Lab Report

Presented by
Ms. Yada Rojanasoontra 5961022
Ms. Patcharipa Chanaturakarnnon 5961106
Ms. Natnicha Kunakornkul 5961025
Ms. Siriyakorn Tongveeraprasert 5961006
Mr. Krittamet Payuhakiat 5961111
Mr. Skypeth Saingthong 5961209

Submitted to
Ms. Patraphorn Sanguansat

Mahidol University International Demonstration

School Academic Year 2017
 Table of Contents

Abstract 3
Introduction 4
Background knowledge 4
Crystallization 4
Chemical structure 4
Balancing equation 4
Calculation 5
Reference citation 6
Objectives 6
Experiment 6
Chemical materials 6
Equipment/Glassware/Instrument 7
Procedures 8
Discussion 10
Discussion and error 11
Conclusion 12
Suggestion 12
References 13
Abstract
This report presents the crystallization of 1.6 grams
tetramethylammonium pentaiodide crystal from a solution of 0.5 grams of
Iodine, 1.3 grams of Tetramethylammonium, and 12 mL of Ethanol. Including
the calculation of limiting reagent, excess reagent, and percent yield. Our
experiment started with all of the material prepared and all the chemical weigh
precisely, following the procedure given. Start with grinding 0.5 grams of
Iodine and 1.3 grams of Tetramethylammonium into fine powder, then add 12
mL of Ethanol to form a solution before putting in on a heat plate using
magnetic bar to stir the solution while heating. After bringing it off heat allow it
to cool using ice bath. Using vacuum filter and hexane extract the crystal out of
the solution. Our result is 1.6 grams of tetramethylammonium pentaiodide in
matt green powder, with small amount of fine shimmer which is almost
invisible. From some calculations we found out that the limiting reagent in this
experiment is Tetramethylammonium, excess reagent is Iodine, and our percent
yield is 59%.
Introduction

● Background knowledge
○ Crystallization
Crystallization is a process which has been used for substance
purification for a long time. It occurs when a heated solution is saturated, cooled
down, and then produce crystals. F ​ irst, atoms or molecules cluster together on the
microscopic scale in a process called ​nucleation.​ If the clusters become stable and
sufficiently large, ​crystal growth may occur.​(​Helmenstine, 2017​) The crystals can
be produced in varied shapes: cubic, tetragonal, orthorhombic, hexagonal,
monoclinic, triclinic, and triagonal. The products from crystallization are
snowflakes, gemstone, synthetic gemstone, syrup in a container, and etc. In this
experiment, the product is a green lattice powder containing lots of glitter.

● Chemical structure
Chemical Structure are the arrangement of chemical bonds between
atoms in a molecule, specifically which atoms are chemically bonded to what
other atoms with what kind of chemical bond. Every molecule or compound
will have its own unique chemical structure. Chemical structure that will be
discussed are Iodine; this chemical has the same crystal structure as chlorine and
bromine, ​Tetramethylammonium; the chemical structure of this chemical is
having Nitrogen as its central atom and four single bonds around it as the
diagram below which also includes the Iodine.

This experiment will show the crystal that are form by combining Iodine and
Tetramethylammonium to form ​tetramethylammonium pentaiodide (Me​4​N​+​I​5​-​).
 ● Balancing equation
Chemical equation needs to be balanced in order to satisfy the law of
conservation of mass. Before balancing chemical equation, the required
information to know the element of a chemical reaction first. The ingredients
are called ‘reactants’, and the results are called ‘products’. A chemical reaction
is needed to be balanced because of the ratio resulting of the balanced equation
will be used in finding the limiting reagent, excess reagent, and percent yield is
important for this lab because after finishing the procedures, in order to
understand more about the chemical reactions and the formation of the crystal,
those knowledge will need to be applied.
"Matter is neither created nor destroyed."
https://www.chemteam.info/Equations/Balance-Equation.html

● Laboratory skills
Since the experiment will involve using chemicals and lab equipments, it is the
best to follow the instructions in the laboratory, know how to use the equipment
proper including wearing safety all the times and be able to use all the lab
equipments properly.

