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The method to measure hardness and other viscoelastic properties of for 9.3% moisture content. Young’s modulus range for soft wheat such as
intact wheat kernels is presented. Wheat with 9.3% moisture showed high Salamanca, Saturno, and Cortazar cultivars was 232.2–308.5 MPa, as
elastic behavior compared with wheat tempered at 22.5 % moisture that compared with Rayón bread wheat at 321.5 MPa and the Altar, Sofía, and
showed a plastic behavior. Load-deformation curves showed that bread Rafi cultivars of durum wheat that had elastic moduli of 438.7–485.8
wheat behaves as a more plastic material than durum wheat, which is a MPa. The compression force and final stress decreased from 69.9 N and
more elastic material. Yield point of all the wheat samples was ≈18.5 N, 40.1 MPa in soft wheat to 90 N and 78.9 MPa in durum, respectively.
independent of wheat type and moisture content. The height of the wheat Total work range was 14.7 MPa/sec in soft wheat to 19.7 MPa/sec for
kernel increased linearly, and the compression area increased exponen- durum wheat and, as expected, was higher in the durum and bread wheat
tially, with increasing moisture content. The modulus of elasticity of than in soft wheat. The plastic part ranged from 2.4 MPa/sec in soft wheat
wheat ranged from 99.2 MPa for 22.5% moisture content to 394.8 MPa to 0.6 MPa/sec in durum wheat.
Wheat physical quality has been tested conventionally using whole corn kernel by Singh et al (1991). In grains, the evaluation
several methods that try to evaluate the hardness. A practical and of mechanical properties is particularly difficult because these
appropriate method to evaluate other fundamental mechanical parameters may be very seriously affected by the percentage of
properties of wheat kernels such as modulus of elasticity, yield strain, drift, temperature, and moisture content. This explains, in
point, yield stress, compressive strength, as well as the viscoelas- part, the ample range of modulus of elasticity values reported
tic properties like elastic and plastic work, may increase the effi- (Shelef and Mohsenin 1967; Singh et al 1991; Haddad et al
ciency of grain selection for processing, marketing, and end use. 1998). In addition, cutting or shaping of a biological material may
Hardness is a grain characteristic defined as the resistance to de- alter its structural mechanics and resultant mechanical behavior,
formation with applied force (stress) and is largely determined by more so for small grains such as cereal grains. Therefore, to ob-
the endosperm properties (Gates and Dobraszczyk 2004; Gref- tain realistic data on the mechanical responses of cereal grains, as
feuille et al 2006). Problems are often encountered when trying to far as possible, intact grains should be tested (Singh et al 1991).
correlate the hardness (compression force obtained from a con- The major objective of this research was to determine the me-
ventional texturometer) and wheat quality. More difficulties were chanical and viscoelastic behavior of intact wheat kernels as a
found when trying to standardize the hardness with the empirical function of wheat type and moisture content.
scales given by the instruments for near-infrared (NIR) and single
kernel characterization system (SKCS). The cause is undoubtedly MATERIALS AND METHODS
the difference in the hardness definitions used in conjunction with
these approaches. Most methods used to assess grain hardness are Materials
empirical and based on the overall properties of the whole grains Three kinds of grains were tested. The wheat samples were
(Gates and Dobraszczyk 2004; Greffeuille et al 2006; Morris et al classified in accordance with the Mexican classification system:
2007). Related to the other mechanical properties of the wheat bread wheat Rayón; soft wheat (Salamanca, Saturno, and Corta-
kernel, several methods have been suggested for the determina- zar cultivars); and durum wheat (Altar, Rafi, and Sofia cultivars).
tion of the elastic modulus of small pieces of agricultural materi- In addition, 250 g of a commercial bread wheat sample with 9.3%
als also using compression tests. Our research here on wheat grain moisture content was conditioned with distilled water to get 17.2,
viscoelastic properties aims to define and measure hardness in 19.5, and 22.5% moisture contents to study the effect of the vis-
terms of mechanical properties. The viscoelastic methods are based coelastic properties of wheat kernels. Samples with 17.2, 19.5,
on the Hertz and Boussineseq assumptions related to deformation and 22.5% moisture contents were prepared in two steps. First,
and elasticity (Pharr et al 1992; Gubicza et al 1996a,b; Wei et al they were placed into airtight containers with distilled water to
2001). These methods include the use of a parallel plate for whole reach ≈14.5% moisture, then they were shaken for a few minutes
grain, spherical indenter, cylindrical indenter, and parallel plate to distribute the water and left to rest 5 hr at 25°C. For the second
for core specimen. step, additional water was added to the sample to desired moisture
The viscoelastic behavior of wheat using the traditional uniax- content, shaken, and kept for additional 12 hr.
