Extraction and Characterization of Terminalia Catappa Seed Oil

EXTRACTION AND CHARACTERIZATION OF TERMINALIA CATAPPA SEED OIL
Extraction and Characterization of Terminalia catappa Seed Oil
Caipang, Cris Jhon G. Radomes, Ma. Vernadith B. Serrano, Romina R. Technological Institute of the Philippines
APPROVAL SHEET
This is to certify that we have supervised the preparation of and read the research paper prepared by Cris John G. Caipang, Ma. Vernadith B. Radomes and Romina R. Serrano entitled Extraction and Characterization of Terminalia Catappa Seed Oil and that the said paper has been submitted for final examination by the Oral Examination Committee. As a member of the Oral Examination Committee, we certify that we have examined this paper and hereby recommend that it be accepted as fulfillment of the research requirement for the Degree of Bachelor of Science in Chemical Engineering.
Engr. Norman Giovanni M. Guevarra Academe Adviser
This research is hereby approved and accepted by the Chemical Engineering Department as fulfillment of the ChE Research Methods requirement for the Degree of Bachelor of Science in Chemical Engineering. ______________________________ Engr. Lorraine A. Carrillo ChE Department Chair
ACKNOWLEDGEMENT Having this research finished is such an accomplishment for the authors. It was undeniably a great occurrence doing this project not only because they were able to generate a superior research but mostly because of the comradeship they developed while working. However, this research would not have been feasible without the support of many people who helped them achieved all of these and with that, they are extending their genuine and heartfelt appreciation to the following. First, to their beloved parents, who, from the start have given their full support in all of the authors endeavors and who have served as their inspiration through the duration of this research. To Engr. Norman Giovanni M. Guevarra, their mentor, who was abundantly helpful and offered invaluable assistance, support, and guidance in teaching them all the things needed for the completion of this research. Deepest gratitude is also due to Ms. Remy, Mr. Ryan, Mr. Danilo, and Mr. Danison for their invaluable help in our laboratory work. The authors would also like to convey thanks to Mr. and Mrs. Rodrigo Pedraza for providing us the Terminalia Catappa Seed for without them this research would not have been successful. To their friends, who, although busy with their project, still manage to lend a hand to them in their own ways. To Jeffrey Lleno, Sarah Garme, and Kristel Ycong for the hilarity as well as gossips which somehow alleviated the pressure and stress while working. And most importantly, to the Almighty God for all the provisions He gave, for the knowledge, wisdom, patience and all the necessities that were provided to the authors before, during and after this research. The Honor and Glory be unto You.
ABSTRACT This research paper carried out experimental study, through extraction and characterization of Terminalia Catappa Seed Oil. Soxhlet apparatus was used as an extractor and methanol as a solvent in extraction process. Separation of oil and methanol occur in distillation process. The oil produced was undergo characterization analysis using different parameters, which includes moisture content 4.57% , specific gravity 0.9162 SG, viscosity 4.8773 cP at 40C, pH 7.29, refractive index 4.8773, acid value 111.9 mg KOH/ 1 g sample, iodine value 10.56 and free fatty acid value such as oleic 42.70%, lauric 30.28% and palmitic 38.76%. According to the Philippine National Standards the acid value of a suitable biodiesel is 0.50max mg/KOH g oil and for Terminalia catappa we have 111.9 mg/KOH g oil. For moisture content the maximum value was 0.05% and we have a 4.57% and for viscosity 2.0-4.5 cP and for Terminalia catappa we have 4.877cP. These properties can be change since the extracted oil is not yet treated to be a biodiesel. Regarding on the free fatty acid previous researches have an analysis of the following palmitic 35.97-37.78%, linoleic 28.93-32.89% and oleic 31.88- 33.12%. Improving the specification will depend on the parameters and process of transesterification. Our results showed that Terminalla catappa have great potential to use as feedstock for biodiesel production. Keywords: Terminalla catappa, extraction, characterization, oil, soxhlet apparatus
TABLE OF CONTENTS
Title Page Approval Sheet Acknowledgement Abstract Table of Contents List of Tables List of Figures Chapter 1: Introduction General Objective Specific Objectives Significance of the Study Scope and Delimitations Chapter 2: Review of Literature Terminalia catappa and Terminalia catappa seed Alternative crops for biodiesel feedstock Ideal biodiesel source Physical and physicochemical properties of oil Physicochemical properties Chemical testing of fats and oil Acid value Free Fatty acid value Iodine value
1 2 3 4 5 6 7 10 11 11 11 12 13 13 15 15 16 17 18 18 18 10
Theoretical framework Definitions Chapter 3: Research Methods Technical/ experimental method Materials and methods Seed processing Terminalia catappa oil extraction Determination of Moisture Content of the Seeds Determination of the Percentage of Terminalia catappa Seed Oil Extracted Characterization of the Extracted Terminalia catappa Oil Determination of acid value Determination of free fatty acid Determination of iodine value Determination of specific gravity Determination of viscosity Determination of refractive index Determination of pH value Chapter 4: Result and Discussion Tabulated data Analysis and Interpretation Chapter 5: Summary of Findings, Conclusion and Recommendation Conclusion Recommendation References
20 21 22 23 26 26 26 27 27 27 27 28 29 29 30 30 31 32 35 40 43 45 46 47
LIST OF TABLES
Table 1: Proximate composition of Terminalia catappa Seed oil Table 2: Physicochemical properties of Terminalia catappa seed oil Table 3: Moisture Content of Terminalia Catappa Oil Table 4: Extraction of Oil using Soxhlet extractor/ Percentage of Oil extracted Table 5: Determination of Specific Gravity Table 6: Determination of pH Value Table 7: Determination of Refractive index Table 8: Determination of Viscosity Table 9: Determination of Acid value Table 10: Determination of Free fatty Acid Value Table 11: Determination of Iodine value Table 12: Summary of Physical Properties of Terminalia Catappa Seed Oil Table 13: Summary of Physico chemical Properties of Terminalia Catappa Seed Oil
17 18 33 34 35 35 36 36 37 38 39 40 41
LIST OF FIGURES
Figure. 1: Teminalia catappa tree Figure 2: Terminalia catappa Seed Figure. 3: Theoretical framework Figure. 4: Solvent extraction Figure. 5: Distillation Figure. 6: Ground Terminalia catappa seed Figure. 7: Mixture of Oil and Methanol after extraction Figure. 8: Chemicals used in extraction and experimentation Figure. 9: Terminalia catappa oil
