Journal of Stored Products Research 59 (2014) 140e145

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Journal of Stored Products Research

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Sorption isotherm and state diagram in evaluating storage stability for

sultana raisins
Mariam Esmaiili Bazardeh, Mohsen Esmaiili*
Food Science and Technology Department, Agricultural Faculty, The University of Urmia, P.O.Box 165, Urmia, Iran

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

Article history: To investigate the optimum storage condition, the interrelation between water activity (aw) and glass
Accepted 3 July 2014 transition temperature (Tg) of sultana raisins were evaluated. Water adsorption isotherms of sultana
Available online 1 August 2014 raisins were measured at 15, 25 and 35
C using an isopiestic method. The measured data were fitted into
BET and GAB models. Thermal transitions of equilibrated raisins and separated crystals of raisins were
Keywords: analyzed using differential scanning calorimetry (DSC). The plasticizing influence of water on glass
Sultana raisin
transition was modeled by GordoneTaylor, Khalloufi and an empirical model. The state diagram was
Sugaring
constructed by adsorption isotherm and the glass line to investigate relation between the two distinct
Glass transition
Sorption isotherm
criteria of the raisins stability. The water sorption data provided the monolayer moisture content values
State diagram of 0.0789 and 0.082 g water/g dry product at 25
C in the BET and GAB models, respectively. The glass
transition temperature of raisins decreased with increasing water contents. According to the state dia-
gram, the predictions of critical water content (Cwc) for stability of raisins at 25
C was underestimated in
comparison with the sorption isotherm. Results showed that the state diagram and water adsorption
data may be used to predict the stability of sultana raisins and both Tg and aw should be considered to
control sugaring phenomenon in raisins.
© 2014 Elsevier Ltd. All rights reserved.

1. Introduction stability being studied (Rahman, 2010). For identifying stability of

In view of the fact that theory of water activity provides a sole
basis for product and process development, the relationship be-
tween rate of physicochemical changes in foods and water activity
(at a given range) guide the development of food products with
prolonged shelf-life and unique quality attributes. Nowadays, these
developments have led to the deeper ideas of glass transition.
Shelf-life of foods is strongly influenced by water content and
temperature. To predict foods stability and calculate the changes of
moisture content during storage, moisture sorption isotherms are
determined (Gal, 1983). To get a better understanding about the
factors governing the stability of foods, it is being recommended
that the concept of water activity be added along with the com-
plementary concept of glass transition (Bhandari and Howes, 1999;
Roos et al., 1996). However, considerable amount of published data
on water activity (aw) and the glass transition indicate that the
relationships between these concepts can be very complex,
depending on the complexity of the food system and on the type of
* Corresponding author. Tel.: þ98 44 3277 5035; fax: þ98 44 3277 9558.
E-mail addresses: esmaili_ma@yahoo.com (M.E. Bazardeh), m.esmaiili@urmia.
ac.ir, esmaiilim@yahoo.ie (M. Esmaiili).
dried foods, the use of the state diagram based on GordoneTaylor
and the GAB (GuggenheimeAndersenede Boer) sorption models
has been proposed (Roos, 1995). The glass transition temperature
(Tg) is mainly a function of moisture content, molecular weight and
nature of the dry matter compounds in a given substance. As a food
material undergoes the glass transition, it changes from a brittle,
highly viscous glassy state to a more elastic liquid-like state.
Sultana raisin is one of the important commercial crops in the
world. For producing sultana raisins, the ripe seedless grapes are
usually dipped in an alkaline emulsion, and then dried by sun
(Esmaiili et al., 2007). Crystallization of sugars in raisins (sugaring)
is one of the major concerns of exporters and consumers due to an
unattractive appearance and disagreeable texture of the raisins.
Sugaring usually is seen in a long time stored raisins, when the
climate becomes relatively warm and humid (e.g. during May and
June). In addition fluctuating storage conditions such as tempera-
ture and humidity, excessive handling and abrasion of raisins and
high moisture content are known to be important factors in sug-
aring (Christensen and Peacock, 2000). It is referred that the overall
rate of crystallization exhibits a maximum between Tg and equi-
librium melting temperature (Tm) (Sperling, 1986). It has to be
considered that in dried fruits (e.g. raisins) sugars are a major

