OPTIMIZATION OF CONCENTRATION OF TOMATO

JUICE BY FREEZE CONCENTRATION

MUHAMMAD HARIZ BIN ABDUL HAMID
A19ET30149
SCHOOL OF CHEMICAL AND ENERGY ENGINEERING
FACULTY OF ENGINEERING

SUPERVISOR : PROF. MADYA DR. MAZURA BINTI JUSOH

CO-SUPERVISOR: DR. AISHAH BINTI ROSLI

1
OUTLINE
INTRODUCTION

LITERATURE REVIEW

METHODOLOGY

RESULT AND DISCUSSION

2
INTRODUCTION

3
BACKGROUND OF STUDY
1. Tomato - highly available in Malaysia

2. Used for - food-industry and variety of forms daily

fresh consumption.

3. Contains important nutrients - vitamin C,

potassium, folate, vitamin K and antioxidant.

4. To maintain the flavour, nutrients, functional

properties of concentrated fruit juices - the right
technique to concentrate the tomato juice needed.

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FREEZE CONCENTRATION

1. Formation ice crystals in crystallizer

2. Convert liquid into ice crystals
3. Separate the ice and concentrate liquid

5
PROBLEM STATEMENT

6
OBJECTIVES

To study the effect of operating conditions on

effective partition constant, K

To optimize operating conditions for

concentration of tomato juice through FC.

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SCOPE OF STUDY

Coolant Response Surface

Stirrer Speed Operation Time Methodology
Temperature

-6 to -14 °C 200 to 450 20 to 60 Design

rpm minutes Expert

8
LITERATURE REVIEW

9
CONCENTRATION TECHNIQUE
METHOD PROCESS ADVANTAGES DISADVANTAGES REFERENCE

Evaporation Concentrate fruit juice by • Easy to use • Destroying vital (Ermolaev et al.,
removing water from the liquid components of the 2022), (Sabanci
phase into the vapour or gas solution fruit juice such & Icier, 2020)
phase as fragrance, taste, and
nutrition due to the high
temperature
• High energy needed due
to heat
Diaphragm Juice pass through smallest • Energy efficient • High expenditures (Soikhedbrod,
membrane holes . The water • Simple operation 2018)
infiltrates and the large
molecules of other substances
of juice remain

Freeze Separates the water from the • Control bacterial (Samsuri et al.,
Concentration liquid solution as ice crystals growth 2018)
and leaving behind a highly • Cost beneficial for
concentrated solution separation process
• Avoid corrosion 10
 FC DESIGN
Crystallizer Application Processing Parameter Cooled Surface Reference
Design
Vertical Vessel Glucose • Stirring speed Cylindrical vessel (Miyawaki &
• Coolant Inakuma, 2020)
temperature
Multiple Probes Cucumber juice • Coolant Bulk flow-tubular (Mohd Rosli et al.,
Cryo-concentrator temperature wall 2022)
• stirring speed
• Operation time
Spiral Finned Glucose solution. • Coolant Bulk flow-cylindrical (Samsuri et al.,
Orange juice temperature with spiral fins 2018)
• time operation
• Circulation flowrate
• Shaking speed
Vertical Finned Concentrate • Coolant Bulk flow-cylindrical (Amran et al., 2018)
apple juice temperature with vertical fins
• Circulation flowrate
11
METHODOLOGY

12
FLOWCHART OF start

METHODOLOGY Formulation of problem

statement

Experimental setup

Crystallizer testing

Ice No Adjust
formation parameters

Ye
s
Raw material preparation Evaluation of effect of parameters
•Coolant temperature
•Operation time
Actual experimental testing •Stirrer speed

Optimization

Analyse concentration of Total

Conclusion Phenolic Content &
Concentration

stop 13
 MATERIALS &
CHEMICALS
Sample Preparation
Extract Tomato juice by the
juicer in about 3 litre.
Coolant Preparation
50 % by volume of Ethylene
Glycol and water solution will
be use as coolant.
Total Phenolic Content
Determination
• Folin-Ciocalteu reagent
(10% (v/v)) 100ml.
• Sodium carbonate
(Na2CO3) solution of
concentration 5 g/L 50ml.
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 APPARATUS
Motorized
stirrer

Refrigerant
Probe
Gas Cooling
System
Refractomete
r

Cylindrical
Tank

Cooling UV-VIS
Waterbath Spectrophotometer
EXPERIMENTAL PROCEDURE

Prepare 3 litre Immersed the Run the FC

tomato juice at
probe in the operation for
desired
desired time
concentration. solution.

1 2 3 4 5 6

Feed the cooled Turn on the

Measure the final
juice into the cooling gas system
concentration of
jacketed tank – & switch on the
ice formed and the
temperature will motorized stirrer
concentrate.
be preserve at 2 °C at desired speed.