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Chapter 1 THE PROBLEM AND ITS BACKGROUND
Introduction Energy is an integral part of a society and plays a pivotal role in its socio-economic development by raising the standard of living and the quality of life. The state of economic development of any region can be assessing from the pattern and consumption quality of its energy. Energy demand increases as the economy grows bringing along a change in the consumption pattern, which in turn varies with the source and availability of its energy, conversion loss and end use efficiency. Through the different stages of development, humankind has experimented with various sources of energy ranging from wood, coal, oil and petroleum to nuclear power. But indiscriminate exploitation of resources and unplanned developmental activities has led to serious ecological and environmental problems. The use of edible vegetable oils and animal fats for biodiesel production has recently been of great concern because they compete with food materials. As the demand for vegetable oils for food has increased tremendously in recent years, it is impossible to justify the use of these oils for fuel use purposes such as biodiesel production. Moreover, these oils could be more expensive to use as fuel. Hence, the contribution of non-edible oils such as Terminalia catappa will be significant as a non edible plant oil source for biodiesel production. Its availability and low cost its one of its advantage to be a good source of biodiesel. Biodiesel was the fuel used in the first diesel engines. Compared to petroleum diesel, biodiesel combustion produces less sulfur oxides, particulate matter, carbon monoxide, and unburned and other hydrocarbons, but more nitrogen oxide. Similar to ethanol, biodiesel use may
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result in lower net-carbon dioxide emission if the sources of biodiesel are oils made from plants, which absorb carbon dioxide. The Talisay tree (Terminalia catappa L.) is also called the "Indian almond", "tropical almond" or "sea almond". It is a deciduous shady tree often grown in the Philippines for ornamental purposes. This tree thrives as an ornamental tree in many tropical cities in the world. Tropical almond is a large deciduous stately tree, originally from India, growing up to 90 feet tall with horizontal whorls of branches offering clusters of foot long; obviate leaves.
Objectives General Objective: The goal of the study is to evaluate the potential of some underutilized oils such as Terminalia catappa as raw material for biodiesel production. Specific Objectives: a. Extraction of Terminalia catappa oil from Terminalia catappa seed through solvent extraction process b. c. To investigate the oil content from the seeds of Terminalia catappa. Characterization of Terminalia catappa seed oil for easy identification, and also to assess its quality.
Significance of the Study With concerns of environmental pollution and high prices of fossil fuels production, use of biodiesel is promoted globally. The use of biodiesel as an alternative source of transportation energy is promoted via national and international legislation and protective measures because; biofuel production enhances sustainability and economic growth (Bezergianni and Kalogianni,
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2009). And using a non food crops as an alternative feedstock to produce biodiesel would reduce the usage of food crops that we need in our daily lives that may can cause unbalance in our food cycle This study serves as a significant basis in discovering new sources of biodiesel by the information that this research will be gained.
Scope and Delimitation of the Study This study focused on extraction and characterization of Terminalia catappa seed oil. By experimentation and investigation of the potential of Terminalia catappa seed as a source of biodiesel, operation on solvent extractor was used to extract oil from the seed and the characterization of the oil was carried out using standard analytical methods such as titration. (acid value, free fatty acid, iodine value) will be determine. Further analysis to convert Terminalia catappa oil to biodiesel were not included, only having an information of its composition whether Terminalia catappa are capable to be one of the sources of biodiesel.
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Chapter 2 THEORETICAL FRAMEWORK AND RELATED LITERATURE
Related Literature / Studies Terminalia catappa Tropical almond (Terminalia catappa) is a large, spreading tree now distributed throughout the tropics in coastal environments. The tree is tolerant of strong winds, salt spray, and moderately high salinity in the root zone. It grows principally in freely drained, well aerated, sandy soils. The species has traditionally been very important for coastal communities, providing a wide range of non-wood products and services. It has a spreading, fibrous root system and plays a vital role in coastline stabilization. It is widely planted throughout the tropics, especially along sandy seashores, for shade, ornamental purposes. The timber makes a useful and decorative generalpurpose hardwood and is well suited for conversion into furniture and interior building timbers. Fruits are produced from about 3 years of age, and the nutritious, tasty seed kernels may be eaten immediately after extraction. Tropical almond is easily propagated from seed, and is fast growing and flourishes with minimal maintenance in suitable environments. Selected cultivars of the species warrant wider commercial planting for joint production of timber and nuts. The tree has a demonstrated potential to naturalize in coastal plant communities, but not to adversely dominate
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. Figure. 1 Terminalia catappa tree
Seeds In the Pacific islands trees exhibit large variations in the size and shape of fruits, nuts, and kernels, but it is difficult to classify this variation. For example, in Vanuatu, the nuts can be 3.9 5.1 long by 2.63.8 cm across (1.52 x 11.5 in) and weigh 714 g (0.250.5 oz). Kernels are in the size range of 2.24.4 x 81.4 cm (0.91.7 x 0.30.6 in) and weigh 0.10.9 g (0.040.32 oz). The percentage kernel content varies from 1% to 10%. The rind of the fruit is a light, pithy, or corky tissue that enables the fruit to float and be dispersed by sea currents. Trees are also found away from coasts due to fruits being carried inland and dropped by frugivorous birds and bats, and as a result of deliberate planting by humans.
