FACULTY OF APPLIED SCIENCES

BACHELOR OF SCIENCE (HONS) IN FOOD SCIENCE AND

TECHNOLOGY

FST 606
INSTRUMENTAL ANALYSIS OF FOOD
INDIVIDUAL LAB REPORT

GROUP MEMBERS:
No. NAME MATRIX ID
1. MUHAMMAD ALIF IQBAL BIN ZALIZAT 2021580847
2. MOHAMAD NUR ARIF BIN NORDIN 2021984377
3. MUHAMMAD FIERDAUS BIN AZMEE 2021739969
4. NURUL AQILAH AZRA BINTI ABDUL SALAM 2021120723
5. NUR ALIFAH ILYANA BINTI ZULKARNAIN 2021321779

NAME : NURUL AQILAH AZRA BINTI ABDUL SALAM

CLASS : 2021120723
LAB TITLE : DETERMINATION OF VISCOELASTIC PROPERTIES FOOD
PRODUCTS USING A RHEOMETER
LECTURER’S NAME : DR SITI ROHA AB MUTALIB
DATE OF SUBMISSION : 19 JANUARY 2023
Table of Contents
1.0 Introduction......................................................................................................... 3
2.0 Objectives ................................................................................................................ 3
3.0 Methodology ............................................................................................................ 4
3.1 Apparatus and Chemicals .............................................................................................. 4
3.2 Procedure ......................................................................................................................... 4
4.0 Results ...................................................................................................................... 5
5.0 Discussion ............................................................................................................. 11
6.0 Conclusion ............................................................................................................. 13
References ................................................................................................................... 13
1.0 Introduction

Rheology studies the movement of complex fluids. The objective of rheology is to determine
the fluid flow that would be produced due to applied forces. When a pressure is applied, fluids
stretch constantly, whereas solids deform briefly before stopping. While fluids do not have an
elastic reaction and constantly deform under tension, solids are said to have a "elastic"
response and can resist an applied stress. Despite the fact that liquids and gases have highly
different molecular properties, the separation between them is less fundamental at the
macroscopic level. Although gases have a far higher deformation rate for a given applied
stress than liquids do, the responses of both liquids and gases to stresses are qualitatively
similar.

The rheological characteristics of the fluids are measured using a Paar Physica MCR300
rheometer. The rheometer is a device that measures air bearing rheology. A 250-lit tank
supplies the necessary air. A set of filters process the air, removing impurities including
moisture and grease. At 5 bar and 110 lit/min, the dry, pure air enters the rheometer. Parallel
plate geometry was already used. The space between the plates is 1 mm. The upper plate
rotates, while the lower plate is fixed. The necessary continuous magnetic field is applied using
a magnetic cell. A water-based heater/cooler system is also employed to maintain a steady
temperature throughout. The fluid temperature can be adjusted by this device at temperatures
between -30oC and 180oC. However, all measurements are carried out at a temperature of
25oC.

2.0 Objectives

The objective of this experiment conducted is:

1. To study the mechanism of rheometer in determining the rheology characteristics of
sample
2. To determine the effect of temperature on viscoelastic properties of the sample
3. To determine the complex viscosity of the sample
3.0 Methodology
3.1 Apparatus and Chemicals
- 5% Xanthan Gum
- 7% Pectin
- The physica
- Viscotherm VT2
- Paar Physica

