Work by Brandon Lam, M15604

Synthesis and characterization

of Tin(IV) Iodide
1 AIM OF EXPERIMENT
The aim of the experiment is to prepare Tin(IV) iodide by redox reaction using Tin
and Iodine. We characterize the product by melting point determination and
calculate the yield of the reaction. Further characterization test are done to study
the properties of Tin(IV) iodide.

2 INTRODUCTION
Tin has atomic number 50 and can be recognized by its silvery-white, soft,
malleable and metallic appearance. Tin has two oxidation states, +2 and the
slightly more stable, +4. Tin is mined from Cassiterite, an ore containing the
oxide form of tin. [1] Due to its many uses and applications, Tin has been mined
excessively over the past decade, and soon its depleting primary source,
cassiterite, would not be able to meet the worlds demand. One of its many uses
include forming an alloy with lead to produce solder. Solder is commonly used for
joining pipes and electrical circuits. Tin is also used for plating steel containers
for food preservation. [1]
Iodine is the 53rd element of the periodic table. It is a halogen bearing the
appearance of a metallic lustrous grey in the solid phase and a violet gas in the
gaseous phase. Sublimation of iodine occurs at standard pressure and room
temperature due to its triple point being above 1 atm. Iodine has a low solubility
in polar solvents like water, owing to its non-polar properties. However, it is
easily solvated by non-polar solvents like hexane. Iodine adopts a variety of
oxidation states, however only the oxidation state of -1 is of significance, being
the form found in iodide salts and organoiodine compound. [2] Iodine plays an
important role in our biological function, it is mainly stored in the thyroid gland,
which has functions in synthesis of hormones for regulating body growth and
temperature.
Tin (IV) iodide is a tetrahedral covalent compound and its salt appears as a bright
orange powder. It can dissolve in non-polar solvent and hydrolyse in water. It is
used in reaction with phosphine for formation of halotin anions. [3] Otherwise, tin
(IV) iodide has little to no real life applications.

3 CHEMICAL REACTION
Sn (s)+2 I 2(s) C H 2 C l 2 Reflux Sn I 4 ( aq)

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Work by Brandon Lam, M15604

The oxidation state of Sn changes from 0 in Sn to +4 in SnI 4, Sn is oxidized as a
result. The oxidation state of I changes from 0 in I 2 to -1 in SnI4, I is reduced as a
result. This is a redox reaction.

4 PROCEDURE
0.1190g of tin was shredded with scissors and added together with 0.4818g of
iodine solid into a 25mL round bottom flask (RBF). 6mL of dichloromethane was
measured out with a graduated cylinder and added to the RBF. A stir bar was
added for stirring the solution.
Reflux was set up by first connecting a water pump to the inlet of the condenser
and rubber tubing out of the outlet. The RBF was securely clamped using a retort
stand and the condenser was attached to the RBF using a keck clip. The water
pump was turned on, pumping water at room temperature. The apparatus was
lowered into a water bath set at 130C with rotation at 1400rpm such that the
content in the RBF is In line with the water bath level. Reflux was achieved and
the mixture was refluxed for 30 minutes until the mixture turned brownishorange.
Gravity filtration was used to filter the mixture into a 25mL RBF. The glass funnel
used had a cotton plug to remove the excess solid from the filtrate. Attached the
RBF to the adaptor head on the rotary evaporator and secured using a keck clip.
Rotation was started and the RBF was lowered into a water bath of 55C until the
content level was aligned with the water bath level. Engaged the vacuum pump
and the pressure decreased till a reading of 600 was achieved. The RBF was
removed when all solvent was removed. The RBF (with the product) was weighed
and the mass of product was calculated to be 0.549g. The purity of the product
was determined using a melting point apparatus. The measured melting point
range was 144C 146.1C
A further characterization test was done. Half a spatula of product was added to
a dry test tube along with 2mL of analytical grade acetone. Following that,
deionised water was added dropwise until no further changes was observed. All
observation was recorded and will be discussed later.
5

RESULT

Theoretical Yield

n Sn=

n I2 =

mass 0.1190
=
=0.001002 mol
M r 118.71

mass 0.4818
=
=0.001898 mol
M r 253.80

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Work by Brandon Lam, M15604

Sn+ 2 I 2 C H 2 C l 2 Reflux Sn I 4

(workings for mole ratio in pen)

