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Labchemistry

This document summarizes a student lab report on the synthesis of tetramethylammonium triiodide. The students used tetramethylammonium iodide and iodine as reactants and crystallization with vacuum filtration to produce the product. Iodine was found to be the limiting reagent based on mass calculations. The actual yield of the product was 0.77 grams, lower than the predicted 1.057 grams, resulting in a 72.85% percent yield. Sources of error that could explain the lower than expected yield are also discussed.

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379 views10 pages

Labchemistry

This document summarizes a student lab report on the synthesis of tetramethylammonium triiodide. The students used tetramethylammonium iodide and iodine as reactants and crystallization with vacuum filtration to produce the product. Iodine was found to be the limiting reagent based on mass calculations. The actual yield of the product was 0.77 grams, lower than the predicted 1.057 grams, resulting in a 72.85% percent yield. Sources of error that could explain the lower than expected yield are also discussed.

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Date: November 28, 2016

Synthesis of tetramethylammonium triiodide

By:
Apisara Yooyuen

#5861004 1102

Korakoch Thangsombat

#5861306 1102

Pin-anong Weesapen

#5861109 1102

Pornpitcha Akkapaiboon

#5861119 1102

Natcha Aphichoksathaphorn #5861067 1102

Chemistry
Ms.Sorasaree Tonsiengsom
Mahidol University International Demonstration School
Semester 1 Academic Year 2016-17

Synthesis of tetramethylammonium triiodide


Abstract
In this lab, we demonstrated formation of tetramethylammonium triiodide by
using crystallization technique to purify the solid compounds based on the principle of
solubility. We mixed all ingredients together in fume hood, filter the product, let it dries
and weigh. Iodine is the limiting reagent and tetramethylammonium iodide is the excess
reagent. This lab has shown the relationship of mass of the reactants and product in
chemical reaction.
Objective
Purpose of the experiment is to understand about mass relationship by
synthesising tetramethylammonium triiodide from tetramethylammonium iodide and
iodine. After we synthesized tetramethylammonium triiodide, then we measured its
mass to find how it relates to mass of both reactants.
Introduction
In the process of synthesis of tetramethylammonium triiodide, we use
tetramethylammonium iodide, iodine and 95 % ethanol to show the technique of
crystallization and vacuum filtration. The crystallization technique is used to purify the
solid compounds based on the principle of solubility; which the solutes tend to be more
soluble in hot liquids than in cool liquids. During the crystallization, to make it form
crystal add hot solvent to dissolve it and wait until it cool down. Furthermore, filtration is
another technique that has been used in this experiment. Filtration is technique to
remove solid from a solution, which help to collect the crystal solid.

Materials
1. 50 mL beaker
2. 0.5 g of tetramethylammonium iodide
3. Stirring rod
4. 0.6 g of iodine (0.6 g)
5. 12 mL of 95 % ethanol
6. Hot plate
7. Ice baht
8. Vacuum filtration
9. 27 mL of hexanes
Method
1. Add 0.5 g of tetramethylammonium iodide to a 50 mL beaker. Use a stirring rod to
break up clumps of Me4N+I-.

2. Add 0.6 g of iodine and 12 mL of 95 % ethanol


3. Gently heat the beaker at a low temperature on a hot plate with stirring for 10 minutes
until tetramethylammonium iodide has dissolved, in the fume hood.

4. Remove from the heat and allow the beaker to cool down undisturbed.
5. Place the beaker in an ice bath for 10 minutes.
6. Using vacuum filtration, collect the crystals and wash them twice with 27 mL of
hexanes.

7. Air-dry the product and weigh.


(Filtration paper + tetramethylammonium triiodide = 1.35 gram
Filtration paper = 0.58 gram

So, tetramethylammonium triiodide = 0.77 gram)


(final product)
8. Hand in a sample, in a capped vial, labelled name, the name of compound and the
date to the lab instructor.

