determination of mechanical and rheological properties of ... · 37 40 48 53 42 45 50 47 32 50...
TRANSCRIPT
35 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
Determination of Mechanical and Rheological Properties of
Cheese by Indentation
Dr. / Prof. Dharmendra C. Kothari,
Department Chemical Engineering &
Technology, Shri Shivaji Education
Society Amravati’s, College of
Engineering & Technology,
Babhulgaon (Jh.), NH 6, Dist.
AKOLA, M.S. INDIA.
Prof. / Dr. Paul Luckham, Professor of Particle Technology,
Department of Chemical Engineering
and Chemical Technology, Imperial
College, London,
SW7 2BY, UK,
Prof. / Dr. Christopher .J. Lawrence,
Department of Chemical Engineering
and Chemical Technology,
Imperial College, London,
SW7 2BY, UK,
ABSTRACT
The mechanical properties of five commercial cheeses
(Mozzarella, Brie, Shropshire Blue, Red Leicester and
Pecorino Romano) are reported based upon studies
using indentation experimentation involving loading-
unloading, and stress relaxation. The conventional
indentation hardness values ranged from “hard” to
“soft” in the order Pecorino Romano, Red Leicester,
Shropshire Blue, Brie and Mozzarella. The hardness is
universally proportional to the moisture content. The
elastic behaviour is characterised by the elastic modulus,
whereas the elasto-plastic behaviour is presented as a
power law with material index n and consistency k. The
elastic modulus of cheeses were found to be proportional
with the hardness values. The general stress relaxation
response approximately followed a power law viscous
relationship; nt kh , where h is the hardness and t is
lapsed time, and k and n are the intercept and power law
indices over a range of five decades in strain rate. The
values of flow index n are seen to be decreasing with the
hardness, whereas the consistency factor k increases
with the hardness values. However, it was observed that
the stress relaxation analysis appears to be sensitive to
the physical structure of the material.
Keywords: Cheese, Elasto-ViscoPlastic, Indentation,
Cone, Sphere.
1. INTRODUCTION
The process of cheese making is an ancient craft
that dates back thousands of years. By even today’s
standards of industrial technology, the process is
still a complicated one, which combines both “Art”
and “Science”, (Ranken, 1989). Cheese is a very
complex, physical, bio-chemical and
microbiological system. It can be considered as a
composite, or a filled gel, in which fat globules and
empty pockets or holes act as the filler entrapped in
a three-dimensional casein network. In general, the
mechanical properties of filled gels are influenced
by the structure of the network and the shape, size,
volume fraction, and deformability, of the filler
particles, as well as the extent and nature of the
filler interactions with the surrounding network,
(Malin and Tunick, 1995).
Most of the cheese cutting systems are empirically
designed and operated. Many cheeses systems use
technology developed in other and often require
pre-processing to give it required properties. This
added pre-processing is costly and time consuming,
and if not carried out correctly can result in serious
reductions in quality, yield and throughput of cut
product. Recently, effective studies of cheese
cutting with wire is carried out by (Kamyab, et. al.,
1998). To optimized the effective processing of the
cheeses it is essential to study its rheological
properties in which hardness is most important.
Hardness which may be defined in many ways is a
significant characteristic of a cheese, which is
important to both consumers and manufacturers.
Hardness clearly corresponds to a mechanical or
rheological response whose attributes will reflect
plastic flow, elasticity, creep and further processes.
It has long been realized that composition and
manufacturing variables, storage temperature and
time, influence the perceived rheological properties
of a cheese such as its firmness, springiness,
stickiness, crumbliness, greasiness, cohesiveness,
and viscosity. The rheological and fracture
properties of many types of cheese change
significantly during maturing mostly because of
protein hydrolysis (Masi, 1989). Therefore, it is
important for the food industry to have a good
understanding and knowledge of the rheological
properties of cheese and to interactive the subjective
assessment criteria with the successfully defined
mechanical characteristics.