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Figure. 2 Terminalia catappa seed
Alternative crops for biodiesel feedstock Biodiesel, the name popularly given to fatty acid alkyl esters, has become an attractive option for the replacement of petroleum diesel (petrodiesel). While its overall impact on the greenhouse effect continues to be debated, other qualities of biodiesel are unquestioned. Biodiesel is biodegradable, generally non-toxic and has superior lubricity to petrodiesel. Overall emissions are greatly reduced. The bulk of the feedstock for its production comes from renewable resources and when biodiesel is used as a blend (up to 20%); no changes are required for existing diesel engines. However, it is still too costly and about 60 80% of the cost for biodiesel comes from the feedstock. Concerns have been raised about the propriety of using food for fuel. Proposed alternative feedstock such as Jatropha curcas address some of these concerns but have their own disadvantages. Legitimate concerns have also been raised about the possible effect of using vegetable oils for fuel on food prices.
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Capacity expansion may lead to a decrease in availability of land for food crops along with the overall negative effect on climate change. The enormous demand for diesel fuel dwarfs the available supply of vegetable oils.
Ideal biodiesel source Though a considerable number of publications about biodiesel can be found in literature, several problems remain unsolved, encompassing economical, social, and technical issues. Thus, the biodiesel industry has come under attack by some environmental associations, and subsidies for biofuel production have been condemned by some governments. Yet, biodiesel may represent a truly competitive alternative to diesel fuel, for which fuel tax exemption and subsidies to energetic crops are needed. Biodiesel must increase its popularity among social movements and governments to constitute a valid alternative of energy source. In this sense, the use of non edible oils to produce biodiesel is proposed in the present review. Moreover, the compromise of non interference between land for energetic and food purposes must be addressed. In most cases, a common recipe to produce biodiesel from any raw material has been adopted, Considering sustainable vegetable oils, biodiesel from Calophyllum inophyllum, Azadirachta indica, Terminalia catappa, Madhuca indica, Pongamia pinnata, and Jatropha curcas oils fits both current biodiesel standards.(European EN 14214 and US ASTM D 6751 02. S. Pinzi)
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Physical and physicochemical properties of oil Table 1. Proximate composition of Terminalia catappa Seed Constituents Oil Protein Carbohydrate Fiber Ash Moisture Percentage composition SEM 56.711.66 26.300.14 6.500.38 4.400.01 4.550.45 1.540.29
The table shows the proximate composition of Terminalia catappa based on Kinetics of autoxidation of an oil extract from Terminalia catappa by Omeje EO, Okide GO, Esimone CO, Ajali U. The different constituents that analyze are the Oil yield, Protein, Carbohydrates, Fiber, Ash and Moisture content of the oil. Table 2: Physicochemical properties of Terminalia catappa seed oil. Analysis/determination Physical state at room temperature Color Odor Specific gravity Density Refractive index Viscosity (cps) Acid value Peroxide value Saponification value Unsaponifiable matter Values SEM Crude oil Liquid Golden Yellow Pleasant 0.95210.08 0.94000.02 1.46460.04 40.791.05 3.53430.14 8.590.06 166.23.69 1.480.002 Refined oil Liquid Golden yellow Pleasant 0.92000.10 0.91200.03 0.46400.06 36.800.94 3.25000.11 8.630.03* 157.82.88 1.020.001
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Iodine value
38.591.14
38.631.06
The table shows the physicochemical properties of Terminalia catappa crude and refined oil. Different analysis was taken to determine the value of each component such as acid value, iodine value, refractive index and determination of viscosity as what the researcher done in their research.
Chemical testing of fats and oils In view of the variety and inherent variability of the sources from which oils and fats are obtained, it is important to characterize these materials using a series of specially designed test procedures.
Acid value Acid value is defined as the number of milligrams of potassium hydroxide required to neutralize 1 gram of the sample under test and is the measure of the total free fatty acids content of the material as a consequent heat damaged and deterioration by fungal. This can impart the higher acid value, odors and color changes to extracted oil. Acid value will vary over a considerable range, depending on the quality of the material being tested, such as the initial moisture content of the seed, storage time and temperature at which the seed is stored. It is necessary to control these conditions in order to maintain the AV value at lower level. Concerning the control of fungal growth, iti is common knowledge that the water activities above 0.65 is needed for corresponding to a moisture content of approximately 9 % dry mass basis at temperature above 25C. Thus the moisture content of the seeds should not excess 8 % dry mass basis for avoiding deterioration during storage caused by fungal growth.
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Free Fatty acid value The fatty acid varied in their carbon chain length and in the number of double bonds. Three fatty acids are linked to one glycerol molecule to form triglyceride which is accounted for 98% of the components found in vegetable oil. It is important to have a simple, reliable and accurate method to estimate the fatty acid and its composition. Saponification is a common and a general step for determination the average molecular weight of fatty acids found in triglyceride molecule.
Iodine value The iodine value is the mass of iodine in grams that is consumed by 100 grams of a chemical substance. An iodine solution is yellow/brown in color and any chemical group in the substance that reacts with iodine will make the color disappear at a precise concentration. The amount of iodine solution thus required to keep the solution yellow/brown is a measure of the amount of iodine sensitive reactive groups. One application of the iodine number is the determination of the amount of unsaturation contained in fatty acids. This unsaturation is in the form of double bonds which react with iodine compounds. The higher the iodine number, the more unsaturated fatty acid bonds are present in a fat. In a typical procedure the acid is treated with an excess of the Hanus solution which is a solution of iodobromine (BrI) (or Wij's iodine solution which a solution of iodine monochloride (ICl) in glacial acetic acid). Unreacted iodobromine (or iodine monochloride) is reacted with potassium iodide which converts it to iodine. The iodine concentration is then determined by titration with sodium thiosulfate.
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Theoretical framework
Raw material: Terminalia Catappa
Terminalia catappa seed are gathered from Nasugbu, Batangas.
