Study of the changes in Mechanical Properties (Texture) of Biscuit

by the sorption of Moisture at different ERH

Kshitij Shrestha1*, Prof. Dr. Dilip Subba2
1
Food Research Officer, Department of Food Technology and Quality Control, HMG/Nepal
2
Assistant Dean, Central Campus of Technology, Dharan, Nepal

Abstract
The study was carried out to study the changes in Mechanical properties (texture) of biscuit by the sorption of
moisture at different ERH(Equilibrium Relative Humidity). The biscuit samples were kept at the ERH of 10, 20, 25, 30,
35, 40, 45, 50, 60 and 75% and stored at room temperature (Avg. 25 oC) until equilibrium is achieved. Then, the samples
were analysed for the Mechanical properties (Breaking force, Elasticity, and Maximum deformation) using Force-
deformation measuring Instrument.
The break and shift was observed in sorption curve in between 35% and 40% ERH and found to be correlated
with the phase transition of sucrose from amorphous (glassy) to crystalline state. The BET monolayer value was
calculated to be 4.77 %. The Mechanical properties (texture) of biscuit were found to be affected significantly by the
phase transition of sucrose. It was observed that crispy and brittle characteristics of the biscuit retain only if sucrose
remains in glassy state but if phase transition of sucrose from glassy to viscous liquid (i.e. rubber) and to crystalline
phase occurs then, there will be corresponding significant change in the mechanical properties of biscuit, which
contribute to the kinaesthetic sensation perceived during eating. It was also concluded that 6 % moisture level was
adequate to control the changes in texture of biscuit.

Key words: - ERH (Equilibrium Relative Humidity), Breaking force, Elasticity, Deformation, EMC (Equilibrium
Moisture Content), Glass transition

Introduction
Water is the most abundant individual constituent in the majority of food. The amount of
water present in many foods can vary over a limited range without causing much apparent
alteration in the product itself. For example, some biscuit can absorb 2 % more moisture than that
presents when they are freshly baked, and consumer would not be able to detect a difference.
However, a distinct lowering of quality would have been noticed above this level (Paine & Paine,
1983). Therefore, it requires defining critical moisture content for a product to be satisfactory to the
consumer. The importance of study of sorption characteristics of biscuit can be seen from the fact
that the most important deterioration index for biscuit is “Moisture changes” and only then
“Oxidative changes” and “Physical damage” comes (Paine & Paine, 1983).
The reason for the moisture change to be most important deterioration index is its direct
influence on the texture of biscuit. Texture is an important aspect of food quality, sometime even
more important than flavour and colour, for example, in the case of biscuit, a crisp and dry food.
Texture is most important in bland foods and foods that are crunchy and crispy (Rangana, 2000).
Subjective evaluation of texture could also be made. The technique, however, is time
consuming, requires considerable trained personnel and may not always be useful in the
standardization of texture of foods. Consequently, objective methods have been made use, to
provide efficient and precise quantitative prescription (Rangana, 2000). The mechanical parameters
that correlate with sensory crispiness are resistance of a food to deformation measured as the slope
of force deformation curve, (Bourne et al., 1966; Iles and Elson, 1972; Brennan et al., 1974) and
also with deformation to fracture (Iles and Elson, 1972; Brennan et al., 1974).Bend deformation to
fracture, a measure of brittleness has also been shown to correlate with sensory crispiness (Iles and
Elson; 1972). It also is an integrated parameter. This Rheological parameter provides excellent
indicators of Crispiness and Crunchiness for a single product type (Vickers, 1979). Consumer
assessment of texture involves large deformation, so obviously measurements of this type are more
likely to correlate with perceived texture than the results of experiments involving small
deformations. As an example, consumer assessment of the hardness of gels correlated with the
rupture strength rather than the elastic modulus. Plastic materials don not have a well-defined
rupture point but brittle material have well-defined rupture points (Mitchell, 1984).
The work was carried out to study the sorption characteristics of the biscuit so as to study
the effect of moisture and ERH on the different mechanical properties (texture) of biscuit.