Table of Data

Reactant
Chemical Formula
Amount (gram)

Product

4 +

0.52

0.59

Amount (mol)

2.587 103

Act as

Excess reagent

2.325 103
Limiting reagent

4 + 3
0.77
1.693 103
-

Calculation

Chemical equation: 4 +

4 + 3

Iodine 0.59gram
mass / molar mass = 0.59 253.8 = 2.325 103 mol
Tetramethylammonium iodide 0.52gram
mass / molar mass = 0.52 201.0 = 2.587 103 mol

4 +
2.587 103 mol

4 + 3

2.325 103 mol

Because; 2.587 103 mol > 2.325 103 mol


Then; 2 is limiting reagent
2 was used all amount which is 0.59 gram,
but 0.52 gram of tetramethylammonium iodide was not used all because is not limiting
reagent.
As we know that tetramethylammonium iodide was used 2.325 103 mol, this
is calculation to find amount of tetramethylammonium iodide in gram unit.
Mass = 2.325 103 mol 201.0
= 0.467 gram
So, 0.467 gram of tetramethylammonium iodide was used in the reaction.
Amount of product in gram unit that we got is 0.77 gram. Molar mass of
tetramethylammonium triiodide is 454.8. Then we can calculate amount of product in
mol unit.
Amount(mol) = mass(gram)/molar mass
= 0.77454.8

= 1.693 103 mol


Amount of product in mol unit should follow amount of limiting reagent
(2.325 103 mol). So, we expect to get 1.057 gram of product according to this
calculation.
Mass = 2.325 103 mol 454.8
= 1.057 gram
The theoretical amount or expected amount is 1.057 gram and the practical
amount that we got from the experiment is 0.77 gram, which is less that the expected
amount. Calculate the percent yield will be equal to (Actual mass/Expected mass)*100
which will be (0.77/1.057)*100 = 72.85%

Discussion

Chemical equation: 4 +

4 + 3

Reactants in this reaction are Iodine and Tetramethylammonium iodide. The


product of this reaction is tetramethylammonium triiodide.
Limiting reagents is the reactant used up first, and its amount will control amount
of product related by mass relationship. Iodine is limiting reagents in this reaction
because we found that its amount (mol) is less than amount of another reactant, so it
means that iodine was used all and tetramethylammonium iodide also have enough
amount for the reaction.
Iodine 0.59gram which is equal to 2.325 103 mol
Tetramethylammonium iodide 0.52 gram which is equal to 2.587 103 mol
Because; 2.587 103 mol > 2.325 103 mol
Then; 2 is limiting reagent
2 was used all amount which is 0.59 gram,
but 0.52 gram of tetramethylammonium iodide was not used all because is not limiting
reagent.
As we know that tetramethylammonium iodide was used 2.325 103 mol, this
is calculation to find amount of tetramethylammonium iodide in gram unit, equal to 0.467
gram.
So, 0.467 gram of tetramethylammonium iodide was used in the reaction.
Amount of product in gram unit that we got is 0.77 gram. Molar mass of
tetramethylammonium triiodide is 454.8. Then we can calculate amount of product in
mol unit.
Amount(mol) = mass(gram)/molar mass that is 0.77454.8 giving the result of
1.693 103 mol
Amount of product in mol unit should follow amount of limiting reagent
7

(2.325 103 mol). So, we expect to get 1.057 gram of product according to this
calculation. Mass = 2.325 103 mol 454.8
= 1.057 gram
The theoretical amount or expected amount is 1.057 gram and the practical
amount that we got from the experiment is 0.77 gram, which is less that the expected
amount. Calculate the percent yield will be equal to (Actual mass/Expected mass)*100
which will be (0.77/1.057)*100 = 72.85%
By calculating the percent yield we can see that the actual amount of the product
is less the amount that we expected because the amount that we calculated is 100%
yield according to the chemical equation. But practically, when the reaction happens,
the reactants might not be the exact amount as in said in the balanced equation, which
means not all of the reactants will be used and that caused the actual products less
than the expectation.
There are lot of factor that can cause the error in this experiment. According to
the theory the color suppose to come up with a dark color that almost black; but in our
experiment it shown up by having many of the spot that contain green color of the
products. Furthermore, this may go back to the step when we try to vacuum filtration it.
Its might not completely cool down since the step before when we put the beaker in the
ice bath. This also affect the process of vacuum filtration when we didnt use enough
amount of the hexane to wash it. So it maybe the factors that cause an error in the
appearance of the products when it done crystallization. Also, for when we try to use a
vacuum filtration to separate the crystal solid from the other chemicals, which can
causes some small pieces of the crystal loss or small enough to pass through the filter.

Conclusion
This lab report has shown the result of our experiment about the relationship of mass of
the reactants and product in chemical reaction, by using tetramethylammonium iodide
and iodine to create tetramethylammonium triiodide. And the result has shown that the
mass of the actual product is less than the predicted (theoretical) product that we
calculated with 72.85% yield.

References
Theoretical Yield and Percent Yield, (2016), Retrieved from
http://www.ck12.org/chemistry/Theoretical-Yield/lesson/Theoretical-Yield-andPercent-Yield-CHEM/

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