● Calculation
This lab consists of calculation. The calculation gives the data and results
which include calculating percent yield, molecular weight, mole, limiting
reagent, excess reagent and the remaining excess reagent. Percent yield is the
percent ratio of actual yield to the theoretical yield. The way to calculate the
percent yield is to subtract the actual yield by the theoretical yield and then
multiply the product by 100 to turn it into percentage, following the formula (
actual yield
percent yield = theoretical yield × 100). The accuracy of the experiment can be
determined by the percent yield. To calculate the molecular weight of a
compound, we need to find the weight of each element on the periodic table and
then sum it together. For instance, CO​2 has 1 carbon and 2 oxygen. Therefore,
the weight of a carbon and 2 oxygens need to be indicated from the periodic
table and their sum will become the molecular weight. The molecular weight
can be further used to calculate the mole. Mole is an unit of measure in the
International System of Units. A mole of every element or compound contains
6.022 x 10​23 atoms and this number is called ​Avogadro’s constant or
mass
Avogadro’s number. The formulation for mole is (​mole = molar mass ) ​which
the given is divided by the molecular mass or molar mass. Limiting reagent is
the compound in a chemical reaction that is used up first. It limits the product’s
production and it can make the least amount of product compared to other
element or compound in the reaction. The excess reagent is the compound that
is not used up or left over in the reaction. It produces the most of the product
compared to other element or compound in the reaction. The calculation can
also be used to help determining the limiting and excess reagent by using the
mole ratio from the balanced chemical reaction. After the excess and limiting
reagent is calculated, we can calculate the amount of the excess reagent that is
left after the reaction by ​calculating how much of the other reactant it must have
reacted with and subtract from the original amount.

● Reference citation
APA citation is the citation format from ​American Psychological Association.
When an information is retrieved from other people’s work an APA citation is
there the format used to give credit to the website, article, author, etc. in order to
prevent plagiarism.

● Objectives
○ To study crystallization.
○ To practice percent yield calculation from the formula
actual yield
(​percent yield= theoretical yield × 100​)
○ To be able to identify errors from the experiment.
○ To be able to calculate mole from the formula.
mass
(​mole= molar mass )
○ To pratice using laboratory equipments.
○ To be able to identify limiting reagent and excess reagent from the
chemical reaction Me​4​N​+​I​-​ + 2I​2​ → Me​4​N​+​I​5-
Experiment

● Chemical materials
○ 0.5 grams of Iodine ○ 12 mL of Ethanol
○ 1.3 grams of ○ Hexane
Tetramethylammonium

● Equipment/Glassware/Instrument
50 mL Beaker
Stirring rod

Fumehood
Hot plate

Magnetic bar Glass dropper

Cylinder Spatula

Filter paper Watch glass

Ice bath Weighing paper

Vacuum filter Scale

 Procedures
1. Add 0.5 grams of tetramethylammonium iodide and 1.3 grams of iodine
into a 50 mL beaker, then break down the lumps using a stirring rod.
2. Pour 12 mL of 95% ethanol into the beaker.
3. Gently heat and stir the heterogeneous solution on a hot plate in a fume
hood for 10 minutes, until the solute dissolves.
4. Use low temperature to prevent pre-crystallization.
5. Take the beaker out of the hot plate and let the solution cool without
disturbance because agitating the solution will affect the size of the
crystals to be smaller. That make them harder to be separated and get
contaminated.
6. Wait for the crystals to form.
7. At room temperature, leaving the beaker in an ice bath for 10 minutes
will make the solution cool faster, or just put it on ice in necessary case. It
is a good chance to set up the equipment for suction filtration while
waiting for the solution to cool.
8. Collect the crystals up, then clean them with 5 mL of hexanes until the
filtrate drop from the tube is clear, the maximum is 5 times.
9. Leave the product until it dries, then weigh its mass.
10.Turn in a sample contained in capped vial and labeled the lists of the
experimenters, the name of the product, and the date to the lab instructor.
Results

