperatures. The isosteric heat of sorption varied between 48.54 and 44.71 kJ/mol at moisture levels varying between 1 and 9 g/g dry
matter for instant green tea powder and 47.96 and 44.10 kJ/mol at moisture level varying between 0.2 and 1.4 g/g dry matter for green tea
granules.
2007 Elsevier Ltd. All rights reserved.
Keywords: Sorption; Instant tea; Tea granules; Isotherms; Equilibrium moisture content; Water activity; Isosteric heat of sorption
1. Introduction
Tea is the most consumed drink in the world after water.
Green tea is a non-fermented tea, and contains more cat-
echins, than black tea or oolong tea. Increasing interest in
its health benets has led to the inclusion of green tea in the
group of beverages with functional properties (Cabrera
et al., 2006). Due to its aroma, stimulatory eect, health
benets and convenience in use green instant tea is now
becoming more and more popular one of the most widely
consumed beverage worldwide. Green instant tea was pro-
duced by freeze drying of juice expressed from macerated,
steamed leaf and green tea granules was produced from the
drying of residue obtained after partial extraction of juice.
The nal target moisture content of dried tea samples
(instant tea powder and tea granules) is around 35% wet
basis (wb). Some sorption of moisture during sorting and
packing takes place but the packed product remains below
7% moisture content wb. As the moisture content is
reduced to such a low level compared to most agricultural
products, equilibrium moisture content (EMC) plays a par-
ticularly important role at the end of drying (Temple and
van Boxtel, 1999). The quality of most foods preserved
by drying depends to a great extent upon their physical,
chemical and microbiological stability. This stability is
mainly a consequence of the relationship between the
EMC of the food material, and its corresponding water
activity, at a given temperature (Myhara et al., 1998). An
addition or removal of water changes the composition
and dimensions of products and may induce phase changes
(Irzyniec and Klimczak, 2003).
Knowledge of the moisture sorption characteristics of
tea is important for predicting its stability during storage
and selecting appropriate packaging materials. Dierent
materials have dierent equilibrium moisture contents.
The EMC is dependent upon the temperature and related
humidity of the environment as well as species, variety
0260-8774/$ - see front matter 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2007.10.026
*
Corresponding author. Tel.: +91 3222 281323; fax: +91 3222 282244.
E-mail address: sinijav@iitkgp.ac.in (V.R. Sinija).
www.elsevier.com/locate/jfoodeng
Available online at www.sciencedirect.com
Journal of Food Engineering 86 (2008) 494500
and maturity of the grain (Chakraverty, 1981). Temple and
van Boxtel (1999) produced data on equilibrium moisture
of tea in a form that can be used in modeling the drying
process. Jayaratham and Kirtisinghe (1974) used saturated
salt solutions to determine the EMC values for a stored
black tea at 20 C. Studies on black teas from Kenya using
the saturated salt method were carried out by Doughan
et al. (1979). Lomauro et al. (1985) attempted to t data
from tea to various equations, concluding that the GAB
model showed the best t, followed by the Oswin model.
The knowledge and understanding of moisture sorption
isotherms for foods is of great importance in food science
and technology for many uses such as the design and opti-
mization of processing as for instance in drying, for assess-
ing the packaging problems, for modeling moisture
changes which occur during drying, for predicting shelf life
stability and for ingredient mixing predictions (Jamali
et al., 2006) The knowledge of sorption isotherms at dier-
ent temperatures enables an evaluation of the heat of sorp-
tion, which determines the interaction between an
adsorbent and adsorbate. Water availability in the reac-
tions of food degradation depends both on water content
and on the properties of the diusion surface, i.e., on the
thermodynamic function of sorbed water. Experimental
sorption data have been used to evaluate the thermody-
namic functions of several foods (Al-Muhtaseb et al.,
2004).
Accurate information on EMC of instant tea at various
relative humidity and temperatures are not available. There
is also a need for comprehensive study of the equilibrium
moisture contents of instant green tea and green tea gran-
ules to understand its drying and storage behaviour. The
present study was carried out with the objective of deter-
mining moisture sorption isotherms for green instant tea
powder and green tea granules and also to analyze the data
with the help of six sorption isotherm equations available
in the literature. Eorts were also made to nd out the
most suitable model describing the isotherms of green
instant tea and green tea granules and to calculate the
net isosteric heat of sorption from the experimental data.
2. Materials and methods
The fresh tea leaves for preparation of tea samples were
plucked from the tea gardens of Indian Institute of Tech-
nology, Kharagpur, India. Fresh tea leaves were steamed
immediately after plucking, to arrest the fermentation reac-
tion and a part of the juice was expressed out from the
