Journal of Cereal Science 49 (2009) 371–377

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Journal of Cereal Science

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Rheological properties of starches with different amylose/amylopectin ratios

Fengwei Xie a, Long Yu a, b, *, Bing Su a, Peng Liu a, Jun Wang a, Hongshen Liu a, b, Ling Chen a
a
Centre for Polymers from Renewable Resources, ERCPSP, School of Light Industry and Food Science, SCUT, Guangzhou, China
b
CSIRO, Materials Science and Engineering, Melbourne, Vic 3168, Australia

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

Article history: The rheological properties of corn starches with different amylose/amylopectin ratios (80/20, 50/50, 23/
Received 2 October 2008 77, and 0/100) were systematically studied by Haake rheometry. The starches were initially pre-com-
Received in revised form pounded with water to designated moisture content levels using a twin-screw extruder. A single-screw
3 January 2009
extruder with a slit capillary die was then used to characterize the shear stress and melt viscosity
Accepted 5 January 2009
characteristics of sample pellets, as a function of both moisture content (19–27%) and extrusion
temperature (110–140  C). The melts exhibited shear thinning behavior under all conditions, with the
Keywords:
power law index (0 < n < 1) increasing with increasing temperature and moisture content in the majority
Starch
Rheometry of cases. The higher the amylose content, the higher is the viscosity (for example, h increases from
Rheological 277 Pa s to 1254 Pa s when amylose content increases from 0% to 80% under a certain condition), which is
Amylose/amylopectin opposite to the sequence of molecular weight; amylopectin-rich starches exhibited increased Newtonian
Extrusion behavior. These rheological behaviors are attributed to the higher gelatinization temperature of amylose-
rich starches, and in particular the multiphase transitions that occur in these starches at higher
temperatures, and the gel-ball structure of gelatinized amylopectin.
Ó 2009 Elsevier Ltd. All rights reserved.

1. Introduction presented examples of viscosity models applied to cooked dough;

Extrusion cooking has been practiced for more than 50 years,
with early developments focused on the preparation of ready-to-
eat cereals (Harper, 1989). Some researchers have investigated the
effects of amylose content in starch or dough on the physical and
functional properties of their extruded products (Guha et al., 2003;
Matthey and Hanna, 1997). Others have analyzed viscoelastic
characterization of different biopolymers and their mixtures with
additives (Bhattacharya and Padmanabhan, 1992; Bhattacharya
et al., 1988; Seethamaju and Bhattacharya, 1994). More recently,
Chanvrier et al. (2007) investigated the effects of starch and protein
on the rheological properties of wheat flour dough during pro-
cessing at low hydration. Different viscosity models have been
proposed to describe the rheological properties of dough based on
the traditional power law function. For example, Jao et al. (1978)
derived a regression model for the die viscosity of soy dough by
considering the effects of temperature, shear rate and moisture
content; Bhattacharya and Hanna (1986, 1987) and Harper (1981)
* Corresponding author. Commonwealth Scientific and Industrial Research
Organization, Materials Science and Engineering, Gate 4, Normanby Rd, Clayton
South, Melbourne, Vic 3168, Australia. Tel.: þ61 3 9545 2777; fax: þ61 3 9544 1128.
E-mail address: long.yu@csiro.au (L. Yu).
and Tomás et al. (1997) derived a regression viscosity model for
extruding rice flour using a stepwise model starting from a power
law equation.
Due to environmental considerations and the shortage of oil,
starches are now attracting increased attention as raw materials in
the production of biodegradable plastics (Arvanitoyannis, 1999;
Signori et al., 2005; Söderqvist Lindblad et al., 2005). In addition,
the water requirements during the thermal processing of these
materials are normally lower than for conventional additives. There
are many reported investigations of the effects of starch type or
amylose/amylopectin ratio on the final properties of starch-based
materials, including:
 Foams (Babin et al., 2007; Chinnaswamy and Hanna, 1988;
Della Valle et al., 1997; Fang and Hanna, 2001a,b; Guan et al.,
2005; Suknark et al., 1997).
 Sheets or films (Fishman et al., 2006; Yu and Christie, 2005; Yu
et al., 2006).
 Lightweight concrete (Glenn et al., 1999).
 Injection-molded products (Funke et al., 1998; de Graaf et al.,
2003).
The melt rheology of starch-based materials has both scientific
and industrial importance, and thus it has been widely