http://dx.doi.org/10.1016/j.jspr.2014.07.001
0022-474X/© 2014 Elsevier Ltd. All rights reserved.
 M.E. Bazardeh, M. Esmaiili / Journal of Stored Products Research 59 (2014) 140e145 141

component and knowledge of Tg has generally been accepted as
being useful in relation to crystallization rates (Canellas et al., 1993).
Time-dependent crystallization of sugars may occur above critical
relative humidity. Moisture content has been shown to have the
most dramatic effect on glass transition as even a marginal increase
in moisture can cause a significant decrease in Tg. The time required
for crystallization decrease rapidly with increasing storage relative
humidity (RH) (Karel, 1973). Since amorphous sugars are more
hygroscopic than crystalline sugars, crystallization may cause
releasing water, thereby increasing water content, which can result
in accelerated reactions in the remaining material (Kilcast and
Subramaniam, 2000). At high RH the crystallized material gained
water due to solubilization.
The exact cause of sugaring is not clear and the optimum storage
condition for prevention of this phenomenon has not yet been
covered in significant details. In this study an attempt is made to
examine the interrelationship between the aw and Tg in evaluating
stability of sultana raisins during storage, to get a better under-
standing about the factors governing the sugaring.
2. Materials and methods
2.1. Materials
Sultana raisins were obtained from the local market in Urmia,
West Azerbaijan province, Iran. The adsorption isotherms were
determined by static gravimetric method. Raisins with initial
moister content of 0.156 (g water/g dry product) were sliced
(1 mm thick) to facilitate diffusion of water. Approximately 1 g of
samples were distributed into weighing plates and placed in
hermetic jars at a known aw Nine different saturated salt solutions
(LiCl, KC2H3O2, MgCl2, K2CO3, Mg[NO3]2, NaNO2, NaCl, KCl, BaCl2)
were selected to give different RH in the range of 0.11e0.90. The
selected salt solutions and their corresponding RH at different
temperatures were taken from data reported by Sablani et al.
(2001). The jars were maintained in a temperature controlled
cabinet (Heraeus, UT 5050 E, W. Germany, with an accuracy of
±1
C) at the constant temperatures 15, 25 and 35
C. Microbial
growth at high aw (aw > 0.6) avoided by using a small amount of
toluene in a special support. Three replications of the same
experiment were carried out. Equilibrium was established be-
tween the environment and the sample when the sample weight
difference between two consecutive measurements was less than
0.001 g. The time required for equilibrium between the environ-
ment and samples was about 5 weeks or more depending on RH
and temperature of the samples. Moisture content of the samples
was measured by Karl Fischer titration method before and after
equilibration.
2.2. Crystal separation
performed with indium and distilled water. Following equilibra-
tion, 15e50 mg of equilibrated raisins at 25
C (0.1 < aw < 0.8) were
placed in pierced lid pans (volume 40 mL) and cooled from room
temperature to 80
C. Then samples were scanned from 80
C to
100
C at a rate of 10
C/min. Triplicate samples were used for
thermal transition experiments. Initially selected sample with aw of
0.44 was scanned at 5, 10, 20, 30, 60, 90, 120, 150, and 180
C/min.
Separated raisin crystals and a-D-glucose monohydrate were
placed in 100 mL pierced lid pans, then scanned from 80
C to
200
C at a rate of 5
C/min. An empty pan was used as a reference
in each test.
2.4. Water sorption modeling
Various equations can be fitted to the experimental sorption
data for grapes and dried grapes (Esmaiili et al., 2007). In this
research the BET (Brunauer, Emmett and Teller) (Eq. (1)) and the
GAB (Eq. (2)) models were used to predict the water sorption
behavior of the samples.
Me ¼ Mb Baw =ð1  aw Þ½1 þ ðB  1Þaw  (1)
where Me is the equilibrium moisture content (g water/g dry
product), aw is water activity, Mb is the BET monolayer moisture
content and B is sorption energy constant:


Me ¼ Mg KCaw ð1  Caw Þ½1 þ ðK  1ÞCaw  (2)
where Mg is the GAB monolayer water content (g water/g dry
product), C is a constant related to monolayer heat of sorption and K
is a constant related to multilayer sorption heat.
2.5. Glass transition modeling
GordoneTaylor and linear GordoneTaylor models (Gordon and
Taylor, 1952) were applied to predict Tg as a function of the solid
fraction. Furthermore Khalloufi model (Khalloufi et al., 2000) and a
new empirical equation were tested to predict Tg as a function of aw
(Table 1).where Tgs is glass transition temperature of anhydrous
solids, Tgw is glass transition temperature of amorphous water
(135
C), Xs is mass fraction of total solids (g solids/g product), Xw
is mass fraction of water (g water/g product) and k1, k2, A, B, C, a and
b are the constant of models. Ckh and Aem parameters in Eqs. (5) and
(6), respectively, are equal to Tgs of the samples. All parameters
were estimated by non-linear regression.
Table 1
Models used for fitting the glass transition temperature of sultana raisins.

Expression Model
Crystals were separated physically from sugared raisins. Resid-
ual flesh removed to some extent by means of washings with
Tgs Xs þ k1 Tgw Xw GordoneTaylor
cooled (20
C) absolute ethanol (Venir et al., 2010). The washing Tg ¼ (3)
Xs þ k1 Xw
process was repeated until white crystals were obtained. Ethanol
was removed from crystal mass by evaporation with dry nitrogen  
flow. Xw Tgw  Tg Linear GordoneTaylor
Tg ¼ Tgs þ k2 (4)
ð1  Xw Þ

2.3. Determination of thermal transitions

Akh a2w þ Bkh aw þ Ckh Khalloufi
Tg ¼ (5)
To determine the glass transition temperature, the thermal aa2w þ baw þ 1

transition experiments in equilibrated raisins were conducted with

a differential scanning calorimeter (DSC823e Mettler Toledo Stare Aem þ Bem aw Empirical model
Tg ¼ (6)
System, USA) provided with a system for temperature control using 1 þ Cem aw þ Dem a2w
liquid nitrogen. Heat flow and temperature calibration was
142 M.E. Bazardeh, M. Esmaiili / Journal of Stored Products Research 59 (2014) 140e145

adsorption isotherms of the samples predicted by the BET (A) and

GAB (B) models, together with experimental data. As shown in this
Fig., BET model was fitted with a good confidence to experimental
data from aw 0.1 to 0.45. Over this range, at high water activity
levels, considerable deviation was observed when dissolution
phenomena become more important than sorption. The GAB model
was successfully used to fit sorption data over evaluated range of aw
(0.1e0.9) with R2 > 0.99. Table 2 shows that water contents asso-
ciated to the monolayer calculated using BET equation (Mb) were
lower than those calculated using GAB equation (Mg) for the whole
temperature range considered.

3.2. Thermal transitions of sultana raisins

3.2.1. Effect of scan rate

The results indicated that Tg value varies depending on the
experimental conditions, such as cooling rate and sample size.
Since the heating rate is a significant factor affecting the calori-
metric determination of Tg, nine different heating rates were
employed during DSC test. The effect of scan rates (SR) on Tg values
of raisin samples is presented in Table 3.
According to Table 3, Tg values increased linearly with increasing
the heating rate (Tgo ¼ 0.4323 SR-33.71). The linear regression co-
efficient is 0.99. Proper selection of conditions is very critical in
determination of Tg and the implementation conditions should
always be reported with Tg values.

