CPB30303 Oil and Fat Process Technology UniKL MICET Experiment 2: Dry fractionation of RBD palm oil full lab report

TABLE OF CONTENTS No. 1 2 3 4 5 6 7 8

Contents Summary/Abstract Introduction and theory Results Discussions Conclusion Recommendations References Appendices

Page Number 2 2 4 7 10 10 11 12

1.0 SUMMARY/ ABSTRACT Dry fractionation is basically the process when the melted oil been crystalized which separation from solid liquid portion of the oil and more specific the dry fractionation of RBD palm oil is needed to obtain solid Stearin or known as cake Stearin and liquid Olein which is the

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

filtrate. Result obtained from this experiment when feed RBDPO 8.00 kg are 4.80 kg soft Olein (liquid), 2.30 kg Stearin (cake) and the yield is 60 %. The highest iodine value obtained for the experiment is Olein which the average is 3.06 and the value is proven when it show the highest the average iodine value. For the average iodine value for stearin is 2.52 and for RBDPO feed is 2.97. The effects of agitation rate on crystallization kinetics of butter fat show that increased agitation rate caused an increase in nucleation rate (more crystals generated per unit time) and an increase in total crystallization (mass deposition) rate. Besides the effects of agitation on growth rates of individual crystals were dependent on temperature of operation. 2.0 INTRODUCTION AND THEORY The rising price of petroleum in the world market, together with the increasing concentration of atmospheric carbon dioxide, has driven the need of biofuels as an alternative to fossil fuels for use in transportation in many countries (Tverbeg, 2013). In Malaysia, Palm oil entered a bull market on rising demand for the edible oil. The price of palm oil according to Bursa Malaysia Derivatives in Kuala Lumpur settled at RM2,643 a tonne. That’s 21% above the closing price of RM2,188 reached on July 12 (Online, 2016). As a consequence, biofuels help, not only reduce crude oil imports, but also boost the economics of the local livelihoods in the country's oil palm plantations areas due to an increased demand for palm oil to produce biodiesel. Since the demand for Para rubber in the world's market has declined and its price lowered, more and more rubber tree cultivating land is being converted to oil palm plantations. Thus, an important advantage for the use of biodiesel is that in addition to money savings from less imported crude oil and reductions of carbon emitted from fossil diesel use, plant growers are given more flexibility in their livelihood because of their ability to convert cultivation to crops suitable for biofuel production. Biofuels also offer a renewable source of energy as compare to fossil fuels (CEF, n.d). Malaysia currently accounts for 39 % of world palm oil production and 44% of world exports. If taken into account of other oils & fats produced in the country, Malaysia accounts for 12% and 27% of the world's total production and exports of oils and fats. Being one of the

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CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

biggest producers and exporters of palm oil and palm oil products, Malaysia has an important role to play in fulfilling the growing global need for oils and fats sustainably (MPOC, n.d). Fractionation Process Basically, palm oil is the liquid fraction obtained from fractionation of palm oil. In edible oil processing, a fractionation process consists of a controlled cooling of the oil, thereby inducing partial or fractional crystallization (Calliauw, 2011). The fractionation process involves a physical process of cooling the oil under controlled conditions to low temperatures, followed by filtration of the crystals through membrane press. Dry fractionation through batch crystallization of oil without using additives by controlled cooling and subsequent continuous filtration. Dry fractionation process is used to separate palm olein and palm stearin from RBDPO produced by physical treatment. Basically, palm oil is the liquid fraction obtained from fractionation of palm oil. The fractionation process involves a physical process of cooling the oil under controlled conditions to low temperatures, followed by filtration of the crystals through membrane press. The remaining liquid palm olein is then separated from the solid fraction palm stearin by means of a filtration or centrifugation (Calliauw, 2011). In this experiment of dry fractionation of RBD palm oil, the products are olein and stearin. The RBDPO is passed through further fractionation process to get various grade of palm olein and palm stearin which the types of olein produced are normal grade olein, super grade olein and olein with cloud point 7-8°e.