MATERIALS
There are more than 2000 varieties of cheese
available around the world; however they are often
36 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
classified into twelve basic categories. Of these
twelve, three main categories have been selected for
the present rheological studies. Five different
commercial cheeses, Pecorino Romano, Red
Leicester, Somerset Brie, Mozzarella (full fat) and
Shropshire Blue were selected on the basis of their
common texture classifications; “very-hard”,
“hard”, and “soft” as well as their moisture and fat
contents, Table [1]. One blue-veined cheese was
selected for the purpose of investigating the effects
of bacteria upon the rheological properties of
cheese.
The Pecorino Romano is an extremely hard cheese.
It is usually grated before being consumed and it
has a strong aroma. Red Leicester is a hard-pressed
cheese manufactured in a similar way to Cheddar up
to the stage of the handling of the curd. The
maximum scald temperature is 370 C and after whey
drainage, the curd is cut into small blocks and
turned at intervals for approximately 1 hour until
the acidity has reached 0.6%. The curd is then
milled, salted, filled into moulds and pressed. The
ripening period is two to three months. Red
Leicester has an open, flaky texture and a mild
mellow flavour. Its characteristic red colour derives
from the use of annatto. Somerset Brie is a soft,
creamy cheese, with a mild, aromatic flavour and a
close, smooth texture. It is manufactured in such a
way that the Brie is covered with a thin
distinguishable white mould-ripened surface layer.
Mozzarella is a soft, un-ripened plastic curd (pasta
filata) cheese. Mozzarella is well known for its
particular use as a cheese for pizza toppings where
its thermo-plasticity gives a characteristic
“stringiness” on heating. The protein network
within the cheese contributes to its thermoplastic
properties. Mozzarella has a soft, waxy body and a
mildly acid flavour. Shropshire Blue has a porous
texture, which allows air to penetrate into the
cheese and enhance the growth of the Penicillium
roqueforti bacteria.
Name Cheese
Type
Moisture
(%)
Fat
(%)
Pecorino Romano
Red Leicester
Somerset Brie
Mozzarella
Shropshire Blue
Very Hard
Hard
Soft
Soft
Blue-
veined
37
40
48
53
42
45
50
47
32
50
Table [1]: - Classification of the five different
cheeses (Approximate Composition, from Potter
and Hotchkiss, 1996).
Indentation responses of Elasto-Viscoplastic
contact
The objective of this paper is to assess the reliability
and reproducibility of indentation measurements
which may be used to characterise the flow
properties of various cheeses. In order to
adequately characterise the material properties, two
distinctly different protocols were followed and are
described. A schematic representation of the two
approaches and their corresponding methodologies
is illustrated in Figure [1]. This figure illustrates the
various indentation histories that may be imposed
on the cheese specimen, such as creep, relaxation,
and constant load rate or constant displacement rate
(Hill, 1992). In the first method, the material is
indented to a prescribed depth at a constant
penetrating velocity and then the direction of
motion is reversed, without any significant dwell
time; this method is well known as “loading and
unloading” (Johnson, 1970). In the second
procedure, once the indenter has reached the set, it
is left in position to sense the “stress relaxation” of
the specimen. Both of these procedures are the
principle flow forms of displacement-controlled
indentation (Briscoe and Sebastian, 1996).
Fig. [1]:- Diagram of experimental protocols, Load
L or Displacement h against time t.
The indentation method adopted provides a contact
compliance characteristic. The indenter moves into
the surface and the reactive load is sensed. For a
wholly elastic cheese, the loading and unloading
curves are identical and there is no stress relaxation.
Conversely, when the deformation is rigid-perfectly
plastic in nature, there is no elastic recovery in the
unloading curve; there is also no stress relaxation.
The nature of the unloading portion is naturally
governed by elastic properties of the material
although various time dependent components may
be evident (Adams and Briscoe, 1993). The elastic
relaxation component associated with regions
outside the contact zone predominates in the initial
portion of the unloading curve, which is
approximately linear. The elastic contribution is
37 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
manifested towards the final part of the loading
curve, when the surrounding surfaces has released
to the planer to be is usually assumed to be due to
the recovery of the actual deformation zone itself.