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RANGE OF PARAMETERS

PARAMETERS RANGE
coolant temperature -6 to -14°C
Stirrer speed 200 to 400 rpm
Operation time 20 to 60 minutes

Coolant -14 Stirrer 200 Operation 20

temperature, -12 speed, 250 time, min 30
°C -10 rpm 300 40
-8 350 50
-6 400 60
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EFFECTIVE PARTITION CONSTANT, K

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OPTIMIZATION OF FREEZE CONCENTRATION

• Design expert software for Response

Surface Methodology (RSM)
• Central Composite Design (CCD) is the
best design in applying response surface
methodology (RSM)
• Interactions of 3 operating conditions was
investigated towards response K value

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RESULTS & DISCUSSION

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EFFECT OF COOLANT TEMPERATURE ON FC SYSTEM
• Operation time at 30 minutes ,
stirrer speed at 350 rpm, and 1.5 brix
% for the initial concentration
• K value decrease from -6 °C to -10 °C
• Best K value recorded at -10 °C which
0.307
• Rise at -10 °C to -14 °C
• This due to the solute being trapped
in the outward movement of the ice
front

21
EFFECT OF OPERATION TIME ON FC SYSTEM

• Coolant temperature at -8 °C , stirrer

speed at 350 rpm, and 1.5 brix % for
the initial concentration
• K value decreases from 20 to 40
minutes
• Best K value - 40 minutes which 0.201
• Increase after 50 minutes of
operation
• The impurity of the ice which grew
with increasing concentration over
time

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EFFECT OF STIRRER SPEED ON FC SYSTEM

• Coolant temperature at -8 °C ,
operation time at 30 minutes, and 1.5
brix % for the initial concentration
• K value decreases from 200 to 250 rpm
• Increase back after 300 rpm
• solute is heavily accumulated at the
ice-liquid interface causing a higher
concentration of solute in the ice
formed
• Best K value recorded at 250 rpm
minutes - 0.362

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DESIGN OF EXPERIMENT
Manipulated variables Range and levels
Variable Symbol
Coolant -α -1 0 1 +α
Run Operation time, Stirrer speed, Response, K
temperatures, Coolant
X2 X3 X1 -14.0 -12. 4 -10 -7.6 -6.0
X1 Temperature, (°C)
1 -12.4 28.1 290.5 0.38 Stirrer speed,
X2 250.0 290.5 350 409.5 450.0
2 -7.62 52.0 409.5 0.33 (rpm)
3 -10.0 20.0 350.0 0.35 Operation time,
X3 20.0 28.1 40 52.0 60.0
4 -10.0 40.0 350.0 0.24 (Minutes)
5 -12.4 28.1 409.5 0.38
6 -7.6 28.1 409.5 0.23 Regression Equation:
7 -10.0 40.0 250.0 0.17
8 -12.4 52.0 290.5 0.35
9 -10.0 40.0 450.0 0.34
10 -10.0 60.0 350.0 0.33
11 -12.4 52.0 409.5 0.27
• Combinations of interactions between parameters by CCD
12 -7.6 52.0 290.5 0.35
• Lower limit, low, centre, high and upper limit which are
13 -6.0 40.0 350.0 0.38 coded as -α, -1. 0. +1 and +α
14 -14.0 40.0 350.0 0.38
• Generate regression equation for K as a function of the
15 -10.0 40.0 350.0 0.24 three variables (X1, X2, X3)
16 -7.6 28.1 290.5 0.33
17 -10.0 40.0 350.0 0.25 24
 MODEL ADEQUACY CHECK (ANOVA)
Sum of Degree of Mean
Sources Squares, Freedom, Squares, F-value F0.05 R2
(SS) (DF) (MS)
Regression
0.1925 9 0.0214 3.77 3.02 0.71
(SSR)

Residual 0.0568 7        

Total (SST) 0.2493 16        

• Value of R2 for the regression model is 0.71.

• most the majority of the observed points are located close to
the linear line.
• F-value recorded higher than F0.05 , 3.77>3.02
• Does prediction mathematical model is appropriate and
accepted

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INTERACTION OF COOLANT TEMPERATURE (X1) AND OPERATION TIME (X2)

• Coolant temperature -7.8 to -11.2 °C • K-value decrease after 30 minutes

• Operation time - 30 to 50 minutes • Some inclusions of the solute in the ice that has
formed
• Increase above 50 minutes and not suitable

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INTERACTION OF COOLANT TEMPERATURE (X1) AND STIRRER SPEED (X3)

