DEPARTMENT OF CHEMISTRY [CHE 323]

EXPERIMENT TITLE: VARIATION OF BOND CHARACTER

WITH OXIDATION STATE: THE PREPARATION OF TIN(II)
CHLORIDE.
EXPERIMENT NO.: 1
SURNAME: Seidisa
INITIALS: T
STUDENT ID: 202103443
LAB GROUP: Monday [0700hrs-1000hrs]
DATE: 21/08/2023
Partners name and ID: Timile S.O. 202101922 and Baleseng K.
20200973
21-08-2023.

VARIATION OF BOND CHARACTER WITH OXIDATION STATE: THE

PREPARATION OF TIN(II) CHLORIDE.

Aim

The aim of this experiment is to explore how changes in oxidation state influence the nature of
chemical bonds by preparing tin(II) chloride and investigating its bonding characteristics.

Abstract

The experiment explores how changes in oxidation state influence the nature of chemical bonds
by preparing tin(II) chloride and investigating its bonding characteristics. Stannous Chloride was
prepared using tin powder and concentrated Hydrochloric acid, and a series of steps were carried
out to obtain anhydrous Stannous Chloride of overall percentage yield of 11.64% . Stannous
Chloride has a melting point of range 216oC – 268oC, and have different bond characteristics in
different solutions; soluble in water, ethanol, acetone, diethyl ether, and insoluble in sodium
hydroxide.

Introduction

Tin,(Sn): atomic weight, 118.69; atomic number, 50; density, 5.8–7.3; melting point, 231.9°C;
boiling point, 2602°C. Tin exists in three allotropic forms: white metallic, tetragonal (tin white),
and white rhombic (tin brittle), and when tin is cooled below 13.2°C, it is converted to allotropic
form called gray tin or a-tin, cubic. Tin is a metal that is insoluble in water, and it is not very
electropositive and, therefore, may be obtained by reduction with a wide variety of reducing
agents, including certain metals (Al, Zn, etc.). Tin may exist either as the metal or in the +2 or +4
oxidation states. Tin forms a large number of inorganic and organic compounds. Inorganic in
compounds are divided into two series: stannous or tin (II) compounds and stannic or tin (IV)
compounds. At pH > 6, stannous compounds are easily oxidized. Tin does not exist in ionized
form, but rather in colloidal complexes. The most common inorganic tin compounds
are stannous chloride (SnCl2), stannous oxide (SnO), stannous fluoride (SnF2), stannic
chloride (SnCl4) and stannic oxide (SnO2),( Ostrakhovitch, et al 2007).

The oxidation states stem from the electron configuration of tin, where it can either lose two or
four electrons to attain a stable configuration. In its +2 oxidation state (Sn2+), tin forms
compounds like tin (II) chloride (SnCl2) and exhibits distinct chemical behaviors due to the
presence of fewer valence electrons, resulting in a different bond character compared to its +4
oxidation state (Sn4+). The Sn2+ ion has a lower charge/radius ratio. Thus, the polarization of the
Cl- by Sn4+ in Tin (IV) Chloride is larger than that of Cl- and Sn2+ in Tin (II) Chloride, which may
be assumed to originally contain Sn4+ ions and Cl- ions. Tin (IV) chloride would then possess a
more covalent nature. Considering the values of the ionization energies, the third and fourth
ionization energies are so high that the total energy required to produce Sn4+ is greater than that
made available by the formation of an ionic lattice. Thus there is little probability of electron loss
from Sn4+, little ionic contribution to the overall bond type, and any Sn (IV) compounds formed
are essentially covalent. The lower values of the first and second ionization energies imply a
greater probability of the formation of Sn2+ , with a consequent increase in the ionic contribution
to the overall bond type (Pass and Sutcliffe, 1987).