Solvent Extraction
Methanol was used to extract the oil from Terminalia catappa seed.
Separation of Solvent
Distillation process was used to separate methanol from oil.
Removal of Solid from Oil
Filter paper was used to remove the solid particles from oil.
Characterization of Extracted Oil
Different parameters such as iodine value, free fatty acid value and acid value were used to characterize the oil.
Fig. 3. Theoretical framework of Extraction and Characterization of Terminalia catappa Seed Oil.
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Definition of Terms
Biodiesel - a fuel made primarily from oily plants (such as the soybean or oil palm) and to a lesser extent from other oily sources (such as waste cooking fat from restaurant deep-frying). Chemical Testing - is a qualitative or quantitative procedure designed to prove the existence of, or to quantify, a chemical compound or chemical group with the aid of a specific reagent. A presumptive test is specifically used in medical science. Distillation- is a method of separating mixtures based on differences in their volatilities in a boiling liquid mixture. Distillation is a unit operation, or a physical separation process, and not a chemical reaction. Extraction - the process of extracting one material from another by washing with a solvent to remove adsorbed material from an adsorbent (as in washing of loaded ion-exchange resins to remove captured ions Iodine Value - or "iodine adsorption value" or "iodine number" or "iodine index") in chemistry is the mass of iodine in grams that is consumed by 100 grams of a chemical substance. pH Value - is a measure of the acidity or basicity of a solution. Refractive Index - or index of refraction of a substance is a measure of the speed of light in that substance. It is expressed as a ratio of the speed of light in vacuum relative to that in the considered medium.
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Titration - is a common laboratory method of quantitative chemical analysis that is used to determine the unknown concentration of a known reactant.
Chapter 3 METHODS OF RESEARCH Technical / Experimental Design Solvent extraction A Soxhlet extractor is a piece of laboratory apparatus invented in 1879 by Franz von Soxhlet. It was originally designed for the extraction of a lipid from a solid material. However, a Soxhlet extractor is not limited to the extraction of lipids. Typically, a Soxhlet extraction is only required where the desired compound has a limited solubility in a solvent, and the impurity is insoluble in that solvent. If the desired compound has a significant solubility in a solvent then a simple distillation can be used to separate the compound from the insoluble substance. Normally a solid material containing some of the desired compound is placed inside a thimble made from thick filter paper, which is loaded into the main chamber of the Soxhlet extractor. The Soxhlet extractor is placed onto a flask containing the extraction solvent. The Soxhlet is then equipped with a condenser. The solvent is heated to reflux, and floods into the chamber housing the thimble of solid. The condenser ensures that any solvent vapor cools, and drips back down into the chamber housing the solid material. The chamber containing the solid material slowly fills with warm solvent. Some of the desired compound will then dissolve in the warm solvent. When the Soxhlet chamber is almost full, the chamber is automatically emptied by a siphon side arm, with the solvent running
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back down to the distilling flask. This cycle may be allowed to repeat many times, over hours or days. As the figure showed the researcher was set up the Soxhlet apparatus to extract oil from Terminalia catappa seed.
Figure. 4 Solvent extraction
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Distillation After extracting the oil from Soxhlet apparatus the researcher used distillation process to separate oil from methanol, methanol that is recovered can used again as a solvent to extract oil from extraction process Distillation is a method of separating mixtures based on differences in their volatilities in a boiling liquid mixture. The vapors of the distilling compounds and the distillate change during the distillation. A still is charged (supplied) with a feed mixture, which is then separated into its component fractions which are collected sequentially from most volatile to less volatile, with the bottoms (remaining least or non-volatile fraction) removed at the end. The still can then be recharged and the process repeated.
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Figure. 5 Distillation
Material and Methods Seed processing The Terminalia catappa seed undergo various processing in the course of its preparation for extraction. The unit operations involved are: Clearing: The Terminalia catappa fruit had some foreign materials and dirt which was separated by hand picking. Drying: The cleaned fruits were sun dried in the open, until the casing splits and sheds the seeds. Winnowing: The separation of the shell from the nibs was carried out using hammer or knife to remove the cover of the seeds.
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Grinding (size reduction): Grinding machine was used to pulverize the seeds.
Terminalia catappa oil extraction 150ml of methanol was poured into round bottom flask. 30g of the Terminalia catappa seed oil was placed in the thimble and was inserted in the centre of the extractor. The Soxhlet was heated at 60 C. When the solvent was boiling, the vapor rises through the vertical tube into the condenser at the top. The liquid condensate drips into the filter paper thimble in the centre, which contains the solid sample to be extracted. The extract seeps through the pores of the thimble and fills the siphon tube, where it flows back down into the round bottom flask. This was allowed to continue for different time interval depending on the ratio of methanol and the seed,. At the end of the extraction, the resulting mixture containing the oil was distilled to recover solvent from the oil.
o
Determination of Moisture Content of the Seeds 40g of the cleaned Terminalia catappa oil was weighed and dried in an oven at 80C for 7hrs and the weight was taken after every 2hrs. The procedure was repeated until a constant weight was obtained. After each 2 hours, the sample was removed from the oven and placed in the dessicator for 30 minutes to cool. It was then removed and re-weighed. The percentage moisture in the seed was calculated from the formula:
where W1 = Original weight of the sample before drying; W2 = Weight of the sample after drying.
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Determination of the Percentage of Terminalia catappa Seed Oil Extracted 30g of the Terminalia catappa oil was placed in the thimble and about 150ml of methanol was poured into the round bottom flask. The apparatus was heated at 60C and allowed for 3hrs continuous extraction using Soxhlet apparatus. The experiment was repeated for different weights of the sample, 35g, 40g and 50g. At the end, the solvent was distilled and the percentage of oil extracted was determined.