As a consequence, neither the depth of penetration
at the maximum load, ht, nor the residual depth of
penetration, hr, shown in Figure [2], provide
directly a means to compute the radius of the
plastically deformed contact region from the
compliance curves.
Figure [2]: - Schematic diagram of the contact
compliance curve: reaction force vs imposed
displacement.
The hardness (plastic component), H, is commonly
defined as
2a
L
A
LH
(1)
where L is the reaction force, A is the contact area,
projected onto the original surface, and a is the
corresponding radius for axially symmetric
indentations. The actual contact radius is
distinguished from the apparent radius of contact,
which corresponds to the value computed from the
total depth of penetration, ht. The means of
computing the hardness for various geometries is
discussed later.
The reduced elastic modulus, E*, is conventionally
obtained from the elastic contact stiffness of the
initial part of the unloading curve, Figure [2];
aESh
L *2
(2)
where )1( 2
*
EE , E is the Young’s modulus,
is Poisson’s ratio and S is the contact stiffness
upon unloading at the maximum penetration depth,
ht.
Evaluation of hp
A means of obtaining the plastic component of the
indentation depth hp, derived to compute the
hardness, H, is to extrapolate the initial linear
unloading portion of the load-displacement curve to
the zero-load axis as shown in Figure [2]. This
method was derived based upon the assumption that
the elastic deformation of the indented material
around the indent may be modelled as that
corresponding to the elastic indentation by an
equivalent cylindrical punch, having an identical
contact radius to that of the imposed indentation.
The computation is invariably subjective. A more
effective procedure for obtaining the value of hp
from the unloading curve is the adoption of an
appropriate curve-fitting method for the
experimental compliance data in order to compute
the intercept, hp.
The Box-Cox transformation method has the
advantages for its purposed and h is described in
detail by Briscoe and Sebastian (1996). The curve
fitting method adopted is of the form;
nhh kL )( 0 (3)
where h0 is the particular zero offset, k is a
coefficient and n is the characteristic load index.
For the loading curve, the equation can be
expressed as
1)( 011
nhhkL (3a)
where subscript 1 indicates loading.
For the unloading curve, the equation can be
expressed as;
2)(22
n
rhhkL (3b)
where subscript 2 indicates unloading.
The computed values of h0 and hr provide the
required numerical values of the zero points for the
loading and unloading curves of the indentation.
The magnitude of the parameter k depends upon the
material properties and also upon the actual indenter
geometry. The value of the index n depends upon
the mode of deformation and also upon the
geometry of the indenter. The value of n2 can be
evaluated by a simple linear regression of log (L) as
a function of log (h-hr). Differentiation of equation
(3b), substitution for Lt, and the simultaneous
solution of the resulting equation relationship with
equation (3b) give;
2nhh
hh
pt
rt
(4)
Contact radius
The computed contact radius is used to evaluate the
hardness of the material, as represented in Figure
[3], in which the cone indentation is represented in
Figure [3a] and the sphere in Figure [3b]. From a
38 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
consideration of the geometry of the indenter used,
the contact radius is given approximately:
Fig. [3a]:-The CONE
indenter geometry.
Fig. [3b]: - The
SPHERE indenter
geometry.
Figure [3]: - Schematic diagram of the indenter
geometries. No surface relaxation on material
displacement is indicated.
for the cone, as: a = h tan (5)
and for the sphere as: a = 22 hRh (6)
where is the semi-included angle of the cone, R is
the radius of the sphere and h is the depth of
indentation, which can be represented as h = V (t-
t0), V is the penetration velocity, t0 is the time zero
offset and (t-t0) is the apparent time of the contact
between the indenter and the specimen. The contact
radius given by (5) and (6) does not account for the
“pile-up” or “sinking-in” of the deformed material
around the impression. To evaluate stress relaxation
the constant value of a corresponds to the last point
of loading, where the loading curve transfers to the
relaxation curve.