Tin production is frequently used in the tin plate, coating, solder, bronze and buckling, metal
alloy, coating for household needs, food packaging, electrical coating (electroplating),
pharmaceutical product, agricultural equipment, tin salt product industry, glaze dye industry, in
the ceramic industry and chemical industry for glass. Stannous chloride (SnCl2) is a tin-derived
compound with applications in various fields, such as catalysts, in surface treatment, as a
reducing agent (Tajuddin, et al. 2021). There are several methods for synthesizing SnCl2 namely
by reacting Sn and HCl to produce SnCl2 in solution. Synthesis of SnCl2 can be done by
recalculating lead powder into 32% HCl and sonication at 800W 24 kHz .SnCl2 is produced by
reacting 60% SnCl4 and lead granules (Wulandari et al 2021). This experiment aims to explore
how changes in oxidation state influence the nature of chemical bonds by preparing tin (II)
chloride and investigating its bonding characteristics.
 [ Sn ] 2+

Figure 1.0: the Oxidation number and

Oxidation state of Tin (II).

Figure 1.1: the structure of Tin (II) Chloride

(SnCl2).

Overall equations:

Sn(s) + 2HCl(l) → SnCl2.2H2O(l) + 2H(g)……………………………….. (1)

SnCl2·2H2O + 2C4H6O3 → SnCl2 + 4C2H4O2............................... (2)

For reaction (1), solid tin (Sn) reacts with liquid hydrochloric acid (HCl) to produce tin (II)
chloride (SnCl2) in liquid state and hydrogen gas (H2) is evolved. This reaction is an example of
a single replacement or displacement reaction, specifically a metal-acid reaction. The tin
displaces hydrogen from hydrochloric acid to form tin chloride and hydrogen gas. The reaction
can be described as an oxidation-reduction reaction, where tin is oxidized from its elemental
state (Sn) to a +2 oxidation state in tin (II) chloride (SnCl2), while hydrogen is reduced from a +1
oxidation state in hydrochloric acid (HCl) to its elemental state as hydrogen gas (H2).

For reaction (2), tin (II) chloride dehydrate (SnCl2•2H2O) reacts with tartaric acid (C4H6O3) to
produce tin (II) chloride (SnCl2) and acetic acid (C2H4O2). The reaction involves the dehydration
of tin (II) chloride dehydrate, where the water molecules are removed from the compound to
form anhydrous tin (II) chloride. The tartaric acid serves as a reactant that provides the necessary
conditions for the dehydration reaction to occur. This type of reaction is a common example of a
dehydration reaction, where a compound loses water molecules to form a different compound.
Materials required:
 Tin powder  Evaporating basin
 Hydrochloric acid  Beaker
 Acetic anhydride  Magnetic stirring rod
 Cold ether  Desiccator (calcium chloride)

Action plan

Dissolve 5g of tin powder in

50ml of concentrated
hydrochloric acid
 Warm the mixture while
constantly stirring
 Filter the hot solution under
gravity
 Reduce the volume of the
solution to about one quarter by
heating
 Cool at room temperature,
then in an ice bath until crystals
form
 Filter off the crystals by
suction, washing with cold ether
 Dry the crystals in a
desiccator and record the yield
 The product was reacted
with acetic anhydride in a
beaker in a fume cupboard
 Filter off the precipitate
formed, washing with cold ether
 Dry on a filter paper and
record the yield
Dissolve 5g of tin powder in
50ml of concentrated
hydrochloric acid
 Warm the mixture while
constantly stirring
 Filter the hot solution under
gravity
 Reduce the volume of the
solution to about one quarter by
heating
 Cool at room temperature,
then in an ice bath until crystals
form
 Filter off the crystals by
suction, washing with cold ether
 Dry the crystals in a
desiccator and record the yield
 React the product with
acetic anhydride in a beaker in a
fume cupboard
 Filter off the precipitate
formed, washing with cold ether
 Dry on a filter paper and
record the yield
 Dissolve 5g of tin powder in 50ml of concentrated hydrochloric acid
 Boil the mixture while constantly stirring(magnetic)
 Filter the hot solution under gravity
 Reduce the volume of the solution to about one quarter by heating(evaporation)
 Cool at room temperature, then in an ice bath until crystals form
 Filter off the crystals by suction, washing with cold ether
 Dry the crystals in a desiccator and record the yield
 React the product with acetic anhydride in a beaker in a fume cupboard
 Filter off the precipitate formed, washing with cold ether
 Dry on a filter paper and record the yield