0733-5210/$ – see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jcs.2009.01.002
372 F. Xie et al. / Journal of Cereal Science 49 (2009) 371–377
investigated. For example, Llo et al. (1996) studied the effects of
extrusion conditions on the apparent viscosity of maize grits,
including the effects of melt temperature, shear rate, material
composition, and extrusion processing history. Willett et al. (1997)
reported that waxy corn starch exhibited shear thinning behavior,
becoming more Newtonian as either temperature or moisture
content was increased. González et al. (2006) investigated the
effects of several factors including screw speed, die restriction (l/r)
and moisture content, together with corn endosperm hardness and
rice amylose content, on apparent melt viscosity using a Brabender
single-screw extruder. Recently, Thuwall et al. (2006) studied the
effects of amylose content, moisture content and starch/glycerol
ratio on the apparent viscosity of potato starch. The effects of
amylose content on reactive extrusion have also been studied
(Wing and Willett, 1997).
Corn starches have attracted particular scientific interests,
because different amylose/amylopectin content materials can be
obtained from natural, renewable resources, and they exhibit
multiphase transitions during thermal processing (Chen et al.,
2006, 2007; Liu et al., 2006). Previous studies have shown that
higher amylose-content starches exhibit superior strength and
toughness in the preparation of starch-based materials and in
producing modified starches by reactive extrusion (Cha et al., 2001;
Dean et al., 2007; Guan and Hanna, 2004; Guan and Hanna, 2006;
Miladinov and Hanna, 2000, 2001; Nabar et al., 2006; van Soest and
Borger, 1997; Yu and Christie, 2005; Yu et al., 2006; Zhou and
Hanna, 2004). However the extrusion of high-amylose starches is
more difficult than that of normal starches, partly due to the higher
die pressure and torque requirements due to the higher melting
temperature and viscosity of these starches (Liu et al., 2006;
Shogren, 1992; Shogren and Jasberg, 1994). In this work, the rheo-
logical properties of corn starches with different amylose/amylo-
pectin ratios (80/20, 50/50, 23/77 and 0/100) were systematically
studied as functions of moisture content and extrusion temperature
using a Haake rheometer. The effects of different amylose/amylo-
pectin ratios on the rheological behaviors will be discussed based
on their microstructures and gelatinization behaviors.
2. Experimental work
2.1. Materials
Four commercially available corn starches with different
amylose/amylopectin ratios were used in this experimental work:
 Gelose 80 (G80, 80/20), supplied by Penford (Australia).
 Gelose 50 (G50, 50/50), supplied by Penford (Australia).
 A normal corn starch (NC, 23/77), supplied by Huanglong Food
Industry Co. Ltd (P.R. China).
 A waxy corn starch (WC, 0/100), supplied by Shanxi Jinli
Industry Group Co. Ltd (P.R. China).
An infra-red heating balance (Model DHS-20) was used to
measure the moisture contents of the original starches during
heating to 110  C for 20 min. All formulations were prepared on
a dry weight basis.
2.2. Sample preparation
Starches were firstly premixed with water to achieve designated
moisture contents. A Haake parallel, co-rotating twin-screw
extruder (Rheomex PTW 24/40p, Ø 30) with a rod die (nozzle L/
D ¼ 3, diameter ¼ 3 mm) was used to produce gelatinized starch
pellets at a screw speed of 90 rpm. The extruder heating barrel
comprises 10 sections. The highest temperature used during
compounding was 160  C, and the die temperature was kept at
105  C to avoid foaming. A gravimetric feeder was used to deliver
the materials into the extruder.
The moisture contents in the compounded pellets were
measured after heating the samples overnight at 130  C in
a vacuum oven.
2.3. Rheological measurements
Compounded pellets were used to study the rheological prop-
erties of various samples. A Haake Rheocord Polylab RC500p
incorporating a single-screw extruder (Rheomex 252p, Ø 19, screw
2:1, L/D 25) with a slit capillary die (20  1 mm) was used to
measure the shear stress and apparent viscosity of samples under
different shear rates at specific temperatures. The screw speed was
varied between 30 and 180 min1, and normally six points were
recorded for each sample using the cutting and manual entry
measurement mode.
Apparent shear rates were calculated by:
6Q
g¼ (1)
WH 2
where g is the shear rate, Q is the volumetric flow rate (in cm3/s), W
is the slit width, and H is the slit height. Shear stress values were
calculated using the following equation:
H$DP
s¼ (2)
2L
in which s is the shear stress, DP is the pressure drop over the
capillary, and L is the slit length.
2.4. Differential scanning calorimetry
A Perkin–Elmer Diamond-I differential scanning calorimeter
(DSC) with an internal coolant (Intercooler 1P), nitrogen purge gas,
and stainless steel sample pans, was used to study the thermal
properties of samples with high moisture content over a high
temperature range (up to 350  C). The melting point and enthalpy
of indium were used for temperature and heat capacity calibrations,
respectively. The detailed methodology and a discussion of some
critical issues are presented elsewhere (Liu et al., 2006; Yu and
Christie, 2001).
3. Results and discussions
3.1. Effects of moisture content
Fig. 1 shows the results for shear stress and melt viscosity as
a function of shear rate for the various corn starches (G80, G50, NC,
and WC) with different moisture contents at an extrusion
temperature of 130  C. It can be seen that, for all moisture contents,
the apparent viscosity decreased with increasing shear rate, and
that, in general, it also decreased with increasing moisture content
in the range studied (19–27%). Similar patterns have been observed
at different extrusion temperatures.
A strong power law dependence of apparent viscosity on shear
rate was observed for all the starch samples and measurement
conditions studied, and this dependence was linear on double-
logarithmic plots, indicating that the power law model of Bird et al.
(1960) could be used to describe the rheological behaviors of
starch-based materials:
h ¼ K gn1 (3)
 F. Xie et al. / Journal of Cereal Science 49 (2009) 371–377 373

