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Identifying the things you will need

Titrating: The first step in preparing your larger
chemicals for production.

The titration is a necessary stage in order to know the quantity
Sodium Hydroxide, NaOH (caustic soda) to be added to your
methanol.
Bio diesel from used cooking oil requires a titration before every batch
is made. With fresh oil, however, this step is unnecessary.

An understanding between the two types of oil, fresh and used, will
help to make this step clearer.

New cooking oil:
Fresh cooking oil has a glycerin backbone and three fatty acid chains
that are connected to this backbone. These components make up a
total vegetable oil molecule, also known as a triglyceride molecule.
When oil is fresh, glycerin and fatty acids are stable.
To make bio diesel with fresh oil, all that is required is:
1 litre of oil, 20% methanol by volume, and 3.5 grams of
caustic soda

The 3.5g of NaOH is sufficient to split the glycerin backbone
away from the fatty acid chains and allow the methanol to
reconnect with these chains. Essentially the methanol pretends to be
glycerin.

Used cooking oil:
In used cooking oil however, once heat is applied to cooking oil, the
bond between glycerin and fatty acids are partially broken,
leaving partial free fatty acids (FFAs) in the vegetable oil.

Not all of the vegetable oil molecules are destroyed this way however,
thus in used cooking oil there will still exist some fresh vegetable oil
molecules. In other words, there are still many stable bonds that
exist even in used oil and it is from these stable bonds that we
make bio diesel.

These stable vegetable oil molecules will follow the same rule as with
fresh cooking oil: 3.5g NaOH and 20% methanol by volume will convert
1 litre of oil to bio diesel.

But, because these stable molecules exist alongside broken vegetable
oil molecules and FFAs, the NaOH will be attracted first to the FFAs in
the oil before it has a chance to work with the stable molecules to
produce bio diesel.
(NaOH is an alkaline and the FFAs are acids. The two are naturally
attracted to each other and will neutralize each other)

Because of this, an excess of NaOH must be added to used
cooking oil, in order to: 1) allow the FFAs to be neutralized, and
2) ensure that 3.5 grams of NaOH is left behind to convert our 1
litre of stable vege oil molecules to bio diesel.

In other words 3.5g NaOH, PLUS excess NaOH, will convert used oil to
biodiesel

Calculating this excess NaOH is the point of titrating our oil.

By not performing this titration, it is possible that insufficient NaOH can
be added and as a result, FFA’s as well as monoglycerides and
diglycerides will exist in partially made bio diesel, resulting in damage
to engines.

What is needed:
Just as the titration allows us to prepare the chemicals for bio diesel
production, there are certain chemicals that have to be prepared for
the titration. These are:
• An indicator
• The solute
• The titrant

The indicator. The indicator indicates by colour, the “end point” of the
titration, or the point at which all the FFA’s have been neutralized,
leaving only stable molecules for conversion. The indicator changes
from yellow, when the oil is acidic, to pink, when most of the acidity is
neutralized. A good indicator that can be home made is one made
using 1 part tumeric to 5 parts alcohol.

The solute is the sample you wish to perform the titration on. It is
always 1ml of vegetable oil, dissolved in 10ml of pure alcohol.

The titrant. The titrant is a solution made up of 1 gram of NaOH,
dissolved in 1 litre of distilled water. The NaOH is dissolved in water
for a number of reasons. The first is because NaOH in solid form will
not react well, and the second, because the quantities used in the
titration are too small to be measured in solid form, whereas in
dissolved form, tiny measured droplets containing even smaller
quantities of NaOH can be used to provide accuracy.
The titrant is added slowly, in very small quantities, to our test sample
being titrated. The more titrant added, the more FFAs are
neutralized and the solution turns more from yellow to pink.

By adding 1 gram of NaOH to 1 litre of water, we actually have an
accurate tool for measuring small quantities of the NaOH dissolved in
it. If we took half of the volume of water, 500ml, we would also have
half the amount of NaOH we added, in otherwords, 0.5g NaOH. If we
took a quarter of the water, 250ml, we would have one quarter the
NaOH, 0.250g.

Let us say for example that in our titration, instead of adding our
titrant slowly, we simply dumped 4ml of our titrant into our solute, and
the solute immediately turned pink.
We could say that 4ml of the titrant was sufficient to neutralize the
FFAs in our sample. However, it is possible it was really only 2.7ml
that was needed, but we did not test accurately enough to determine
that.

What is done therefore, is to add the titrant slowly, about 0.1ml drops
at a time. As mentioned above, every time we take a known volume of
water out of our water/NaOH solution, we are also taking out a known
amount of NaOH. So if we add drops of 0.1ml of water, we are also
taking 0.001g of NaOH in each drop.

By adding such small quantities slowly, we can determine the exact
moment and amount of NaOH that will change the solution
from yellow to pink, thus neutralizing the FFAs.

Once the FFAs are neutralized, from yellow to pink, we take note of
how much of the titrant was used for this colour change to occur. If it
took ten 0.1ml drops of the titrant (1ml), we add 1 gram to the
3.5 grams we already know about. It the titration took twenty
0.1ml drops (2ml) we add 2 grams to our 3.5 grams. And so on.

• Step 1: Prepare the indicator. Measure 1 part tumeric to 5 parts
alcohol. A measuring spoon works best. Wait for all the tumeric
to settle to the bottom of vial before using. The alcohol should
be yellow and not cloudy.

• Step 2: Prepare the titrant. Using an accurate scale, weigh 1
gram of NaOH. Dissolve the NaOH into 1 litre of distilled water.

• Step 3: Prepare the solute.
• Step 3.1: Measure 10ml of pure alcohol. (This is not the
same as surgical or rubbing alcohol.)

• Step 3.2: Neutralize the acidity of the alcohol. As alcohol
ages, it becomes slightly acidic. This can give inaccurate
readings. To neutralize, add one to two small drops of the
indicator to the alcohol and afterwards, add, slowly, measured
drops of the titrant to the alcohol until it goes from yellow to
pink.

• Step 3.3: Add to the neutralized alcohol, 1ml of the
vegetable oil sample. Mix thoroughly. The sample will turn
from pink back to yellow again.

• Step 4: Once the solute is ready, begin adding slowly, and
counting, 0.1ml drops of the titrant to the solute. The solute will
require stirring or mixing while adding the titrant. Continue
adding until the solute can remain pink for a pprox. 30 seconds.

• Step 5: Record the amount of the titrant that was added to the
solute.

• Step 6: Repeat steps 4 and 5 three more times.
• Step 7: Perform final calculations.

E.g. Let us say that we added 1.2ml of titrant in the first trial, 1.4ml in
the second trial and 1.2ml again in the third trial. The average here is
1.3ml. Therefore we know that 1.3ml or 1.3 EXTRA grams is
required to neutralize JUST the FFAs in 1 litre of our oil sample.

We add 1.3 to our 3.5 grams (the amount needed for our stable vege
oil molecules) to have a total of 4.8 grams that would be needed
to neutralize the FFAs AND convert the stable oil to bio diesel.

• Step 8: Determine how many litres of oil you will be processing.
• Step 9: Multiply the number of litres of oil to be converted, by the
amount of NaOH needed to convert 1 litre. For e.g., assuming
that we were making 40 gallons. So 40 gallons x 3.78 = 151.2
litres. 4.8g x 151.2 = 725.76g of NaOH.

Preparing the Methoxide

Once the methanol (20% of the total volume of vegetable oil to be
processed) is ready, the NaOH must be added and mixed thoroughly
until dissolved.