Experimental Procedure
In the analytical balance, precisely 4.9900g of tin powder was meticulously measured and
subsequently dissolved in 50.0 ml of concentrated Hydrochloric acid (HCl). The resulting
mixture was heated on a hot plate while being stirred with a magnetic rod, until complete
dissolution of the tin powder was achieved. Subsequent to dissolution, gravity filtration was
executed while the solution remained hot, and the filtrate was collected in an evaporating basin.
The solution was then evaporated to approximately one quarter of its original volume. Following
evaporation, the solution was allowed to cool to room temperature and was subsequently placed
in an ice bath, inducing crystallization. The resulting crystals were subjected to suction filtration,
followed by a thorough wash with cold ether under suction. The obtained product was then dried
within a desiccator containing calcium chloride, a process that spanned approximately 24 hours.
Upon completion of drying, the yield was quantified and subsequently, to convert the product
(SnCl2.H2O) to its anhydrous form, 2.2088g of the product was reacted with 4.4176 ml of acetic
anhydride. Once the reaction concluded, the precipitated salt was filtered under suction, washed
with cold ether, and eventually dried on filter paper. The final yield was recorded.

Results
Sn(s) + 2HCl(aq) → SnCl2.2H2O(s) + H2(g)
HCl has SG value of 1.18g/ml
Therefore: mass of HCl ¿ 1.18 g ml−1 ×50.0 ml
¿ 59.00 g
mass
Moles of HCl used ¿
molar mass
59.00 g
¿
36.458 g mol−1
¿ 1.618 mol
mass
Moles of Sn used ¿
molar mass
4.9900 g
¿ −1
118.7100 g mol
¿ 0.04204 mol

Therefore: the limiting reactant is tin (Sn) given the calculations above.
Hence;
Moles of SnCl2.2H2O = (1mol of SnCl2 = 1 mol of Sn)
=0.04204 moles
Theoretical mass of SnCl2.2H2O ¿ moles × molar mass
= 0.04204 mol × 225.63 g/mol
= 9.4855g
Actual mass of product one = 2.2088g
Percentage yield 1 = (actual yield / theoretical yield) ×100%
= (2.2088g/9.4855g) × 100%
= 23.29%

For the second reaction of the dehydration of the crystalline tin (II) chloride using
acetic anhydride;
SnCl2.2H2O + 2C4H6O3 → SnCl2 + 4C2H4O2
Moles of SnCl2.2H2O = mass / molar mass
= 2.2088g / 225.63 gmol-1
= 0.009789mols

