Journal of Food Engineering 69 (2005) 453–459

www.elsevier.com/locate/jfoodeng

Thermal characterization and phase behavior of cornstarch

studied by differential scanning calorimetry q
Zhikai Zhong, X. Susan Sun *

Department of Grain Science and Industry, Kansas State University, Manhattan, KS 66506, United States

Received 30 November 2002; received in revised form 18 March 2004; accepted 14 July 2004

Abstract

A cornstarch–water system was characterized by differential scanning calorimetry (DSC). Glass transition and melting transitions
of starch crystals and amylose–lipid complexes were observed in native cornstarch with moisture content (MC) between 11.9% and
24%. At medium to high MC levels, the glass transition was not detectable, but melting of ice and gelatinization of starch (G endo-
therm) were observed. The gelatinized cornstarch was completely amorphous and retrogradation was not observed under the exper-
imental conditions. As expected, phase behavior and thermal properties of cornstarch–water system were significantly dependent on
water content, composition, and gelatinization. The gelatinized cornstarch had higher glass transition temperature than the native
cornstarch. Nonfreezing water of starch increased as MC increased and leveled off at 29.5% MC. The gelatinized cornstarch had less
nonfreezing water at low MC and had more nonfreezing water at high MC compared to the native cornstarch. Water in the system
was thought to exist in three forms: bound water, loosely bound water, and free water, all of which were MC dependent. State dia-
grams for the native and gelatinized cornstarch were configured out of the data obtained in this study.
Ó 2004 Elsevier Ltd. All rights reserved.

Keywords: Cornstarch; Nonfreezing water; Thermal properties; Phase behavior; State diagram

1. Introduction and phase transition of starch (Roos, 1995). Endother-

Thermal properties are important in starch and have
been a primary area of starch research for many years
(Roos, 1995; Whistler, BeMiller, & Paschall, 1984).
Study of thermal properties can provide guides for
processing and utilization of starch and also informa-
tion for exploring and understanding the structure of
starch. Differential scanning calorimetry (DSC) is a
powerful tool used to investigate thermal properties
q
Contribution 03-161-J from the Kansas Agricultural Experiment
Station, Manhattan, KS 66506, United States.
*
Corresponding author. Tel.: +1 785 532 4077; fax: +1 785 532
7010.
E-mail address: xss@wheat.ksu.edu (X.S. Sun).
mal and exothermal changes in a DSC thermograph re-
veal transitions or reactions occurring during DSC
testing, such as glass transition, gelatinization, and melt-
ing. DSC thus can directly provide the temperature and
enthalpy of transition/reaction, as well as capacities.
Analysis of DSC data can provide additional informa-
tion about starch, such as its structure and composition,
its interaction with other components, the effects of
water, and related properties.
The most frequent use of DSC with starch is to
investigate its gelatinization behavior. Usually, starch
has been mixed with water in a 1:3 ratio and then
subjected to DSC testing. These types of DSC thermo-
graphs exhibit only one gelatinization peak at 50–
80 °C. Studies on wheat, potato, and rice starches with
reduced water content showed two transition peaks,
i.e. gelatinization transition (G endotherm) and melting