3.2 Procedure
1. Firstly, the compressed air supply was turned on and let the pressure rise up until
reach 5 bar.
2. Next, the Physica, Viscotherm VT2, Paar Physica and Rheometer, and fluid
circulator was turned on.
3. The computer was switched on.
4. After the desktop shown, rheoplus was clicked and the TEK150P was installed into
the measuring plate.
5. Before the experiment was begin, the instrument was first calibrated.
6. The sample was put on top of the measuring plate.
7. The ‘zero gap’ button were clicked to produce a gap of 1 mm
8. Next, the lift position button was clicked.
9. The sample were measured by clicking control panel button and sample name
were changed accordingly.
10. The data of each sample were recorded in the rheoplus software.
11. The torque sweep, temperature sweet and frequency sweep of the sample were
carried out.
4.0 Results
Table 1.1 Average Data of the 7% Pectin by using Rheometer
Average Average Average Average Loss Average
Measure Points Frequency (Hz) Storage Modulus (Pa) Complex
Modulus (Pa) Viscosity (Pa.s)
1 1 5.21E+01 5.90E+01 12.9
2 6.21 2.03E+02 1.57E+02 6.63
3 11.4 3.42E+02 2.71E+02 6.11
4 16.6 4.32E+02 2.87E+02 4.99
5 21.8 4.42E+02 3.49E+02 4.16
6 27.1 4.46E+02 4.14E+02 3.71
7 32.3 4.18E+02 4.81E+02 3.40
8 37.5 4.23E+02 5.54E+02 3.27
9 42.7 4.24E+02 6.43E+02 3.23
10 47.9 4.40E+02 7.33E+02 3.26
11 53.1 4.83E+02 8.22E+02 3.29
12 58.3 5.43E+02 8.95E+02 3.31
13 63.5 6.17E+02 9.29E+02 3.28
14 68.7 7.03E+02 9.05E+02 3.19
15 73.9 8.13E+02 8.27E+02 3.06
16 79.2 1.02E+03 6.27E+02 2.87
17 84.4 1.53E+03 1.09E+02 2.90
18 89.6 1.85E+02 1.82E+03 3.42
19 94.8 1.29E+02 2.56E+03 4.34
20 100 8.37E+00 3.82E+03 6.08

Rheoplus

1 4
10 10

7% Pectin Tue pm 1
Pa
PP25; [d=1 mm]

3 G' Storage Modulus

10
G'' Loss Modulus

7% Pectin 2 Tue pm 1
G' PP25; [d=1 mm]
2
10 G' Storage Modulus

G'' Loss Modulus

G''
7% Pectin 2 Tue pm 2

PP25; [d=1 mm]

1
10 G' Storage Modulus

G'' Loss Modulus

0 0
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 1: Combination graph of triplicate 7% Pectin data by using rheometer

 Rheoplus

1 4
10 10

Pa

3
10
7% Pectin Tue pm 1

PP25; [d=1 mm]

G'
G' Storage Modulus

G'' Loss Modulus

G''
2
10

0 1
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 2: Graph of first replicate for 7% Pectin data by using rheometer

Rheoplus

1 4
10 10

Pa

3
10

7% Pectin 2 Tue pm 1

PP25; [d=1 mm]

2 G'
10 G' Storage Modulus

G'' Loss Modulus

G''

1
10

0 0
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 3: Graph of second replicate for 7% Pectin data by using rheometer

 Rheoplus

1 4
10 10

Pa

7% Pectin 2 Tue pm 2

PP25; [d=1 mm]

3 G'
10 G' Storage Modulus

G'' Loss Modulus

G''

0 2
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 4: Graph of third replicate for 7% Pectin data by using rheometer

Graph of Frequency (Hz) Versus Complex

Viscosity (Pa.s)
14
12
Complex Viscosity (Pa.s)

10
8
6
4
2
0
0 20 40 60 80 100 120
Frequency (Hz)

Figure 5: Graph of Frequency (Hz) versus Complex Viscosity (Pa.s) of 7% Pectin

Table 1.2 Average Data of the 5% Xanthan Gum by using Rheometer
Average Average Average Average Loss Average
Measure Points Frequency (Hz) Storage Modulus (Pa) Complex
Modulus (Pa) Viscosity (Pa.s)
1 1 1.74E+03 2.45E+02 280
2 6.21 2.06E+03 2.52E+02 53.2
3 11.4 2.16E+03 2.81E+02 30.4
4 16.6 2.29E+03 3.15E+02 22.1
5 21.8 2.26E+03 3.06E+02 16.6
6 27.1 2.21E+03 3.52E+02 13.1
7 32.3 2.12E+03 4.03E+02 10.7
8 37.5 2.01E+03 4.58E+02 8.76
9 42.7 1.88E+03 5.21E+02 7.28
10 47.9 1.75E+03 5.84E+02 6.13
11 53.1 1.61E+03 6.42E+02 5.21
12 58.3 1.49E+03 6.86E+02 4.47
13 63.5 1.39E+03 7.01E+02 3.90
14 68.7 1.32E+03 6.68E+02 3.43
15 73.9 1.31E+03 5.83E+02 3.09
16 79.2 1.37E+03 3.78E+02 2.87
17 84.4 1.17E+03 3.56E+02 2.72
18 89.6 0.00E+00 1.78E+03 3.17
19 94.8 0.00E+00 2.24E+03 3.76
20 100 0.00E+00 3.20E+03 5.09
Rheoplus