1
Materials and Methods
Sample
The biscuit chosen for the study was the Glucose Biscuit (soft dough) obtained from the
local market.

Study of sorption behaviour of biscuit

For the determination of Equilibrium moisture content, Wink's weight Equilibrium method,
as described by Rangana (2000) was followed.

Study of mechanical properties of biscuits

For the study of mechanical properties, a simple instrument was designed. The important
part of the arrangement was the measurement of force and corresponding measurement of
deformation of the material. Mitchell (1984) observed that both the stress and strain at rupture
depend on the rate of deformation. So, to keep the constant rate of stress, constant water flow rate
was maintained and stored in water holding bin as source of force. The balance tank was used to
keep the constant level of water by over-flowing the excess water. The height of water level to the
level of output nozzle (h) was adjusted and kept constant so as to keep constant water output rate
(5ml/sec). Timer was used to measure the time as an index of water deposited in the water holding
bin i.e. force being directly applied to the biscuit. For the measurement of deformation, a needle
was connected to the moving prove. The adjustment was done in such a way that small deformation
was magnified linearly, as shown in figure 1.
Force due to weight of water
C
Actual deformation O B
A Observed
Deformation
Biscuit
D

Fig. 1. Experimental arrangement for measurement of actual deformation

From figure 1 we can write

AC = AO = K (Constant)
BD BO
So, AC = K × BD
i.e. Actual deformation = K × Observed deformation
The value for the designed instrument was calculated to be 0.097.

The Force acting on biscuit at any instant is given by

Force (N) = Time (t) × Rate of water flow (R) × acceleration due to gravity (g)

For each sample of different humidity, at least 10 biscuits were tested for mechanical
properties. The graph was drawn between force and deformation for each reading and the slope of
the first straight portion was taken by linear regression on computer for the computation of
elasticity.

Chemical Analysis
Analytical procedures were carried out as per Rangana (2000) and AOAC (1975). All the
moisture content data are expressed in dry basis.

Statistical analysis
Statistical analyses were carried out using Genstat 5 Release 3.2 software, Lawes
Agricultural Trust (Rothamsted Experimental Station).

2
Results and discussion
The sorption curve of Biscuit
After the attainment of equilibrium (wt. variation of <1mg), Moisture content of each sample was
determined. The observed results are tabulated below:

Table.2. Equilibrium moisture content of Biscuit at room temperature (avg. 25oC)

Relative Humidity Equilibrium Moisture Content aw
(%) (%d.b.) X (1 - aw)
10 3.27 0.034
20 4.52 0.055
25 5.13 0.065
30 5.88 0.073
35 6.86 0.079
40 6.99 0.095
45 8.06 0.102
50 8.48 0.118
60 10.87 0.138
75 17.34 0.170

The observed sorption curve is shown in figure 2.

20

18
Equilibrium Moisture Content (%)

16

14 Sucrose Crystallization
12

10

4
Crystalline state of Sucrose
2 Glassy State of Sucrose

0
0 10 20 30 40 50 60 70 80
Equilibrium Relative Humidity (%)

Fig.2 Sorption curve of Biscuit

The graph shows linear increment in the moisture content with the RH in the region of 10
to 30%. The moisture content of 5.88% was found to be critical moisture content, the ERH of
which corresponds to 30%. This is because, above this level, a higher rate of uptake of moisture
with slight increment of RH occurs and enters into a very significant portion of graph, which is
break and shift in the sorption curve in between 35 and 40% ERH. At this point, moisture content
has decreased slightly and again started to increase with increasing ERH.
The break and shift obtained was compared with the sorption behaviour of sucrose. This
observation was related to the phase change in the sucrose molecule from amorphous to crystalline
structure i.e. crystallization of sucrose (Karel, 1993). During baking, the drying rate is such a high
that sugar can’t crystallize and remain as amorphous structure (Peleg & Bagley, 1999). Karel
(1993) also observed similar results. He observed that sucrose crystallization occurs in 2 days at
35% RH, whereas it takes 100 days to crystallize at 30 % RH, during which it releases moisture.
The moisture content of crystalline sugar is below 0.5%.