Plasticity index
A plasticity index, , is a parameter which
characterises the relative plastic and elastic
behaviour of the material under the action of
prescribed external strains. In the case of
indentation, the plasticity index can be usefully
expressed as the ratio of the elastic component of
the work done to the plastic component of the work
done, (Bower et. al, 1993). Using the parametric
relationship for the loading curves, the plasticity
index can be approximated in terms of the hardness
and the reduced elastic modulus.
H
E*
tan (7)
where is the angle of inclination of the indenter to
the sample surface and E* is again the reduced
elastic modulus. The effective contact strain is taken
as 0.2 tan (Briscoe and Sebastian, 1996).
For the cones the angle is not a function of depth
for large penetrations, the indentations are said to be
“self similar”. In the case of the sphere the
corresponding angle decreases with the depth of the
penetration; at a given depth, h, the strain in the h/R,
where R is the spheres values. Thus the effective
strains are constant for cone ~ 0.2 tan and are
typically ~ 0.35 for the sphere.
Stress Relaxation
An elasto-viscoplastic model for indentation is
shown in Figure [4], which comprise of the
conventional elastic and plastic descriptors. The
first term on the right-hand side of the equation
(Figure 4) represents the elastic component of the
strain, which responds instantaneously to the
applied stress, whilst the second term expresses the
viscous component, which depends on the duration
of the stress.
Figure [4]:- Schematic representation of a non-
linear Maxwell model for elasto-viscoplastic
materials.
If the stress is removed after some time, the spring,
no longer constrained, returns to its original length
immediately, but that part of the displacement due
to the dashpot creep remains. Extensive work has
been performed to characterise both the elastic and
viscous properties of soft-solid materials, using a
simple wedge-indentation stress relaxation method,
by Lawrence et. al, (1998).
In a general case, it is expected that the imposed
strain and strain rate will induce both elastic and
plastic contributions to the deformation, in different
proportions throughout the material. As long as a
material is uniform, it can be expected that the
nominal stress, , is related to some nominal strain
rate .
by a simple relationship.
)(
FCP . (8)
where CP is the plastic constraint factor ( a term to
include geometric factors and interface friction) and
F is a non-linear material function.
Similarly, for an essentially elastic response to
indentation, the nominal stress would be related to
some nominal strain by a simple relationship.
39 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
*ECE (9)
where CE is the elastic constraint factor which also,
like CP, embodies geometrical and frictional effects,
E* is an effective elastic modulus.
It is supposed that, during the indentation phase, the
elastic component of the strain is small, so that an
approximate relationship for the mean indentation
pressure is obtained as:
a
V FC
A
LP (10)
where V is the indentation velocity.
However, during the relaxation phase, the elastic
stress is equally important, and a relationship for the
indentation pressure is given as:
*
.
EC A
P FC
A
L
E
P (11)
where L is the load registered, and
.
L is the rate
of relaxation of the load. The equation (11) provides
quantitative values of the power law index q and the
intercept k, (Holdsworth, 1993).
q Lk
.
(12)
Equation (9) will be used in the stress relaxation
analysis in order to characterise elastic properties.
By the form of equations (10) and (11), it is noted
that plotting the mean indentation pressure against
nominal strain rate for the indentation phase, all the
different loading curves for a given material should,
in principle, collapse into a single master curve.
Similarly, a plot of the indentation pressure against
the rate of decrease of the load in the relaxation
curves phase for all different velocity curves should
also collapse upon a single master curve.
Furthermore the two master curves should have the
same shape. Subsequently, by choosing an
appropriate value of CEE*, the two sets of data may
be combined to give an overall single master curve.
The flow consistency and the material index are
then obtained from the equation of the master curve.
EXPERIMENTS
Sample Preparation
All the cheeses were removed from their
packages just before the experiment. In order to
prevent significant drying and consequent
rheological changes, once a cheese was un-
wrapped, the experiments were carried out within a
period of two hours. All the cheeses were cut into
blocks of 150 mm length, by 70 mm width by 70
mm height. The ambient temperature was in the
range 20-240C.