0260-8774/$ - see front matter Ó 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2004.07.023
454 Z. Zhong, X.S. Sun / Journal of Food Engineering 69 (2005) 453–459
of starch crystals (M1 endotherm), related to starch
crystallites at intermediate water content and only
one peak at both low and high water contents (Burt
& Russell, 1983; Chungcharoen & Lund, 1987; Dono-
van, 1979; Donovan & Mapes, 1980; Eliasson, 1980).
Another study showed second peak at high tempera-
ture for some starches, which was attributed to the
melting transition of amylose–lipid complex (Kugi-
miya, Donovan, & Wong, 1980). Studies on the glass
transition of starches reported difficulty in determining
the glass transition with high MC starch because of an
overlap with gelatinization or ice melting transition
(Biliaderis, Page, Maurice, & Juliano, 1986; Slade &
Levine, 1988).
Water is a primary plasticizer used in processing and
manufacturing starch and its products and greatly af-
fects various properties of starch. In a starch–water sys-
tem, some water interacts directly or indirectly with
starch and has detectable property differences from bulk
phase water. The water that remains unfrozen even at
subfreezing temperature is called ‘‘nonfreezing water’’
or ‘‘bound water’’. Determination of nonfreezing water
is the most simple and straightforward way to estimate
hydration and nonfreezing water can provide important
information on structure and functional properties of
starch (French, 1984). Information on nonfreezing
water also can be used in establishing proper processing
and storage conditions for dehydrated and frozen foods
(Roos, 1995).
Although lots of works have been done to starch sys-
tem, knowledge about starch is far away from complete,
such as water status, interactions between water and
starch, glass transition of starch at high water content,
and phase behavior between the native and gelatinized
starches. The objectives of this work were to systemati-
cally investigate the thermal behavior of cornstarch at
various hydration levels and large temperature scan
ranges, to determine the amount of nonfreezing water
and water status as affected by starch gelatinization
and water content, and to measure and predict glass
transition temperature. The data obtained from this
study can be used to generate a state diagram for a sys-
tem containing native or gelatinized starch alone or as a
major component. The diagram could be useful refer-
ence in predicting phase behavior and properties of the
starch-containing system and selecting processing/stor-
age conditions.
2. Materials and methods
2.1. Materials
Food grade Silver Medal Pearl cornstarch 2000 was
obtained from Cargill Foods (Cedar Rapids, IA). It
was made from common dent corn and contained be-
tween 26–31 wt% amylose, 69–74 wt% amylopectin,
and 0.3% lipid based on dry weight. Moisture content
(MC) of the starch was 11.9 wt% as measured by an
air-oven method (AACC, 2000).
2.2. Sample preparation
The cornstarch was used as received. Low MC
(<30 wt%) samples were obtained by exposing the as-
received cornstarch in a desiccator with 95% relative
humidity atmosphere for various times. Other samples
were obtained by mixing the as-received cornstarch with
appropriate amounts of distilled water. All samples ob-
tained were then sealed and stored in a refrigerator for
one week to reach equilibrium. The actual MC of these
samples was determined by an air-oven method (AACC,
2000).
2.3. DSC measurement
A DSC (differential scanning calorimeter) (Pyris-1
Perkin-Elmer, Norwalk, CT) was used for calorimetric
measurements. The instrument was calibrated with in-
dium and zinc standards before sample measurements,
and all measurements were conducted under a nitrogen
atmosphere. All samples first were quenched to
70 °C
and held at that temperature for 1 min. Then the sam-
ples were scanned at 10 °C/min to 220 °C, quenched
again to
70 °C and held there for 1 min, and finally re-
heated at 10 °C/min. The temperature at the midpoint of
the change in slope of the DSC heat-capacity change
was taken as the glass transition temperature (Tg). The
temperature at the maximum value of the corresponding
endothermic peak was taken as either the gelatinization
temperature or melting temperature of amylose–lipid
complexes. The melting-point temperature of frozen
water of each sample was the temperature at the maxi-
mum value of the endothermic transition in the vicinity
of 0 °C. Enthalpies of the gelatinization, of the melting
of amylose–lipid complexes, and of the frozen water fu-
sion were calculated from the areas encompassed by the
baseline and thermogram of the corresponding transi-
tion, respectively.
Nonfreezing water was determined using the DSC
data following the method described by Ross (1978)
and Zhong and Sun (2000). The same calorimetric meas-
urements were carried out for pure water. The melting
enthalpy of pure water was obtained and used as the ref-
erence enthalpy.
All samples were duplicated and the reported values
are the average of the two DSC measurements. The
length of error bar reported in Figs. 4–6 presented the
difference between the maximum and minimum value
of obtained data.
 Z. Zhong, X.S. Sun / Journal of Food Engineering 69 (2005) 453–459 455

3. Results

The first DSC scan of cornstarch with 11.9% MC pre-

sented a glass transition, located at 60 °C, and two endo-
thermic peaks, located at 182 °C and 195 °C,
respectively (Fig. 1). The peak at 182 °C was due to
the melting of cornstarch crystals, and the one at
195 °C was due to melting of the amylose–lipid com-
plexes. The second DSC scan of the same cornstarch
had a glass transition occurring at a much higher tem-
G
perature (100 °C) compared to the one in the first
F
DSC scan (Fig. 1). No endothermic transition beyond
the glass transition was observed from the second scan, E
indicating that no re-crystallization of cornstarch mole-