steamed leaves for production of instant tea. The juice with
a total solid content of 79% was freeze dried to obtain
instant tea powder and the pressed leaf residue with a mois-
ture content of 6364% (wb) was subjected to hot air dry-
ing in order to get the tea granules. The instant tea (mc 6
8% (wb)) and green tea granules (mc 56% (wb)) thus pro-
duced were used for adsorption isotherm generation and
the juice and pressed leaf residue were used for desorption
isotherm generation.
A sorption isotherm represents the relationship between
EMC of a material with the relative humidity (RH) of the
surrounding environment at a particular temperature.
These are useful in determining several product parameters
related to sorption process. The procedure suggested by
Iglesias and Chirife (1982) was followed for deriving sorp-
tion isotherms at 20, 30, 40 and 50 C. Two to three grams
samples of juice, pressed leaf residue and its powders
(instant tea powder and tea granules) lled in sterilized
glass weighing bottles were placed in seven separate desic-
cators containing saturated salt solutions (LiCl, KC
2
H
3
O
2
,
MgCl
2
, Mg (NO
3
)
2
, NaCl, KCl and KNO
3
) for maintain-
ing equilibrium relative humidity (ERH) levels from 10%
to 90% (Greenspan, 1977; Palipane and Driscoll, 1992;
Young, 1967). The air inside the desiccators was sucked
with the help of a vacuum pump.
All these seven desiccators were put in an incubator set
at 20 C and the gain or loss in weights of all these samples
in each desiccator was monitored for every three days. The
EMC was noticed when three consecutive weight measure-
ments showed a dierence of less than 0.001 g. This took
about 1619 days, depending on the nature of the samples
and the temperature inside the incubator. Two replications
were kept for each sample and the average values of EMC
have been reported. The EMC of each sample was deter-
mined by gravimetric method, by keeping the sample over-
night in a hot air oven in which temperature was xed at
105 C. The temperature of the incubator was changed,
and the same experiment was conducted for sorption pro-
cess at 30, 40 and 50 C. A glass dish containing 5 ml tolu-
ene was placed in desiccator with relative humidity higher
than 75% to check mold growth (Labuza, 1984). When
moisture content of the tea samples reached equilibrium
with the relative humidity of the atmosphere maintained
in desiccator, the water activity (a
w
) of the sample was
equal to the relative humidity (fraction) of the atmosphere
inside the desiccators. To establish moisture sorption iso-
therms, the equilibrium moisture contents were plotted
against water activity.
2.1. Analysis of sorption data
A large number of models have been proposed in the
literature for the sorption isotherms. The relationship
between the total moisture content and water activity of
the food, over a range of values, at a constant temperature
and under equilibrium conditions yields a moisture sorp-
tion isotherm when expressed graphically. The typical
shape of an isotherm reects the manner in which the
water is bound to the system. In the eld of water vapor
sorption by a solid sorbent, moisture sorption hysteresis
is the phenomenon by which two dierent paths exist
between the adsorption and desorption isotherms. It has
been stated that the extent of hysteresis is related to the
nature and state of the components in a food, reecting
their potential for structural and conformational rear-
rangements, which alter the accessibility of energetically
V.R. Sinija, H.N. Mishra / Journal of Food Engineering 86 (2008) 494500 495
favourable polar sites (Al-Muhtaseb et al., 2004; Kapsalis,
1981).
Temple and van Boxtel (1999) used Halsey, GAB, Hen-
derson and Oswin equations to t experimental sorption
data of tea. The dierent models were chosen to t the
experimental sorption data as shown in Table 1 (Sinija
and Mishra, 2007). M
e
, X
m
, a
w
and t represent equilibrium
moisture content, monolayer moisture content, water activ-
ity and temperature (C), respectively. The other symbols
(A, B, C, K, K
1
, K
2
, n
1
, n
2
) are isotherm constants.
2.2. Validation of sorption models
The coecients of various sorption equations were
determined by means of standard regression technique
using Origin 7.5 software. The various sorption models
were evaluated for their suitability in predicting the sorp-
tion behaviour of the sample on the basis of the coecient
of determination (r
2
) and reduced v
2
values and also on the
basis of residual plots. The dierence between the measured
and predicted EMC values at various water activities were
dened as residuals. The residuals were plotted against pre-
dicted values of EMC. A model is considered acceptable if
the residual values fell in horizontal band centered around
zero, displaying no systematic tendencies (i.e., random in
nature) towards a clear pattern. If residual plot indicates
clear pattern, the model is not acceptable.
2.3. Heat of sorption
The isosteric heat of sorption is a dierential molar
quantity derived from the temperature dependence of the
isotherm, which represents the energies for water molecules
binding at a particular hydration level (Beristain et al.,
2002). The net isosteric heat of sorption (q
st
) was deter-
mined using the ClausiusClapeyron equation (Labuza
et al., 1985):
ln
a
w1
a
w2