3
Fitting of BET equation
0.18

0.16
y = 0.2097x + 0.0111
0.14 R2 = 0.9959
0.12
aw/x(1-aw)

0.10

0.08

0.06

0.04

0.02

0.00
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Water Activity

Fig.3. Fitting of BET Equation for Biscuit

The observed data were analysed for fitting of BET equation. A very good fitting of
equation over wide range of ERH was found (Corr. Coeff. of 0.9976).

The observed BET equation is aw = 0.0111+ 0.2095 aw

X (1 - aw)
From calculation, the BET monolayer value was observed to be 4.77%. This is the most
stable moisture content. Similar monolayer values for biscuit were also observed by Rahman and
Labuza (1999).

Chemical composétion
The biscuit under observation was the soft dough glucose biscuit i.e. high sugar high fat
biscuit. The chemical composition of Biscuit was carried out. The chemical composition was
within the range of soft dough glucose biscuit. The results obtained are tabulated below:

Table.1. Chemical composition of biscuit (Glucose) under study

Parameters Observed Value
Moisture Content 4.7 %
Fat Content 12.1 %
Sucrose Content 23.3 %
Protein Content 8.2 %
Ash Content 0.9 %

Effect of ERH (and EMC) on Mechanical Properties of Biscuit

Kase (1953) observed that even when measurements are made at a constant rate of strain, rupture
strength are much less reproducible than small deformation parameters because failure takes place
as a defect in the sample and the number and extent of such defect varies considerably from sample
to sample. The distribution of rupture strength is represented by a double exponential frequency
distribution function. Its integral form is following

σ b (n) = σ b + S ln –ln( n – 0.5 )

N
Where, σ b (n) = Stress or strain at rupture of the nth sample. When N samples are ranked in order
of decreasing magnitude.

4
σ b = Mode (Most Probable Value) of the distribution
S = Standard Deviation of the distribution.
Both these parameters can be obtained from a plot of ln –ln ( n – 0.5 ) against σ b (n).
(Kase, 1953). N
Hence, using the Kase’s equation, the modal values of breaking force and maximum
deformation was calculated and used for the comparison purposes. The modal values as given by
Kase’s equation from the ten observations from each sample of different ERH were calculated. The
observed result is presented below:

Table. Effect of ERH and EMC on different Mechanical Parameters

ERH Moisture Breaking force Mean value Maximum deformation
(%) content (gm) of Elasticity (mm)
(%) Modal Mean (dyne cm-2) Modal Mean
value Value
10 3.27 1540 1492.5±102.1a (13.0±0.75)×107a 5.78 5.6±0.37a
b
20 4.52 1327 1298.0±66.7 (11.3±0.36)×107b 5.81 5.6±0.49a
c
25 5.13 1223 1175.5±102.0 (10.2±0.66)×107c 6.10 5.8±0.68a
d
30 5.88 1142 1098.5±92.9 (5.67±0.40)×107d 9.69 9.0±1.41b
e
35 6.86 752 720.5±67.6 (1.87±0.16)×107e 19.23 18.4±1.62c
e
40 6.99 747 717.5±61.8 (2.31±0.13)×107e 20.22 19.0±2.76c
f
45 8.06 500 472.5±61.2 (1.21±0.18)×107f 31.25 29.6±3.50d
50 8.48 389 363.0±58.0g (0.97±0.07)×107f 34.79 33.6±2.42e

Dimensions: Biscuit breadth 2.87cm, thickness 0.64cm and distance between supporting edges 3cm
Note: Values in column with different superscripts differ significantly at 5% level of significance

Effect on breaking force

The breaking force was found to decrease linearly with the moisture content and also with
ERH up to moisture content of 5.88% i.e. ERH of 30% with very high correlation coefficient
(>0.99). This shows that breaking force can be a good indicator of the moisture content of the
biscuit. From the Regression analysis, the straight line equation of breaking force obtained were
tabulated below:

Table .4. Linear Regression analysis of graph of breaking force with EMC and ERH
Relation of breaking Range Equation Regression coeff.
force with (r)
Moisture Content 3.27 to 5.88% y = -155.31 x + 2038 - 0.995
” 6.86 to 8.48% y = - 225.62 x +2309.5 -0.998
Equilibrium RH 10 to 30% y = -20.137 x + 1735.9 - 0.998
” 40 to 75% y = -35.2 x + 2127.3 -0.977
The dependable variable y is for breaking force, and x is corresponding independent variable.

