Experiment 4

Preparation of Biodiesel
Renewable Feedstocks for Fuel Production

adapted from Sally A. Meyer and Mark A. Morgenstern, Colorado College,

Colorado, USA

Introduction

As concerns about our environment and the use of non-renewable energy

sources have increased over the past ten years, scientists have begun to look at
new fuel sources. As an example, the production of biodiesel fuel from used
vegetable oil has been studied. Western universities, industries and even
individual people have begun making biodiesel to power their vehicles.
Diesel comes from petroleum and contains hydrocarbons of a higher
molecular weight than in gasoline (petro). It is used for trucks. The burning of
diesel from petroleum sources is known to contribute particulate matter as well
as carcinogenic hydrocarbons to the environment. Biodiesel creates less of these
hazardous materials, but has higher nitrogen oxide emissions. As with the
burning of all fossil fuels, the burning of petroleum diesel increases the carbon
dioxide in the environment as well. In contrast the burning of biodiesel, derived
from vegetable oil, does not increase the net carbon dioxide level in the
environment because everything is grown, produced, and burned within the
present day carbon cycle. It is, however, not a good idea to produce fuel from
food sources when people are starving. The production of biodiesel from waste
oil, or other waste streams may be a viable alternative for a small part of our
energy needs.
In this laboratory, you will prepare biodiesel from new vegetable oil as
the use of waste cooking oil is more complicated. Biodiesel is a collection of
methyl or ethyl esters from the fatty acids found in plant and animal fats. It is
produced via a base-catalyzed transesterification reaction between the
triglyceride (the fat) and sodium methoxide. Sodium methoxide can be prepared
from sodium hydroxide and methanol. The byproduct of the reaction is glycerol,
a product that is often used in cosmetics and soaps. The reaction below
illustrates the chemistry. Remember, the length of the carbon chains in the fatty
acid is dependent on the specific oil used. In addition, in vegetable oils, there
are often double bonds as well.
Procedure

Measure 14 ml methanol into a 125 or 250 ml Erlenmeyer flask. Weigh

0.5 g sodium hydroxide (NaOH) and crush into a powder using a mortar and
pestle. (NaOH can cause burns. Make sure you do not get it on your hands.)
Add the sodium hydroxide to the methanol. Stir slowly with a magnetic stirrer
for 5 – 10 minutes to dissolve the sodium hydroxide. When this is completed,
you have used your base catalyst to make the reactant, sodium methoxide.
Use a graduate cylinder to measure 60 ml vegetable oil. Add this to the
methanol solution and heat on your hot plate for 20 – 30 minutes at 35 – 50
degrees C. Keep stirring so that the mixture does not separate into layers.
Pour the mixture into a 125 ml separatory funnel and allow the solution to
cool and the layers to separate. Remove the bottom layer, which contains
glycerol, methanol, water, and the salts into a small beaker.
The top layer from your separatory funnel is your biodiesel fuel. Vacuum
filter this layer into a clean, dry filter flask using a Buchner funnel. Note the
appearance (color, clear? cloudy?) of your product. Measure the volume of
biodiesel and calculate the percent conversion based on the volume of your
vegetable oil only. The expected yield for this conversion is around 70%.

Waste Disposal
Both your byproduct layer and your biodiesel should be placed in the
containers provided in the lab. Do not pour them down the sink. Perhaps the
biodiesel will be used in the department’s oil burners.

Report

You will be required to submit a lab report for this experiment, in English.
It should include a title, a short introduction section, an experimental section
(how you did the experiment) and your results. Write it in your own words.
 Experiment 4
Preparation of Biodiesel
Equipment Needed (Things in bold are not currently in 506)

Hot plate stirrer and magnetic stir bar (7 of them)

Balance
Vacuum source

Supplies Needed (per group)

125 or 250 ml Erlenmeyer flask

Mortar and pestle (1 for the class would work here)
100 ml graduate cylinder (1 for the class)
25 ml graduate cylinder (1 for the class)
thermometer
125 ml separatory funnel
small beaker
Buchner funnel (1 for class)
Vacuum flask (1 for class)
Filter paper

Chemicals Needed (per group)

14 ml methanol
0.5 g sodium hydroxide (Important! Use this from a new bottle, where pellets
are not stuck together. Otherwise there is too much water in the reaction and it
doesn’t work well. Probably need to ask department head to buy new.)
60 ml vegetable oil

Total Needs (20 groups)

300 ml methanol
10 g NaOH
1.5 l vegetable oil

Helpful Hints

If it is warm, it may be helpful to cover the flask when dissolving the sodium
hydroxide so that methanol isn’t lost to the air. However, do not stopper tightly.

Encourage students to watch temperature carefully so as to not heat above 50

degrees. If heated higher than 50 degrees, the lower layer may become a solid
in the separatory funnel, and you will not be able to drain it. Then pour into a
new funnel and continue.