1000000 10000 1000000 10000

Shear stress (Pa) τ (19% mc) τ (19% mc)

Shear stress (Pa)

τ (23% mc)

Viscosity (Pa·s)

Viscosity (Pa·s)
τ (23% mc)
τ (27% mc) τ (27% mc)
η (19% mc) η (19% mc)
100000 η (23% mc) 1000 100000 η (23% mc) 1000
η (27% mc) η (27% mc)

G80 G50
10000 100 10000 100
10 100 1000 10 100 1000
Shear rate (-s) Shear rate (-s)

1000000 10000 1000000 10000

τ (19% mc) τ (19% mc)
Shear stress (Pa)

Shear stress (Pa)

τ (23% mc)

Viscosity (Pa·s)
τ (23% mc)

Viscosity (Pa·s)
τ (27% mc) τ (27% mc)
η (19% mc) η (19% mc)
100000 η (23% mc) 1000 100000 η (23% mc) 1000
η (27% mc) η (27% mc)

NC WC
10000 100 10000 100
10 100 1000 10 100 1000
Shear rate (-s) Shear rate (-s)

Fig. 1. Effect of moisture content on shear stress and melt viscosity of various starches (extrusion temperature 130  C).

where h is the melt viscosity, K is the consistency, g is the shear rate,
and n is the pseudoplastic index. The corresponding consistency
and pseudoplastic index can be determined individually from the
intercept and the slope of each single straight line in the double-log
plots. For starch-based materials in this study, values of n are
between 0 and 1, and when n < 1, the apparent viscosity will
decrease with increasing shear rate and the materials will undergo
shear thinning (Tanner, 2000).
a function of shear rate. It can be seen that the apparent viscosity
generally decreased with increasing temperature from 110 to
140  C. A strong power law dependence of apparent viscosity on
shear rate is observed. For all the starch samples and measurement
conditions studied, the dependence of apparent viscosity on the
shear rate was linear on double-logarithmic plots, again indicating
that the power law model could describe the rheological behaviors
of the molten starches.