q
st
R
1
T
1

1
T
2

; 1
where a
w1
and a
w2
are water activities at temperatures T
1
and T
2
, respectively and R is the universal gas constant
(8.314 J/mol K). The isosteric heat of sorption (Q
st
) was
calculated from the relationship Q
st
= q
st
+ DH
v
, where
DH
v
is the latent heat of vaporization of pure water at
35 C (43.53 kJ/mol), the average of the two temperatures
used in the study (20 and 50 C).
3. Results and discussion
3.1. Sorption curves
The results of the sorption experiments are presented in
Figs. 14. The EMC increases with decreasing temperature,
at constant equilibrium relative humidity (ERH). This
result may be explained by the higher excitation state of
water molecules at higher temperature thus decreasing
the attractive forces between them (Mohamed et al.,
2004). Furthermore, at constant temperature, the EMC
increases with increasing ERH. Similar results have been
reported in the literature for the sorption curves (Arslan
and Togrul, 2006; Basunia and Abe, 2001; Ghodake
Table 1
Dierent sorption models tted to the experimental data of tea samples
Model Mathematical expression
GAB M
e
= X
m
CKa
w
/[(1 Ka
w
)(1 Ka
w
+ CKa
w
)]
BET M
e
= X
m
Ca
w
/[(1 a
w
)(1 a
w
+ Ca
w
)]
Oswin M
e
= A[a
w
/(1 a
w
)]
B
Peleg M
e
K
1
a
n
w1
K
2
a
n
w2
Modied Henderson M
e
= [ln(1 a
w
)/(A(t + C))]
1/B
Modied Halsey M
e
= [exp(A + Bt)/ln(a
w
)]
1/C
0.0 0.2 0.4 0.6 0.8 1.0
0
2
4
6
8
10
12
14
20C
30C
40C
50C
m
o
i
s
t
u
r
e

C
o
n
t
e
n
t
(
g
/
g

d
r
y

m
a
t
t
e
r
)
a
w
Fig. 1. Desorption isotherms of tea leaf juice at dierent temperatures.
0.0 0.2 0.4 0.6 0.8 1.0
0
2
4
6
8
10
20C
30C
40C
50C
m
o
i
s
t
u
r
e