RBD palm olein and RBD palm stearin

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CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

The olein is fully liquid at ambient temperature in warm climates. It can be blended with various vegetable oils in different proportions to obtain liquid oils which can withstand lower temperatures. For example, blends of palm olein with more than 70% soft oils such as soybean oil, corn oil or canola oil remain clear at 0°C for at least 5 hr. Oxidative stability of soft oils are also extended and improved by the palm olein (MPOB, 2016). RBD Palm Stearin is solid fraction obtained by the fractionation of palm oil after crystallization at controlled temperatures. The application of RBD palm stearin is for shortenings and margarine. RBD Palm Olein is the liquid fraction obtained by the fractionation of palm oil after crystallization at controlled temperatures. It is especially suitable for frying and cooking. Main applications of RBD Palm Olein include salad and cooking oils in households, industrial frying fat of instant noodles, potato chips, doughnuts and condensed milk. Crystallization Process Crystallization is a separation technique that is being used to separate solid that has dissolved in the dry fractionation which the temperature of the solution is being lowered causing the solution to melt. The product fractions are both being influenced by the crystallization temperature, cooling rate and agitation speed. For the stearin fraction, it is only being affected by the cooling rate and on the other hand, olein fraction is affected by the crystallization temperature and cooling rate (Peer, 2013). The stearin can then be separated from oil olein by different methods and the oil is thus divided into two fractions which are stearin with a high melting point and olein with a low cloud and melting points. The fractional crystallization and used to obtain oils or fats more suitable for example, as cooking oils or for margarine/shortening production. Filtration Process Filtration is the process where the solid matter is being separated from a liquid by causing the latter to pass through the pores of substances. The crystal slurry will go through the membrane filter, where it will separate the stearin fraction and olein fraction. Iodine Value 4

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

Quality parameters for fractionation are Iodine Value (IV). Iodine value is number of centigrams of iodine absorbed per gram of sample which represents degree of saturation of an oil or fat which lower IV means the oil of high saturation and vice versa. IV for RBD palm oil is 52 and IV for palm olein is 56. Natural oils and fats have different characteristics due to the fact that they are composed of a great number of different triglycerides. These contain fatty acids with carbon chins of different lengths and with different degrees of unsaturation. Triglycerides with a high degree of unsaturation, indicated by a high iodine value, have a lower melting point than those containing more saturated fatty acids. Iodine Value Rbd Palm Oil Feed Iodine value for RBD palm oil feed by using Wijs’ method is in range 50-55 Wijs which is 52 Wijs. Iodine Value Rbd Palm Olein Basically, there are two major grades of palm olein: standard olein and super olein (iodine value greater than 60). The standard olein has an iodine value of about 56.0-59.1 Wijs and cloud point of 10°C max. The specifications are given in Malaysian Standard MS816:2007(Table 3). Super olein is more suited to cooler climates and has cloud points of about 2°C-5°C. Iodine Value Rbd Palm Stearin The range iodine value RBD palm stearin in Malaysia is 27.8-45.1 Wijs (MPOB, 2016).

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CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

3.0 RESULTS AND ANALYSIS (with calculation)

Program Pattern 80 80 70 70 60 60 50 50 30

30 30

25 25

20 20

Table 1: Data of experiment Segmen t Starting

0

1

2

3

4

5

6

7

8

9

10

11

12

13

set point 30

30

80

80

70

70

60

60

50

50

30

30

25

25

80

80

70

70

60

60

50

50

30

30

25

25

20

25

30

53

30

46

30

30

30

138

60

100

60

30

(oC) Target set point 30 (oC) Time (min)

0

Weight of RBD Palm Oil feed:

8.00 kg

Weight of RBD Palm Olein

4.80 kg

:

Weight of RBD palm Stearin: 2.30 kg 6

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

Production Yield (%)

:

60 %

Iodine Value Analysis Table 2: Result of iodine value for RBD Palm Oil Feed RBD Palm Oil

Volume of sodium thiosulphate solution used (ml)

Mass of test

Iodine

Blank sample, V1

Palm oil feed, V2

sample, M (g)

value

25.1 25.1 25.1

17.9 18.8 17.5

3.0 3.0 3.0

3.05 2.66 3.21 2.97

Mass of test

Iodine

Feed Sample 1 Sample 2 Sample 3

Average

Table 3: Result of iodine value for RBD Palm Olein RBD Palm Oil

Volume of sodium thiosulphate solution used (ml) Blank sample, V1

Palm olein, V2

sample, M (g)

value

25.1 25.1 25.1

18.2 17.5 17.9

3.0 3.0 3.0

2.92 3.21 3.05 3.06

Feed Sample 1 Sample 2 Sample 3

Average Table 4: Result of iodine value for RBD Palm Stearin RBD Palm Oil

Volume of sodium thiosulphate solution used (ml)

Mass of test

Iodine

Blank sample, V1

Palm stearin, V2

sample, M (g)

value

25.1 25.1 25.1

19.1 19.3 19.0

3.0 3.0 3.0

2.54 2.45 2.58 2.52

Feed Sample 1 Sample 2 Sample 3

Average

Analysis of Result 7

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

The weight of RBD Palm Oil Feed is 8.00 kg, weight of RBD Palm Olein is 4.80 kg and the weight of RBD Palm Stearin produced is 2.30 kg. Thus, the measured production yield is 60%. Table 2 shows the iodine value for palm oil feed for sample 1, sample 2, and sample 3. The values obtained by calculation for three samples are 3.05, 2.66 and 3.21 respectively with the average value of 2.97. Besides, Table 3 shows the iodine value for palm oil olein for sample 1, sample 2, and sample 3. The values obtained are 2.92. 3.21 and 3.05 respectively with average value of 3.06. Table 4 shows the iodine value for palm oil stearin for sample 1, sample 2, and sample 3 which are 2.54, 2.45 and 2.58 respectively with average value is 2.52. It shows that palm olein has the highest iodine value followed by palm oil feed and palm stearin.

4.0 DISCUSSIONS Basically, dry fractionation is the process in which separation from solid liquid portion of the oil is achieved by a process of gradual cooling preheated oil (MPOB, 2010). The process actually separates RBD palm oil into olein and stearin. A typical plant consists of crystallisation and filtration sections. During crystallisation, RBD palm oil is being heated up first and then cooled under a controlled cooling program inside the crystallisers. At the end of this cooling program, the oil becomes slurry of crystal and liquid oil. The slurry is then fed into the filtration section which consists of membrane filters to separate the olein which is the liquid oil) and stearin which is the crystal. It is fair to state that other typical fat crystallization phenomena such as polymorphism are of secondary importance compared to intersolubility; typical fractionation conditions are generally sufficiently restricted in time and temperature range to only allow one type of molecular arrangement to form. For palm oil, this is typically in a β’-form from start to finish. [1] RBD-palm oil was fractionated into stearin fraction (the cake, as solid phase) and olein fraction (the filtrate, as liquid phase). Physical appearances in room temperature (25-30°C), the 8

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

stearin was solid while the olein was liquid compared to the initial palm oil that was semi-solid. The physical changes of the fractions compared to the initial RBD-palm oil were influenced mainly by shifted in the chemical compositions. To start the operation, RBDPO obtained from a local palm oil refinery was pumped by a peristaltic pump into the CC until the crystalliser is completely filled. Then, it was immersed in a refrigerated water bath. The CC was connected to a peristaltic pump by a silicone tube and the RBDPO was circulated in the system for a period of an hour. Before starting the circulation at the desired temperature, the CC containing RBDPO must first be heated at a temperature of 80°C to avoid the presence of unwanted crystal and also to remove previous thermal history. After that, the process proceeds to the designated reducedMtemperature, usually from 28°C until 24°C, which corresponds to the melting point of stearin and olein, which are about 48 °C and 20°C, respectively.

