This study aims to extract and characterize biodiesel from Musa paradisiaca (banana) fruit peel. Banana peel oil will be obtained using a Soxhlet extractor with natural hexane as the solvent. Purification of extracted oil will be done using 0.73 % and 0.58% NaCl solutions. Extracted oil will be esterified using Sodium hydroxide as a catalyst producing biodiesel. Water wash method will be used to further purify the biodiesel. The volume (mL) and percent yield (%) of both banana peel oil and biodiesel will be computed. Characterization of biodiesel will be based on the values given by ASTM (American Society for Testing and Materials), AOCS (American Oil Chemists Society), ISO (International Organization for Standardization) and EN (European Standard).
Time and Place of Study
The study will be conducted at the Research Laboratory, Philippine Science High School Western Visayas, Jaro, and Iloilo City from March to April 2012.
A. Preparation of Materials and Equipment A.1. Preparation of Raw Material (Musa paradisiaca) Forty kilos of banana peel (Musa paradisiaca) will be obtained from a bananacue stall. The banana peelings will be put in a plastic sack and transported back to Philippine Science High School Western Visayas Campus in the Research Laboratory.
A.2. Preparation of Banana Peel for Extraction A.2.1 Cleaning, Cutting, Blending The banana peels will be washed in distilled water and roughly chopped. Then the peels are soaked within minimum quantity of distilled water. The entire mixture is homogenized in a blender. The homogenized mixture or peel paste should be now transferred in a beaker.
A.2.2 Drying and Pulverization of Banana Peel Peel paste should be dried in the oven at a temperature not greater than 50 C. Dried peels should be grounded to obtain fine powder so that maximum particle exposure will be gotten for extraction of oil.
B. Extraction and Purification of Oil from Banana Peel B.1 Preparation of Materials and Equipment for Extraction and Purification of Oil Powdered banana peel will be used for the Soxhlet extraction. The following materials and equipment are needed: 10 g banana peel powder, normal Hexane, cellulose extraction thimbles, glass wool, condenser, 500-mL round-bottom flask (predried with boiling chips), heating mantle, Soxhlet extraction unit, rotary evaporator.
B.2 Extraction of Oil by Soxhlet extraction Pour 300 mL of normal hexane into the round bottom flask. Ten grams of the sample should be placed in the thimble and is inserted in the center of the extractor. The Soxhlet should be heated at 60 C. When the solvent is already boiling, the vapor will rise through the vertical tube into the condenser at the top. The liquid condensate will drip into the filter paper through the pores of the thimble and fills the siphon tube, where it flows back down into the round bottom flask. This will continue for 30 minutes. It is then removed from the tube, dried in the oven, cooled in the desiccators and weighed again to determine the amount of oil extracted. Further extraction should be carried out at 30 minutes interval until sample weight at a further extraction and previous weight becomes equal. The weight of oil extracted is determined for each 30 minutes interval. At the end of the extraction, the resulting mixture containing the oil should be heated to recover solvent from the oil. The low boiling point of hexane (50 to 70C) and the high solubility of oils and fats in it make it a suitable solvent for extraction. They are widely used as cheap, relatively safe, largely unreactive and easily evaporated non-polar solvents.
B.3 Purification of extracted Oil Briefly, 0.73 % of NaCl solution should be added to the oil solvent mixture in a separating funnel. This will be separated into two layers: the upper (organic phase) and the lower (aqueous phase). The lower phase is run-off and chloroform: methanol: 0.58 % NaCl solution was added for the purification of the organic phase. This again will be separated into two layers after which the lower layer was again run-off leaving the upper phase of the mixture containing the purified oil and solvent. The solvent should be driven off by placing the oil solvent mixture in a bath leaving behind the purified oil.
B.4 Determination of percent yield of Purified Oil from banana peel Percent yield of the purified oil will be measured using the following formula:
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C. Production of Biodiesel C.1 Transesterification Three and a half grams of sodium hydroxide (NaOH) catalyst should be mixed for ten minutes with 200 mL of ethanol inside a beaker using a magnetic stirrer to create sodium methoxide. The resulting solution is then mixed for an hour with 1000 mL banana peel oil using the same instruments. The mixture will be heated to 40 C while mixing. After an hour of mixing, the resulting mixture will be allowed to settle for eight hours.
C.2 Separation of Glycerine and Biodiesel After allowing the mixture to settle for eight hours, the mixture inside the beaker must have settled into a layer of glycerine and biodiesel fuel. A centrifuge will be used to easily separate the layer of glycerine from the layer of biodiesel fuel. The layer of biodiesel fuel should be decanted to a separate container for storage.
C.3 Removal of Alcohol from the Biodiesel Fuel Phase Once the glycerine and biodiesel phases have been separated, the excess alcohol in each phase is removed by distillation. Distillation is a commonly used method for purifying liquids and separating mixtures of liquid into their individual components.
C.4 Purification of Biodiesel C.4.1 Addition of Acid to Biodiesel After separation, acid (HCl) is added to the biodiesel to neutralize any residual catalyst and to split any soap that may have formed during the reaction period. Soaps will react with the acid to form water soluble salts and free fatty acids. Neutralization before washing reduces the water required and minimizes the potential for emulsions to form.
C.4.2.Water Washing The salts will be removed during the water washing step and the free fatty acids will stay in the biodiesel. The water washing step is intended to remove any remaining catalyst, soap, salts, methanol, or free glycerol from the biodiesel. Following the wash process, any remaining water is removed from the biodiesel by a vacuum flash process. This is the normally the end of the production process, resulting in a clear amber-yellow liquid with a viscosity similar to petro diesel.