After the filtration, we got a green muddy product. When it dried, the
product turned into green powder, it was matt with small amount of fine
shimmer which is almost invisible. The actual yield was 1.05 grams
Discussion
- calculation
mass
From mole = molar mass
0.5
mole of Me​4​N​+​I​-​ = (12.01)×4 + 3×(1.008)×4 + (14.01) + 126.9
0.5
=​ 201.05 mol
= 2.49 × 10​-3 ​mol
Me​4​N​+​I​-​ = Me​4​N​+​I​5-
​
1 : 1
1
2.49 × 10​-3 × 1 = ​2.49 × 10​-3 ​
mol

mass of Me​4​N​+​I​- ​= (2.49 × 10​-3 ​) × 708.67

= 1.76 g limiting reagent and theoretical yield
1.3 1.3
mole of I​2 = 2(126.9) = 253.8
= 5.12 × 10​-3​ mol
2 I​2 ​ : Me​4​N​+​I​5-
5.12×10−3
2 = ​2.561 × 10​-3 ​ mole excess reagent

From the limiting and excess reagent above, we can find out the amount
of the excess reagent that remains after the reaction occurs by:

Me​4​N​+​I​- + 2I​2 → Me​4​N​+​I​5-

ratio 1 : 2
​
usage 2.49 × 10​-3 (2.49 × 10​-3​) × ​2
(4.98 × 10​-3​) × 126.9
0.632 g
remaining 0 1.3 - 0.632 = 0.668 grams

From the calculation, Iodine will be left for 0.668 grams from 1.3 grams as the
excess reagent of this reaction.

We can find the percent yield of this experiment from:

 actual yield
percent yield = theoretical yield × 100
1.05
= 1.76 × 100
= 59.66 %

- Discussion and error

From the calculation above, we found out that our theoretical yield was 1.77
grams, and the actual yield was 1.05 grams. So the percent yield was 59.577%.
There was almost no crystal that were formed and could be seen. Which means
that during the experiment something went wrong and caused an error as a
result. The mistakes were mainly from human failures, but there was also an
environmental factor which was the airflow from air conditioners in the
laboratory that hit the scale and affected the weights of the reactants and filter
paper to be inaccurate causing the result to not come out in the way it should be.
Anyway the major fault was a human error. First, the process of grinding with a
stirring rod, the reactants might not be thoroughly grinded, which cause the
solution to be a heterogeneous, therefore some parts of the reactant might not
dissolve because they had bigger surface area, and the reaction was not likely to
be 100% completed. The second defect was timing; we reckoned the time too
early, so we took the solution out of a hot plate before the right time, it led to
incomplete chemical reaction. The last factor that made the error product was
that the solution were disturb during the state of crystallization, we might move
it too strong, so the crystal could not form properly.
Conclusion
From this crystallization lab, 1.05 grams of tetramethylammonium
pentaiodide was produced from 0.5 grams(5.122 x 10​-3 ​mole) of iodine(excess
reagent of 12.37 grams) and 1.3 grams(2.487 x 10​-3 ​mole) of
tetramethylammonium(limiting reagent) with a percent yield of 59.577 percent.
From our observation, the result came out as that it was green lattice powder
with almost invisible shimmer.

Suggestion
Since we got a low percent yield from the experiment, we noticed that we
could make it much more better by reducing the human errors during the
experiment. We would be need to be more circumspectly in every procedures
because all of them can cause an error to the result. Weighing, and measurement
must be accurate. While handling the solution we must be very careful since a
slightly gentle bump could disturb the formation of the crystal. By using an
advance technology in either measuring or handling the solution could also help
prevent any errors and gave out a more accurate result.
References
- Britannica (2017). Mole. Retrieved from
https://www.britannica.com/science/mole-chemistry
- ChemTeam (n.d.). Balancing Chemical Equations: Discussion and Fifteen
Examples. Retrieved from
https://www.chemteam.info/Equations/Balance-Equation.html
- Helmenstine (2017). Balancing Chemical Equations. Retrieved from
https://www.thoughtco.com/balancing-chemical-equations-introductio
n-602380
- Helmenstine, Anne Marie, Ph.D. (2017). Crystallize Definition
(Crystallization). Retrieved from
https://www.thoughtco.com/definition-of-crystallize-605854
- Karger B. (2014). Separation and purification. Retrieved from
https://www.britannica.com/science/separation-and-purification/
Exclusion-and-clathration#ref619631