The limiting reagent is I2 and the maximum moles of SnI4 formed is

0.00094917 mol

mass Sn I 4 =0.00094917 636.328=0.5945 g

Percentage Yield & Melting Point

yield=

Actual yield
0.5490
=
=92.3
Theoretical yield 0.5945

Theoretical melting point: 144.0C

Experimental melting point range: 144.0C 146.1C
Table of results:
Percentage
yield
92.3%

Melting
point
range (C)
144.0 146.1

6 DISCUSSION
Observations
When CH2Cl2 in liquid phase is added to iodine solid, the solution turns purple as
iodine is a non-polar molecule and thus dissolves in a solvent with similar
polarity like dichloromethane (DCM). Tin is insoluble in DCM thus it remains as a
solid at the bottom of the RBF. A reflux was set up for the maintenance of the
reaction at a temperature higher than the boiling point of the solvent (DCM). This
is also done so that the solvent is not lost to the atmosphere in the gaseous
phase.
The water pumped into the condenser was at room temperature. This was to
ensure no condensation occurs at the cooling coils. The solvent used was DCM,
not water, thus condensation will cause water droplets to form on the cooling
coils, drip back into the RBF and contaminate the reaction mixture. Furthermore,
from the characterization test, we see that the product reacts with water, so
water should not be part of the reaction mixture.
In order to increase the rate of reaction, the temperature of reaction must be
moderately high. However, since DCM has a low boiling point (39.8C), a reflux
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Work by Brandon Lam, M15604

was set up so that the reaction could still take place at a high temperature. The
reaction proceeded for around 30 minutes at 120C. In the process, I2 and Sn is
consumed as SnI4 is produced as the concentration of I 2 decreases and that of
SnI4 increases. Consequently the reaction mixture turns from purple to brownishorange. The SnI4 dissolved in DCM takes the appearance of a brownish-orange
solution. At the end of the reaction, black solid was observed at the bottom of
the RBF. This black solid is the unreacted tin metal. This makes sense as iodine is
the limiting reagent (as calculated above), leaving tin in excess.
In order to remove the excess reactants, gravity filtration was used and the
mixture in the RBF was pass through a cotton plug into a clean and dry RBF. After
transferring the solution into the RBF, orange precipitate was observed to form
on the walls of the RBF. This is probably due to the lower surrounding
temperature which decreases the solubility of SnI 4 in DCM, causing its
precipitation.
Next, in order to purify the product, removal of the solvent is required. Therefore,
we boil the product obtained from gravity filtration using the rotary evaporator.
To quickly remove the solvent, a high temperature is needed, however, this may
decompose the product. Thus the product is boiled under sub atmospheric
pressure instead. At a lower pressure, a lower temperature is needed to boil the
DCM away. After the DCM was removed, precipitation of SnI 4 crystals were
observed, it appeared bright orange.
The characterization test included adding half a spatula of the final product to
2mL of analytical grade acetone in a test tube. Acetone solvated the final
product (SnI4 crystals), forming a dark brown solution. It may seem odd that
acetone, a polar solvent, can solvate SnI4, a non-polar compound. But, acetone
(CH3COCH3), has two non-polar and hydrophobic methyl groups, which help in
the solute-solvent interactions between itself and SnI 4. Deionised water was
added to the test tube, while agitating it continuously. The solution turned from
dark brown to light brown then yellow as the concentration of SnI 4 decreases.
Upon further addition of water, white precipitate formed. Tin(IV) hydroxide is the
white precipitate and is formed as described by the equation below. [4]

OH 4 +4 HI
Sn I 4 + 4 H 2 O Sn
Precaution and measures
Some precautions were needed to prevent loss in percentage yield of the
product. Weighing and addition of iodine solid was done after all required
apparatus was properly set up in order to reduce the time it was left exposed as
iodine solid has the ability to sublime under room temperature and pressure.
Also, the heat setting on the heating unit was set to be slightly higher than the
required temperature for reflux as heat may be lost to its surroundings, causing
the temperature of reaction to be lower than the heat setting, lowering the rate
of reaction.
Experimental Flaws and improvement

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Work by Brandon Lam, M15604

Tin has two possible oxidation states, which makes the reaction between Tin and
Iodine produce more than one product. The alternate reaction produces SnI 2 as
described by the chemical equation below.