ial compression of various loading devices, including parallel
plate, was determined in cut samples of the hard endosperm Grain Characterization
(Shelef and Mohsenin 1967; Haddad et al 1998, 2001), and in Moisture content was determined by Approved Methods 55-10
and 44-15A, respectively (AACC International 2000). Kernel
height was measured using a digital caliper (model CD-6 CS,
1 DIPA, Universidad Autónoma de Querétaro. Centro Universitario, Cerro de las Mitutoyo, Japan).
Campanas S/N, Querétaro, Qro., CP 76010. A TA-XT2 texture analyzer (Texture Technologies Corporation,
2 Centro de Investigación y de Estudios Avanzados (CINVESTAV-IPN), Libra-
miento Norponiente 2000, Fracc. Real de Juriquilla, Querétaro, C.P. 76230 Qro.,
Stable Micro Systems, Surrey, England) was used to measure the
México. kernel response to compressive loadings between two parallel
3 Corresponding author. E-mail: jfigueroa@qro.cinvestav.mx plates (an aluminum probe 50 mm in diameter [model P/50] and
4 Facultad de Químico-Farmacobiología, Universidad Michoacana de San Nicolás
the plate). The technique used to determine the contact area (load-
de Hidalgo, Morelia, Mich., México. bearing area) of the individual kernels during the loading process
doi:10.1094 / CCHEM-85-5-0667 first used an ink pad to paint the grain, then pieces of paper 30
© 2008 AACC International, Inc. mm × 30 mm were taped onto the loading face of the top plate to
Statistical Analyses
Data was analyzed using Tukey’s test with SAS general linear
model (GLM). Simple Pearson’s correlations were performed using
PROC CORR and were significant and highly significant at P ≤
0.05, and P ≤ 0.001, respectively (SAS Institute, Cary, NC).
Fig. 2. Behavior schematic of various materials during compression load. A, ideal plastic; B, elastoplastic; and C, ideal elastic.
TABLE I
Mean Values for Physical and Mechanical Properties of Bread Wheat Conditioned at Different Water Contentsa,b
Kernel Compression Compression Modulus of
Moisture (%) Height (mm) Area (mm2) Force (N) Final Stress (MPa) Final Strain (%) Elasticity (MPa)
9.3 3.08 ± 0.16b 0.99 ± 0.36b 58.09 ± 9.33a 62.49 ± 12.99a 16.27 ± 0.9a 394.8 ± 49.67a
17.2 3.12 ± 0.09ab 1.05 ± 0.27b 45.02 ± 6.37b 44.26 ± 7.78b 15.99 ± 1.1a 292.7 ± 38.43b
19.5 3.25 ± 0.16ab 1.48 ± 0.18a 39.91 ± 5.15b 26.11 ± 3.31c 15.34 ± 1.2a 150.3 ± 24.42c
22.5 3.28 ± 0.11a 1.52 ± 0.24a 23.21 ± 3.07c 15.67 ± 3.38c 15.23 ± 1.1a 99.2 ± 19.84d
a Measured using a uniaxial cell with strain of 0.5 mm and 0.1 mm/sec of deformation velocity.
b Means ± standard deviation followed by the same letter are not significantly different at P ≤ 0.05 (analyzed using Tukey’s test).
Fig. 4. Typical force displacement curves of wheats. A, Soft wheat Saturno; B, bread wheat Rayón; C, durum wheat Rafi. Arrow indicates yield point.
