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Melting Point
(F)
37.4
3.2
70
14
Density (g/mL),
25C
0.917
0.920 0.925
0.9 0.915
0.920 0.925
Procedure:
1. Develop an experiment (test) to determine the relative melting points of the four
unknown oils. Record your results and verify your answers with your instructor.
Test (please describe):
Unknown Oil #
1
Observations
Melting Point
2
3
4
2. Develop an experiment (test) to determine the density of the unknown oils. Record you
results and verify your answers with your instructor.
Test (please describe):
Unknown Oil #
1
Observations
Density
2
3
4
Melting Point
(F)
37.4
3.2
70
14
Density (g/mL),
25C
0.917
0.920 0.925
0.9 0.915
0.920 0.925
Procedure:
1. Develop an experiment (test) to determine the relative melting points of the four
unknown oils. Record your results and verify your answers with your instructor.
Test (please describe):
Unknown Oil
#
1
Observations
Melting Point
2
3
4
2. Develop an experiment (test) to determine the density of the unknown oils. Record you
results and verify your answers with your instructor.
Test (please describe):
Unknown Oil
#
1
Observations
Density
2
3
4
Student Questions
1. Based on your experiments, identify the unknown oils:
Unknown Oil
#
1
Oil Name
2
3
4
2. Are you able to distinguish between the oils by using density and melting point alone?
If not, what other tests would you propose to determine which oil is which?
3. If you are investigating the use of these four vegetable oils for the use in a biodiesel
engine, which one(s) would you recommend? Why?
4. What benefits do you think using biodiesel has compared to using traditional diesel
fuel?
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Name:_____________________________________
1) Complete the following reaction for the titration of a carboxylic acid with NaOH
(acid/base reaction):
O
R
OH
+ NaOH
____________________________moles
6) We are using KOH as catalyst. How many moles of KOH will be needed for 10.0 mL
of PURE veggie oil?
___________________________moles KOH catalyst for 10.0 mL pure veggie oil
7) NOW, how many TOTAL moles of KOH will be needed for the transesterification
reaction:
moles KOH to neutralize fatty acids + moles KOH as reaction catalyst =
___________________total moles
8) The KOH for transesterification is provided as a 10.0 M aqueous solution. How many
mL and mL of 10.0 M KOH will be needed?
______________________________mL
_____________________________mL
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*KOH is corrosive and can cause burns on the skin. If contact with skin is made, wash
with copious amounts of water immediately. Be sure to read safety information regarding
this chemical and to take the appropriate safety precautions before using in the
classroom.
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Note that three fatty acids are used to form the triglyceride. Depending on the oil or fat,
the lengths of the fatty acid chains will vary and the three fatty acids that make up the
triglyceride can be three different fatty acids. Because they can be three different fatty
acids, the term R is used to represent the carbon chain. R, R1 and R2 all represent
different lengths of carbon chains. These oils and fats are commonly found in plants and
in our bodies.
In order to make biodiesel the triglyceride molecules can be converted into a simpler
form through what is called a transesterification reaction. This reaction converts one type
of ester group to another. In the reaction scheme below you can see that the ester groups
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that are attached to the glycerol portion of the molecule are broken and converted to a
different type of ester.
The reaction scheme above shows that we use an alcohol, such as ethanol (CH3CH2OH)
and a catalyst (potassium hydroxide, KOH) to convert the vegetable oil into biodiesel and
glycerol, a by-product of the reaction. You can see that since the starting material on the
left side of the equation had three fatty acid hanging off the glycerol that we needed 3
ethanol molecules to produce 3 biodiesel molecules.
Keep in mind that since biodiesel is actually a mixture of esters, different types of
vegetable oils can produce fuels with different properties.
You are now ready to make your own biodiesel fuel from WVO.
Experimental Procedure:
1) Determine the mass of a clean, dry 25 mL Erlenmeyer flask. Add to this flask 10.0
mL of WVO using the bottle dispenser, and record the exact mass of the WVO. Add a
stir bar to the WVO, 2.0 mL of ethanol, and the appropriate volume of 10.0 M KOH
calculated in PART I. Stir the reaction mixture vigorously (setting of 8-9) at 50oC for 60
minutes. Record all observed changes during the reaction.
2. Transfer the reaction mixture to two centrifuge tubes, and centrifuge for 5 minutes.
You should end up with two layers, with the biodiesel on top. Using a pipet, discard the
lower layer which contains glycerol and KOH catalyst into the labeled waste container.
3. Combine the crude biodiesel into one centrifuge tube. Add 1 mL of 0.1M acetic acid
to the biodiesel, cap the tube, invert gently five times (do not shake), then centrifuge for 5
minutes. Discard the bottom, aqueous layer into the labeled waste container. Repeat the
extraction step using 1 mL of distilled water.
The extraction or washing in step 3 removes flammable ethanol, glycerol byproduct,
catalyst, and fatty acid salts (soaps) from your biodiesel. If the water wash is not done
properly, contaminating ethanol could create a fire hazard, and contaminating glycerol,
catalyst, and soaps will negatively affect combustion and engine performance.
Furthermore, mixtures of biodiesel and water will form an emulsion if shaken. Fuel
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emulsions with water would be disastrous in a diesel engine. Finally, all traces of water
must be removed from the washed biodiesel before use in a diesel engine is possible.
4. Using a pipet transfer the washed biodiesel to a pre-weighed 25 or 50 mL Erlenmeyer
flask. Heat this sample at 70-80oC for 10-15 minutes to evaporate residual water. Obtain
the mass of your dry biodiesel.
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Name:_____________________________________
Color of purified
biodiesel________________________________________________________________
_
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4. Explain the purpose of the acid wash in step #3. Write a balanced chemical equation
as part of your explanation.
6. In the commercial production of biodiesel, 1.20 x 103 kg of vegetable oil produces 1.10
x 103 kg of biodiesel. How does your yield compare to this
7. One argument against biodiesel being a green fuel is that combustion produces CO2,
which is a greenhouse gas. Is it possible to counter this argument from the standpoint of
using renewable resources?
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