UNIT II- Characterization

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 Standards used in biodiesel characterization
The properties of biodiesel were determined by standard test methods as follows;

• Fatty acid profile AOAC (2000);

• Density ASTM D 1298;

• Kinematic viscosity ASTM D 445;

• Calorific value ASTM D 5865;

• Flash point ASTM D93;

• Cloud point ASTM D2500;

• Pour point ASTM D90;

• Cetane number ASTM D613;

• Acid value ASTM D664;

• Iodine value EN 14111;

• Copper strip corrosion;

• Biodiesel Rancimet EN 14112 and

• Ester content EN 14103.

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 Measured Biodiesel properties
Standard Diesel
B100 used in the
Properties Limit
present study

FAME content EN 14103 96.5 98.33 -

Density at 15 oC, kg/m3 ASTM D4052 860-900 890 820

ASTM D445 2.5
Kinematic Viscosity at 40 oC, mm2/s 1.9-6.0 4.83

Acid value, mg KOH/g ASTM D974 Max.0.5 0.38 -

Calorific value, MJ/kg ASTM D4809 - 43.4 45

Flash point , oC ASTM D93 Min 130 174 55

Cloud point, oC ASTM D2500 Report 5 -16

Pour point, oC ASTMD97 -15-10 2 -21

Cetane number ASTM D613 Min. 51 53 51

Oxidation stability at 110 oC,h EN ISO 14112 Min. 6 2.1 -

Copper strip corrosion ASTM D130 Max. 1 1

EN 14111 -
Iodine value g I2/100 g Max.120 37
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 GC-MS

Gas Chromotography-Mass Spectroscopy

(GCMS)
Table : Fatty acid profile of VODD biodiesel

Fatty acid Formula Structure Wt.%

Palmitate C17H34O2 17:0 14.90
Stearate C19H38O2 19:0 2.50
Oleate C19H36O2 19:1 30.00
Linoleate C19H34O2 19:2 50.93

*Fatty acid profile results matches with Moser et al (2011)

studied for soybean oil methyl ester 6
TLC
 Thin Layer Chromatography (TLC)
• TLC is a chromatography technique used to
determine the conversion of raw feedstock into
biodiesel.
• TLC is performed on a sheet of glass, plastic, or
aluminium foil, which is coated with a thin layer
of adsorbent material, usually silica
gel, aluminium oxide, or cellulose (blotter paper).
• This layer of adsorbent is known as the stationary
phase.
 Thin Layer Chromatography (TLC)
• After the sample has been applied on the
plate, a solvent or solvent mixture (known as
the mobile phase) is drawn up the plate
via capillary action.
• Because different analyses ascend the TLC
plate at different rates, separation is achieved.
 Thin Layer Chromatography (TLC)
• Thin layer chromatography can be used to
monitor the progress of a reaction, identify
compounds present in a given mixture, and
determine the purity of a substance. In the
present study, TLC was used to determine the
conversion of raw oil into biodiesel i.e. FAME.
 Procedure to run a thin layer
chromatography
• A small spot of solution containing the sample
(Biodiesel and Raw feedstock oil) is applied to a
plate, about 1.5 centimeters from the bottom
edge.
• The solvent is allowed to completely evaporate
off, otherwise a very poor or no separation will
be achieved.
• If a non-volatile solvent was used to apply the
sample, the plate needs to be dried in a vacuum
chamber.
 TLC PROCEDURE
• A small amount of an appropriate solvent (petroleum ether) is poured in
to a glass beaker or any other suitable transparent container (separation
chamber) to a depth of less than 1 centimeter.
• The container is closed with a cover glass or any other lid and is left for a
few minutes to let the solvent vapors ascend the filter paper and saturate
the air in the chamber.
• The TLC plate is then placed in the chamber so that the spot(s) of the
sample do not touch the surface of the elutant in the chamber, and the lid
is closed.
• The solvent moves up the plate by capillary action, meets the sample
mixture and carries it up the plate (elutes the sample).
• When the solvent front reaches no higher than the top of the filter paper
in the chamber, the plate should be removed (continuation of the elution
will give a misleading result) and dried.
• The photograph 6.3 shows the conversion of raw high FFA oil (Left side)
into FAME (Right side).