Characterization of the Extracted Terminalia catappa Oil Determination of Acid Value Potassium Phthalate is heated in the oven at 100C for 2 hours then place in dessicator to cool, 0.5 g Potassium Phthalate is weigh to dissolve in 50 ml distilled water in an Erlenmeyer flask. 4 drops of phenolphthalein indicator is added then titrate to Potassium Hydroxide solution to its end point (pale pink).
2 grams of sample was weigh in an Erlenmeyer flask, 50 ml dissolving solution was added and shake it vigorously .4 drops of phenolphthalein indicator was added then titrated it to KOH solution until its end point. Computation:
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Determination of Free Fatty acid Two grams of the Terminalia catappa oil was weighed into a 250 ml Erlenmeyer flask. 50 ml of neutralized Ethyl Alcohol and 2ml phenolphthalein indicator was then added. Standard sodium hydroxide is titrated in a vigorously shaking until the appearance of the first permanent color of the same intensity as that of the neutralized alcohol before the addition of sample. The color must persist for 30 seconds. Calculations:
Determination of Iodine Value 25ml of standard dichromate solution is pipette to Erlenmeyer flask.5 ml of HCl and 10 ml of KI solution is added and mix thoroughly allow to stand for 5 minutes then 100 ml distilled water is added. Sodium thiosulfate solution is titrated in a shaking motion continuously until the yellow color has almost disappeared.
10ml chloroform is added in weigh sample in iodine flask of, then 10 ml of 0.1 mol Wijs solution is added also. Put stopper in the flask then mix and stand on the dark for 30 minutes. 10ml of KI
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solution was added. Then 0.1 N sodium thiosulfate is titrated to become faint yellow color.2ml of starch solution is added and titrated to the end point.(Vs). Run a blank (Vb) using the same quantities of reagents under the same conditions.
Determination of Specific Gravity Density bottle was used to determine the density of the Terminalia catappa oil. A clean and dry bottle of 25ml capacity was weighed (W0) and then filled with the oil, stopper inserted and reweighed to give (W1). The oil was substituted with water after washing and drying the bottle and weighed to give (W2). The expression for specific gravity (Sp.gr) is:
Determination of Viscosity A clean, dried viscometer with a flow time above 200 seconds for the fluid to be tested was elected. The Terminalia catappa oil was filtered through a sintered glass (fine mesh screen) to eliminate dust and other solid material in the liquid sample. The viscosity meter was charged with the sample by inverting the tubes thinner arm into the liquid sample and suction force was draw n up to the upper timing mark of the viscometer, after which the instrument was turned to its normal vertical position. The viscometer was placed into a holder and inserted to a constant temperature bath set at 40C and allowed approximately 10 minutes for the sample to come to the bath temperature at 40C. The suction force was then applied to the thinner arm to draw the sample
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slightly above the upper timing mark. The afflux time by timing the flow of the sample as it flow freely from the upper timing mark to the lower timing mark was recorded. Determination of Refractive Index Refractometer was used in this determination. Few drops of the Terminalia catappa oil were transferred into the glass slide of the refractometer. Water at 30C was circulated round the glass slide to keep its temperature uniform. Through the eyepiece of the refractometer, the dark portion viewed was adjusted to be in line with the intersection of the cross. At no parallax error, the pointer on the scale pointed to the refractive index. This was repeated and the mean value noted and recorded as the refractive index. Determination of pH Value 2g of the Terminalia catappa oil was poured into a clean dry 25ml beaker and 13ml of hot distilled water was added to the sample in the beaker and stirred slowly. It was then cooled in a cold-water bath to 25C. The pH electrode was standardized with buffer solution and the electrode immersed into the sample and the pH value was read and recorded. Chapter 4 PRESENTATION, ANALYSIS AND INTERPRETATION Terminalia catappa seed was easily to crushed like peanut. The researcher used grinding machine to ground the seed after that the seed should place in a warm and open bin for it will not moist in plastic container after grinding. The seed is place in the thimble inside the soxhlet apparatus.
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Figure. 6 Ground Terminalia catappa seed The figure shows the mixture of oil and methanol after extraction process the researcher have 3 to 4 batches of 50 grams and 150 ml of methanol everyday and the extraction process was operating 8 to 12 hours per day and after one week we attain this amount of mixture. Oil was obtained using soxhlet apparatus for extraction.
Figure. 7 Terminalia catappa oil with methanol after extraction Methanol was used as a solvent for extraction process; the researchers consume 1 liter of methanol per day depending on the batches of extraction. The chemicals that used in characterization are 0.1 N Sodium thiosulfate, 1 % starch indicator, Chloroform, Potassium iodide etc. in different analysis conducted All of the chemicals were bought at Crismon Enterprise Bambang, Manila
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Figure. 8 Chemicals used in Extraction and Experimentation After extraction the researcher get the oil and methanol mixture This mixuture is distilled to separate the oil from methanol. The distillation process takes 1 to 2 hours depending on the volume of mixture you pour on the distilling flask and it should not take too long for the oil will be burn and change it physical properties as what we observe.
Figure. 9 Terminalia catappa seed oil Tabulated data Results are obtained from various tests carried out on the sample are tabulated below. Using the formulas as indicated in the Methods and Materials, physical properties of the Terminalia Catappa Seed Oil were evaluated and results are presented in a Table4.1.1-Table 4.1.5 separately.
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Table 3. Moisture Content of Terminalia Catappa Oil
Sample (W1) a. 40.2042 grams weight sample b. 40.3002 grams weight sample c. 40.2165 grams weight sample
Time 2 hours in oven then 30 mins. in dessicator 2 hours in oven then 30 mins. in dessicator 2 hours in oven then 30 mins. in dessicator
Weight after (W2) 39.1526 grams
Moisture Content 2.69%
38.843 grams
3.75%
37.494 grams
7.26%
Average Moisture Content:
4.57%
Determination of moisture content takes 3 trials at 40 grams Terminalia catappa oil sample. The Terminalia catappa oil place in oven at 2 hours and after that it place in dessicator at 30 minutes and weigh. To get the percent moisture content equation 3.2.3 was used. Based on the tabulated data, the results obtained showed that the seeds contained the average of 4.57% moisture content.