c
o
n
t
e
n
t
(
g
/
g

d
r
y

m
a
t
t
e
r
)
a
w
Fig. 2. Adsorption isotherms of instant green tea powder at dierent
temperatures.
496 V.R. Sinija, H.N. Mishra / Journal of Food Engineering 86 (2008) 494500
et al., 2007; Lahsasni et al., 2003; Mohamed et al., 2004;
Stencl et al., 1999).
Figs. 5 and 6 show the adsorption and desorption curves
at 30 C for instant green tea powder and green tea gran-
ules. Similar behaviour of adsorption and desorption iso-
therms was observed for other temperatures also. The
gure clearly shows that the EMC for desorption was
higher than that for adsorption, at a particular water activ-
ity. Hysteresis existed over the entire water activity range.
Some thermodynamically irreversible processes must occur
during desorption or adsorption. Polar sites in the molecu-
lar structure of the material are almost entirely occupied by
adsorbed water in the wet condition. Upon drying and
shrinkage, the molecules and their water holding sites are
drawn closely enough together to satisfy each other. This
reduces the water holding capacity of the material upon
subsequent adsorption (Mohsenin, 1986).
3.2. Fitting of sorption models to experimental sorption data
The sorption curves for tea juice, residue, instant green
tea powder and green tea granules are drawn as EMC
against the a
w
(ERH). These curves are used to estimate
the coecients of the dierent sorption models and it was
found that Peleg model (M
e
K
1
a
n
w1
K
2
a
n
w2
, where M
e
and a
w
represent equilibrium moisture content and water
activity, respectively and other symbols are isotherm con-
stants) gives best t to the experimental data for instant
tea powder and green tea granules, with highest values of
r
2
and lowest values of v
2
than other models for sorption
isotherms for a wide range of water activity. Values of
the various coecients, regression coecient (r
2
) and
0.0 0.2 0.4 0.6 0.8 1.0
0.0
0.5
1.0
1.5
2.0
2.5
m
o
i
s
t
u
r
e

c
o
n
t
e
n
t
(
g
/
g

d
r
y

m
a
t
t
e
r
)
a
w
20C
30C
40C
50C
Fig. 3. Desorption isotherms of pressed leaf residue at dierent
temperatures.
0.0 0.2 0.4 0.6 0.8 1.0
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
1.8
20C
30C
40C
50C
m
o
i
s
t
u
r
e

c
o
n
t
e
n
t
(
g
/
g

d
r
y

m
a
t
t
e
r
)
a
w
Fig. 4. Adsorption isotherms of green tea granules at dierent
temperatures.
0.0 0.2 0.4 0.6 0.8 1.0
0
2
4
6
8
10
12
desorption
adsorption
m
o
i
s
t
u
r
e

c
o
n
t
e
n
t
(
g
/
g

d
r
y

m
a
t
t
e
r
)
a
w
Fig. 5. Hysteresis eect at 30 C for tea leaf juice and instant tea powder.
0.0 0.2 0.4 0.6 0.8 1.0
0.0
0.5
1.0
1.5
2.0
desorption
adsorption
m
o
i
s
t
u
r
e