Endo
cules (retrogradation) occurred during cooling in the D

DSC measurement. However, there was a small endo-

C
thermic peak at about 0 °C in the second scan (Fig. 1).
This peak was attributed to ice melting. B
The first scan and second scan of DSC thermographs
of other samples with different MC are presented in A

Figs. 2 and 3, respectively. As MC increased, all glass

-50 0 50 100 150 200
transition, melting of starch crystals, and melting of
o
amylose–lipid complexes shifted toward lower tempera- Temperature ( C)
tures (Fig. 2). Two new endothermic peaks appeared at Fig. 2. The first scan DSC thermograms of the cornstarch with
medium to high MC levels: one located at about 71 °C, moisture content: (A) 18.5%, (B) 24.0%, (C) 29.5%, (D) 39.3%, (E)
the other at about 0 °C. The peak at 71 °C was attrib- 49.1%, (F) 59.5%, and (G) 75.9%. Arrows indicated location of peaks
uted to gelatinization of cornstarch, while the peak at related to starch or amylose–lipid complexes.
0 °C was attributed to the ice melting. As MC further in-
creased, the ice melting and starch gelatinization peaks

G
B
F

E
Endo
Endo

C
A
B

-50 0 50 100 150 200

-50 0 50 100 150 200
Temperature (oC)
Temperature (oC)
Fig. 3. The second scan DSC thermograms of the cornstarch with
Fig. 1. DSC thermograms of the cornstarch with 11.9% MC: (A) the moisture content: (A) 18.5%, (B) 24.0%, (C) 29.5%, (D) 39.3%, (E)
first scan and (B) the second scan. 49.1%, (F) 59.5%, and (G) 75.9%.
456 Z. Zhong, X.S. Sun / Journal of Food Engineering 69 (2005) 453–459

remained at the same temperature range and became 160

more significant. However, the melting peak of starch
crystals continued to shift toward lower temperature 140

and merged with the gelatinization peak finally at about 120

60% MC. The melting peak of the amylose–lipid com-
plex also shifted toward lower temperature (Fig. 2). 100
As to the second DSC scan, glass transition shifted
toward lower temperature as MC increased and was 80

Temperature ( C)
no longer observable as MC was about 30% (Fig. 3).

o
60
No endothermic peak related to starch was observed
for all MC levels. The ice melting peak remained at 40
about 0 °C and became larger and larger as MC in-
20 A
creased. An exothermic peak appeared at subfreezing
temperature as MC was 30% or above (Fig. 3). This exo-
0
thermic peak could be attributed to crystallization of
water in the sample during the second DSC scan. Tran- -20
sition temperatures from the first and second scans are
summarized in Figs. 4 and 5 against water content. -40
From the enthalpy of ice melting, nonfreezing water
-60
was calculated and plotted against water content in 0 10 20 30 40 50 60 70 80
Fig. 6. Error bars associated with data were also re- Water content (wt%)
ported in the Figs. 4–6 to indicate if the data were signif-
Fig. 5. Thermal properties of the gelatinized cornstarch against
icantly different. The nonfreezing water content moisture content: the crystallization temperature of water (m), the
increased substantially between MCs of 11.9% and melting temperature of ice (d), the experimental glass transition
24%, with the amount more than doubling over that temperature (j), and the calculated glass transition temperature (h).
range (Fig. 6; Table 1). However, as MC continued to Point A: 23 °C and 50% MC.

