CRYSTALLISATION BEHAVIOUR OF PALM OIL:

Crystal Size Distribution of Palm Oil and the

Ternary Blends during Isothermal Crystallization
using Focused Beam Reflectance Measurement
(FBRM) system
Zaliha Omar, Elina Hishamuddin and Norizzah Abd Rashid

Product Development & Advisory

Services Division, Malaysian Palm Oil Board, Malaysia
 PRESENTATION OUTLINE

Introduction
Objectives
Materials and Methods
Results and Discussion
Conclusion
Acknowledgements
 INTRODUCTION

Palm oil

Semi-solid at ambient temperature (25C), consisting of low

and high melting triacylglycerols (TAGs).

Crystallized in either ' or mixture of (' + ) or

polymorphic forms depending on the crystallization
temperature.

Can be fractionated into liquid fraction (olein) and solid

fraction (stearin).

These unique characteristics make palm oil a versatile

ingredient in food and non-food products.
 The crystallization process is a controlled cooling
process from a higher to lower temperature to
obtain the desired:-

o crystal number, size distribution, polymorph, TAGs,

FAC to form different functional of palm fractions

o textural properties and physical characteristics of

food products.
Crystallisation process of oils and fats:-

super cooling from melt

CRYSTALLISATION PROCESS
Nucleation
( )
Monotropic manner

Crystal growth

Aggregation of crystal

Crystal network
 Palm oil slurry after
crystallization process

Filtration

Olein Soft stearin Hard stearin

(liquid 55-65%) Palm-mid fraction (Solid 10-15%)
(semi-solid 25-30%)
SMP 56-58C
SMP (low) 19.4-23.5C SMP 45-48C IV 10
IV 63 IV 33
Factors influencing the Macroscopic properties of
fat crystal networks

Macroscopic Properties
(end products), eg. Texture,
rheology

Microstructure
(Sizes)

Polymorphism Processing conditions

, , Temperature
Polyptism
Agitation
Cooling rate
Lipid Composition Cooling profile etc.
(TAG, FAC))

(Marangoni, 2001)
Recent study

FBRM capable of assessing changes in particle size

of palm oil crystals and in detecting multiple
crystallization events in palm oil system
(Hishamuddin et al., 2011).

FBRM is becoming a more popular technique to

measure particle size on-line in different applications.

The technique gives information on online

monitoring of particle numbers and size distributions
during the crystallisation process.
 OBJECTIVES

To measure the total particle counts and chord length

distribution (CLD) of Palm Oil and ternary blends
using FBRM under isothermal crystallisation.

To determine the effects of blending palm oil, palm

stearin, palm olein and soya bean oil on the particle
size, triacylglycerol, polymorphic form and fatty acid
composition.
Materials
Palm oil (PO, IV 53.5), palm stearin (PS, IV38), palm olein
(POo, IV59) - Jomalina Sdn. Bhd. Port Klang, Msia.
Soybean oil (SBO) from local supermarket.

Blends preparation:-
PO:PS: POo and PO:PS:SBO at weight ratio
of 50, 30 and 20 (w/w)

Methods
Crystal size distribution (CLD) under isothermal
crystallisation process - FBRM
Triacylglycerol (TAG) profiles HPLC
Fatty acid composition (FAC) GC
Microscopic observation PLM
Polymorphic form X-ray diffractometer
continue

Isothermal crystallisation of
palm oil and ternary blends
from melt was monitored
online using a Lasentec
FBRM probe inserted into
the stirred reactor (100rpm).

The crystallisation were

carried out at 28, 30 and
32C

Schematic diagram of FBRM probe

RESULTS AND DISCUSSION

Nucleation
induction time

Total particle counts of Palm Oil during

isothermal crystallisation pocess
continue

Total particle counts of Total particle counts of

PO:PS:POo(50:30:20) blend PO:PS:SBO(50:30:20) blend
 PO
21m and 61m

PO:PS:POo(50:30:20)
51m

PO:PS:SBO (50:30:20)
65 m

RBDPO [A] PO:PS:POo(50:30:20)[B PO:PS:SBO(50:30:20

] )
The chord length distributions (CLD) -
isothermal crystallisation at 30c
 FATTY ACID COMPOSITION (%)

