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Received 25 June 2007; received in revised form 5 October 2007; accepted 8 November 2007
Abstract
A simple tensile test set-up was built and attached to an Instron 5566 to determine gluten extensibility, comparing the performance of
strong and weak flour mixed for various mixing time. In this work, the gluten strip was clamped at two ends and extended upward at the
centre by a hook at speed of 300 mm min1. Parameters such as gluten length at fracture, measured force, actual force acting on the
gluten strips, strain, strain rate and stress were obtained. Gluten obtained from strong flour has greater extensibility compared to weak
flour. The extensibility of gluten from both strong and weak flour dough increased as dough mixing time increased before decreasing at a
peak of 8 min. The results demonstrated the capability of the tensile test set-up to describe the development of gluten during mixing of
dough. Rheological characteristic of gluten indicated that gluten exhibited strain hardening effect during extension.
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doi:10.1016/j.jfoodeng.2007.11.005
Please cite this article in press as: Abang Zaidel, D.N. et al., Rheological characterisation of gluten from extensibility measurement,
Journal of Food Engineering (2007), doi:10.1016/j.jfoodeng.2007.11.005
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Nomenclature
2004a,b). Tronsmo et al. (2003) performed a uniaxial Thus, optimum water level must be used in developing
extension on dough and gluten using the Kieffer dough cohesive, viscoelastic dough with optimum gluten
and gluten extensibility rig for the TA.TX2i texture ana- strength. As mixing proceeds, more protein become
lyser to test the rheological properties. They used six differ- hydrated and the glutenins tend to align because of the
ent wheat flours to study the difference in the breadmaking shear and stretching forces imposed. At this stage, gluten
performance and determined the maximum resistance to networks are more developed by the cross-linking of pro-
extension and total extensibility. Another extensional tein with disulphide bonds. At optimum dough develop-
instrument used to determine the extensibility of wheat ment, the interactions between the polymers cross-links
flour dough was Sentmanat Extensional Rheometer become stronger and that leads to an increased dough
(SER) (Trevor et al., 2006). In this test, a rectangular strength, maximum resistance to extension and restoring
dough sample was mounted onto two cylindrical drums force after deformation. When the dough is mixed past
and was stretched until it fractured. its optimum development, the cross-links begin to break
The main problem encountered in performing gluten due to the breaking of disulphide bonds. The glutenins
and dough extensibility tests is to hold the sample so that become depolymerised and the dough is overmixed.
it breaks within the sample and not at the jaws that hold The presence of smaller chains in the dough makes the
the sample. This paper focuses on gluten extensibility mea- dough stickier. Two types of flour were used in this
surement using a new tensile test set-up attached to Instron study as different wheat flour has different optimum mix-
(5566 series, Instron Corporation, USA) and also its rheo- ing time (Hoseney, 1985). Longer mixing time is expected
logical characterisation. Using this set-up, gluten extensi- for mixing dough from strong flour. It is probably due
bility was determined by studying the effect of various to the dense particles of strong flour through which
mixing times on the development of gluten during dough water penetrates slowly (Hoseney, 1985). Sliwinski et al.
mixing. Four rheological characteristics were determined: (2004a) reported that a positive correlation was observed
fracture strain, fracture stress, the coefficient, k and index, between mixing time and the percentage of glutenin pro-
n. Fracture strain and fracture stress are the points when tein on total protein in flour. The effect of mixing time
gluten fractured at its maximum extensibility. k and n, on the rheological properties of gluten has been investi-
which indicate the extensional stiffness and strain harden- gated by Amemiya and Menjivar (1992), Janssen et al.
ing of gluten respectively, were determined from curve-fit- (1996) and Létang et al. (1999).
ting of stress–strain curve following exponential equation,
r = kene. Previous studies on biaxial extension of dough 2. Materials and methods
(Chin and Campbell, 2005; Dobraszczyk et al., 2003) fit
the stress–strain curves following the exponential equation 2.1. Dough preparation
to obtain k and n.
