ABSTRACT

In this experiment we use tetramethylammonium

iodide, iodine and ethanol - which are the solvent -
as the reactants to create tetramethylammonium
pentaiodide. Firstly, we break down clumps of
tetramethylammonium iodide and iodine that are
put in the beaker into a small powder. Then we add
ethanol by pouring it into the beaker. Secondly, we
put a small magnet into the beaker, put them in the
fume hood, and heat them up for ten minutes. After
ten minutes, we allow the solution to cool down
outside the fume hood and let the crystal form. To
make the crystal form quicker, we put the beaker in
an ice bath to cool it down. Next, we pour the
solution into the vacuum filtration to collect the
crystal by using hexane to wash the product down.
We leave the product for a few hours to let it dry. The
result is that the product is formed into shimmering,
crystal shape.
 OBJECTIVE
- To study the crystallization, the
mole calculation, the limiting
reagent identification, and the
percent yield of experiment work
calculation.
-To understand more about the
topic that we study

-To applied our knowledge in

class to use in real experiment
such as the calculation of percent
yield and limiting reagent.

-To make a crystal from chemicals

by using many methods
 INTRODUCTION
Chemistry is one of the science subjects that has to
deal with chemicals. It is very fantastic that one
chemical can form many products. Also, the amount of
the reactant has to associate with it which will affect
the on the amount of product. There are plenty of
method that we can use to create product. For
example, combustion reaction, synthesis reaction,
decomposition reaction, and acid-base reaction. We
can use more than two reactants in one chemical
reaction. In chemical reaction, the reactant that can
produce less amount of product will be the limiting
reagent while the reactant that can produce the higher
amount of product will be the excess reagent.
Therefore all of the limiting reagent is going to get
absolutely consumed and the excess reagent will be
left at the end of the reaction. In our experiment, we
use crystallization method to create crystal.
Crystallization is a process that atoms gather to make
tightly bonded or connected group. In order for the
crystallization process to occur, the solution needs to
be supersaturated. The term supersaturated means
there is too much solute in the solvent. Supersaturated
solution can be created by adding heat to the solution
which will make the atoms in the solution move
rapidly, therefore, more reactant can be added. As the
solute tends to have more solubility in the heated
 INTRODUCTION
solvent, the heat is removed and the solute is no longer
soluble in the solution. Then the pure crystal will start
to form. Filtration process will be used to separate the
crystal from the solution to get the product.

In the experiment, we use tetramethylammonium

iodide, iodine, and ethanol as the reactants and the
tetramethylammonium pentaiodide as a product. First
and foremost, we put 0.5 grams of
tetramethylammonium iodide and 1.3 grams of iodine
together in a beaker and use a stirring rod to break all
the clumps down. After that, we add 12 mL of ethanol,
which is the solvent, into the beaker. The solution that
we now have is a supersaturated. To dissolve all the
reactants, we heat the beaker up for a while then
quickly it cool down. The crystallization process will
occur. Crystal will form after the solution are cool down
with enough time and without disturbance. Finally, we
pour the solution into the vacuum filtration, which is
needed to separate the crystal from the solution, and
wash the solution with hexane. Then leave the product
in the petri dish. After we are done with all the
processes, we measure the amount of the product in
the petri dish and calculate the percent yield.
 Materials

Iodine (1.3g) Ethanol (12mL)

Tetramethylammonium
Hexane
iodide (0.5g)
 EQUIPMENT

50ML BEAKER

STIRRING
ROD

HOT-PLATE

PETRI DISH

ELECTRIC
BALANCE

VACUUM
FILTRATION
(FUNNEL
VACUUM)