Figure [5]:- Schematic diagram of the experimental
set-up.
Description of the Apparatus Used
The principal device used was a standard universal-
testing machine (Instron 1122, Instron Ltd. High
Wycombe, UK), equipped with a 50N transducer
(bottom load cell) of accuracy 0.01N. A schematic
diagram of the experimental arrangement is shown
in Figure [5].
The instrument incorporates an electronic data
collection system with load cells detecting the load
applied to the specimen. Two geometries of
indenter were used: a stainless steel cone of
included angle 90o and a sphere of diameter 12.7
mm (1/2”). The specimens were supported on the
bottom platform. The machine was configured to
operate at constant indentation speeds of 2, 5, 10, 50
and 100 mm/min up to a prescribed depth of 5 mm,
i.e. the experiments were displacement controlled.
The reaction load was recorded at suitable intervals
automatically using analogue sensors. Force and
corresponding time data were recorded
simultaneously by a host computer, via a terminal
panel T31 (analogue to digital converter) connected
to the Instron interface.
Description of the Experimental Procedure
In a representative experiment the load cell output
was zeroed with the sample on the platform and the
indenter was brought to the sample surface by
moving the crosshead. Then, the required
indentation speed was set, and the indenter was
moved into the material at the chosen constant
speed. The displacement may be deduced from the
speed and lapsed time data. However, a separate
40 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
LVDT (linear variable displacement transducer)
was used to measure the imposed displacement.
The data acquisition rate was adjusted according to
the values of the imposed nominal strain rate.
RESULTS AND DISCUSSION
The indentation experiments were carried out on the
five chosen cheeses with two protocols i.e. loading-
unloading and loading-stress relaxation;
Loading and Unloading
The initial data were obtained in the form of time
series of load, and the corresponding displacement.
Figure [6] shows typical examples of loading and
unloading curves, where the total load (N) for the
constant depth is plotted against the indentation
displacement (mm) for a Red Leicester using
conical (Figure [6a]) and spherical (Figure [6b])
indenters at five different penetration velocities.
(6a): - For 900 cone
Indenter.
(6b) :- For ½” sphere
Indenter.
Figure [6] :- Loading-unloading curves of load
against displacement load for several indenter
speeds for Red Leicester Cheese.
The curves indicate that there is a little elastic
recovery of the material during unloading, which
tends to increase as the indentation rate is increased.
However, there is a significant energy loss and
permanent deformation during the indentation
cycle. The general trends for the other cheeses were
similar. All the compliance curves obtained
indicate, as expected, that the maximum indentation
force is much higher when using a spherical
indenter; because the contact area is larger. The
curves showed that Mozzarella was the most elastic
material of the set, with the least amount of plastic
deformation. The Pecorino Romano was the
hardest, with the highest indentation forces.
The parameters of the fitting curves
The Box-Cox transformation method was adopted
for the analysis of the unloading curves. A simple
linear regression of log (L) against log (h-hr) was
used to evaluate the parameter n2 (subscript 2
represents the unloading phase). Table [2] shows
the n2 values obtained from the fitted curves for all
the cheeses under both geometries of indenter. The
values of n2, for both geometric forms of indenter,
are generally less than 2. The results reflect the
relative insensitivity of the unloading curve to the
indenter geometry but values of the parameters are
dependent on the indenting speed. There may be
two reasons for the variation in the values of n2. The
determination of the residual depth of penetration hr
is subject to experimental uncertainties, and the set
depth of penetration was not reached exactly; both
influence the curve fitting. The latter was more
evident at higher indention speeds. These two
factors would have a significant effect on the values
of n2. The theoretically expected n2 values for the
case of purely elastic deformation are 1.5 and 2 for
a spherical and conical indenter respectively.
Hence from the values of n2, it can be concluded
that the deformation of all the cheeses was not
perfectly elastic, but a combination of elastic and
plastic.
Table [2]: - Parameter (n2) of fitted curves for
unloading.