1 4
10 10

Pa

5% xanthan gum Tue pm 2

3 PP25; [d=1 mm]

10
G' Storage Modulus

G'' Loss Modulus

5% xanthan gum Tue pm 4

G' PP25; [d=1 mm]

G' Storage Modulus

G'' Loss Modulus

G''
5% xanthan gum Tue pm 7

PP25; [d=1 mm]

2 G' Storage Modulus

10
G'' Loss Modulus

0 1
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 6: Combination graph of triplicate 5% Xanthan Gum data by using rheometer

 Rheoplus

1 4
10 10

Pa

3
10

5% xanthan gum Tue pm 2

PP25; [d=1 mm]

G'
G' Storage Modulus

G'' Loss Modulus

G''

2
10

0 1
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 7: Graph of first replicate for 5% Xanthan Gum data by using rheometer

Rheoplus

1 4
10 10

Pa

5% xanthan gum Tue pm 4

PP25; [d=1 mm]

3 G'
10 G' Storage Modulus

G'' Loss Modulus

G''

0 2
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 8: Graph of second replicate for 5% Xanthan Gum data by using rheometer
 Rheoplus

1 4
10 10

Pa

5% xanthan gum Tue pm 7

PP25; [d=1 mm]

3 G'
10 G' Storage Modulus

G'' Loss Modulus

G''

0 2
10 10
1 10 Hz 100
Frequency f
Anton Paar GmbH

Figure 9: Graph of third replicate for 5% Xanthan Gum data by using rheometer

Graph of Frequency (Hz) Versus Complex

Viscosity (Pa.s)
30
Complex Viscosity (Pa.s)

25

20

15

10

0
0 20 40 60 80 100 120
Frequency (Hz)

Figure 10: Graph of Frequency (Hz) versus Complex Viscosity (Pa.s) of 5% Xanthan Gum
5.0 Discussion
The Rheoplus software rheometer with series MCR300 was utilised in this experiment. The
measuring tool is a PP25 parallel plate and TEK150P paltier. The objectives of this experiment
are to determine the sample's complex viscosity and the impact of temperature on its
viscoelastic characteristics. 5% and 7% of Xanthan Gum and Pectin were utilised as samples.
To obtain an accurate result, the experiment was repeated three times for each sample.
Xanthan gum and pectin are both utilised as thickening agents in various food applications.
Although xanthan gum can effectively replace pectin, the optimal composition frequently
combines xanthan, inulin, and pectin.

In order for the objectives of the experiment determine, both xanthan gum and pectin were
analysed using the rheometer. Firstly, the rheometer was turned on starting from the air
pressure in order to rise the pressure up to 5 bar. Next, the Physica, Viscotherm VT2, Paar
Physica and Rheometer, and fluid circulator was turned on. Later, the computer for displaying
the rheometer data was turned on. The ‘rheoplus’ was clicked and next the rheometer was
calibrated before the sample were analysed. The reason of calibration check performed is to
quantify and improve the measurement accuracy of the instrument itself. After done calibrated,
the parallel plate was inserted into the lifting post. Before the analysis begin, the temperature,
frequency are all set inside the computer system. After done, the sample was put in the middle
on the rheometer plate. The ‘meas. position’ was then clicked and the lifting arm started to
move downward which giving only 1mm gap. The excess sample that presence on the outer
parallel plate was cleaned by using spatula. After done, the sample was ready to be analysed
and all of the data sample been analysed and person in charged were filled in the form inside
the system. All of the sample were analysed for 3 consecutives times in order to get the
average result. As been tabulated in the result, Figure 1 and 6 illustrated the 3 graph that been
combined after the pectin and xanthan gum undergo rheometer analysis. Both graph shown
different trend, where the pectin is more likely to rise and have some crossing between the
storage modulus and loss modulus, meanwhile for xanthan gum, no crossing occurred
between the storage modulus and loss modulus as there have a gap in between both of the
line.