3.2. Effects of extrusion temperature 3.3. Effects of amylose content

Fig. 2 shows the effect of temperature on the rheological prop- Fig. 3 shows the effect of amylose content on the shear stress
erties of the different starches at 23% moisture content, as and melt viscosity of various samples at a moisture content of 23%

1000000 10000 1000000 10000

τ 110°C
Shear stress (Pa)

τ 110°C
Shear stress (Pa)

Viscosity (Pa·s)

τ 120 °C τ 120 °C

Viscosity (Pa·s)
τ 130 °C τ 130 °C
τ 140 °C τ 140 °C
η 110°C η 110°C
100000 η 120 °C 1000 100000 η 120 °C 1000
η 130 °C η 130 °C
η 140 °C η 140 °C

G80 G50

10000 100 10000 100

10 100 1000 10 100 1000
Shear rate (-s) Shear rate (-s)

1000000 10000 1000000 10000

τ 110°C
Shear stress (Pa)

τ 110°C
Viscosity (Pa·s)

τ 120 °C
Shear stress (Pa)

τ 120 °C
Viscosity (Pa·s)

τ 130 °C τ 130 °C
τ 140 °C τ 140 °C
η 110°C η 110°C
100000 η 120 °C 1000 100000 η 120 °C 1000
η 130 °C η 130 °C
η 140 °C η 140 °C

NC WC

10000 100 10000 100

10 100 1000 10 100 1000
Shear rate (-s) Shear rate (-s)

Fig. 2. Effect of temperature on shear stress and melt viscosity of various starches (moisture content 23%).
374 F. Xie et al. / Journal of Cereal Science 49 (2009) 371–377

1000000 10000 and extrusion temperature of 130  C, as a function of shear rate. It

τ G80 was found that higher amylose content resulted in a higher
τ G50 apparent viscosity over the same shear rate range. For example, at
τ NC
a shear rate of 100 S1, h is 277, 635, 1008, and 1254 Pa s for WC, NC,
Shear stress (Pa)

Viscosity (Pa·s)
τ WS
η G80
G50, and G80 respectively under the condition of 23% moisture
η G50 content and 130  C extrusion temperature.
100000 η NC 1000
η WS
3.4. Power law parameters

Table 1 lists the detailed parameters of regression power law for

the different samples and extrusion conditions investigated. It can
10000 100 be seen that, in most cases, n was higher when the moisture
10 100 1000 content was higher, which is to be expected, since increased water
Shear rate (-s) content in starches could make them more Newtonian. This
corresponds with most previous studies (Della Valle et al., 1996a;
Fig. 3. Effect of amylose content on shear stress and melt viscosity of various starches González et al., 2006; Kokini et al., 1992; Lai and Kokini, 1990),
(moisture content 23%; extrusion temperature 130  C).
although Willett et al. (1997) reported that the effect of moisture on
n was not clear in their study of waxy corn starch. The results in this
experimental work show that there are only a few conditions (e.g.

Table 1
Power law parameters of the various starches.

