LAB REPORT

Synthesis of

Tetramethylammonium pentaiodide

By

Vipada Davies

Kannicha Eksuwancharoen

Warinthorn Samerpak

Akarapon Amnajsongserm

Bhitchayoot Sima-aree

Teeranut Sawanyawat

Room: 1107

Submitted to

Miss Patraphorn Sanguansat

General Chemistry 11

Mahidol University International school

Page

Abstract 3

Introduction 4

Experiment 5-7

Solution 8

Result and Discussion 9-10

Conclusion 10-11

Suggestion 12

Reference 13
 Abstract

Our purpose for this experiment is to create crystal like particles by using

Tetramethylammonium iodide, 1.3 grams of Iodine and Ethanol 95% which is 12 mL. The

product that was supposed to come out was a crystal like substance once the procedure was

finished. Depending on how well the instructions were followed the product will vary. The

essential points of the procedure was weighing the correct amount of substances. Mixing the

substance by order and knowing how to filter the mixture to get your final product. The results

for this experiment did not go as planned. The product came out not crystal like but dull instead.

There was an error in either the material that were used or the procedure. Recommendations are

to be careful mixing the substances and grinding them. It is important to weigh the amount of the

substances properly you that it can be sure that nothing would go out of plan.
 Introduction

The main purpose of this task is to study a process of crystallisation, the process by

which a solid forms where atoms or molecules are highly organized into a structure known as
−
crystal, in this case, heating and cooling our reactants, M e4 N + I and 2I 2 , in order to get

tetramethylammonium pentaiodide or M e4 N + I 5− as a form of crystal. However, in order to

conduct the experiment, we need to know the basic information of Halogen, the 7A group in the

periodic table first. Because every element in the Halogen group requires only one electron to

become stable, it acts like an important component to react and oxidize with other elements.

Moreover, if an element from the Halogen group is mixed with a halide solution, it will resulted

in the displacement reaction of element. Also, in the periodic table, the M e stands for methyl (

CH 3 ). During the crystallisation, the temperature of elements, mixing together to form a crystal,

should always be monitored because if the temperature has been lowered, the result of

crystallisation will resulted in getting an immature crystal.

1. 0.5 grams of m

2. Tetramethylammonium iodide

3. 1.3 grams of Iodine

4. 12 mL of Ethanol 95%

Equipments

1. Vacuum filtration 2. A beaker 3. Stirring rod 10. Ice bath

4. Magnetic rod 5. Petri dish 6. Weighing Paper

7. Filter paper 8. Hot-plate 9. Capped via

2. Add 1.3 grams of Iodine and 12 mLs of 95% in the same beaker

3. Heat up the beaker by using a stirring rod and shot plate for about 10 minutes until the
Tetramethylammonium Iodine has dissolved.

4. Heat at a low temperature to prevent premature crystallisation.

5. Remove from the heat and allow the beaker to cools undisturbed. (agitating the solution
can cause smaller crystals to form which are more difficult to isolate and tend to occlude
impurities)

6. The crystals should form during this time.

7. Once at room temperature, further cooling can be achieved by placing the beaker in an
ice bath for about 10 minutes. Only put the solution on ice if necessary. During this time,
set up the apparatus for suction filtration

8. Using vacuum filtration, collect the crystals and wash them with hexanes (5 ml portions
until filtrate dropping from funnel is colourless, max. 5 washings.)

9. Air-dry the product with weight.

10. Hand in a sample, in a capped vial, labelled with your name, the name of the compound
add the date of the lab instructor.
 Solution

−
M e4 N + I → N (CH 3 )4 I

0.5
N (CH 3 )4 I : Mole = 201 = 0.002487 → ​0.002487 x 709 = 1.763283 gram

1.3
I2 : Mole =
254 = 0.0051181 → ​0.0051181 x 709 = 3.62874 gram

−
M e4 N + I is limiting reagent, I 2 is excess reagent

Actual Y ield
% Yield = T heoretical Y ield x 100 :

1.24
% Yield = 1.763 x 100 = 70.32 %

I 2 left

Mol of 2I 2 : 0.0051181*2 = 0.102362 mol

Mol of 2I 2 − N (CH 3 )4 I = 0.102362 - ​0.002487 = 0.0077492 mol

0.0077492 x 254 = 1.9682968 grams of I 2 are left.

The physical properties tetramethylammonium pentaiodide is presented by the color and

shape. Which the shape of tetramethylammonium pentaiodide is not likely crystal 100%, most of

it are similar to dust. Moreover, the color of it is kind of black-green and white.

Chemical Properties

Balance Equations: N (CH 3 )4 I + 2I 2 ➡ N (CH 3 )4 I 5

Theoretical Yield: 1.763 gram

Actual Yield: 1.24 gram

Reaction Yield: 70.32%

In the theory, the result of product need to

contain a dark colour and rod shape, but for our group,

this might come when filter it in the vacuum and didn’t

completely wash it with hexane. This can cause the

impurity. This happened when we put it in the fume

hood which it will be very hard to control and it’s

easier to get contaminated from other substance. Other

substance might be spilled into the crystal and this

cause the inaccurate information. Moreover, our

percent yield is about 70.3% . We think that we used

too much of iodine. When we measure the iodine, the filter paper was blowing by the air

conditioner which made an inaccurate measuring of iodine. This made information inaccurate.
 Conclusion
From the experiment we used a total amount of 0.5 grams of Tetramethylammonium

iodide which is equal to 0.002487 mol and 1.3 grams of Iodine which is equal to 0.0051181 mol.

The limiting reagent was the Tetramethylammonium Iodide because it could only produce 1.763

grams of Tetramethylammonium pentaiodide while iodine can produce 3.529 grams. The final

product of this experiment was Tetramethylammonium pentaiodide but for us there was an error

in the procedure so the product didn’t come out as planned instead of having little crystal like

particles in the product there were no crystal particles at all. The product was the color of green it

was in a powdered substance. The amount of product is 1.24 grams which is 70.32 % of the

Theoretical yield.
 Suggestion
For the suggestion, we found out that we needed to turn off the air conditioner when we

were measuring the filter paper due to the wind that blew through the paper and making an

inaccuracy mass of the filter paper. Furthermore, we needed to be more careful on eighth step

because we needed as close to 100% pure crystal without contaminate. We also needed to use

proper equipment because it would made our process easier and gave out more efficiency to earn

nearly pure product. Moreover, when we moved the product through other places, we should be

more careful to prevent the crystal to fragile.

Anne Marie Helmenstine, Ph.D.(2017 ,April 4). Understanding Crystallization in Science.

Retrieved from, http​://www.thoughtco.com/definition-of-crystallize-605854

Hallas, N,J (n.d.). CRYSTALLIZATION. Retrieved from,

​http://www.thermopedia.com/content/679/