Based on the result of 7% pectin, the viscosity of pectin solutions decreased with rising
frequency but however rising at frequency 84.4 Hz (2.90 Pa.s) until 100 Hz (6.08 Pa.s). The
behaviour of pectin in aqueous solutions, specifically its form and hydrodynamic volume,
determines its functional qualities. Using the intrinsic viscosity measurement, pectin solutions
are categorised as hydrocolloids. Generally speaking, the viscosity increased as the pectin
concentration increased. pH, pectin concentration, and temperature all had an impact on the
impact of buffer concentration on viscosity. The intermolecular interactions and strength of the
water-solute hydrogen bonds, which limit molecular motion, may be to account for the
concentration's influence. The increase in hydrogen bonding with the pectin hydroxyl groups
causes the viscosity to increase when a high amount of pectin is dissolved in water. On the
other side, for 5% xanthan gum, the viscosity was recorded started to rise again at frequency
89.6 Hz (3.17 Pa.s), 94.8 Hz (3.76 Pa.s) and 100 Hz (5.09 Pa.s). The rheological behavior of
xanthan gum solutions at the studied temperatures decreased with increasing shear rate from
0 to 300 s-1 due to their pseudoplastic fluid rheology (Figure 6). The dissociation of the side
chain carbonium ions and the creation of aggregates through many hydrogen bonds are
thought to be the causes of the influence of xanthan gum concentration on pseudo plasticity.

The amount of energy that is stored in a sample and released following mechanical stress is
measured by the storage modulus (G'). The viscose portion of the sample, on the other hand,
is described by the loss modulus and is related to the loss of energy converted through friction
into heat (Centre for Industrial Rheology, 2022). The viscoelastic behaviour of the sample is
most closely resembled by the solid-state behaviour, which is represented by the storage
modulus G' (G prime, in Pa). The viscous component of viscoelastic behaviour, which can be
understood as the sample's liquid-state behaviour, is characterised by the loss modulus G" (G
double prime, in Pa). According to the experimental data, since Xanthan Gum 5% has a
storage modulus, G', that is greater than its loss modulus, G" (G' > G"), it is a solid light sample
with elastic behaviour. The loss modulus and the stored deformation energy are both indicated
by the term modulus of storage G'. G" stands for the deformation energy lost (dissipated)
during flow as a result of internal friction. When G' > G'' is present, the storage modulus
outweighs the loss modulus in viscoelastic solids. Internal connections inside the substance,
such as chemical bonding or physical-chemical interactions, are to blame for this. Pectin 7%
has a loss modulus of G" that is greater than its storage modulus of G' (G" > G'), making it a
liquid light sample with viscous behaviour. On the other hand, viscoelastic liquids with G" > G'
have a higher loss modulus than storage modulus.

Important micro-structural characteristics are measured since the tensile stress in the Linear
Viscoelastic Region are inadequate to produce structural breakdown of the structure. When
applied stresses are greater than the yield stress, non-linearities develop and measurements
are no longer easily associated with microstructural characteristics. The amount of force
delivered on a well-defined cross-sectional sample is referred to as stress. Strength is equal
to force/area. Samples with circular or rectangular cross sections can be stretched or
compressed. Up to ten times their initial length can be achieved by stretching rubber and other
elastic materials. By conducting a stress or strain sweep test and measuring the point at which
the structure starts to deteriorate, the linear visco-elastic area often is identified. The limit of
the linear viscoelastic area corresponds to the stress or strain dependence of G'. According
to the viscoelastic area, the complex viscosity of 5% Xanthan Gum and 7% Pectin is more
dominating at high frequency than at low frequency.

During conducting this experiment, there may be some error been occurred which resulting in
data error. For example, overfilling the sample using parallel plate in rotational rheometry. The
measured viscosity increases due to greater drag force produced by an overfilled sample,
especially if the sample wets the geometrical rim. Moreover, to minimize error from occurring,
the sample should then be stirred before being poured into the measurement device because
the result won't be accurate otherwise.

6.0 Conclusion

In conclusion, the objectives of this experiment were achieved. It can be concluded xanthan
gum 5% is a solid, light sample with elastic behaviour because its storage modulus, G', is
greater than its loss modulus, G" (G' > G"). Since the loss modulus, G," of pectin at 7% is
more than the storage modulus, G', (G" > G'), hence it is a liquid light sample with viscous
behaviour. The complex viscosity of Xanthan Gum 5% and Pectin 7% is more dominating at
high frequency than at low frequency, according to the viscoelastic area.

References

Basics of rheology :: Anton Paar Wiki. (n.d.). Anton Paar. Retrieved from https://wiki.anton-
paar.com/my-en/basics-of-rheology/
Centre for Industrial Rheology. (2022b, January 4). Storage modulus (G’) and loss modulus
(G”) for beginners. Rheology Lab. Retrieved from
https://www.rheologylab.com/videos/storage-and-loss-modulus-for-beginners/
Heney, P. (2021, November 3). What is a rheometer? Research & Development World.
https://www.rdworldonline.com/what-is-a-rheometer/