Starch Extrusion conditions Power law index (n) K (¼h at 1 s1) Correlation coefficient (R2)

Temperature ( C) % MC
G80 110 19 – – –
110 23 0.161 97,500 0.9670
110 27 0.197 65,300 0.9800
120 23 0.206 65,500 0.9805
120 27 0.284 300 0.9823
130 19 0.031 201,000 0.9950
130 23 0.259 38,000 0.9768
130 27 0.386 14,400 0.9677
140 23 0.316 22,800 0.9898
140 27 0.431 8510 0.9734

G50 110 19 – – –
110 23 0.102 119,000 0.9897
110 27 0.243 28,300 0.9961
120 23 0.217 50,200 0.9932
120 27 0.263 19,500 0.9956
130 19 0.154 59,400 0.9633
130 23 0.266 29,600 0.9916
130 27 0.345 10,400 0.9959
140 19 0.562 3660 0.8273
140 23 0.322 17,400 0.9975
140 27 0.400 5480 0.9990

NC 110 19 0.289 43,900 0.9654

110 23 0.331 25,300 0.9768
110 27 0.351 15,900 0.9938
120 19 0.383 20,400 0.9819
120 23 0.434 10,900 0.9963
120 27 0.475 5970 0.9590
130 19 0.411 13,800 0.9963
130 23 0.435 8560 0.9399
130 27 0.589 2390 0.9599
140 19 0.535 5570 0.9736
140 23 0.494 5590 0.9889
140 27 0.571 2260 0.9856

WC 110 19 0.477 14,000 0.9503

110 23 0.455 8020 0.9564
110 27 0.458 7400 0.9715
120 19 0.549 5950 0.9296
120 23 0.658 2060 0.9196
120 27 0.492 4290 0.9930
130 19 0.780 1260 0.9551
130 23 0.741 913 0.9503
130 27 0.504 2800 0.9479
140 19 0.825 710 0.8592
140 23 0.847 366 0.9618
140 27 0.680 835 0.9701

