Moiss Avila Rehlaender | Principle #1 of Green Chemistry | Laboratory Practice

Analysis of biodiesel synthesized from canola oil.

Introduccin
Creation of a cost-effective and greener alternative fuel is a major focus of science today.
One of the more often used greener fuels is biodiesel.
It is made from new or used vegetable oils and animal fats, and is biodegradable and
nontoxic. This means it meets the criteria for several of the
12 principles of green chemistry, including the use of renewable feedstock and design for
degradation.

The simplest way to produce biodiesel uses what is called a transesterification reaction. In
this particular reaction, a base catalyst (KOH) is used to convert the triglycerides into three
smaller separate ester molecules, with each one ending in a OCH3. A molecule of glycerol,
a trialcohol, is also formed as a by-product. This is a reversible reaction, so excess methanol
is added to drive the reaction toward the product.
Any water in the process promotes soap making (via saponification) and inhibits
transesterification. This means the methanol used must be dry and the KOH weighed out
quickly since it is hygroscopic.

Procedure
Part 1: Synthesis of biodiesel
1. Obtain approximately 9.5 ml canola oil in a clean and dry 10 ml graduated cylinder.
Record the exact amount of canola oil obtained. Calculate the number of moles of canola
oil this is.
Use 880 g/mole for the average molar mass of a canola oil molecule.
2. Add the canola oil into a 15 ml conical plastic centrifuge tube. Be sure to give it adequate
time to drain into the centrifuge tube. Use the average molar mass of a canola oil molecule
and the average density of canola oil given in prelab question 2 to calculate the grams and
moles of canola oil obtained.
3. Acquire 3.50 ml of red methanol/KOH solution in the 10 ml graduated cylinder used to
obtain the canola oil. Be sure you obtain 3.50 ml of the red methanol/KOH solution in
addition to any residual canola oil. Add this to the centrifuge tube and place the cap securely
on the tube.
4. Shake the centrifuge tube vigorously for 5 minutes. Shake it in different ways and
directions to avoid catching any of the solution in the tip of the centrifuge tube.
 Moiss Avila Rehlaender | Principle #1 of Green Chemistry | Laboratory Practice

5. Place the centrifuge tube in a centrifuge, and balance it using a counterweight. Run the
centrifuge for 30 seconds. Determine and record the volume of the glycerol layer, which is
the red bottom layer.
6. Repeat steps 35 two additional times. All of the red should be at the bottom of the
centrifuge tube. If it is not, repeat steps 35 until it is.
7. Carefully pour all of the contents of the centrifuge tube into a 25 ml buret. Allow extra
drain time if needed. Let the biodiesel rest for at least 5 minutes to allow it to drain off the
sides of the buret and settle into two distinct layers. Determine and record in Table 21.1
the quantity of the top biodiesel layer.

Part 2: Calculation of yield using glycerol calibration curve

1. Carefully drain down the red bottom (glycerol) layer to the end of the tip of the buret. A
very small amount of only the red bottom layer may need to be drained into a waste beaker
to remove air bubbles. Add this back into the buret and allow it time to settle to the bottom.
2. Obtain a buret reading at the top of the biodiesel to the hundreths place. Record this
value as buret.
3. Obtain and record the mass of a small test tube.
4. Drain approximately 1.0 ml of the red bottom layer into the preweighed test tube. Obtain
a buret reading at the top of the biodiesel to the hundreths place, and record it as buret
reading 2.
5. Determine and record exactly how much red bottom layer was drained into the test tube
by subtracting buret reading 2 from buret reading 1. Do not get any of the top biodiesel
layer into the test tube.
6. Obtain and record the mass of the test tube with the red bottom layer. This can be
accomplished by taring a small beaker on the balance and then placing the test tube in it
and obtaining the mass. Calculate and record the mass of the contents.
7. Calculate and record the red bottom layers density.
8. Carefully drain the rest of the red bottom layer into a waste beaker.
Obtain and record the volume reading of the biodiesel on the buret as buret reading 3.
Subtract this from buret reading 1 to determine the volume of the red bottom layer. Enter
this volume under Total volume of red bottom layer.
9. Obtain and record the mass of another small test tube. Into this test tube drain 2.0 ml of
provided 50/50 glycerol/methanol solution located in a buret. Record the exact volume
obtained.
10. Obtain and record the mass of the test tube with the glycerol/methanol solution, and
calculate the mixtures density in g/ml.
11. The densities of glycerol and methanol are 1.261 and 0.791 g/ml, respectively. Use these
densities and the density you determined for the 50/50 glycerol/methanol solution to
create a calibration curve that compares percent glycerol to density. Record the equation
of the line of best fit.
12. Using the equation of the line, calculate the percent glycerol by volume in the red layer.
Do this by inserting the density of the glycerol layer that was calculated in step 7 into the
equation.
 Moiss Avila Rehlaender | Principle #1 of Green Chemistry | Laboratory Practice

13. Use the percent glycerol by volume to calculate the milliliters of glycerol present in the
red layer. Do this by multiplying the total volume of the red layer by the percent glycerol by
volume.
14. Calculate the moles of glycerol produced, using 1.261 g/ml as the density and 92.09
g/mole as the molar mass. From this, determine the moles of biodiesel produced. Next, use
this and the moles of canola oil used that was calculated in Part 1 to determine the percent
yield. Remember you get 3 moles of biodiesel for every 1 mole of glycerol.

References
Sally A. Henrie, Green Chemistry Laboratory Manual for General Chemistry (2015)
pp. 315-323.