0.50
200

180 0.45

160
Nonfreezing water (g water/g starch)

0.40
140

0.35
120
Temperature ( C)
o

100 0.30

80 B
0.25
60

40 0.20

20 A
0.15
0

0.10
-20 0 10 20 30 40 50 60 70 80
0 10 20 30 40 50 60 70 80
Water content (wt%)
Water content (wt%)

Fig. 4. Thermal properties of the native cornstarch against moisture
content: the melting temperature of ice (d), the glass transition
temperature (j), the gelatinization (G endotherm) temperature of
cornstarch (n), the melting (M1 endotherm) temperature of cornstarch
(m), and the melting (M2 endotherm) temperature of the amylose–lipid
complex (.). Point A: 23 °C and 15% MC; Point B: 80 °C and 50%
MC.
Fig. 6. Nonfreezing water of the native and the gelatinized cornstarch
against moisture content: the native cornstarch (d) and the gelatinized
cornstarch (s).
increase, the amount of nonfreezing water leveled off,
remaining near 0.4 g water/g dry starch (Fig. 6).
 Z. Zhong, X.S. Sun / Journal of Food Engineering 69 (2005) 453–459
Table 1
Calculated glass transition temperature (Tg) for the gelatinized cornstarch based on the Gordon–Taylor equation
Overall water content (%) Nonfreezing water (g water/g dry starch)
11.9 0.1345 ± 0.001
18.5 0.225 ± 0.002
24.0 0.291 ± 0.002
29.5 0.380 ± 0.020
39.3 0.389 ± 0.026
49.1 0.405 ± 0.013
59.5 0.386 ± 0.004
75.9 0.397 ± 0.017
a
Experimental data from this work.
4. Discussion
When heated and cooled in the presence of water,
starch undergoes a series of thermal transitions; the
associated thermal properties also change with the in-
crease in temperature. Thermal transitions include crys-
tallization of water, melting of ice, glass transition of
starch, gelatinization transition of starch (G endo-
therm), melting of starch crystals (M1 endotherm),
and melting of the amylose–lipid complexes (M2 endo-
therm). Usually several, but sometimes only one, of
these transitions occur for a given sample, and occur-
rence depends on starch composition, MC, and thermal
history. Also, these thermal transitions occur in a certain
order.
At low moisture content (11.9% and 18.5%), all water
molecules were absorbed and bounded with starch mol-
ecules in amorphous phase. Thus no free water was
available to form ice and no ice melting was observed
(Figs. 1A and 2A). Because of the lack of available
water, starch granules could not swell and no G endo-
therm was observed; therefore, the melting peak oc-
curred at an elevated temperature (M1 endotherm)
(Figs. 1A and 2A). As MC increased to 24.0%, extra
water became available for ice forming during DSC
cooling (Fig. 2B). With a further increase in MC, water
was sufficient for starch granules to swell, leading to a
partial loss of crystallinity as proposed by Donovan
(1979) and Jenkins and Donald (1998). This was the
physical initiation of G endotherm as shown in Fig.
2C. Then, the remaining starch crystals melted at a high-
er temperature and appeared as M1 endotherm on the
DSC curve (Fig. 2C). As MC continued to increase,
more water molecules were free (not bound or loosely
bound to starch) to crystallize. A greater number of
starch granules also swelled and more starch crystals
were destroyed (Fig. 2D and E). At high MC, granules
swelled fully at G endotherm and all cornstarch crystals
were destroyed during the swelling. Therefore, no M1
endotherm was detected (Fig. 2F and G).
Water acts as a plasticizer in the starch–water system
by depressing the glass transition temperature (Maurice,
Slade, Sirett, & Page, 1985). Therefore, Tg of cornstarch
decreased as MC increased (Fig. 4). The glass transition
457
Nonfreezing water (%) Tg (°C)
11.86 ± 0.03 98.3 ± 1.8a
18.4 ± 0.1 47.5 ± 4.6a
22.5 ± 0.1 19.1 ± 3.8a
27.5 ± 0.7
4.6 ± 3.3
28.0 ± 1.0
6.6 ± 4.2
28.8 ± 0.5
10.2 ± 1.9
27.9 ± 0.2
5.9 ± 0.7
28.4 ± 0.9
8.4 ± 3.8
for the cornstarch with 29.5% MC or more (Fig. 2C) was
not detectable because the Tg was below room tempera-
ture and the transition was overlapped with the ice melt-
ing transition on the DSC curve. Zeleznak and Hoseney
(1987) have reported that Tg of wheat starch occurred
below room temperature at moisture levels greater than
22%. Levine and Slade (1990) used Tg of
5 °C for
starch with 28% MC to propose their starch state dia-
gram. The plasticization effect of water also depressed
melting temperatures of starch crystals and amylose–