Mixing time is one of the processing factors that influ- Two types of flour, Diamond N (12.33% protein) and
ence the gluten development during mixing other than SP-3 (8.81% protein), were used in this study and they
work input, mixer type and temperature. The molecular are referred as strong and weak flour, respectively.
model proposed by Belton (1999) and Létang et al. Doughs were prepared by mixing 200 g flour with water
(1999) suggested that at early stage of mixing, gluten fibrils (63.4% for strong flour; 59.5% for weak flour) in mixer
are formed as the water is in contact with flour particles. (5K5SS, KitchenAid, Belgium) for various mixing times:
Water is responsible in hydrating the protein fibrils and 3, 5, 8, 11 and 15 min. Treated drinking water was used
started the interactions between the proteins cross-links to avoid any effect or reaction from other minerals on
with the disulphide bonds. Too much water added to the the protein of flour during flour–water mixing. Dough
flour will result in slurry and too little water results in was left to stand in water for 1 h at room temperature
slightly cohesive powder (Faubion and Hoseney, 1989). to rest (AACC, 1976).
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4 D.N. Abang Zaidel et al. / Journal of Food Engineering xxx (2007) xxx–xxx
Fig. 3. Schematic diagram of forces acting on gluten and the length of gluten during tensile test (Dunnewind et al., 2004).
2.3.2. Derivation of rheological parameters (ANOVA), at alpha level = 0.05 (P < 0.05), was performed
The extension parameters obtained earlier were used to using a statistical software, Design Expert (Version 6.0.4,
determine the rheological parameters such as strain, strain State-Ease Inc., Minneapolis, USA). The force-extension
rate and stress. The Hencky strain (eH) acting on gluten graphs were plotted from data obtained from Instron
was calculated using the Eq. (5): which were also used to calculate the extensibility parame-
0qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi1 ters. Curves of strain-hook displacement, strain rate-hook
2 2
lt B ðd=2Þ þ ðy o þ y t Þ C displacement and stress–strain were obtained to study the
eH ¼ ln ¼ ln @ qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi A ð5Þ performance of the tensile test set-up.
lo
ðd=2Þ2 þ ðy o Þ2
3. Results and discussion
The strain rate was calculated by differentiating of Hencky
strain (_e) with time as shown in Eq. (6):
3.1. Dough and gluten preparation
deH dl 1 2ðy t þ y o Þ dy
e_ ¼ ¼ ffi t
¼ qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
dt lt dt lt 2 2 dt Observations made during washing of gluten shows that
9 þ ðy t þ y o Þ
washing time to obtain starch-free gluten for strong flour
4vðy t þ y o Þ was longer than weak flour. This suggests that washing
¼ ð6Þ
l2t time is influenced by the flour type and its protein content.
With the same dough dimensions before washing, the
where v is the speed of hook (mm min1). The final cross-
weight of gluten obtained from strong flour was slightly
sectional area of gluten strip was calculated by assuming
higher compared to weak flour. This explains that the
the volume of gluten was constant throughout the test
quantity of wet gluten is higher from a higher protein con-
(Muller et al., 1961; Sliwinski et al., 2004a) as provided
tent flour (Ćurić et al., 2001).
in the Eq. (7).
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a 1.6 b 1.6
2 min 2 min
5 min 5 min
8 min 8 min
1.2 11 min 1.2 11 min
15 min 15 min
Fm (N)
Fm (N)
0.8 0.8
0.4 0.4
0.0 0.0
0 50 100 150 200 0 50 100 150 200
y t (mm) y t (mm)
Fig. 4. Measured force-hook displacement curves for gluten from doughs mixed using (a) strong and (b) weak flour at various mixing times.
but it was not obvious for the weak flour. The curves of
250 strain rate versus hook displacement in Fig. 7 shows that
as the hook displacement increased, the strain rate
200
increased up to a peak before decreasing as the hook dis-
placed further. Glutens from weak flour gave higher strain
150
0 4 8 12 16 rates compared to glutens from the strong flour for all the
Mixing time (min) mixing times.
Fig. 5. The gluten length at fracture from doughs mixed for various
mixing times. 3.2.2. Rheological characterisation
Fig. 8 illustrates the stress–strain curves of glutens
obtained from strong and weak doughs mixed for various
strength as influenced by the flour protein content (Ćurić mixing times. The stress increased with increasing strain
et al., 2001). with maximum values at sample fracture. The gradient of
Fig. 5 shows the effects of various mixing times on glu- the curve is related to the modulus of gluten. The curves
ten extensibility. The length of gluten at fracture (lt) displayed a curvature up to fracture indicating that the
increased as mixing time increased, reaching a peak before modulus increased with extension. This behaviour is
it decreased in further mixing indicating a typical dough known as strain hardening, where the force to extend the
development process. Gluten from both flours, mixed for material needs to increase for additional strain to occur
8 min gave the highest value of lt. This suggests that dough and the stress increases more than proportional with the
mixed for 8 min reached the optimum development and at strain (Sliwinski et al., 2004c). This result was also reported
this stage, the interactions between the polymers cross-links in previous studies on uniaxial extension test on dough and
became strong and leads to an increased dough strength, gluten (Sliwinski et al., 2004a,b,c) and biaxial extension of
maximum resistance to extension and restoring force after dough (Janssen et al., 1996; Chin and Campbell, 2005; Sli-
deformation (Létang et al., 1999). Gluten mixed for times winski et al., 2004b). Trevor et al. (2006) reported that
exceeding 8 min had lower extensibility values. Létang strain hardening occurred at high strain rates where the
et al. (1999) explained that when the dough is mixed longer stress increases more rapidly than linearly with the strain.