Table 4. Extraction of Oil using Soxhlet extractor/ Percentage of Oil extracted
Sample
Time of extraction
Oil produce (not distilled)
Time of distillation
Oil produce (pure)
% Oil Extracted
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35 grams of seed,150ml methanol
8am to 1pm
112ml
1:28pm to 2:14 pm
Oil produce: 25ml Recovered methanol: 81ml Oil produce: 22ml Recovered methanol: 62 ml Oil produce: 30ml Recovered methanol: 65ml
22.32%
45 grams of seed, 150 ml. methanol
8am to 12pm
102ml
1:28pm to 2:14 pm
21.57%
50 grams of seed, 150 ml methanol
8:15 am to 12pm
105ml
8:48am to 10:30am
28.57%
Average Percentage Oil Yield:
24.15%
Percentage of oil takes place in three different weigh sample, 35 grams, 45 grams and 50 grams. The solvent used was methanol and each sample has same volume which is 150 ml. each. The time of extracting the oil takes place at 8am to 12pm, the oil produce was tabulated and after the extraction process the mixture of oil and methanol is distilled to separate oil from methanol. The methanol that is recovered can be used in another extraction process. Based on the data gathered, the results showed that the Terminalia Catappa seed oil contained the average of 24.15% oil yield. Variation in oil yield may be due to the differences of time extraction using soxhlet apparatus.
Table 5. Determination of Specific Gravity
Sample
Values Obtained
Computed Specific gravity
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a.
Wo: 21.2244 grams W1: 51.5959 grams W2: 54.4098 grams Wo: 21.2244 grams W1: 51.7920 grams W2: 54.5197 grams Wo: 21.2244 grams W1: 51.6090grams W2: 54.4132 grams Average Specific Gravity:
0.9152
b.
0.9178 0.9155
c.
0.9162 SG
Equation 3.3.5 was used to compute the specific gravity of the oil. The three samples were taken and reweigh using the density bottle. The following procedure was detailed on Materials and Methods the computed specific gravity showed 0.9162.
Table 6. Determination of Refractive index Sample 1 2 3 Average: Refractive index 1.460 1.390 1.420 1.423
The average refractive index of the oil was 1.423, it was determine using refractometer. Table 7. Determination of pH Value Trial 1 pH 7.68 Temp. 24.7C
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2 3 Average pH:
7.09 7.10 7.29
24.3C 24.5C
pH value was determine to know if the oil is to acidic or basic three samples were taken at the same volume of oil, using a pH meter the pH of oil were determine and based on the tabulated data the average pH is 7.29.
Table 8. Determination of Viscosity Sample 1 2 3 Average: 33.8 / 5.17 33.8 / 5.20 33.8 / 4.54 Viscosity 5.073 5.1033 4.4556 4.8773 cP
Viscosity is more commonly known as resistance to flow, the viscosity of the oil is a measure of the resistance to flow between the individual layers. A high viscosity implies a high resistance to flow while a low viscosity indicates a low resistance flow. Viscosity varies inversely with temperature, In this research the viscosity of oil was determined using a viscometer the experimentation was done in Chemrez Laboratories Inc. and data showed that the average viscosity of Terminalia catappa oil is 6.82 cP. Chemical Analysis
Table 9. Determination of Acid value
36
Trial TRIAL 1 Beq= 1.8 Veq= 28.5 Wt of Sample = 2.0023 g TRIAL 2 Beq= 1.8 Veq= 28.8 Wt of Sample = 2.0038 g TRIAL 3 Beq= 1.8 Veq= 29.2 Wt of Sample = 2.0041 g Average
Acid value
110.58
111.74
113.38 111.9
The acid content in alimentary oil is given by the quantity of free fatty acids deriving from the hydrolytic going rancid of the triglycerides. This alteration occurs under unsuitable conditions of treatment and preservation of the fats and thus the acidity represents a basic indicator of the genuineness of the product. Substances with high water content, such as butter, are more subject to hydrolysis of the fats, and they can alter more easily, assuming the typical unpleasant smell and taste. Oil can reach a high free acid content when they have not been gathered and processed correctly. Furthermore In dried fruit bad storage as, for example, in a damp place causes the hydrolysis of the fats increasing the concentration of non esterifies acids and therefore total acidity. Equation 3.3.1.2 was used to determine the acid value of the oil in three trials the resulting data shown that the average of Acid value of oil is 111.9.
Table 10. Determination of Free Fatty acid
37
Trial TRIAL 1 Wt. of sample=2.0035 g Vol. of NaOH= 30.6 mL TRIAL 2 Wt. of sample= 2.0053 g Vol of NaOH= 30.2 mL
FFA as OLEIC, % FFA as LAURIC, % FFA as PALMITIC, %
TRIAL 3 Wt of sample= 2.0012 g Vol of NaOH= 30.3 mL
Average
42.70%
30.28%
38.76%
The measurement of free fatty acid concentration is important in refining of edible oils and in manufacture of biodiesel. The free fatty acid as Oleic, Lauric and Palmitic was taken in the analysis; equation 3.3.2.1 to 3.3.2.3 was used to determine the free fatty acid. The higher percentage is the Oleic acid which has 42.70%. It is important to know the level of free fatty acid present in the feed stock so the appropriate amount of caustic can be added to react with the FFA and still provide enough concentration to catalyze the reaction between the oil and methanol to produce the maximum amount of the desired biodiesel final product. And as what the tabulated data shown Terminalia catappa have a lower free fatty acid and it is a Oleic- Palmitic acid group.