The ANOVA analysis of the breaking force data of different ERH indicated that they were
significantly different from each other (p>0.05). The l.s.d showed that only data obtained for ERH
of 35 and 40% were not significantly different from each other, at 5 % level of significance
(p<0.05).
From the comparison of the straight lines of two different ranges of moisture content in
above table, it was observed that slope of second line was greater than that of first line, indicating
the more prominent effect of moisture in second stage.
The graph indicated a drastic variation in the breaking force in between ERH of 30 to 40%,
where the sucrose crystallization had taken place.

5
 18 4

Max. Deformation (mm)

16 3.5

14
Breaking force (x100 gm) and

3
Elasticity (x10 dyne cm )

12
-2

Glass transition region for sucrose 2.5

10 Sucrose Crystallization
2
7

8
1.5
6
1
4
Crystalline state
2 of sucrose 0.5
Glassy state of sucrose

0 0
0 10 20 30 40 50 60
ERH (%)

Breaking Force Elasticity Max. Deformation

Fig.4. Effect of ERH on mechanical properties of biscuit

18 4

16 3.5

Max. Deformation (mm)

14
Breaking force (x100gm) and

3
Elasticity (x107 dyne cm-2 )

12
Glass transition region for sucrose 2.5
10
Sucrose crystallization
2
8
1.5
6

1
4 Crystalline
state of sucrose
2 Glassy state of sucrose 0.5

0 0
3 4 5 6 7 8 9
EMC (% d.b.)

Breaking Force Elasticity Max. Deformation

Fig.5. Effect of EMC on mechanical properties of biscuit

6
Effect on Elasticity
It was observed that elasticity doesn’t follow the straight-line function with both moisture
content and ERH. Elasticity was found to decrease very slowly at first, up to the moisture content
of 5.13% i.e. ERH of 25%. Above this, elasticity was found to decrease at a very high rate, linearly
and steeply. The decrease in elasticity is the result of the plasticizing effect of water, the more the
moisture content more plastic the material will be. It can be seen clearly in the graph.
In the region of 10% to 35% ERH, ANOVA analysis showed significant difference between
different observation (p>0.05) with coeff. of variation below 8.89%.Above this region, the ANOVA
analysis showed no significant difference in the observation of 35% and 40% ERH, and again that
of 40% and 45% ERH (p<0.05). This indicates the plateau region, called rubbery plateau, which
can be observed in graph.
Literature shows that elasticity is a good measure of crispiness characteristics of the crispy
material. For a material to be crispy, it must have the certain degree of elasticity with brittle failure
(Jowitt, 1979). It indicates the importance of study of elastic nature of biscuit sample. Hence, the
legal limit i.e. 6% moisture content level can be considered to control the crispy characteristic of
biscuits.

Effect on maximum deformation before breaking

It was observed that deformation was very small until the moisture content of 5.13% (i.e.
25% ERH). There was little or no significant effect of moisture sorption up to that level. ANOVA
analysis also indicated no significant difference between the deformation data obtained up to that
level.
Crispiness is always associated with the brittle failure and also the high rates of failure and
strain energy release so, for crispiness, deformation before breaking should be low (Jowitt, 1979).
The increase in deformation is always associated with the rubbery characteristics or plasticity of
the material. Hence, deformation study shows that the crispy or brittle characteristic of the biscuit
retains very well up to 5.88% moisture content above which there is linear increase in deformation
and so rubbery characteristic. So, biscuit should not have moisture content of more than 6 %.
Above that level, the deformation was found to increase sharply with sorption of moisture. A very
good linear relationship has been found between the moisture content and the deformation before
breaking. The correlation coeff. is very high (r = 0.99). The observed regression equation is:
y = 0.946 x – 4.63 , (r = 0.99)
Where y is for deformation and x is for moisture content.