• Coolant temperature factors at -8 to -10 ˚C and stirrer • The PFC process become less efficient when highest
speed 230 to 380 rpm X1 and X3 or the lowest X1 and X3
• Lower K-value can get with higher stirrer speed and lower • This means the appropriate range is at a value that
coolant temperature falls halfway between two factors

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INTERACTION OF OPERATION TIME (X2) AND STIRRER SPEED (X3)

• Operation time at 33 to 45 minutes and stirrer speed at • K value increase when operation is too high and too low
230 to 350 rpm similar with stirrer speed
• K value reach lowest response • Best K value show at intermediate levels of operation time
and stirrer speed
• Better heat transfer occur for accelerate the growth of ice
layer at probe

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VALIDATION OF EXPERIMENT

Coolant
Operation Stirrer Validatio
Response temperature, Predicted
time, X2 speed, X3 n
X1
K -9.4 49.0 375.0 0.267 0.282
• Optimum conditions at -9.4 ˚C, 49 min and 275 rpm

• Predicted response of K is 0.267 and validation is 0.308

• Percentage error for this 15.36%

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 CONCLUSION &
RECOMMENDATION

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• Coolant temperature - K value decrease at -6 °C to -10 °C and increase at -12 °C to -14 °C
which recorded the best K value at - 10 °C.

• Operation time - K value decrease at 20 to 40 minutes and increase at 50 to 60 minutes

which recorded the best K value at 40 minutes.

• Stirrer speed - K value decrease at 200 to 250 rpm and increase at 300 to 400 rpm which
recorded the best K value at 250 rpm.

• The optimum conditions for K value - coolant temperature at-9.4 °C, an operation time at 49
minutes, and a stirrer speed at 375 rpm

• MPCC system should be installed with efficient cooling gas system that can be set with
different decimal temperature range for cooling process.

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REFERENCES
1. Ermolaev, A. E., Krysanov, K. S., Tekiev, M. V., Silaev, V. I., & Zaseev, S. G. (2022). Vacuum-evaporative method
of juice concentration. IOP Conference Series: Earth and Environmental Science, 954(1), 012028.
https://doi.org/10.1088/1755-1315/954/1/012028
2. Sabanci, S., & Icier, F. (2020). Rheological behavior of sour cherry juices concentrated by ohmic and
conventional evaporation processes under vacuum. Journal of Food Processing and Preservation, 44(10).
https://doi.org/10.1111/jfpp.14832
3. Soikhedbrod, M. (2018). The new method of Juice Concentration. Journal of Food Processing & Technology,
09(05). https://doi.org/10.4172/2157-7110.1000731
4. Samsuri, S., Amran, N. A., & Jusoh, M. (2018). Optimization of progressive freeze concentration on Apple Juice
via response surface methodology. IOP Conference Series: Materials Science and Engineering, 358, 012042.
https://doi.org/10.1088/1757-899x/358/1/012042
5. Miyawaki, O., & Inakuma, T. (2020). Development of progressive freeze concentration and its application: A
Review. Food and Bioprocess Technology, 14(1), 39–51. https://doi.org/10.1007/s11947-020-02517-7
6. Mohd Rosli, N. N., Harun, N. H., Abdul Rahman, R., Ngadi, N., Samsuri, S., Amran, N. A., Safiei, N. Z., Ab Hamid,
F. H., Zakaria, Z. Y., & Jusoh, M. (2022). Preservation of total phenolic content (TPC) in cucumber juice
concentrate using non-thermal progressive freeze concentration: Quantitative design characteristics and
process optimization. Journal of Cleaner Production, 330, 129705.
https://doi.org/10.1016/j.jclepro.2021.129705
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REFERENCES
7. Samsuri, S. (2016). Development of Spiral Finned Crystallizer for Progressive Freeze Concentration
Process (Doctoral dissertation, Universiti Teknologi Malaysia).
8. Amran, N. A. (2015). Development of Vertical Finned Crystallizer for Progressive Freeze Concentration
Process (Doctoral dissertation, Universiti Teknologi Malaysia).
9. Ibrahim, S. A. (2012). Effect of Coolant Temperature and Intial Concentration on Progessive Freeze
Concentration of Simulated Dairy Wastewater by Using Aluminium Crystallizer (Doctoral dissertation,
Universiti Teknologi Malaysia).
10. YAHYA, N. B. (2020). DEVELOPMENT OF MULTIPLE PROBE CRYO-CONCENTRATION SYSTEM FOR PROGRESSIVE
FREEZE CONCENTRATION OF LYSOZYME AQUEOUS SOLUTION (Doctoral dissertation, Universiti Teknologi
Malaysia).
11. Safiei, N. Z. (2016). Progressive Freeze Concentrator Prototype for Preservation of Phenolic Content in Grape
Juice (Doctoral dissertation, Universiti Teknologi Malaysia).

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THANK YOU

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