lipid complexes (Figs. 2 and 4).
After the cornstarch–water system was heated to a
higher temperature and then cooled, a totally different
thermal behavior was observed upon re-heating (Figs.
1B and 3). First, the melted endotherms of cornstarch
crystals and amylose–lipid complexes were not observed
on the second DSC scan, meaning that the melting of
the crystals and complexes were not reversible within
such a short time. Recovery of the crystals and com-
plexes might need a longer time, such as retrogradation.
Second, an ice melting endothermic transition was ob-
served for the starch with low MC (Figs. 1 and 3). Keep-
ing in mind that the MC of 11.9% was far lower than the
water content (about 30%) required for fully hydrating
starch, the appearance of free water after the first scan
seemed unusual. One possible reason was melting of
the amylose–lipid complexes, which would release free
lipid molecules to the system. Because of incompatibility
between lipid and water, some water molecules may
have been repelled, causing their crystallizing and then
melting. Third, there appeared to be water at medium
to high MC levels, that was neither bound water nor free
water, as shown by the exothermic DSC peak (Fig. 3).
These water molecules were relatively loosely bound to
starch molecules and they could not crystallize as did
the totally free water during fast cooling (quenching) be-
cause of the restriction of the starch molecules, low
mobility, and short time scale. However, they could
crystallize when they were heated again to temperatures
higher than
50 °C (Fig. 3C–G). The heating at 10 °C/
min gave the loosely bound water molecules more
mobility and more time to crystallize. Finally, the glass
transition of cornstarch occurred at a much higher tem-
perature compared to that observed in the first scan
458 Z. Zhong, X.S. Sun / Journal of Food Engineering 69 (2005) 453–459
(Figs. 4 and 5). The higher Tg in the second scan could
be attributed to lower water content in the amorphous
water–starch–lipid phase. At the same overall MC, the
gelatinized cornstarch amorphous phase should have
lower water content than that in the native amorphous
starch phase. Clearly, the cornstarch–water system had
different Tg before and after starch gelatinization. There-
fore, it was not appropriate for Zeleznak and Hoseney
(1987) to use the temperature from the second DSC scan
as Tg for native wheat starch.
The total water in the system (WT ) is the sum of free
water (WF), loosely bound water (WLB), and bound
water (WB):
W T ¼ W F þ W LB þ W B ð1Þ
The free water has the same properties as the bulk phase
water. The loosely bound water has similar properties as
the free water and can also crystallize. However, the
loosely bound water interacts with cornstarch mole-
cules; as a result the water crystallizes at more restricted
conditions. The bound water has strong interaction with
cornstarch molecules and cannot crystallize to ice. It is
therefore also called ‘‘nonfreezing water’’. Because both
the free water and loosely bound water can freeze under
the experimental conditions, and then melt at about
0 °C, subtracting these two parts of water from the total
water should equal the nonfreezing water. The nonfreez-
ing water increased as MC increased in the system and
then leveled off at 30% MC because at this point, suffi-
cient water was available to cornstarch (Fig. 6). The
nonfreezing water at high MC for the native cornstarch
and the gelatinized cornstarch was 0.32 and 0.39 g wa-
ter/g dry starch, respectively (Fig. 6). Wootton and
Bamunuarachchi (1978) reported 0.30 and 0.32 g wa-
ter/g dry starch for native maize and waxy maize,
respectively, and 0.33 and 0.35–0.42 g water/g dry starch
for the native and pregelatinized wheat starch, respec-
tively. The greater amount of nonfreezing water for
the gelatinized starch was attributed to the gelatiniza-
tion, which results in disruption of the weak associative
bonds in the amorphous region of the granule, enabling
increased hydration of starch molecules and exposure of
more starch molecules to water (Wootton & Bamunu-
arachchi, 1978). In our study, at lower MC, the value
of nonfreezing water of molten cornstarch was smaller
than that of native cornstarch, which has not been re-
ported in the literature. As discussed before, the released