Table 11. Determination of Iodine value
38
Trial 1 2 3 Average
Result 10.62 10.52 10.55 10.56
Iodine value is measure of unsaturated oil take up iodine the more iodine is attached, the higher the iodine value, the more reactive, less stable, softer and more susceptible to oxidation and rancidification of the oil. In performing the test, a known excess of iodine, usually in the form of iodine monochloride also known as Wijs solution, is allowed to react with a known weight of the oil and then the amount of iodine remaining unreacted is determined by titration. But in researcher case the Wijs solution is not available in laboratory thats why it had been tested on Accuserv Testing Laboratories and as the data shown that the average iodine value is 10.56.
Table 12. Summary of Physical Properties of Terminalia Catappa Seed Oil
39
Property
Terminalia Catappa Seed Oil 4.57% 0.9162
Moisture Content Specific Gravity
Refractive Index
1.42
pH
7.29
Oil Yield
24.15%
Color
Golden yellow
Based on the characterization of oil done in the research the values are partially the same on the value of Terminalia catappa based on the literature that is tabulated in 2.4.1. Table1. Proximate composition of Terminalia catappa seed.
Table 13: Summary of Physicochemical Properties of Terminalia Catappa Seed Oil
40
Experimental data: Property Acid Value Terminalia Catappa Seed Oil 4.57% Oleic: 42.70% Lauric: 30.28% Palmitic: 38.76% 4.8773 4.57% 10.56
Free Fatty Acid Viscosity Moisture Iodine Value
Data from Philippine National Standard for Biodiesel (PNS)

Property Acid value Free fatty acid Viscosity Moisture Iodine value Specifications for Biodiesel 0.50 max 96.5 min. 2.0-4.5 0.05 max 12.0 max
The tabulated shows the Chemical Properties of Terminalia catappa seed oil after the researcher made the characterization some of the analysis was similar to the based on the data of PNS for the specifications of biodiesel.
Chapter 5 SUMMARY OF FINDINGS, CONCLUSIONS, AND RECOMMENDATIONS
41
Summary of Findings Characterization of Terminalia catappa seed oil was done through experimentation, three trials was tested in every characterization of oil and for the result of moisture content the average value was 4.57%. In percentage of oil extracted the average value was 24.15% it was taken after the oil and methanol separated through distillation process and the average specific gravity was 0.9162 SG. The refractive index value was 1.423, pH had an average value of 7.29 using a pH meter, and the average viscosity was 4.8773 cP at 40C. In chemical analysis of Terminalia catappa seed oil the acid value had an average value of 111.9 the free fatty acid value was divided into three analyses which is the free fatty as oleic had an average value of 42.70%, lauric 30.28% and Palmitic 38.76%. And for the determination of iodine value the average value was 10.56 the result is from Accuserv laboratories for it was tested. The researcher was also compared the data result from experimentation to the value of Philippines National Standard for biodiesel. The researcher found out that some of the result in experimentation has differences in value in chemical characteristic of the oil, since the oil is not refined yet. But mostly the value in physical characteristics of oil was the same.
Conclusions
42
The Terminalia catappa seed oil produced in this research work was analyzed for specific gravity of 0.9162, Viscosity at 40C of 4.8773 cP, refractive index at 28C of 1.42, pH of 7.29, moisture content of 4.57%,, acid value of 111.9, free fatty acid value such as oleic 42.70% , lauric 38.76% , and palmitic 30.28%.(mg KOH/g oil) and iodine value 10.56 (mg Na2SO3/g oil). Terminalia catappa L. seed oil is of unsaturated type and contains mainly the fatty acids oleic C18:1(42.70%). The oil can be classified in the oleic-linoleic acid group. Most of the values comply with the previous study Composition and Nutritional Properties of Seeds and Oil From Terminalia catappa L. by L. Matos,et.al. The oil extracts exhibited good physicochemical properties and could be useful for industrial applications. Based on evaluation of data in Philippine National Standard (PNS) for Biodiesel it shows that the acid value required for a biodiesel has a maximum of 0.50, a 111.4 difference on the data of Terminalia catappa seed oil also the iodine value required has a maximum of 12 and the data for Terminalia catappa is 10.56. Basis on Philippine National Standard for Biodiesel is refined oil difference in value may occur because Terminalia catappa seed oil did not undergo the transesterification process, Improving the specification will depend on the parameters and process of transesterification. Results showed that it is the most effective and feasible method to produce the biodiesel using the extracted Terminalia catappa seed oil.
Recommendations
43
The researchers recommend for further study for the physical and chemical properties of Terminalia Catappa Seed Oil for the production of biodiesel. Since analysis to convert Terminalia catappa oil to biodiesel are not included in this research we recommend to research on how the oil from Terminalia catappa will be converted to biodiesel. Also to improve its properties in order to acquire the specifications suitable for a competitive quality of biodiesel.On the extraction process of oil we recommend to use other solvent such as ethanol and hexane aside from methanol, to determine if it is more efficient than methanol as a solvent in extracting oil. Also we recommend using another extractor aside from Soxhlet apparatus to analyze the volume and quality it produces. Methanol that is recovered by separation of oil and methanol in distillation process can be used as a solvent in extraction process. Heating the steam supplied in the distilling flask should be minimal in order not to burn the oil and prevent the changes on physical characteristics of oil such as color.