3.2.2. Effect of water content

Table 4 shows the onset and mid-point temperatures of the
glass transition for the analyzed samples, which occurred over a
temperature range of 80e100
C. DSC data were obtained in raisin
samples presumably without freezable water content. Within wa-
Fig. 1. Comparison of experimental (Exp.) and predicted (Pre.) adsorption data of ter activities range of 0.1e0.7, thermograms exhibited only one
sultana raisins by BET (A, fitted till aw z 0.45) and GAB (B, fitted till aw z 0.9) models transition and no formation of ice and no ice melting endotherm. Tg
at 15, 25, 35
C.
values were found to decrease with increased moisture content. In
present study, we consider Tgm as the characteristic of the glass
Evaluation of predictions from models with experimental data transition. Thus dependence of the Tgm on water activity (aw) can be
was carried out using determination coefficient (R2) and the mean shown by Tg ¼ 95.95 aw þ 16.04 (R2 ¼ 0.933).
relative percentage deviation (P value) was assessed: The GordoneTaylor and linear GordoneTaylor models (Eqs. (3)
  and (4)) were used to fit the experimental TgeXw data, and Khal-
N 
100 X YExp  YPre  loufi and empirical models (Eqs. (5) and (6)) were used to predict
P% ¼ (7)
N i¼1 YExp the Tg of raisins as a function of aw. All of the applied equations were
fitted with a very close agreement between experimental and
where YExp and YPre are the experimental and predicted values predicted values (Fig. 2 A, B, Table 5) nevertheless the estimated Tgs
respectively and N is the number of experimental data. A model is values were significantly different between applied models
considered acceptable if the P values were below 10% (Chirife and (Table 5). Due to these differences among the predicted data, use of
Iglesias, 1978). All analyses were performed using Statistica soft- the experimental values of Tgs is suggested. The value of k1
ware, release 7, StatSoft, Inc., USA. parameter was given as 4.23. A series of k2 values was estimated
using linear GordoneTaylor relevant to each aw (k2 average ¼ 2.45).
3. Results
3.2.3. Raisin crystals
3.1. Sorption isotherm DSC scan of raisin crystals shows two melting peaks at
approximately 73 and 146
C (Fig. 3A). Existent base line deviation
The water adsorption behavior of sultana raisins was modeled in DSC thermogram of raisin crystals can be related to residual
using BET (Eq. (1)) and GAB (Eq. (2)) models. Fig. 1 shows the impurities in the separated crystals. DSC test performed on glucose

Table 2
Model parameters of adsorption isotherms of sultana raisins at 15, 25 and 35
C.

Temperature (
C) GAB parameters BET parameters

K C Mg R2 P% B Mb R2 P%

35 1.034 10.78 0.076 0.990 3.32 11.18 0.075 0.999 0.94

25 0.986 17.98 0.082 0.999 1.85 20.85 0.079 0.993 1.86
15 0.898 18.78 0.098 0.993 1.90 27.34 0.088 0.997 1.34
 M.E. Bazardeh, M. Esmaiili / Journal of Stored Products Research 59 (2014) 140e145 143

Table 3
Experimental onset and midpoint Tg data of sultana raisins at selected scan rates.
(Samples equilibrated at aw z 0.536).

Scan rate (
C/min) Tg onset (
C) Tg midpoint (
C)

5 35.51 32.33
10 32.28 28.38
20 24.15 20.01
30 19.00 14.81
60 4.27 0.27
90 8.47 17.76
120 19.38 29.36
150 30.80 39.11
180 40.65 50.31

monohydrate also gave two endothermic peaks at about the same

temperatures (Fig. 3B), indicating that raisin crystals may be
composed of glucose monohydrate. In this study, water content of
separated raisin crystals was 0.1 (dry base).

3.3. Comparison of raisins stability criteria based on the concepts of

water activity and glass transition

Figure 4 shows the interrelationship of Tg-Me-aw, were exam-

ined for raisins. The sorption isotherm predicts that sultana raisins
are stable at GAB monolayer water content (Mg) of 0.082 g water/g
dry product at 25
C (point C in Fig. 4). However at an equivalent
water content, the Tg value from the glass line was 4
C (point E)
and Caw was 0.22 (point D). Interpretation of state diagram con-
cludes samples with 0.025 g water/g dry product are stable at
25
C or below (point B). According to this criterion Caw is 0.02
which is lower than nominated one by sorption isotherm Fig. 2. Comparison between experimental and predicted data of Tg for sultana raisins;
(Caw ¼ 0.22, point D). A: Tg vs equilibrium moisture content (Me) and B: Tg vs aw.