past its optimum development, the cross-links begin to The failure stress and strain were obtained from the
break due to the breaking of disulphide bonds and the stress–strain values at gluten fracture. Fig. 9a and b show
glutenins becomes depolymerised and overmixed. Table 1 that for both flours, the failure stress and strain increased
shows the extensibility of gluten of strong and weak flour as the mixing time increased to 8 min before started
mixed for various mixing times at optimum water level. decreasing. This agrees with Fig. 5 showing gluten mixed
Analysis of variance shows that the effect of mixing time for 8 min reaching its optimum development. At this stage,
on gluten extensibility was more significant for the strong the interactions between the polymers cross-links become
flour gluten (P < 0.003) than the weak flour gluten strong and it leads to increased dough strength, maximum
(P < 0.37). resistance to extension and restoring force after deforma-
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Journal of Food Engineering (2007), doi:10.1016/j.jfoodeng.2007.11.005
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Table 1
Extensibility parameters of gluten at fracture from strong and weak flour at various mixing times
Flour Mixing time (min) yt (mm) Fm (N) lt (mm) Fa (N) eH e_ (s1) r (N mm2)
Strong 2 136.1 ± 5.6 1.40 ± 0.21 287.0 ± 11.0 0.71 ± 0.06 1.93 ± 0.04 2.08 ± 0.08 0.0489 ± 0.0058
5 136.1 ± 2.8 1.41 ± 0.16 287.0 ± 5.5 0.71 ± 0.05 1.93 ± 0.02 2.07 ± 0.04 0.0491 ± 0.0043
8 172.2 ± 5.6 1.43 ± 0.26 358.7 ± 11.0 0.72 ± 0.08 2.15 ± 0.03 1.86 ± 0.05 0.0618 ± 0.0059
11 140.3 ± 9.1 1.37 ± 0.14 295.3 ± 18.1 0.69 ± 0.04 1.95 ± 0.06 2.03 ± 0.12 0.0490 ± 0.0053
15 137.5 ± 7.2 1.49 ± 0.08 289.8 ± 14.3 0.77 ± 0.02 1.93 ± 0.05 2.09 ± 0.10 0.0523 ± 0.0038
Weak 2 90.3 ± 2.8 0.57 ± 0.04 196.7 ± 5.4 0.29 ± 0.02 1.55 ± 0.03 2.99 ± 0.08 0.0137 ± 0.0008
5 83.3 ± 4.8 0.58 ± 0.05 183.1 ± 9.4 0.30 ± 0.03 1.48 ± 0.05 3.21 ± 0.16 0.0131 ± 0.0012
8 97.2 ± 2.8 0.91 ± 0.07 210.3 ± 5.5 0.46 ± 0.04 1.62 ± 0.03 2.80 ± 0.07 0.0234 ± 0.0023
11 94.4 ± 7.3 0.78 ± 0.09 204.9 ± 14.4 0.40 ± 0.05 1.59 ± 0.07 2.90 ± 0.19 0.0193 ± 0.0015
15 94.4 ± 5.6 0.84 ± 0.05 204.9 ± 10.9 0.43 ± 0.02 1.59 ± 0.05 2.89 ± 0.16 0.0210 ± 0.0020
± Standard deviation of mean of three replicates.
a 2.5 b 2.5
2.0 2.0
Fig. 6. Strain versus hook displacement for gluten from doughs mixed using (a) strong and (b) weak flour at various mixing times.
a 8 b 8
2 min
5 min 2 min
6 6 5 min
8 min
8 min
Strain rate (s-1)
11 min
15 min 11 min
15 min
4 4
2 2
0 0
0 50 100 150 200 0 50 100 150 200
yt (mm) yt (mm)
Fig. 7. Strain rate versus hook displacement for gluten from doughs mixed using (a) strong and (b) weak flour at various mixing times.