C.5. Determination of Volume and Percent Yield of Biodiesel extracted from Banana Peel Volume of the biodiesel will be measured using a glass graduated cylinder. Percent yield of the final product will be measured using the following formula:
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D. Characterization of Biodiesel Quality D.1 Determination of properties of Biodiesel using the standards in Table 1. Table 1. Chemical and Physical Requirements of Biodiesel in the Philippines. Property Limit Test Method Flash point, closed cup(C) 130(minimum) ASTM D 93 Water and sediment(% volume) 0.050(maximum) ASTM D 2709 Kinematic viscosity @ 40C (mm 2 /s) 1.9-6.0 ASTM D 445 Sulfated ash(%mass) 0.020(maximum) ASTM D 874 Total sulfur(%mass) 0.05(maximum) ASTM D 5453 ASTM D 2622 ASTM D 4294 Copper strip corrosion (3 hrs.@ 50C) No. 1 ASTM D 130 Cetane number(min.) 47-51 ASTM D 613 Cloud point(C) ------- ASTM D 2500 Carbon residue(% mass) 0.050 ASTM D 4530 ISO 10370 Acid number(mg KOH/g) 0.50-0.80 ASTM D 664 ASTM D 974 EN 14104 Free glycerin(%mass) 0.020 AOCS Ea 6-94(1997) ASTM D 6584 modified Total glycerin(%mass) 0.240 AOCS Ca 14-56(1997) ASTM D 6584 modified Phosphorus 0.0010 ASTM D 4951 Storage Stability To be determined To be determined Density @ 15C (kg/L) 0.86-0.90 ASTM D 1298 ISO 3675
Legend: ASTM - American Society for Testing and Materials AOCS - American Oil Chemists' Society ISO - International Organization for Standardization EN - European Standard
D.2 Comparing of amount of determined properties with its corresponding limits The amount of determined properties will depend upon the ASTM method to be used.
E. Storage of Biodiesel E.1 Determination of source facility and container All biodiesel production facilities should be equipped with a laboratory so that the quality of the final biodiesel product can be monitored. Biodiesel should be stored in closed containers or cans that are completely filled to the top. Storing biodiesel in partially filled containers is not recommended because condensation can build up on the inside of the container and cause the biodiesel to deteriorate over a long period of time and can possibly cause the growth of bacteria and mold. When storing biodiesel containers or cans, it's important to keep them away from direct sunlight and insulated from low temperatures. Biodiesel will gel at a higher temperature than petroleum-based diesel fuel, but it will return to its liquid state when it is heated or allowed to gradually warm up. Biodiesel containers should also be protected from precipitation and excess moisture because of the aforementioned issues with condensation.
E.2 Storage of Biodiesel The chemical stability of biodiesel depends on the oil from which it was derived. Biodiesel from oils that naturally contain the antioxidant tocopherol or vitamin E remain usable longer than biodiesel from other types of vegetable oils. Banana peels are said to have tocopherol while vitamin E is found in bananas. According to at least one source stability is noticeably diminished after 10 days and the fuel may be unusable after 2 months. Temperature also affects fuel stability in that excessive temperatures may denature the fuel. Any fuel that will be stored for more than 6 months, whether it is diesel fuel or biodiesel, should be treated with an antioxidant additive.
Precautionary Measures
A. Safe Handling of Chemicals Chemicals will be transported using bottle carriers with caps closed tightly. Decantation of chemicals should be done properly with acid being added to water. All bottles will be labeled accurately for identifying chemicals. Labels should include the name of the chemical, the date it was initially opened and received. Chemicals, especially n- hexane and ethanol, should be placed inside a glass bottle separately with 100% leak proof cap. N- hexane and ethanol are highly flammable. To avoid explosion of chemicals, the containers should be securely closed and kept in a well-ventilated area. Avoid skin contact to all chemicals to prevent irritation and burns.
B. Safety Procedures in the Laboratory Sanitation should be practiced inside the laboratory. Hands should be washed thoroughly before entering the laboratory and after each procedure. Dress appropriately inside the laboratory at all times. To prevent skin or eye contact with chemicals the use of impervious gloves, laboratory gowns, safety goggles, face masks, and closed shoes should be strictly followed. Hair of girls should be tied back. The labels on reagent bottles should not be removed and always read to make sure it is the chemical that will be used. Bottles should be in order and then be put back in its original place after use. Laboratory equipment should be inspected before using. Glass wares should be handled with care. Tables, floors and aisles should be kept dry and clear from any unnecessary materials. After each use, laboratory surfaces will be kept clean using applicable disinfectants. Horse playing inside the laboratory is strictly prohibited.
C. Waste Disposal Sodium chloride and Sodium hydroxide will be diluted in water and disposed in the sink drains, accompanied by substantial water flush. Ethanol, n-hexane and hydrochloric acid are disposed of as a hazardous waste. Containers and other materials that are contaminated with these reagents must also be treated as hazardous waste. Waste acid should be separated from combustible substances, strong oxidants, strong bases, and metals. D. After-care of the Laboratory Chemicals will be disposed properly. Area must be clean after the study. All equipment should be returned to its original area or to Sir Rusty Balcoba and Maam Lani Estilo. If required, the Research laboratory should be locked after leaving.