Sn+ I 2 C H 2 C l 2 Reflux Sn I 2

Although, the +4 oxidation state that tin takes is more stable, making SnI 4 the
main product, the side reaction produces a significant amount of SnI 2. This
affects the purity and yield of the final product. One way to reduce the alternate
product is to use I2 in excess such that the side reaction is minimized and a
larger yield of SnI4 can be obtained.
Another method to improve on the purity of the final product is to perform
recrystallization. This aids in removing the SnI2 and other impurities. SnI2 is polar,
SnI4 is non-polar, and hence SnI2 is more soluble than SnI4 in CH2Cl2. By using the
differing solubility of SnI2 and SnI4, we can separate both of the compound and
isolate the latter.
Finally, cotton plug used for gravity filtration absorbed a significant amount of
filtrate. It is highly possible that cotton absorbs more filtrate than a simple filter
paper, given its size and volume. Furthermore, cotton wool is fibrous and fluffy,
there are multiple large air pockets that will allow contaminants to pass through,
affecting the purity of the end product. An alternative method is to replace the
cotton with filter paper, which has smaller pores and less absorbance.

7 CONCLUSION
SnI4 was successfully synthesized using tin metal and iodine solid with a mass of
0.549g and 92.3% yield. The final product was reasonably pure as the melting
point range, 144.0oC 146.1oC is small with margin of error 2.1. Thus it can be
concluded that the product, SnI4 was produced with high yield and moderate
purity. SnI4 was also characterized for its hydrolysis reacction and some various
properties.

8 POST-LAB QUESTIONS
1. SnI4 consist of four Sn-I bonds and each bond is polar covalent, with a
dipole moment in each of them. Although each Sn-I bond has a dipole
moment, because SnI4 has a tetrahedral symmetrical geometry, the
dipoles cancel each other out. Thus SnI 4 is a non-polar molecule with no
net dipole moment and has polar covalent bonding. SnI 4 has a relatively
large Mr of 636.33g/mol, thus the London Dispersion Forces (LDF) between
the molecules will be relatively strong. Consequently, a relatively high
temperature is required to break the LDF interactions between the SnI 4
molecules, making the melting point of SnI4 relatively high.
2.

Sn I 4 ( s)+2 KI (aq) K 2 [Sn I 6 ]( aq)

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Work by Brandon Lam, M15604

9 REFERENCES
[1]RSC.ORG,. TIN - ELEMENT INFORMATION, PROPERTIES AND USES | PERIODIC TABLE
HTTP://WWW.RSC.ORG/PERIODIC-TABLE/ELEMENT/50/TIN (ACCESSED JUL 9, 2015).
[2]RSC.ORG,. IODINE - ELEMENT INFORMATION, PROPERTIES AND USES | PERIODIC TABLE
HTTP://WWW.RSC.ORG/PERIODIC-TABLE/ELEMENT/53/IODINE (ACCESSED JUL 9, 2015).
[3] APOSTOLICO, L.; KOCIOK-KHN, G.; MOLLOY, K.; BLACKMAN, C.; CARMALT, C.; PARKIN, I.
DALTON TRANS. 2009, 10486.
[4] HYDROLYSIS OF SNI4 HTTPS://UK.ANSWERS.YAHOO.COM/QUESTION/INDEX?
QID=20090119104630AAEBRK1 (ACCESSED JUL 13, 2015).
[5] HARLANFALCONS.ORG,. SYNTHESIS OF TIN(IV) IODIDE AND COMPARISON OF REACTIVITY
AMONG TIN(II) CHLORIDE, TIN (IV) CHLORIDE, AND TIN (IV IODIDE)
HTTP://HARLANFALCONS.ORG/OURPAGES/AUTO/2010/10/13/45969889/AP_LAB%20REPORT
%20EXAMPLE.DOC (ACCESSED JUL 13, 2015).

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