Discussion on the effect of ERH on Mechanical Properties of Biscuits

The overall result can be correlated with the physical state of sucrose in the biscuit sample.
Up to nearly 6% moisture content, sucrose is completely in glassy (amorphous) state and the slope of
breaking force, elasticity and deformation curve are all small. This is because, during baking, the
drying rate is such a high that sugar can’t crystallize and remain as amorphous structure. The glassy
state is brittle and hard and so the crispy characteristics of the biscuit retain (Peleg & Bagley, 1999).
That is why all mechanical parameters were changing at very small rate with sorption of moisture in
this region.
The large change in all mechanical properties between moisture content of 5.88% and
6.86% (i.e. ERH if 30% and 35%) was found to be correlated with the phase change in the sugar
from glassy state to rubbery state i.e. glass transition of sucrose. The sugar remained at glassy state
up to moisture content of 5.88% and above that, it was converted to super cooled amorphous
solutions or very viscous liquid which have the properties similar to rubber so also called rubbery
state (Karel, 1993). This is the reason to have a significant great change in the mechanical
properties of biscuit.
After the glass transition, crystallization is the time dependent phenomenon. The
crystallization of sugar has been found to be in between 35% and 40% ERH (moisture content of
6.88% and 6.988%) from the sorption curve. Palmer et al. (1956) also studied the crystallization of
sucrose at 24oC and nearly 32.5% RH.
During crystallization moisture is released and so moisture content decreases and again the
sorption occurs at 40% RH. It has been found that there is very small change in moisture content

7
between ERH of 35% and 40% and also, all the mechanical properties have been found to be
insignificant (p<0.05). This may be due to the fact that mechanical properties are more related to
moisture content than ERH.
After crystallization, again the mechanical properties have been found to change with
increase in moisture content but the effect is more prominent. This fact may be explained from the
sorption studies of glassy and crystalline sugar. Amorphous sucrose begins absorbing water already
at aw = 0.1 with major rise in moisture content at aw = 0.3, but crystalline sucrose remains
eventually dry until about aw = 0.84 and meet amorphous sucrose at aw = 0.9 (Peleg and Bagley,
1999). This means, glassy state absorbs water and less water is available for polymer to change in
mechanical properties, while crystalline sugar doesn’t absorb it and more free moisture to affect the
polymer to change in mechanical properties such as breaking force (hardness), elasticity and
deformation before breaking (Crispiness).
This shows that sucrose combined with water contributes to the plasticization of
biopolymer because the sugar will shift the transition towards lower temperature. The plasticizing
effect of sugar will depend on the water / sugar / biopolymer mass ratio.
In this way, in many different cereals based foods containing relatively high percentage of
sugar (such as cookies, crackers and cakes) this carbohydrate contributes significantly to the
overall texture to the food by affecting the thermo mechanical behaviour of the products.

Conclusions
The Mechanical properties (texture) of biscuit are affected significantly by the phase
transition of sucrose. The crispy and brittle characteristics of the biscuit retain only if sucrose
remains in glassy state but if phase transition of sucrose from glassy to viscous liquid (i.e. rubber)
and to crystalline phase occurs then, there will be corresponding significant change in the
mechanical properties of biscuit, which contribute to the kinaesthetic sensation perceived during
eating. It was also concluded that 6 % moisture level was adequate to control the changes in texture
of biscuit. The phase transition of sucrose was observed above 35% ERH, so package design
should not allow to increase the internal humidity level above that one, so as to control the effect of
moisture on biscuit quality.

Acknowledgement
I would like to express sincere gratitude to my guide Pro. Dr. Dilip Subba (Asst. Dean, Central
Campus of Technology, Dharan), other lecturers of the campus and my colleagues for their constant
support, inspiration, encouragement and help during my dissertation.

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