tion (Létang et al., 1999). Failure stress and strain for trend from k. The strong flour seems to have a slight fall in
strong flour gluten were higher than weak flour gluten the n value for 15 min mixing. k value for weak flour was
for all mixing times (Sliwinski et al., 2004b). Coefficient, higher than strong flour and the opposite was found for
k and index, n were determined by fitting the stress–strain n value which is also reported for biaxial extension study
curves using an exponential equation, r = kene. The coeffi- of dough (Chin and Campbell, 2005). Higher k values in
cient of determination (R2) of the fitted stress obtained for the weak flour gluten compared to the strong flour gluten
various mixing times was in the range of 0.91–0.99 as pre- suggest that the earlier was extensionally stiffer. Higher n
sented in Fig. 8. Fig. 9c and d show that k increased and value was found in strong flour explains that the strong
then decreased with mixing time while n shows an opposite flour gluten exhibit higher strain hardening properties than
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a 0.08 b 0. 08
2 min R2= 0.9987 2 min R 2= 0.9943
5 min R2= 0.9993 5 min R 2= 0.9827
0.06 8 min R2= 0.9355 0. 06 8 min R 2= 0.9933
11 min R2= 0.9796
Stress (N mm-2)
11 min R 2= 0.9960
Stress (N mm-2)
15 min R2= 0.9988 15 min R 2= 0.9168
0.04 0. 04
0.02 0. 02
0.00 0. 00
0.0 0.5 1.0 1.5 2.0 2.5 0.0 0.5 1.0 1.5 2.0 2.5
Strain Strain
Fig. 8. Stress–strain curves for gluten from doughs mixed using (a) strong and (b) weak flour at various mixing times.
a 2.5 b 0.08
strong strong
weak weak
0.04
1.5
0.02
1.0 0.00
0 4 8 12 16 0 4 8 12 16
Mixing time (min) Mixing time (min)
c 0.0025 d 3.0
strong strong
0.0020 weak weak
Coefficient, k
2.5
0.0015
Index,n
0.0010
2.0
0.0005
0.0000 1.5
0 4 8 12 16 0 4 8 12 16
Mixing time (min) Mixing time (min)
Fig. 9. Graph of (a) failure strain, (b) failure stress, (c) k, and (d) n for gluten from doughs mixed using (a) strong and (b) weak flour at various mixing
times.
the weak flour gluten, of which is in agreement with Sliwin- to a peak of 8 min before decreasing. At this stage the gluten
ski et al. (2004c). Strain hardening prevents premature frac- development is at its optimum and further mixing of dough
tures of dough and gluten and allow large extensions before beyond this optimum time results in reduction in gluten
rupture (Chin and Campbell, 2005; Sliwinski et al., 2004c). extensibility. The extensibility parameters of gluten from
strong flour gave higher values than weak flour in term of
4. Conclusions the length at fracture, measured and actual force, strain
and also stress. These results are supported by the higher
Determining the extensibility of gluten using the tensile strain hardening properties of the strong flour gluten, which
test set-up was successful in terms of providing the extensibil- prevents early fracture of gluten samples. This work illus-
ity measurements where gluten do not fracture at the clamp- trated that the behaviour of gluten development during mix-
ing areas. The extensibility of gluten from both strong and ing can be predicted by the rheological characterisation of
weak flour dough increased as dough mixing time increased gluten. Thus, the results also demonstrated the capability
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of the tensile test set-up to describe the development of gluten doughs at elevated temperatures in relation to breadmaking perfor-
during mixing of dough. mance. Cereal Chemistry 80, 218–224.
Dunnewind, B., Sliwinski, E.L., Grolle, K., Van Vliet, T., 2004. The
Kieffer dough and gluten extensibility rig – An experimental evalua-
Acknowledgement tion. Journal of Texture Studies 34, 537–560.
Faubion, J.M., Hoseney, R.C., 1989. The viscoelastic properties of wheat
The authors wish to thank Malayan Flour Mill Sdn flour doughs. In: Faridi, H.A., Faubion, J.M. (Eds.), Dough Rheology
Bhd, Malaysia for supplying the flour for this study. and Baked Product Texture. Van Nostrand Reinhold, New York,
USA, pp. 29–66.
References Hoseney, R.C., 1985. The mixing phenomenon. Cereal Foods World 30
(7), 453–457.
Janssen, A.M., van Vliet, T., Vereijken, J.M., 1996. Rheological behaviour
AACC, 1976. Method 38-10. Gluten – Hand washing method. In:
of wheat glutens at small and large deformations. Comparison of two
Approved Methods of the American Association of Cereal Chemists,
glutens differing in bread making potential. Journal of Cereal Science
vol. 1. seventh ed., AACC, Inc., Minnesota, USA.