4. Discussion 25 and 35
C are given in Table 2. As shown in Table 2, water

The characteristics of sorption isotherms of fresh and dried
grapes are affected by the influence of amount and form (amor-
phous and crystalline) of sugars, moisture content and physico-
chemical pretreatments (Esmaiili et al., 2007). As shown in Fig. 1,
sultana raisins presented the typical behavior of products with high
sugar content: a slow increase in the equilibrium moisture content
at the low aw ranges and a sharp increase at intermediate aw values.
A comparison between adsorption isotherms at different temper-
ature showed that water adsorption decreased when increasing the
temperature until aw ¼ 0.65. From this value up, the crossing-over
phenomenon is observed and the equilibrium moisture content
increased with increasing temperature from 15 to 35
C. Such
inversion is related to increasing in the number of adsorption sites
and leaching of sugars at high water contents and temperatures.
These results corroborate the findings of a great deal of the previ-
ous works in this field (Saravacos et al., 1986; Tsami et al., 1990).
Model parameters of adsorption isotherms of sultana raisins at 15,
Table 4
Glass transition temperatures (onset, Tgo, mid, Tgm), average value, of sultana raisins
influenced by water content (scan rate 10
C/min).
contents associated to the monolayer calculated using BET equation
(Mb) are lower than those calculated using GAB equation (Mg) for
the whole temperature range considered, which is in agreement
with results observed by several authors and summarized by
Timmermann et al. (2001). For dried foods the concept of mono-
layer water content is considered to be critical limit when the rate
of deteriorative reactions during preservation starts increasing
significantly. The GAB monolayer and the C value decrease with
increasing temperature while the K parameter of this model in-
crease slightly. The K values of the samples presented small varia-
tions, all near 0.9 to 1.
From investigation of thermal transitions of sultana raisins it
was concluded that Tg values reduced with increasing aw. The
relationship between Tg and aw is linear at intermediate moisture
contents. However, the true relationship is sigmoid in the whole
range of water activity. Direct plasticizing effect of increased
moisture content leads to increased segmental mobility of chains in
amorphous region of glassy and partially crystalline systems. The
plasticizing effect of water, inducing depression of the Tg down to a
temperature lower than storage temperature, is redound to sugar
crystallization in amorphous products (Roos and Karel, 1991).

