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CHAPTER 3

Overview of the Study



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:


()
()


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:


()
()





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.

E. Data Organization

Table 1. Percent Yield
Weight (g) Volume (mL) Percent Yield (%)
Banana Peel -------------
Oil
Biodiesel

Table 2. Properties of Biodiesel
Property Limit
Measured Value
Trial 1 Trial 2 Trial 3 Average
Flash point, closed cup(C) 130(minimum)
Water and sediment(%
volume)
0.050(maximum)
Kinematic viscosity @
40C (mm
2
/s)
1.9-6.0
Sulfated ash(%mass) 0.020(maximum)
Total sulfur(%mass) 0.05(maximum)
Copper strip corrosion (3
hrs.@ 50C)
No. 1
Cetane number(min.) 47-51
Cloud point(C) -------------
Carbon residue(% mass) 0.050
Acid number(mg KOH/g) 0.50-0.80
Free glycerin(%mass) 0.020
Total glycerin(%mass) 0.240
Phosphorus 0.0010
Density @ 15C (kg/L) 0.86-0.90

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