Velocity Mozzarella. Brie Shrop. Blue Red Leicester Pecorino
mm/min
Cone Sphere Cone Sphe
re Cone
Sphere
Con
e
Sphere
Cone Sphe
re
2 0.44 0.57 0.36 0.65 0.30 0.61 0.86 0.54 0.69 0.76
5 0.47 0.65 0.81 0.79 0.56 0.44 0.63 0.44 0.75 0.61
10 0.42 0.36 0.69 0.87 0.54 0.37 0.75 0.55 0.70 0.49
50 0.71 0.65 0.86 0.53 0.55 0.39 0.84 0.55 0.70 0.96
100 1.54 1.53 1.27 1.68 1.82 0.60 1.82 1.47 2.96 1.66
The values of hp were evaluated using equation (4),
and are listed Table [3]. The results indicate an
obvious decreasing trend of hp with the increase of
the indentation rate. In other words, there is more
elastic recovery of the materials at the higher
indenting speeds. Such a trend is verified by the
nature of the loading and unloading curves.
Table [3]: - Values of hp, (mm). Velocity Mozzarella. Brie Shrop. Blue Red Leicester Pecorino
mm/min Cone
Sphere
Cone
Sphere
Cone
Sphere
Con
e
Sphere
Cone
Sphere
2 3.40 3.46 3.80 3.72 4.18 3.99 4.19 3.40 4.09 3.74
5 3.29 3.73 3.40 3.20 4.16 3.77 3.97 3.19 4.12 3.48
10 2.92 2.72 3.33 3.18 4.00 3.82 3.97 3.10 4.06 3.44
50 2.97 2.59 2.78 3.51 3.81 3.74 3.89 2.93 3.71 3.25
100 2.91 2.38 2.88 3.10 3.78 2.90 3.66 3.11 3.57 3.15
The difference in hp values between the indenters is
mainly due to their geometric differences. The
computed values of hp also confirm that Mozzarella
is the most elastic of the cheeses, as it has the
smallest amount of permanent plastic deformation.
41 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
Table [4]: - Computed values of mechanical
properties of cheeses using conical and spherical
indenters average of the five velocities. Cheese M.P. Mozzarell
a. Brie
Shrop.
Blue
Red
Leicester Pecorino
For 900 Conical Indenter
Elastic
Modulus,
MPa
0.334 0.149 0.842 1.227 1.313
Stiffness
MN/m
0.004 0.019 0.106 0.166 0.167
Plasticity
Index
0.5 0.7 0.9 0.8 0.8
Hardness,
MPa
0.009 0.026 0.134 0.222 0.227
For ½” Spherical Indenter
Elastic
Modulus MPa
0.058 0.297 1.135 1.327 1.462
Stiffness,
MN/m
0.089 0.484 0.182 0.141 0.242
Plasticity
Index
0.7 0.7 0.5 0.6 0.7
Hardness
MPa
0.0124 0.0574 0.0789 0.201 0.263
Hardness
The computed mean hardness values of all the
cheeses, obtained using both indenters, are
summarised in Table [4]. The variation in hardness
with speed is relatively small, as seen in Figure [6].
The result also reflects that the hardness is inversely
proportional to the moisture content of cheese,
which agrees with the general consensus; the higher
the moisture content, the softer the cheese. The
discrepancy in the hardness values measured by the
cone and sphere is mainly due to deflections with
imposed effective contact strain; see earlier.
Elastic Modulus
The elastic modulus is calculated according to
equation (2) and associated procedures. The
stiffness is computed from the slope of the
unloading curve, using the equation
SP
h h
t
t p
.
By definition, a material is said to be stiff when a
large force is required to produce a small strain;
Table [4]. The Poisson’s ratio was taken to be 0.45
for all the cheeses for the purpose of calculating the
Elastic modulus.
The value of the elastic modulus for different
indentation velocities for all the cheeses indicates
that there is a slight increase in the value with
indentation speed for the spherical indenter. This
variation indicates either that the strain imposed on
the cheese is dependent on the indentation rate, or a
degree of inaccuracy of the computed values at
higher speed. A more significant variation in the
computed values for the conical indenter is a
reflection of the difficulty of accurately specifying
the parameters required to define the slope at
unloading, as well as the corresponding values of
the contact area.