5 (figure not shown here), it can be seen that higher amylose content
4
Heat Flow Endo Up (mW)
WC
3
NC
2
1 gelatinization endotherms of the various starches as measured by
M2
G M
0 second endotherm, M2, was detected for NC at about 90  C, which
50 100
Temperature (ºC)
Fig. 4. Gelatinization endotherms of different starches.
at 140  C) that produce abnormal effects of moisture content on the
power law index n. One explanation could relate to the slight
expansion at the higher temperature and the enhancement of
moisture evaporation during measurement. Variations of volume
or mass at higher temperatures will affect the shear rate, which will
in turn affect the exponent n (see Eqs. (1) and (3)).
Increasing temperature will increase the power law index n and
thus make the starch melt less pseudoplastic and more Newtonian.
Similar results have been reported for both waxy corn starch (Della
Valle et al., 1996b; Willett et al., 1997) and normal corn starch
(Willett et al., 1994, 1995). An increase in n with increasing
temperature has also been observed with waxy corn starch during
first-pass twin-screw extrusion (Della Valle et al., 1996b; Lai and
Kokini, 1990).
It is important to note that n became higher with decreasing
amylose content for the studied corn starches, clearly indicating
that lower amylose-content corn starch has a more Newtonian
behavior in its melting state. Similar results have been observed in
previous studies (Della Valle et al., 1996b; Lai and Kokini, 1990). The
decrease in the power law index with increasing amylose content
was generally attributed to an increase in entanglements between
amylose chains, since the highly branched amylopectin was not
expected to form effective entanglements (Willett et al., 1997; Yu
and Christie, 2005).
Table 1 also shows that the power law consistency value K
decreased with increasing moisture content and extrusion
temperature. Since the K value has a direct relationship with
viscosity (see Eq. (3)), it can be used to represent the viscosity
characteristics of a material under certain conditions. The K results
are as expected, since both water (as plasticizer) and temperature
will normally decrease the viscosity of a polymeric material. By
plotting the effects of amylose content and temperature on K
Fig. 5. Schematic representation of microstructure and phase transition of starch during gelatinization.
F. Xie et al. / Journal of Cereal Science 49 (2009) 371–377 375
resulted in a higher K value. For example, K increased from 103 for
WC to 105 for G80 at the highest temperature investigated (140  C).
However, all starches recorded a lower K value with increasing
temperature, although the decrease in K was not linear for starches
with different amylose/amylopectin ratios. It should be pointed out
that there were a few anomalies for the waxy starch at higher
temperature, which could be explained by the expansion of the
material during extrusion, as discussed earlier.
Gelatinization during thermal processing is one of the unique
G50
characteristics of starch-based materials, and Fig. 4 shows the
G80 DSC. It can be seen that for the waxy and normal corn starches,
a large gelatinization endotherm, G, appeared at about 70  C. A
150 was considered to be a phase transition within an amylose–lipid
complex (Biliaderis et al., 1985; Jovanovich and Añón, 1999; Liu
et al., 2006; Raphaelides and Karkalas, 1988). A very broad endo-
therm was observed in the temperature range of 65–115  C for both
high amylose-content starches (G50 and G80), which represents
a composite of gelatinization endotherm G and a phase transition
within the amylose–lipid complex M2. For G80, a small endotherm,
M, was also detected at about 155  C, which was considered to be
amylose melting (Liu et al., 2006). The higher temperature detected
for the amylose-rich starches can be used to explain their higher
viscosity and less Newtonian behavior.
It is has been noticed that the higher the amylose content, the
higher the viscosity, which is opposite to the sequence of molecular
weight (see Fig. 3) (Liu et al., 2006). The unique microstructure and
phase transition can be used to explain this phenomenon. Fig. 5
shows a schematic representation of the microstructure and phase
transition of starch during gelatinization, in which the double
helical, crystalline structure formed by the short branched chains in
amylopectin are torn apart. However, these short branched chains
remain in a regular pattern by retaining a certain ‘‘memory’’. French
(1984) reported that the thickness of crystalline lamellae in native
amylopectin and recrystallized amylopectin is the same (about
50 Å), which supports the ‘‘memory’’ theory. In a previous study, Yu
and Christie (2005) indicated that these short branched chains
form gel-balls that are comprised mainly of chains from the same
sub-main chain. In addition, one amylopectin molecule may form
a relatively separate super-globe. The molecular entanglements
between gel-balls and super-globes are much less than those
between linear polymer chains, due to their size and the length of
the chains (only 4–6 glucose).
These gel-balls require less energy to move than long linear
chains, especially when they are lubricated by a plasticizer (water).
Because of the highly branched microstructure of starch, and the
formation of gel-balls and super-globes after gelatinization, the
entanglement of polymer chains in amylopectin-rich starch is
much less than that in amylose-rich linear starch. This could
explain why amylopectin-rich materials initially have lower
376 F. Xie et al. / Journal of Cereal Science 49 (2009) 371–377
modulus and higher elongation, and lower viscosity during extru-
sion (Yu and Christie, 2005). It could also explain why amylopectin-
rich starches exhibit increased Newtonian behavior.
4. Conclusions
In this work, the rheological properties of various corn starches
with different amylose/amylopectin ratios (0/100, 23/77, 50/50, and
80/20) were firstly systematically studied using a Haake rheometer.
A single-screw extruder with a slit capillary die was used to char-
acterize shear stress and apparent melt viscosity as functions of
moisture content (19–27  C) and extrusion temperature (110–
140  C). The melts exhibited shear thinning behavior under all
conditions, with the power law index n (0 < n < 1) increasing with
increasing temperature and moisture content in most cases; and it
decreased as amylose content increased. The K value decreased
with increasing moisture content and extrusion temperature; and
it increased with increasing amylose content (for example, K
increased from 103 for WC to 105 for G80 at 140  C). The amylose-
rich corn starches showed higher viscosity and less Newtonian
behavior, which can be explained by its higher gelatinization
temperature (and in particular multiphase transition at higher
temperature), greater molecular entanglements between linear
polymer chains, and less gel-balls and super-globes that are much
easier to move than long linear chains. The results of this work have
confirmed some previously reported results, and have addressed
some earlier confusion.
Acknowledgement
The authors from SCUT, China, would like to acknowledge the
research funds NRDPHT (863) (2007AA10Z312, 2007AA100407),
GNSF (05200617) and ETRFNK (2006C40038).
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