c
o
n
t
e
n
t
(
g
/
g

d
r
y

m
a
t
t
e
r
)
a
w
Fig. 6. Hysteresis eect at 30 C for pressed leaf residue and green tea
granules.
V.R. Sinija, H.N. Mishra / Journal of Food Engineering 86 (2008) 494500 497
reduced chi square (v
2
) for Peleg model, are presented in
Table 2. Fig. 7 shows the residual plots for tea juice, resi-
due, instant tea powder and green tea granules.
3.3. Heat of sorption
The study of sorption isotherms at least at two dierent
temperatures provides thermodynamic data on isosteric
heat of sorption through the use of ClausiusClapeyron
equation. The isosteric heat of sorption varies with the
amount of water adsorbed by the substrate. The calcula-
tion of the variation of net isosteric heat of sorption as a
function of moisture content, at the mean temperature of
30 C, was done by Eq. (1). The relationship between isos-
teric heat of sorption and moisture content is plotted in
Fig. 8a and b. At moisture content below 7 g/g dry matter
and 1 g/g dry matter, the isosteric heat of sorption
increased sharply for instant tea and green tea granules,
respectively, and values of 48.54 kJ/mol and 47.96 kJ/mol
were estimated. However, at moisture content above that
the isosteric heat of sorption fell almost in line with the
heat of vaporization of pure water. The decrease in the
isosteric heat of sorption with increase in amount of water
sorbed is due to the fact that initially, sorption occurs on
Table 2
Estimated parameters of the Peleg model tted to sorption data for instant green tea powder and green tea granules
Sample Constants Adsorption Desorption
20 C 30 C 40 C 50 C 20 C 30 C 40 C 50 C
Instant tea powder and tea leaf juice K
1
11.051 55.363 19.159 1316.4 13.943 13.381 12.381 11.131
K
2
7.8599 8.9701 8.3889 8.2039 50.180 51.896 84.905 39.639
n
1
12.520 31.069 23.389 64.949 2.0639 2.1961 2.2331 2.1909
n
2
2.1587 2.5193 2.5815 2.5390 32.401 151.28 82.858 139.04
r
2
0.9998 0.9996 0.9997 0.9992 0.9996 0.9971 0.9982 0.9972
v
2
0.0463 0.0102 0.0069 0.0139 0.0229 0.1325 0.0722 0.0938
Green tea granules and pressed leaf residue K
1
1.7266 1.1804 1.9023 1.7112 3.8765 2.5932 1.9906 1.5863
K
2
3.8739 2.5932 0.0639 0.0246 1.7269 1.1805 0.0365 2494.7
n
1
1.5540 1.39029 3.2476 2.8741 16.555 9.0178 2.5936 1.9529
n
2
16.545 0.0173 0.199 0.6180 1.5544 1.3903 0.448 93.716
r
2
0.9984 0.9973 0.9925 0.9898 0.9984 0.9973 0.9967 0.9931
v
2
0.0020 0.0031 0.0047 0.0054 0.0020 0.0031 0.0025 0.0042
-0.06
-0.04
-0.02
0
0.02
0.04
0.06
0 0.5 1 1.5 2 2.5
r
e
s
i
d
u
a
l
s
Peleg at 30C for pressed leaf residue
-0.15
-0.1
-0.05
0
0.05
0.1
0.15
0 0.5 1 1.5 2
r
e
s
i
d
u
a
l
s
Peleg at 30C for green tea granules
-0.4
-0.3
-0.2
-0.1
0
0.1
0.2
0.3
0 10 8 6 4 2 12
r
e
s
i
d
u
e
s
Peleg at 30C for tea juice
Predicted EMC values (g/g dry matter)
-0.15
-0.1
-0.05
0
0.05
0.1
0.15
0 2 4 8 6 10
r
e
s
i
d
u
a
l
s
Peleg at 30C for instant green tea
Predicted EMC values (g/g dry matter)
Fig. 7. Residual plot for various tea samples.
498 V.R. Sinija, H.N. Mishra / Journal of Food Engineering 86 (2008) 494500
the most active sites, giving rise to higher energy of interac-
tion between the sorbate and the sorption sites. As these
active sites become occupied, sorption subsequently occurs
on the less active sites giving lower heats of sorption (Igle-
sias & Chirife, 1982). The net isosteric heat of sorption ran-
ged from 5.01 kJ/mol at moisture content of 1 g/g dry
matter to 1.10 kJ/mol at a moisture content of 9 g/g dry
matter for instant tea powder and the corresponding value
for tea granules was 4.43 kJ/mol at moisture content of
0.2 g/g dry matter and 0.58 kJ/mol at moisture content of
1.4 g/g dry matter.
4. Conclusions
The moisture sorption isotherms of various tea samples
presented a sigmoid shape and belong to type II of BET
classication. The experimental results illustrated that
EMC increased with decreasing temperature, at constant
ERH. Furthermore, at constant temperature, the EMC
increased with increasing ERH. Various models were tested
for their ability to t the experimental sorption data. The
sorption data were in good agreement with popular sorp-
tion models like Peleg, modied Henderson and GAB
equations. However, the Peleg model could be found best
to describe the sorption isotherm at all the temperatures
studied for both instant green tea powder and green tea
granules. The isosteric heat of sorption curve showed a reg-
ular fall with increasing moisture content and approached
the heat of vaporization of free water at higher moisture
content.
Acknowledgement
The rst author is grateful to All India Council for
Technical Education (AICTE), for the nancial assistance
received in the form of National Doctoral Fellowship to
pursue her doctoral programme.
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44
45
46
47
48
49
1 2 8 7 3 4 5 6 9
Moisture content, g/g dry matter
I
s
o
s
t
e
r
i
c

h
e
a
t

o
f

s
o
r
p
t
i
o
n
,
K
J
/
m
o
l
44
45
46
47
48
49
1 2 3 4 5 7 6 8 9
Moisture content, g/g dry matter
I
s
o
s
t
e
r
i
c

h
e
a
t

o
f

s
o
r
p
t
i
o
n
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K
J
/
m
o
l
Fig. 8. Variation of isosteric heat of sorption with moisture content for (a) instant green tea powder and (b) green tea granules.
V.R. Sinija, H.N. Mishra / Journal of Food Engineering 86 (2008) 494500 499
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