Loading and Relaxation
The relaxation response was observed by holding
the indenter within the sample for a period of 400
seconds after the set depth of 5 mm was reached. In
contrast to a typical loading and unloading curve,
Figure [7] shows a gradual elastic-plastic relaxation.
There are three aspects about the general shape of
the stress relaxation curve, which are worthy of
mention. First, as can be seen in the Figure [7], the
load raises during the indentation phase until the
prescribed depth is reached.
[7a]:- For a 900 cone
indenter.
[7b]:- For a ½” sphere
indenter.
Figure [7]:- Loading and relaxation curves for Red
Leicester, Using two indenters at 5 different speeds.
The curve is slightly concave for the cone
indentation and convex for the sphere indentation.
This is mainly due to the way in which the contact
radius changes with time. As was noted earlier, the
indentation load is proportional to the contact area
of an indenter. Secondly, during the relaxation
phase, when the loading motion ceases, the
indentation load falls rapidly at first, followed by a
long gradually decaying tail. This relaxation phase
indicates that the reaction to the load is partly
elastic and partly viscoplastic. The ratio of the
elastic and viscoplastic components depends on the
time-scale of the measurement.
The data of load and displacement were analysed
using equation (10) for the loading period and (11)
for the relaxation data. According to equation (10),
plots of the mean indentation pressure (nominal
stress) against nominal strain rate for different
speeds should collapse to a single master curve,
where strain rate is defined as the argument of the
function F. Similarly, by an inspection of equation
(11) the mean indentation pressure in the relaxation
phase is a function of the rate of decrease of the
load. First, the time dependent response was
42 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
characterized by examining the relaxation behavior.
A typical result for the relaxation phase is plotted in
Figure [8] as the mean stress (MPa) against the
unloading rate (N/s) on log-log axes.
[8a]: - For 900 cone
indenter.
[8b]:- For ½” sphere
indenter.
Figure [8]:- Mean indentation pressure vs. load
relaxation rate for Red Leister, using two indenters
at 5 different speeds.
The various curves are seen to lie closely to each
other. It can therefore be concluded that all the
curves collapse onto a single master curve and the
trend of this master curve obeys a power law
relationship. The relationship is fitted
approximately, over three decades of strain rate,
using 19.0q for cone and 17.0q for the
sphere. Since the form of the function F must be the
same for the loading phase as well as for the
relaxation phase, the slope of the trend line in
Figure [8] was used to estimate an approximate
value of t0, which accounts for an arbitrary zero
offset in the time variable in the loading phase.
This term was incorporated into the time data for
equation (10). The t0 values were chosen separately
for each indentation speed to give the best fit of all
the curves to a single master curve. Figure [9] is a
plot of indentation pressure (MPa) against the
nominal strain rate (1/s) for Red Leicester on log-
log axes.
[9a]:- For 900 cone
indenter.
[9b]:- For ½” sphere
indenter.
Figure [9] :- Mean indentation pressure vs. strain
rate for Red Leicester, using two indenters at five
different speeds.
As is evident in Figure [9], the data collapse better
for the cone than for the sphere, and for larger
indentation depths (lower stress and strain rate). A
power trend was fitted to these data to represent the
single master curve. The value of the consistency k
was obtained from the equation of the trend line, as
the plastic flow intercept; k = 0.33 MPa.sn for the
cone and k = 0.05 MPa. sn.