TABLE II
Mean Values for Elastic Modulus in Wheat Kernels Measured in a Single Kernela
Kernel Compression Compression Final Stress Final Strain Modulus of
Cultivar Thickness (mm) Area (mm2) Force (N) (MPa) (%) Elasticity (MPa)
Saturno 2.90 ± 0.16ab 1.83 ± 0.43a 69.92 ± 8.75d 40.00 ± 1.07d 17.23 ± 1.0ab 232.14 ± 55.41d
Salamanca 2.97 ± 0.20ab 1.78 ± 0.28ab 75.13 ± 7.79cd 43.30 ± 9.09d 16.81 ± 1.2ab 244.65 ± 45.81cd
Cortazar 3.06 ± 0.14a 1.56 ± 0.21a–c 80.24 ± 5.83cd 50.05 ± 9.46cd 16.09 ± 1.0 b 308.54 ± 29.92bc
Rayón 2.82 ± 0.14b 1.47 ± 0.12b–d 86.93 ± 5.82ab 63.23 ± 1.39bc 17.71 ± 0.9a 321.46 ± 32.54b
Altar 3.00 ± 0.13ab 1.29 ± 0.13c–e 92.58 ± 3.66a 71.05 ± 8.88ab 16.61 ± 0.7ab 438.65 ± 50.03a
Sofía 3.03 ± 0.16a 1.22 ± 0.17de 88.74 ± 6.72ab 71.53 ± 1.45ab 16.61 ± 1.0ab 454.14 ± 79.36a
Rafi 2.97 ± 0.13ab 1.15 ± 0.16e 90.94 ± 6.20a 78.95 ± 1.24a 16.87 ± 0.8ab 485.80 ± 54.33a
a Means ± standard deviation followed by the same letter are not significantly different at P ≤ 0.05 (analyzed using Tukey’s test).
Therefore, durum wheat kernels have a higher maximum stress niques using the wheat kernel as an indenter. The use of load and
(strength), modulus of elasticity (stiffness), and toughness than displacement sensing indentation techniques are becoming in-
the mealy soft wheat and bread wheat cultivars. creasingly popular for measuring the elastic moduli of materials.
Delwiche (2000) used wheat endosperm cylinders compressed These techniques rely on the fact that the displacements recovered
at a velocity of 0.5 mm/min and reported modulus of elasticity during loading and unloading are largely elastic, in which case,
values of ≈805–1,130 MPa for soft wheat and 1,850–2,050 MPa the elastic punch theory can be used to determine the viscoelastic
for HRS for 9–10% moisture content. Glenn et al (1991) reported parameters.
the modulus of elasticity of core endosperm of bread wheat and Several authors have proposed estimation of hardness in soft
durum wheat of 500–1,500 MPa for American wheats, which are materials in terms of the maximum applied load divided by the
higher than those found for Mexican wheats and those reported projected area of the permanent impression being equivalent to
for French wheats by Kang et al (1995) and Haddad et al (1998, the plastic work divided by plastically deformed volume (Pharr et
2001). This is due to different breeding conditions and low com- al 1992; Tuck et al 2001). If we relate that to the loading area, we
pression velocity used by Delwiche (2000) but it does follow the have the formula Load P (N)/deformation (mm) = plastic work
tendency that hard wheats usually present higher modulus of elas- Wp (J)/plastic area (mm2)
ticity than soft wheats at the same moisture content. In Fig. 5, for example, we present loading and unloading data
Regarding elastic behavior of wheat, in most cases, the initial for wheat kernels. The loading curve passes through the origin.
portion of the curve is approximately nonlinear up to certain lev- The data can be fitted well to the quadratic equation P = c2h +
els of deformation, beyond which it becomes linear (Fig. 4). We c3h2; r2 = 0.999, especially the loading, before reaching the yield
observed that durum wheat is more linear than the soft and bread point (Fig. 5A). Pharr et al (1992) reported that linear unloading
wheats, which showed a small curvature before reaching the yield is observed in metals over most of the unloading range. There are,
point. This means that durum wheat follows the Hookean behav- however, many materials like cereals for which unloading curves
ior better than soft and bread wheats. For ideal elastic materials, are not completely linear (Fig. 5B). However, the experimental
stress is directly proportional to strain according to Hooke’s law. results showed a good approximation to a linear relationship (r2 =
Usually, for other types of material, the Young’s modulus should 0.9957; P < 0.001) between unloading and deformation (Fig. 5B).