The effects of agitation rate on crystallization kinetics of butter fat were studied by Grall and Hartel (64). In a 2 L batch crystallizer, increased agitation rate caused an increase in nucleation rate (more crystals generated per unit time) and an increase in total crystallization (mass deposition) rate. [3] However, the effects of agitation on growth rates of individual crystals were dependent on temperature of operation. At 30°C, increased agitation led to a decrease in growth rate, whereas for crystallization at either 15°C or 20°C, increased agitation caused an increase in growth rate. These results may be related to the different composition effects at the different temperatures (different TAGs cocrystallize). [2] Furthermore, the quality parameter that is nominally monitored for fractionation is Iodine Value (IV) and Cloud point. Iodine value is defined as the number of centigrams of iodine absorbed per gram of sample. It represents the degree of saturation of oil or fat. Lower IV means the oil is of high saturation and vice versa. The theoretical IV for RBD Sterin is 48 and for palm olein is 56. Other quality parameters which are quite important but cannot be controlled in fractionation plant are colour and Free Fatty Acid. Besides checking the ICV, the cloud point of 9

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

the oil is another way to check the quality of the palm oil. The cloud point test is done by slowly cooling the oil sample. The temperature of the oil when it changes from clear liquid to cloudy is recorded. This temperature is taken as the cloud point. Palm stearin is the solid phase of RBD-palm oil fractionation while palm mid fraction is the solid phase of palm olein fractionation. Even though both palm stearin and palm mid fraction are the solid phases of the dry fractionation process, it seems that they have different physicochemical properties. The main reason is RBD-palm oil and palm olein which served as raw materials for dry fractionation have different levels of unsaturation.

At the end of the experiment, we have obtained the IVs of olein and stearin are 3.06 and 2.52 respectively. From the first dry fractionation, According to Knothe (2002), IV was used as a general measure of the unsaturation of the oil. IV shows the amount of double bonds present in the fatty acids. As the oil is more liquid (less saturated), it will impart a higher IV. So the IV of olein must be higher than the stearin. This is due to the composition of stearin which is more saturated than olein and super olein respectively.

Yield becomes higher when coolant temperature increased. This confirms the theory that the yield has a correlation with coolant temperature, where a better yield needs high range of temperature. The common yield of olein from dry fractionation or conventional fractionation using vacuum suction filter gives a yield of 65-68%. Therefore, the results obtained from this study are acceptable because the production of yield that we get are 60% that are near to theoretical.

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CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

5.0 CONCLUSION This experiment was assigned in order for the student to understand more about the concept of the dry fractionation of the RBD oil. The fractionation itself are the process where there is a procedure for adding value to an oil or fat by separating it into two (or more) fractions differing in fatty acid and triacylglycerol composition where this will change affect the physical properties and so increase oil range of usefulness. Theoretically, it can be said, from the fractionation it will produce two different phase which are solid known as the stearin fraction and also the liquid which are the olein fraction. Stearin is said to be a crystal which less soluble, higher melting and also more saturated compared to he olein fraction. From the result, it can be conclude that result of iodine value RBD palm olein have recorded the highest iodine value which is 3.06 compared to RBD palm oil feed and RBD palm oil stearin which is 2.97 and 2.52. The influence of these parameters such as crystallization temperature, cooling rate and agitation speed during the fractionation process need to be taken into consideration in order to obtain a good quality olein and stearin fraction. Based on the past study, Crystallisation temperature and cooling has an influence on the chemical property of the olein fraction but not for the stearin fraction. On the 11

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

other hand, agitation speed does not have any effect on both the chemical properties of olein and stearin fraction. 6.0 RECOMMENDATIONS In order to obtain a good results in this experiment, some errors should be avoided and precaution steps must be taken throughout the experiment. Firstly, ensure the filter press have optimum pressure so that the oil can be separated nicely. Then, ensure the filter press is clean before proceeding the experiment to avoid any presence of contaminant in the final product. The temperature must be controlled correctly in order to have a good texture of product. Next, during the analysis, the titration method must be done by dropping the potassium hydroxide, KOH slowly while shaking the conical flask to observe the change. Besides, the volume of any chemicals used must be accurate to the amount required. Therefore, by following these recommendations, the results obtained might be accurate or closer to the theoretical value.