Table [5]: - Results of stress relaxation experiment. Cheese
Selections
Sphere Cone Spher
e
Cone Sphere Cone
q K (MPa.sn) CEE (MPa)
Mozzaller
a
0.289 0.278 0.05 0.22 0.007 0.096
Somerset
Brie
0.186 0.247 0.10 0.40 0.075 0.051
Shropshire
Blue
0.163 0.211 0.03 0.13 0.155 0.089
Red
Leicester
0.166 0.192 0.05 0.33 0.080 0.036
Pecorino
Romano
0.182 0.184 0.09 0.43 0.170 0.159
The result of the stress relaxation analysis for Red
Leicester indicates that the power law relationship
is a sufficient description over the entire
experimental strain rate range of five decades; as is
shown in Figure [10]. It also confirms that the
assumption that n is reasonably constant over the
investigated range is valid. On the whole, the value
of n decreases with the hardness of the cheese;
while the value of k, on the other hand, increases
with the hardness. Thus both the n and k are related
to the hardness of the material.
[10a]:- For 900 cone
indenter.
[10b]:- For ½” Sphere
indenter.
Figure [10]:- Combined plot of data from
indentation and relaxation for Red Leicester, using
two indenters at five different speeds.
The forms of equation (10) and (11) both show the
shape of the viscosity function F. Choosing an
appropriate value of CEE, which is incorporated in
the relaxation equation, the various loading and
relaxation data may be combined as is shown in
Figure [10]. The values for red leicester and the
product of the elastic modulus and elastic constraint
factor was evaluated to be 0.106 MPa for sphere
and 0.044 for cone indenter. Values of the material
index and CEE for all the cheeses are tabulated in
Table [5].
43 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
5. CONCLUSIONS
The various protocols for indentation studies, such
as loading and unloading and stress relaxation, were
investigated to characterise the elastic and
viscoplastic properties of several cheeses. The order
of cheese from the softest to the hardest was found
to be; Mozzarella, Brie, Shropshire Blue, Red
Leicester and Pecorino Romano. We have carried
out similar studies on Feta, Edam, Stilton, Chedder,
and Cheshire, and obtained similar results. The
computed values of hardness indicate that the
hardness of a cheese is dependent upon its moisture
content. The higher the moisture content is, the
softer is the cheese.
The Box-Cox transformation method provides the
hardness and the elastic properties from the
compliance data, as it eliminates some of the
ambiguity in selecting the linear portion of the
unloading curves for the usual graphical
extrapolation. It was noted that the values of
contact radius and the actual value of the set depth
reached played a significant part in determining the
computed results.
The stress relaxation analysis provides a means of
computing elastic properties of these elasto-
viscoplastic materials since it takes the inherent
large strain and strain rate of the material into
account. The elastic behaviour of a material is
characterised by the elastic modulus, whereas the
elasto-plastic behaviour is presented as a power law
with material index q and consistency k which are
the power law relationship parameters. All of the
cheeses were found to follow the power law
relationship over a range of five decades in strain
rate. The values of q decrease in an order with the
hardness of cheese, on the other hand the values of
k increase with the hardness. However, it was
observed that the stress relaxation analysis appears
to be sensitive to the physical structure of a
material. For instance, Shropshire Blue, which has a
porous structure, does not respond well to the
analysis because the cheese showed signs of
cracking; and “pile-up” effects were also noticed
during the indentation phase. As a result, a
significant discontinuity of the strain rate was seen
when combining the indentation and relaxation data
together.
NOMENCLATURE
A
a
nominal contact area
contact radius
CP
CE
D
E
E*
plastic consistency
elastic consistency
indenter diameters
Modulus of Elasticity
reduced elastic modulus
F
hE
h
h0
hp
hr
ht
H
function
elastic indentation depth or displacement
indentation depth, displacement
zero offset
plastic penetration depth
residual depth of penetration
penetration at maximum load
hardness
k
n
L
flow consistency or the flow intercept
flow index
Indentation load
R
S
t
t0
V
radius of spherical indenter
contact stiffness
time
zero offset
indentation velocity
poisson’s ratio
cone semi angle
stress
y yield stress
plasticity index
.
strain rate
strain
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44 Dr. / Prof. Dharmendra C. Kothari, Prof. / Dr. Paul Luckham, Prof. / Dr. Christopher .J. Lawrence
International Journal of Computer & Mathematical Sciences
IJCMS
ISSN 2347 – 8527
Volume 5, Issue 4
April 2016
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