REFERENCES
44
Pandey A., Boca R. Handbook of Plant-Based Biofuels. CRC Press. 2009
Species Profiles for Pacific Island Agroforestry, Advance Journal of Food Science and Technology Maxwell Scientific Organization 1(1): 72-77, 2009 ISSN: 2042-4876 ver. 2.2, 2006- 2009
Kyari, M.Z, Extraction and characterization of seed oils, Department of Science Laboratory Technology, Ramat Polytechnic, Maiduguri, Nigeria .2008
Akpan, U.G., Jimoh A., and Mohammed A. D. Extraction, Characterization and Modification of Castor Seed Oil Department of Chemical Engineering, Federal University of Technology, Minna P.M.B. 65, Niger State, Nigeria, 2007
Acosta A., Maricela R., Ramrez A., Jess S., Daz P., Reyna Z.J. Extraction and Characterization of Oils from Three Mexican Jatropha Species Mex. Chem. Soc. 2010, 54(2), 88-91 2010, Sociedad Qumica de Mxico ISSN 1870-249X. 2010
Agatemor E., Christian B., Ukhun, Mark E., Nutritional Potential of the Nut of Tropical Almond (Terminalia Catappia L.) Department of Chemistry, Faculty of Physical Sciences, University of Benin, Benin City, Nigeria Pakistan Journal of Nutrition Asian Network for Scientific Information. 5 (4): 334-336, 2006 ISSN 1680-5194. 2006 Studies of Selected Physicochemical Properties of Fluted Pumpkin (Telfairia occidentalis Hook F.) Seed Oil and Tropical Almond (Terminalia catappia L.) Asian Network for Scientific Information Seed Oil Pakistan Journal of Nutrition 5 (4): 306-307, 2006 ISSN 1680-5194
45
Da Silva N., Jhosianna P.V., Serra L., Tatiana. M., Moringa oleifera oil: Studies of characterization and biodiesel production Gossmann Marcelo et.al 2010
Buikema, Brooke., Gabbadon, Stephen., Workman, Produced from Jatropa Seed Oil. 2008
Michael., Lee, Hwok-Chuen., Biodiesel
Thomson , Lex A. J., Evans, Barry. Species Profiles for Pacific Island Agroforestry 2006
Matos L., Nzikou J.M., Kimbonguila A., Composition and Nutritional Properties of Seeds and Oil From Terminalia catappa 2009
Nikoli, Nada ., Caki M, Suzana M., Novakovi, Sanja M., Effect of Extraction Techniques on Yield and Composition of Soybean. 2009
APPENDIX A Sample Problem 1. Determination of moisture content
46
Using this equation:
In trial 1 we have the following value: Sample weight ; W1= 40.2042 grams Weight after the seed places in oven for 2 hours and in dessicator for 30 minutes; W2= 39.1526 grams
Moisture content = 2.69%
2. Determination of Specific Gravity Using this equation:
In trial 1 we have the following value: Weight of the dry bottle, Wo: 21.2244 grams Weight of the dry bottle with Terminalia catappa seed oil, W1: 51.5959 grams Weight of water substituted after the oil was washed in dry bottle, W2: 54.4098 grams
Specific gravity= 0.9152 SG 3. Determination of Free fatty acid value Using this equation:
47
In trial 1 we have the following value: Weight of sample: 2.0035 grams Volume of NaOH titrated: 30.6 ml For Free Fatty acid as Oleic %
For Free Fatty acid as Lauric %
For Free Fatty as Palmitic %
APPENDIX B
48
CFAR No. 04-04-011-CME
CA # DR-11-0111 31 January 2011
CERTIFICATE OF QUALITY
Product Code Description Job Order No. Delivery Receipt No. Lot Number Quantity Customer : : : : : : : Bio-Activ BD 100 Coconut Methyl Ester E216289 28867 1006270628 40,000 L Petron Corporation Bataan
PROPERTIES Clear 0.41 sample,
Test Results
Specification: Clear
Appearance Acid Number, mg KOH/g Carbon Residue on 100%
PNS/DOE QS 002:2007
0.50 max. 0.05 max. 55 min. 5 max.
0.001 70 -4 No. 1a 0.8735
Cetane %mass Number Cloud Point, C Copper Strip Corrosion, 3hrs @ 50C Density @ 15C, kg/L Distillation AET, C 90% volume
No. 1 max. 0.86-0.90 360 max. 96.5 min. 100 min. 0.02 max. 0.24 max.
356 97.12 109 0.004 0.22
FAME Content, %mass recovered Flash Point, C Free Glycerin, %mass Total Glycerin, %mass Glyceride Content, % mass Monoglyceride content Diglyceride content Triglyceride content Group Metals, mg/kg Group I Metals (Na + K) Group II Metals (Ca + Mg)
0.21 0.02 0.04
0.80 max. 0.20 max. 0.20 max.
<1 <1
5.0 max. 5.0 max.
49
Iodine Value, g I2/100g Methanol Content, % m/m Methyl Laurate C12:0, %mass Oxidation Stability @ 110 C, hrs Phosphorus, %mass Pour Point, C Sulfated Ash, %mass Sulfur, %mass Viscosity @ 40C, mm2/s Water & Sediments, % volume 0.01 45.86 11.30 0.00004 -7 0.001 0.00 2.62 0.03
8.05
12.0 max. 0.20 max. 45.0 min. 6.0 min. 0.001 max. To report 0.02 max. 0.05 max. 2.0-4.5 0.05 max.
This Certificate has been issued and found to comply with PNS specifications. Further certify that this material is a fatty acid methyl ester derived from coconut-based feedstock with an ester content of 96.5 mass percent minimum and is not diluted with diesel.
Certified by: Medwin Diogenes E. Visaya QC Chemist I
Noted by: Edgar A. Pantino QC Superviso
CHEMREZ TECHNOLOGIES, INC. QUALITY CONTROL LABORATORY
31 January 2011 Product Code Sampling Date Sampling Time Truck Plate Number Reference CA# : : : : : BioActiv BD100 30 January 2011 2300H ZTU 284 / PUN 964 DR 10 0111
APPENDIX C Sampling Method
50
Fig. 10 Gathering of Seeds Terminalia catappa tree is a large, spreading tree distributed throughout the tropics in coastal environments. The researchers gathered the seeds in Nasugbu, Batangas near the beach. Some of the seeds we found are on the ground that already falls from the tree.
Fig. 11 Drying of Terminalia catappa seed After gathering the seed it should be dried before winnowing, for the shell will easily remove using hammer.
51

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EXTRACTION AND CHARACTERIZATION OF TERMINALIA CATAPPA SEED OIL