lipid molecules after melting of the amylose–lipid com-
plexes might repel some bond water from cornstarch,
which may reduce the level of nonfreezing water at low-
er MC, but would not have any significant effect on non-
freezing water at higher MC due to abundance of water
and corrupted starch granules. In addition, no gelatini-
zation occurred at low MC. All these may reduce the
nonfreezing water amount for molten starches at low
MC.
As the amount of nonfreezing water levels at high
MC, the Tg of the water–starch also should level off.
The Tg of gelatinized cornstarch could be calculated
from the Gordon–Taylor equation (Gordon & Taylor,
1952):
W 1 T g1 þ kW 2 T g2
Tg ¼ ð2Þ
W 1 þ kW 2
where Tg, Tg1, and Tg2 are glass transition temperatures
of the starch–water amorphous phase, pure water, and
pure starch, respectively; W is the weight fraction and
k is a constant. Taking Tg1 =
135 °C for pure water,
we fitted the experimental Tg data (MC = 11.9%,
18.5%, and 24.0%) using Eq. (2) and obtained
k = 0.176 and Tg2 = 277.8 °C with R2 = 0.9999. By using
the obtained k and Tg2, we calculated glass transition
temperature for the gelatinized starch–water system
based on the amount of nonfreezing water (Table 1;
Fig. 5). The Tg for gelatinized cornstarch at MC of
29.5% or above ranged from
5 to
10 °C, which was
close to the
5 °C proposed by Slade and Levine
(1988) for their gelatinized starch.
It was inappropriate to use Eq. (2) for native corn-
starch because the Gordon–Taylor equation could only
be applied to an amorphous system. The native starch
has starch crystalline and amylose–lipid complexes,
which might act as physical cross-linking. Furthermore,
percentage of amorphous phase in native starch and
accurate water content in the amorphous phase were
unavailable. The actual water content in the amorphous
starch–water phase should be higher than that calcu-
lated from the nonfreezing water content. All of these
excluded the application of the Gordon–Taylor equa-
tion in native starch system.
As discussed above, the cornstarch–water system had
different phase behavior before and after starch gelatini-
zation. The phase behavior also depended on MC level
and small ingredients (such as lipid). Figs. 4 and 5 could
be used as state diagrams for the native and the gelati-
nized cornstarch–water system, respectively, showing
the physical state of the system at different temperatures
and compositions. For example, at room temperature
(23 °C), there existed a glassy starch–water mixture,
starch crystals, and amylose–lipid complexes in the na-
tive cornstarch–water system with 15% MC (Fig. 4,
Point A). At 80 °C and 50% MC, there existed free
water, rubbery partially gelatinized cornstarch–water
mixture, starch crystals, and amylose–lipid complexes
in the starch/water system (Fig. 4, Point B). At room
temperature, there existed free water, loosely bound
water, and rubbery starch–water–lipid mixture in the
gelatinized starch/water system with 50% MC (Fig. 5,
Point A). The state diagrams can be used in selecting
processing and storage conditions of starch as a major
component of a product.
 Z. Zhong, X.S. Sun / Journal of Food Engineering 69 (2005) 453–459
5. Conclusions
Phase behavior and thermal properties of cornstarch–
water were dependent on water content, composition,
and gelatinization. The gelatinized cornstarch had high-
er Tg than the native cornstarch at the same overall MC.
The nonfreezing water content increased as MCs in-
creased and equilibrated at high MCs. The gelatinized
cornstarch had higher equilibratory nonfreezing water
than the native starch. At low MC levels, some water
was repelled out of the starch after heating, and the mol-
ten cornstarch had a lower amount of nonfreezing water
than the native cornstarch. The gelatinized cornstarch
was amorphous; while in the native cornstarch there ex-
isted amorphous starch, crystalline starch, and amylose–
lipid complexes. Water in the system existed as bound
water, loosely bound water, and free water, the amounts
of which depended on MC level.
Acknowledgements
The authors greatly appreciated Dr. Paul Seib for his
valuable comments. The authors also are grateful to
Cargill Foods (Cedar Rapids, IA) for supplying the
cornstarch.
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