To determine the percentage of oxalic acid and sodium oxalate in a

mixture.
Introduction
Titration is a laboratory method to be used for quantitative
analysis. Hence, titrametric analysis is extremely important for chemists
to determine the concentration of analyte in a given solution, the
stoichiometry of a reaction, the number of electrons gained or accepted
in a redox reaction, the solubility products and so on. Generally, titration
involves the use of two solutions: an analyte solution and a standard
solution. An analyte solution is the constituent of interest that is to be
studied. The concentration of the analyte is usually unknown. In
contrast, standard solution is defined as the solution for which the
identity and concentration of the solution are known.
During a titration, the equivalence point or endpoint is observed,
indicating that the chemical reaction is complete. However, the
equivalence point and endpoint are both different terms. Equivalence
point is explained as the theoretical completion of a chemical reaction,
while endpoint is defined as the point in a titration at which a reaction is
complete which is to be determined experimentally.
In this experiment, potassium permanganate and sodium hydroxide
are used to determine the percentage of oxalic acid and sodium oxalate
in a mixture. Both oxalic acid and sodium oxalate react with potassium
permanganate :
2 KMnO
4
+ 5 H
2
C
2
O
4
+ 3 H
2
SO
4
----> K
2
SO
4
+ 2 MnSO
4
+ 8 H
2
O + 10
CO
2

or, ionically
2 MnO
4
-
+ 5 C
2
O
4
2-
+ 16 H
+
----> 2 Mn
2+
+ 8 H
2
O + 10 CO
2

Both oxalic acid and sodium oxalate contain one oxalate ion in a
molecule; so the volume of potassium permanganate can be separated
into the portions reacting with oxalic acid and sodium oxalate.
Only oxalic acid will react with sodium hydroxide, thus can be
determined separately.
H
2
C
2
O
4
+ 2 NaOH ----> Na
2
C
2
O
4
+ 2 H
2
O
Apparatus
Pipette, conical flask, hot plate, burette, thermometer.
Materials
Sample consists of oxalic acid and sodium oxalate, 0.02 M potassium
permanganate, 1 M sulphuric acid, 0.1 M sodium hydroxide,
Phenolphthalein indicator.
Procedures
A) Titration 1
1) 25 cm
3
of the sample was pipetted into a conical flask.
2) The solution was acidified with about 15 cm
3
of dilute sulphuric acid.
3) The flask was heated until the flask was too hot to touch (~80C), and
titrated with potassium permanganate.
4) The titration was repeated twice.
B)
1) 25 cm
3
of the sample was pipetted into a conical flask.
2) A few drops of phenolphthalein indicator was added and titrated with
sodium hydroxide until the colour of the solution just turned pink.
3) The titration was repeated twice.
Results and Calculations
A) Titration 1
Titration number 1 2 3
Initial volume of burette (ml) 5.30 22.10 30.50
Final volume of burette (ml) 20.40 37.20 45.60
Total volume of KMnO
4
used
(ml)
15.10 15.10 15.10

Average volume of KMnO
4
required for titration = 15.10 ml
B) Titration 2
Titration number 1 2 3
Initial volume of burette (ml) 0.40 8.80 17.40
Final volume of burette (ml) 8.80 17.40 25.90
Total volume of NaOH used
(ml)
8.40 8.60 8.50

Average volume of NaOH required for titration =
()

= 8.50 ml
Molarity of KMnO
4
, M
1
= 0.02 M
Volume of KMnO
4
used, V
1
= 15.10 cm
3

Volume of sample used, V
2
= 25 cm
3

2 MnO
4
-
+ 5 C
2
O
4
2-
+ 16 H
+
----> 2 Mn
2+
+ 8 H
2
O + 10 CO
2
Since 2 moles MnO
4
-
ions react with 5 moles of C
2
O
4
2-
ions, thus

( )(

)
=

M
2
= 0.0302 M
Concentration of oxalate ions = 0.0302 M = 0.0302 mol dm
-3


From the result of titration 2,
Molarity of NaOH used, M
1
= 0.1 M
Volume of NaOH used, V
1
= 8.50 cm
3

Volume of sample used, V
2
= 25 cm
3

H
2
C
2
O
4
+ 2 NaOH Na
2
C
2
O
4
+ 2 H
2
O
Since 2 moles NaOH react with 1 mole oxalic acid,

= 2
( )(

)
= 2
M
2
= 0.017 M
Concentration of Oxalic acid = 0.017 M = 0.017 mol dm
-3


Concentration of Na
2
C
2
O
4
= Conc. of oxalate ions - Conc. of oxalic acid
= 0.0302 M - 0.017 M
= 0.0132 M
= 0.0132 mol dm
-3

Concentration of oxalic acid = 0.017 mol dm
-3
x [2(1.00794) +
2(12.0107) + 4(15.9994)] g/mol
= 1.5306 g dm
-3