Moles of SnCl2 = 0.009789mols

Theoretical mass/yield of SnCl2 = Moles × molar mass
= 0.009789mols ×189.616g/mol
= 1.8561g
Actual yield of product two = 1.1043g
Percentage yield of product two = (actual yield / theoretical yield) × 100%
= (1.1043g /1.8561g) × 100%
= 59.50%
From the Overall reaction 1.1043g was the actual yield of SnCl2 obtained from the 4.9900g of
Sn powder that reacted with 50ml of the hydrochloric acid and the expected mass was 9.4855g,
Therefore overall percentage yield will therefore be;
Percentage yield = (actual yield/theoretical yield) ×100%
 = (1.1043g /9.4855g) × 100%
= 11.64%
Discussion
The results suggest that the experimental yield of the first product, SnCl2.2H2O, was 23.29% of
the theoretically expected yield. This lower yield might be attributed to factors such as
incomplete reaction conversion, side reactions, or losses of the product during purification. The
second reaction, involving the dehydration of SnCl2.2H2O, yielded an anhydrous SnCl2 product
with a higher yield of 59.50%, possibly indicating improved reaction efficiency or purification in
this step. Both reactions showed yields below 100%, indicating that the desired products were
not fully obtained. These discrepancies between theoretical and actual yields could arise from
multiple sources, including incomplete reaction due to limited time during the experiment, and
procedural imperfections like purity of the reactants. Further investigation and optimization of
reaction conditions may enhance the overall efficiency and yield of these chemical processes.
Complementary work was done on the anhydrous Stannous(II) Chloride(SnCl2) and potrayed
different bond character; the product is soluble in water forming a milky solution, it is insoluble
in sodium hydroxide(NaOH), and for solubility in different organic compounds, i) the product is
soluble in acetone giving a milky solution, ii) insoluble in ether, iii) soluble in ethanol, giving a
colourless solution. The mixture of Iron (III) Chloride and potassium hexa-cyanoferrate(III),
coordinate with Tin (II) Chloride forming a dark blue solution. The melting point of the
product ,Stannous(II) Chloride(SnCl2), was ranging from 216oC – 268oC in contrast the melting
point of Tin(IV) Chloride is -33 °C (National Center for Biotechnology Information 2023),
tin(II) chloride, has a higher melting point than tin(IV) chloride, because of the different types of
bonding present in each compound. SnCl2 is held together by ionic bonds, which are strong and
require a lot of energy to break. These bonds are formed by the attraction between the positively
charged tin ions and the negatively charged chloride ions. SnCl4, on the other hand, is held
together by covalent bonds, which are weaker and require less energy to break. These bonds are
formed by the sharing of electrons between the tin and chloride atoms. Because of the stronger
ionic bonds in SnCl2, it requires more energy to separate the ions and melt the compound,
resulting in a higher melting point. According to (Faul and Thiel 2005) conducted a same
research on Tin (II) Chloride and found out that the physical properties of Stannous(II) chloride
are, melting point 246.8 °C; boiling point 623 °C and density of 3.95 gcm−3. Solubility: soluble in
water, ethanol, acetone, diethyl ether, methyl acrylate, methyl ethyl ketone, and isobutyl alcohol.
National Center for Biotechnology Information (2023) Stannous(II) chloride, solid appears as
crystalline mass or flaky solid with a fatty appearance. Density 3.95gcm-3,melting point 247 °C,
boiling point 623 °C and soluble in less than its own weight of water, but it forms an insoluble
basic salt with excess water; Ethanol: soluble.

Conclusion

Tin(II) Chloride was successfully prepared and it was found out to have different bond
characteristics in different solutions; soluble in water, ethanol, acetone, diethyl ether, and
insoluble in sodium hydroxide and had a high melting point ranging from 216 oC – 268 oC,
which is close to the literature value of 247 oC, hence there is variation of bond character with
oxidation state.

References

1. Ostrakhovitch, E. A., & Cherian, M. G. (2007). Chapter 42 - Tin. In G. F. Nordberg, B. A.

Fowler, M. Nordberg, & L. T. Friberg (Eds.), Handbook on the Toxicology of Metals (Third
Edition) (pp. 839-859). Academic Press. ISBN: 9780123694133.
https://doi.org/10.1016/B978-012369413-3/50097-5.
2. Pass, G., and Sutcliffe, H. (1987). Practical Inorganic Chemistry: Preparations, reactions and
instrumental methods. InnChemBook(2nd ed.). Springer Science+Busimess Media B.V.
https://doi.org/10.1038/053243a0
3. Tajuddin, C., Amal, Muhamad, Widayatno, Wahyu, Wulandari, N., Purnomo, D., & Nasikin,
M. (2021). Stannous chloride (SnCl2) and stannous sulfate (SnSO4) synthesis from tin
powderization waste. IOP Conference Series: Earth and Environmental Science, 749,
012025. https://doi.org/10.1088/1755-1315/749/1/012025
4. Wulandari, N., et al. (2021). Optimization Process In The Synthesis of Stannous Chloride
(SnCl2) by Redox Method In The Context of Downstream Tin Derivative Product. Journal of
Physics: Conference Series, 1764, 012034. https://doi.org/10.1088/1742-6596/1764/1/012034
5. National Center for Biotechnology Information (2023). PubChem Compound Summary for
CID 24287, Tin tetrachloride. Retrieved August 27, 2023
from https://pubchem.ncbi.nlm.nih.gov/compound/Tin-tetrachloride.
6. Margaret M. F. and Oliver R. T. (2005) Tin(II) Chloride. Encyclopedia of reagents for oganic
synthesis. https://doi.org/10.1002/047084289X.rt112.pub2
7. National Center for Biotechnology Information (2023). PubChem Compound Summary for
CID 24479, Stannous Chloride. Retrieved August 27, 2023
from https://pubchem.ncbi.nlm.nih.gov/compound/Stannous-Chloride.