SPATULA
 EQUIPMENT

ICE BATH
FUME HOOD

WEIGHING FILTER
PAPER PAPER

CYLINDER DROPPER

GLOVES GOGGLES
 PROCEDURE
1. Add 0.5 g of tetramethylammonium to a 50
ml beaker. Use a stirring rod break up clumps.
2. Add 1.3 g of iodine and 12 mL of 95% ethanol.
3. Heat the beaker on a hot-plate and stirring it
along for about 10 mins until
tetramethylammonium iodide has dissolved.
4. In order to prevent premature crystallization,
heat at a low temp.
5. Let the beaker to cool undisturbed after
removing from the heat unless a crystal would
be small and tend to become impurities.
6. The crystals should form during this time.
7. Place the beaker at room temp (can put on
ice for 10 mins if necessary). Set up the
apparatus for suction filtration.
8. Collect the crystals and wash them with
hexanes using vacuum filtration.
9. Air-dry the product with weigh.
10. Turn in the sample with our name on, the
name of the compound and the date to the lab
instructor.
 RESULT - WHAT DO
WE GET FROM
EXPERIMENT?
The result of our experiment is after mixing
tetramethylammonium iodide, iodide, and ethanol, we
could see that the color of those reactants are black
and yellow which is similar to betadine. There are some
big pieces sticking together. Then we heat the beaker
on the hot plate for 10 minutes. The color of our
reactants has become dark olive green and it looks a
little green. After that we put our beaker in the ice bath
in order to cool down solution, the crystal start to form
faster during this process. The color still looks the same
as before we put in the ice bath but it look less gray
now. After that, we put the solution into the filtration
and wait for 1 night. The color turns to dark green, and
the solution does not has a proper shape as shown in
the picture below. After we subtract the mass of the
filter paper, the amount of product that we get is 1.08
g. Add a little bit of body text
 DISCUSSION
Calculate the number of mole of each compound
Me4N+I- + I2 Me4N+I5-

Me4N+I- is given 0.5 grams

1 mole of Me4N+I- = 2.4875 * 10-3 mol

I2 is given 1.3 grams

1 mole of I2 = 5.1220 * 10-3 mol

Indicate the limiting reagent

 DISCUSSION
According to the calculation, Me4N+I- is limiting
reagent because it can produce less amount of
product than I2. Therefore, Me4N+I- is considered
as limiting reagent while I2 is excess reagent.

- Express the amount of excess reagent remaining

The amount of I2 is used in the reaction

= 2.4875 * 10-3 mol * 253.808 g
= 0.6313 g
The amount of excess reagent remaining
=1.3 g - 0.6313 g
=0.6687 g

- Discuss the % yield

%yield = Actual Yield * 100

Theoretical yield
= 1.08 g * 100
1.763 g
= 61.26 %

Actual yield: 1.08g (Result - Weighting paper =

1.08g) Result = 1.66 g,
paper = 0.58 g
 DISCUSSION
- Error

In the experiment, we got a human error during

synthesis of tetramethylammonium pentaiodide.
Therefore, our product is not as shine as other
groups that has the same reactant. In addition, our
groups crystal is not form well. The possibility of
human error in this experiment are we dont have
enough time to let the solution to cool down, dont
hold the solution stable enough so the forming
crystal breakdown into smaller pieces.
 CONCLUSION

In this reaction we mix the 0.5

grams or 2.4875*10^-3 mole of
tetramethylammonium iodide and
1.3 grams or 5.12198*10^-3 mole of
iodine. The crystal that our group
form has dark green color, no shape,
and slightly shinny. The limiting
reagent in this reaction is the
tetramethylammonium iodide and
the excess reagent is the iodine. The
amount of the excess reagent left
over is 0.6687 g grams. The percent
yield is 61.26%.
 SUGGESTION
- Unstable hand holding the beaker
while waiting for it to form the crystal so
the crystal break into smaller pieces.
Therefore, our crystal has a slightly
shiness.

- We noticed the problem that our

crystal has only slightly shiness. It
happen because we did not hold it
stably while the crystal is forming so the
forming crystal break apart.We should
use the beaker holder to hold it in the
ice bath. Also, we should let the beaker
heat up and let it cool down longer.
Another mistakes is when we pour the
solution into the vacuum filtration. We
use the stirring rod to spread the
solution down so, the crystal might
break down while we were using the
stirring rod. It might hit the crystal and
broke it.
 REFERENCE

Reciprocal Net. (n.d.). Crystallization.

Retrieved from
http://www.reciprocalnet.org/edumodu
les/crystallization/

Crystallization (n.d.). Retrieved from

http://orgchemboulder.com/Technique/
Procedures/Crystallization/Crystallizati
on.shtml

Helmenstine, Ph.D. (2017). Crystallize

Definition (Crystallization). Retrieved
from
https://www.thoughtco.com/definition-
of-crystallize-605854
WORK LOG