be determined from the initial section of the loading stress-strain Pharr et al (1992) investigated the validity of load approxima-
curve at relatively low deformation, at the section before the yield tion to the linearity of different indenters and realized that the
point. However, in wheat kernel samples, that region does not methodology is more universal than generally recognized. In fact,
follow the elastic profile well and it behaves as a plastic material. the equations presented are perfectly valid for any indenter. Thus,
In inorganic materials, it is helpful to calculate Young’s modulus the relationship between the loading and contact area is geometri-
from Equation 1 or to use the slope of the section after the yield cally independent, at least in the selected linear part of the curve,
point of the unloading stress-strain curve. and an analysis used to extract moduli and contact areas using the
slope of the linear part of the loading or unloading curves is not
Viscoelastic Properties of Wheat Kernels limited just to the flat punch geometry. This also means that
Several methods have been suggested for the determination of curved data shown in Fig. 5 is expected because of the curvature
the elastic modulus of small pieces of agricultural materials using and geometry, except for the flat punch. However, in the present
compression tests. The methods are based on the assumptions of case, the spherical or ellipsoidal geometry of the wheat kernel is
Hertz and Boussineseq (Pharr et al 1992; Gubicza et al 1996a,b; substituted for the indenter regular shape.
Wei et al 2001). The test methods include the use of a parallel Various types of continuous tests have come into general use
plate for whole grain, with a spherical indenter and a cylindrical for the determination of mechanical properties of materials. The
indenter, and a parallel plate on core specimens. Despite succes- common feature of these tests is that the applied load is registered
sive improvements, the methods based on the Hertz and Boussi- as a function of indentation depth (deformation herein) during
neseq theory all have problems due to the whole structure of the both the loading and unloading periods (Gubicza et al 1996a,b). A
wheat grain (Haddad et al 1998). Any variability in the form of schematic load-penetration depth curve was reported by several
the grain or the properties induces errors in the measurement of researchers (Pharr et al 1992; Gubicza et al 1996a,b; Tuck et al
the viscoelastic characteristics of the endosperm (Haddad et al 2001) and is shown in Fig. 2.
1998). The effect of moisture on the load-deformation curve of wheat
To overcome these problems, we are proposing to take into ac- is shown in Fig. 6. We observed that wheat with low moisture
count the whole grain and apply the load and displacement tech- content showed high elastic behavior compared with the wheat
Fig. 7. Load vs. deformation curves of wheat types. A, Soft wheat Saturno; B, bread wheat Rayón; C, durum wheat Rafi.
TABLE III
Mean Values for Viscoelastic Components in Wheat Measured in Intact Kernelsa,b
Area of Total Area of Elastic Area of Plastic Area Curve
Cultivar Work (MPa/sec) Work (MPa/sec) Work (MPa/sec) Yield Point (N) Load Time (N/sec)
Saturno 14.74 ± 2.31c 12.30 ± 2.22d 2.44 ± 0.87ab 18.19 ± 0.52b 143.2 ± 19.29d
Salamanca 16.24 ± 2.26bc 13.38 ± 2.17cd 2.86 ± 0.97a 18.81 ± 0.50ab 159.9 ± 19.91cd
Cortazar 17.79 ± 1.40ab 14.99 ± 1.75bc 2.79 ± 1.26a 19.68 ± 0.61a 178.5 ± 9.60cd
Rayón 18.89 ± 1.53a 17.16 ± 1.86ab 1.74 ± 0.74bc 18.21 ± 0.37b 186.5 ± 13.03ab
Altar 19.65 ± 1.26a 19.07 ± 1.25a 0.58 ± 0.23cd 17.95 ± 1.04b 197.0 ± 12.55b
Sofía 18.92 ± 1.98a 18.01 ± 2.15a 0.91 ± 0.44cd 18.17 ± 0.58b 193.5 ± 16.53ab
Rafi 19.68 ± 1.68a 18.71 ± 1.82a 0.98 ± 0.30d 18.21 ± 0.55b 202.4 ± 6.80a
a Measured using uniaxial cell with strain of 0.5 mm and 0.1 mm/sec of deformation velocity.
b Means ± standard deviation followed by the same letter are not significantly different at P ≤ 0.05 (analyzed using Tukey’s test).