23, 19–31.
Abang Zaidel, D.N., Chin, N.L., Abdul Rahman, R., Karim, R., 2007.
Kieffer, R., Wieser, H., Henderson, M.H., Graveland, A., 1998. Corre-
Development of gluten extensibility measurement using tensile test. In:
lations of the breadmaking performance of wheat flour with rheolog-
Mustapa Kamal, S.M., Hussain, S.A., Chin, N.L., Abdul Rashid, S.,
ical measurements on a micro-scale. Journal of Cereal Science 27, 53–
Sobri, S., Yusof, Y.A., Taip, F.S., Abdullah, L.C. (Eds.), Proceedings
60.
of the World Engineering Congress 2007, 5–9 August, Penang,
Létang, C., Piau, M., Verdie, C., 1999. Characterization of wheat flour–
Malaysia, pp. 1–8.
water doughs. Part I: Rheometry and microstructure. Journal of Food
Amemiya, J.I., Menjivar, J.A., 1992. Comparison of small and large
Engineering 41, 121–132.
deformation measurements to characterize the rheology of wheat flour
Muller, H.G., Williams, M.V., Russell Eggitt, P.W., Coppock, J.B.M.,
doughs. Journal of Food Engineering 16, 91–108.
1961. Fundamental studies on dough with the Brabender Extensog-
Anderssen, R.S., Bekes, F., Gras, P.W., Nikolov, A., Wood, J.T., 2004.
raph. I – Determination of stress–strain curves. Journal of the Science
Wheat–flour dough extensibility as a discriminator for wheat varieties.
and Food Agriculture 12, 513–523.
Journal of Cereal Science 39 (2), 195–203.
Sliwinski, E.L., Kolster, P., Prins, A., van Vliet, T., 2004a. On the
Belton, P.S., 1999. On the elasticity of wheat gluten. Journal of Cereal
relationship between gluten protein composition of wheat flours and
Science 29, 103–107.
large-deformation properties of their doughs. Journal of Cereal
Chen, C.S., Chen, J.J., Wu, T.P., Chang, C.Y., 1998. Optimising the frying
Science 39, 247–264.
temperature of gluten balls using response surface methodology.
Sliwinski, E.L., Kolster, P., van Vliet, T., 2004b. Large-deformation
Journal of the Science of Food and Agriculture 77, 64–70.
properties of wheat flour dough in uni- and biaxial extension. Part I.
Chiang, S.H., Chen, C.S., Chang, C.Y., 2006. Effect of wheat flour protein
Flour dough. Rheologica Acta 43, 306–320.
compositions on the quality of deep-fried gluten balls. Journal of Food
Sliwinski, E.L., Kolster, P., van Vliet, T., 2004c. On the relationship
Chemistry 97 (4), 666–673.
between large-deformation properties of wheat flour dough and baking
Chin, N.L., Campbell, G.M., 2005. Dough aeration and rheology. II.
quality. Journal of Cereal Science 39, 231–245.
Effects of flour type, mixing speed and total work input on aeration
Trevor, S.K.N., Gareth, H.M., Madesh, P., 2006. Linear to non-
and rheology of bread dough. Journal of the Science of Food and
linear rheology of wheat flour dough. Applied Rheology 16 (5),
Agriculture 85, 2194–2202.
1–7.
Ćurić, D., Karlović, D., Tušak, D., Petrović, B., Dugum, J., 2001. Gluten
Tronsmo, K.M., Magnus, E.M., Baardseth, P., Schofield, J.D., 2003.
as a standard of wheat flour quality. Journal of Food Technology
Comparison of small and large deformation rheological properties
Biotechnology 39 (4), 353–361.
of wheat dough and gluten. Cereal Chemistry 80 (5),
Day, L., Augustin, M.A., Batey, I.L., Wrigley, C.W., 2006. Wheat-gluten
587–595.
uses and industry needs. Trends in Food Science and Technology
Uthayakumaran, S., Newberry, M., Phan-Thien, N., Tanner, R., 2002.
Journal 17 (2), 82–90.
Small and large strain rheology of wheat gluten. Rheologica Acta 41,
Dobraszczyk, B.J., Smewing, J., Albertini, M., Maesmans, G., Schofield,
162–172.
J.D., 2003. Extensional rheology and stability of gas cell walls in bread
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