7.0 REFERENCES 1. Dry Fractionation. (n.d.). Retrieved December 18, 2016, from http://lipidlibrary.aocs.org/OilsFats/content.cfm?ItemNumber=40328 2. Radiation Pneumonitis. (n.d.). Encyclopedia of Cancer, 2520-2520. doi:10.1007/978-3540-47648-1_4904 3. Crystallization of Fats and Oils. (n.d.). Retrieved December 18, 2016, from http://onlinelibrary.wiley.com/doi/10.1002/047167849X.bio021/full 4. Razam, Ab. Latib (2013). Journal of Peer-Reviewed & Open Access: Palm -based diacylglycerol fat dry fractionation: effect of crystallisation temperature, cooling rate and agitation speed on physical and chemical properties of fractions. Retrieved from 5. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3654720/ 6. Nusantoro, B. P. (2007). DRY FRACTIONATION OF RBD . Agritech, 171-175. 7. Ribeiro, A. P. (2015). Crystallization modifiers in lipid systems. PMC, 3925– 3946.

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CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

8. CEF. (n.d). What is Biodiesel? Retrieved December 21, 2016, from Conserve Energy Future: http://www.conserve-energyfuture.com/Advantages_Disadvantages_Biodiesel.php 9. MPOC. (n.d). ONE OF THE WORLD'S LARGEST PALM OIL EXPORT. Retrieved December 21, 2016, from Malaysia Palm Oil Industry: http://www.mpoc.org.my/Malaysian_Palm_Oil_Industry.aspx 10. MPOB. (2016). About palm oil. Retrieved from http://www.palmoilworld.org/about_palmoil.html

11. Online, T. S. (2016, August 18). Palm oil enters bull market as demand rises. Retrieved December 21, 2016, from The Star Online: http://www.thestar.com.my/business/businessnews/2016/08/18/palm-oil-enters-bull-market-as-demand-rises/ 12. Tverbeg, G. (2013, January 17). Ten Reasons Why High Oil Prices are a Problem. Retrieved December 21, 2016, from Our Finite World: https://ourfiniteworld.com/2013/01/17/ten-reasons-why-high-oil-prices-are-a-problem/

8.0 APPENDICES

Figure 1: Stearin (solid-phase) 13

CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

Figure 2: Group members with the product of dry fractionation(stearin)

Sample Calculation Production Yield

Weight of Olein Produced ×100 Weight of RBD palm oil feed

=

=

4.80 × 100 8.00

= 60 % Iodine Value, IV IV =

12.69 C (V 1−V 2 ) M

Where,

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CPB30303- Oil and Fat Process Technology Experiment 1: DRY FRACTIONATION of RBD OIL

C: concentration of the sodium thiosulphate solution (mol/L) V1: volume of sodium thiosulphate solution used for blank sample (ml) V2: volume of sodium thiosulphate solution used for the determination (ml) M: mass of the test sample (g) Sample calculation of IV value of RBD Palm Oil Feed: IV =

12.69( 0.1 mol/ L)(25.1 ml−18.8 ml) = 3.05 3.0 g

Sample calculation of IV value of RBD Palm Olein: IV =

12.69(0.1 mol/ L)(25.1 ml−18.2 ml) 3.0 g

= 2.92

Sample calculation of IV value of RBD Palm Stearin: IV =

12.69(0.1 mol/ L)(25.1 ml−19.1 ml) 3.0 g

= 2.54

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