Sample C12:0 C14:0 C16:0 C18:0 C18:1 C18:2 C18:3 C20:0

PO 0.2 1.1 45.2 4.1 38.8 9.9 0.2 0.3

PS 0.2 1.4 59.3 4.7 27.4 6.3 0.1 0.3

POo 0.2 1.0 39.7 4.0 44.0 10.1 0.3 0.4

SBO - - 10.9 4.4 22.1 53.8 7.5 0.3

PO:PS:SBO 0.2 1.0 43.9 4.6 32.4 17.3 1.4 0.3

(50:30:20)

PO:PS:POo 0.3 1.1 45.4 4.7 37.6 9.9 0.2 0.4

(50:30:20)

PO and PS rich in palmitic and oleic acids

SBO contains mainly oleic and linoleic acids
Both blends high amounts of palmitic and oleic acids
 TRIACYLGLYCEROL COMPOSITION (%)

Sample OLL PLL OOL/ PLO PLP OOO POO POP PPP SOO POS PPS
OLO

PO 0.36 2.20 1.68 9.46 9.44 4.90 24.30 30.6 5.07 2.51 4.96 0.91
(Palm oil)
PS 0.22 1.13 0.79 4.88 6.51 3.84 12.61 27.99 22.18 1.44 5.13 4.45
(Palm stearin)
POo - 0.5 1.80 11.8 10.4 4.1 36.21 32.1 0.60 2.60 5.5 -
(Palm olein)
SBO 16.0 14.0 7.30 11.11 2.10 2.60 4.71 0.60 0.31 0.90 0.31 -
(soyabean oil)
PO:PS:SBO 4.2 5.2 3.6 8.8 7.6 4.1 15.7 23.0 11.1 1.9 3.9 2.0
(50:30:20)

PO:PS:POo 0.4 2.4 1.4 9.5 9.5 4.6 23.4 27.9 10.0 2.7 5.0 2.0
(50:30:20)

P=Palmitic acid, S=stearic acid, L=Linoleic acid, O=Oleic acid.

POLYMORPHIC FORM

Samples Polymorphic form

PO

POo

SBO

PO:PS:SBO (50:30:20) (+ )

PO:PS:POo (50:30:20)

X-ray relative intensity (short spacings):-

at 4.2 and 3.8 and
at 4.6
 CONCLUSION

The difference in the induction times and the CLD of Palm Oil
and the ternary blends were possibly due to the chemical
characteristics such as the triacylglycerol composition and fatty
acid profile of each type of oil in the blends.

The faster nucleation rate could be due to the higher content of

high melting TAGs of the blends such as PPP and PPS as
compared to Palm Oil which also caused the blends slurry to be
more denser.

The chord length distribution (CLD) of PO at the end of

crystallisation process were shorter than ternary blend
containing SBO but longer than blend with palm olein .

Palm stearin, Palm olein and soya bean oil altered the crystal
size distribution of Palm Oil.
 REFERENCES

1. Braatz, R.D. (2002) Advanced control of crystallization processes

Annual Reviews in Control 26:87-99.

2. Hishamuddin, E., Andrew, Stapley, G.F., and Zoltan K.N. (2011).

Application of laser backscattering for monitoring of palm oil
crystallisation from melt Journal of Crystal Growth 335:172-180.

3. Simmons, M.J.H., Langston, P.A. and Burbidge, A.S. (1999). Particle

and droplet size analysis from chord distributions Journal of Powder
Technology 102:75-83.

4. Stphanie, B. and Ronald W. R. Rousseau (2006). Utilization of Focused

Beam Reflectance Measurement in the Control of Crystal Size
Distribution in a Batch Cooled Crystallizer Chem. Eng. Technol. 29(2) pp
206-211.
 ACKNOWLEDGEMENTS

Special thanks to:-

The Director General of Malaysian Palm oil

Board (MPOB)

The Head of Faculty of Applied Sciences of

Universiti Teknologi MARA Shah Alam, Malaysia
for permission to present this paper

All the Physics and Chemistry Laboratory staff of

MPOB for their assistance.