Concentration of sodium oxalate = 0.0132 mol dm
-3
x [2(23) +
2(12.0107) + 4(15.9994)] g/mol
= 1.7691 g dm
-3
Percentage of oxalic acid =

()

x 100 %
= 46.39 %
Percentage of sodium oxalate =

()

x 100 %
= 53.61 %




Objective
To synthesize the pentaaminechlorocobalt(III) chloride complex.
Introduction
Coordination compounds are called such as they contain ions or
molecules, coordinated, or linked to a transition metal. They are also
known as coordination complexes or complex ions because they are
Lewis acid-base complexes. The ions or molecules that bound to the
central transition metal ion are known as ligands while coordination
number is defined as the number of ligands bound to the central
transition metal ion.
Complex compounds comprise of a large group of chemical
compounds and is derived from chemical elements, primarily from
metals and in particular transition metals. Coordination complexes exists
in different forms, such as SO
4
2-
, MnO
4
-
, [FeCN
6
]
2-
, etc.
Many metallic salts exists in the hydrated form, for instance,
CoCl
2
.6H
2
O and consists of the complex ion such as [Co(H
2
O)
6
]
2+
here,
six water molecules act as the ligand bonding directly to the central
metal ion, Co
2+
, by coordinate bond through the donor atom from the
ligand, that is, the oxygen atom from the H
2
O ligand.
The ligands are arranged in an ordered manner around the central
metal atom. Although there are a number of stereochemistry's associated
with these complexes but the most common ones are those of
coordination number 4 ( with tetrahedral or square planar geometries )
and 6 ( with geometries that approximate an octahedron ).
The objective of this experiment is to synthesize the
chloropentaaminecobalt(III) chloride complex. The scheme of the
reactions for the preparation is given below:
2 CoCl
2
.6H
2
O + 2 NH
4
Cl + 8 NH
3
+ H
2
O
2
---> 2 [Co(NH
3
)
5
(H
2
O)]Cl
3
+
12 H
2
O
[Co(NH
3
)
5
(H
2
O)]Cl
3
----> [Co(NH
3
)
5
Cl]Cl
2
+ H
2
O

Apparatus
Beaker
Glass rod
Buchner funnel
Vacuum pump
Materials
Aqueous concentrate ammonia solution
Ammonium chloride
Cobalt (II) chloride 6-hydrate
Hydrogen peroxide solution
Concentrated hydrochloric acid
Procedures
1) In 7.5 ml aqueous concentrated ammonia solution, 1.25 g
ammonium chloride was added.
2) With stirring, 2.5 g cobalt (II) chloride 6-hydrate was added in
small portion. The next portion was not added until the added
portion had dissolved. A yellow precipitate was formed easily.
3) To the slurry above, with stirring, hydrogen peroxide solution (2.0
ml, 30% v/v) was added slowly. A strong reaction occurred.
4) After the reaction had stopped, 7.5 ml concentrated hydrochloric
acid was added slowly to the red aquapentaamine solution.
5) The product was heated on a hot water bath for 20 minutes.
6) The product was then filtered off by vacuum suction and washed
with cold water.
Results and Calculations
Mass of cobalt (II) chloride 6-hydrate used = 2.4878 g
Mass of ammonium chloride = 1.2504 g
Mass of watch glass = 30.7527 g
Mass of watch glass + product = 31.8420 g
Mass of product = 1.0893 g

No. of mole of cobalt (II) chloride 6-hydrate used =



= 0.0105 mol
No. of mole of ammonium chloride =



= 0.0234 mol
2 CoCl
2
.6H
2
O + 2 NH
4
Cl + 8 NH
3
+ H
2
O
2
---> 2 [Co(NH
3
)
5
(H
2
O)]Cl
3
+
12 H
2
O
[Co(NH
3
)
5
(H
2
O)]Cl
3
----> [Co(NH
3
)
5
Cl]Cl
2
+ H
2
O
Cobalt (II) chloride 6-hydrate is the limiting agent in this experiment as
ammonium chloride was added in excess.
2 moles CoCl
2
.6H
2
O produce 2 moles [Co(NH
3
)
5
(H
2
O)]Cl
3
.
0.0105 mole CoCl
2
.6H
2
O produce 0.0105 mole [Co(NH
3
)
5
(H
2
O)]Cl
3
.
1 mole [Co(NH
3
)
5
(H
2
O)]Cl
3
produces 1 mole [Co(NH
3
)
5
Cl]Cl
2
.
Hence, no. of mole of [Co(NH
3
)
5
Cl]Cl
2
produced =

= 0.00525
mol

Molar mass of product, [Co(NH
3
)
5
Cl]Cl
2
= 250.44 g/mol
Theoretical mass of product, [Co(NH
3
)
5
Cl]Cl
2
= 250.44 g/mol x 0.00525
mol
= 1.3148 g