Xs (g solids/g product) Xw (g water/g product) Tgo (
C) Tgm (
C) Table 5

0.94 0.059 4.97 3.39 Predicted Tgs (
C) by four mathematical models for sultana raisins.
0.92 0.082 9.68 4.28
Model Tgs P% R2
0.90 0.097 16.50 11.59
0.88 0.012 27.45 23.23 GordoneTaylor 40.00 1.30 0.970
0.86 0.014 32.89 28.70 Linear GordoneTaylor 14.16 1.04 0.982
0.82 0.018 50.99 46.91 Khalloufi 2.30 0.28 0.997
0.76 0.024 69.68 65.03 Empirical 1.18 0.46 0.994
144 M.E. Bazardeh, M. Esmaiili / Journal of Stored Products Research 59 (2014) 140e145
Fig. 3. DSC thermograms of separated raisin crystals (A) and glucose monohydrate
crystals (B) scanned in pierced lid pans (SR ¼ 5
C/min).
DSC scanning of extracted crystals from raisins indicated that
crystals should be mainly composed by glucose monohydrate.
Glucose monohydrate is composed by 1:1 molecules of glucose and
water (Venir et al., 2010). Glucose and fructose in raisin are present
in about equal concentrations (Zhao and Hall, 2008) but the lower
solubility enables glucose to be the crystallizing sugar. Glucose may
crystallize as a-D-glucose monohydrate with the stable crystalline
form below 50
C and anhydrous form, stable above 80
C (Young,
1957).
State diagram was depicted in present study to identifying rai-
sins stability during storage as well as to select a suitable condition
of temperature and moisture content for processing. It can also
Fig. 4. State diagram indicating variation of glass transition temperature (Tgm); GeT
(GordoneTaylor); Caw: critical water activity; Cwc: critical water content; Mg: GAB
monolayer water content.
assist in understanding the complex changes when product's water
content and temperature are changed. State diagram is the map of
different states of a food as a function of water or solids content and
temperature (Rahman, 2006). Based on modified state diagram
(which is constructed by GordoneTaylor and GAB models) foods
can be defined as having a critical water activity (Caw), where Tg falls
below ambient or storage temperature, and critical water content
(Cwc) which corresponds to Caw (Roos, 1995). Recently this proce-
dure has been followed by some researchers for determining sta-
bility of selected foods (Moraga et al., 2011; Rahman, 2012; Sablani
et al., 2004). The findings in this study are consistent with other
studies which pointed that the glass transition concept un-
derestimates the stability temperature for dried fruits containing
large concentration of sugars (Roos, 1993; Sablani et al., 2007).
5. Conclusion
In this study, to investigate the optimum storage condition for
prevention of sugaring phenomenon, temperature dependence of
sorption isotherms, glass transition models and the interrelation-
ship of Tg-Me-aw were examined for sultana raisins. The results
regard the effect of water content and scan rate on Tg. The findings
of the present study show that the Tg of raisins decreased linearly
from 3
C to 65
C as the water content increased from 0.06 to
0.32 g water/g dry product and also Tg increased linearly
from 32
C to 50
C as the scan rate increased from 5 to 180
C/
min. The sorption isotherm predicts that sultana raisins are stable
at GAB monolayer water content (Mg) of 0.082 g water/g dry
product at 25
C. DSC scanning indicated that extracted crystals
from raisins should be mainly composed by glucose monohydrate.
Sorption isotherm and glass transition line has been combined to
predict stability of raisins (assumed preserving from sugaring). It
sounds that further work is required on the relationships between
glass transition, water activity and raisins stability, with more focus
on experimental measurement of sugaring in raisins around Tg.
Acknowledgment
Valuable comments provided by the reviewer are gratefully
acknowledged. The authors gratefully thank also Dr. Ali Hassanza-
deh (Nanotechnology Lab. of Urmia University) for his valuable
comments and appreciate University of Urmia to provide the
financial support.
Nomenclature
AKh,BKh,CKh,a,b Khalloufi Eq. constants
Aem,Bem,Cem,Dem empirical Eq. constants
aw water activity
B constant related to net heat of sorption in BET Eq.
C constant related to first layer heat of sorption in GAB Eq.
Caw critical water activity
Cwc critical water content
DSC differential scanning calorimetry
Eq. Equation
Exp experimental data
GeT GordoneTaylor model
K constant related to heat of sorption of multilayer in GAB
Eq.
k1 empirical constant in GordoneTaylor Eq.
k2 empirical constant in linear GordoneTaylor Eq.
Me equilibrium moisture content (g water/g dry product)
Mb monolayer moisture content in BET Eq. (g water/g dry
product)
 M.E. Bazardeh, M. Esmaiili / Journal of Stored Products Research 59 (2014) 140e145
Mg monolayer moisture content in GAB Eq. (g water/g dry
product)
N number of experimental data
P% mean relative percentage deviation
Pre predicted value
RH relative humidity
SR scan rate (
C/min)
Tg glass transition temperature (
C)
Tgw glass transition temperature of amorphous water (
C)
Tgs glass transition temperature of anhydrous solids (
C)
Tgo onset point of glass transition temperature (
C)
Tgm midpoint of glass transition temperature (
C)
Xw mass fraction of water (g water/g product)
Xs mass fraction of soluble solids in the product (g solids/g
product)
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