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 KMnO4 + 5 H2C2O4 + 3 H2SO4 ----> K2SO4 + 2 MnSO4 + 8 H2O + 10

CO2

or, ionically

2 MnO4- + 5 C2O42- + 16 H+ ----> 2 Mn2+ + 8 H2O + 10 CO2

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.

H2C2O4 + 2 NaOH ----> Na2C2O4 + 2 H2O

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 cm3 of the sample was pipetted into a conical flask.

2) The solution was acidified with about 15 cm3 of dilute sulphuric acid.

3) The flask was heated until the flask was too hot to touch (~80˚C), and

titrated with potassium permanganate.

4) The titration was repeated twice.

B)

1) 25 cm3 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 KMnO4 used 15.10 15.10 15.10

(ml)

Average volume of KMnO4 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 8.40 8.60 8.50

(ml)

(8.40+8.60+8.50)ml
Average volume of NaOH required for titration =
3

= 8.50 ml

Molarity of KMnO4 , M1 = 0.02 M

Volume of KMnO4 used, V1 = 15.10 cm3

Volume of sample used, V2 = 25 cm3

2 MnO4- + 5 C2O42- + 16 H+ ----> 2 Mn2+ + 8 H2O + 10 CO2

M1 V1
Since 2 moles MnO4- ions react with 5 moles of C2O42- ions, thus =
M2 V2

2
5

(0.02 M)(15.10 cm3 ) 2

=
M2 (25 cm3 ) 5

M2 = 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, M1 = 0.1 M

Volume of NaOH used, V1 = 8.50 cm3

Volume of sample used, V2 = 25 cm3

H2C2O4 + 2 NaOH  Na2C2O4 + 2 H2O

M1 V1
Since 2 moles NaOH react with 1 mole oxalic acid, =2
M2 V2

(0.1 M)(8.50 cm3 )

=2
M2 (25 cm3 )

M2 = 0.017 M

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

Concentration of Na2C2O4 = 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

1.5306 g dm−3
Percentage of oxalic acid = (1.5306+1.7691)g x 100 %
dm−3

= 46.39 %

1.7691 g dm−3
Percentage of sodium oxalate = (1.5306+1.7691)g x 100 %
dm−3

= 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 SO42-, MnO4-, [FeCN6]2-, etc.

Many metallic salts exists in the hydrated form, for instance,

CoCl2.6H2O and consists of the complex ion such as [Co(H 2O)6]2+ here,

six water molecules act as the ligand bonding directly to the central

metal ion, Co2+, by coordinate bond through the donor atom from the

ligand, that is, the oxygen atom from the H2O 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 CoCl2.6H2O + 2 NH4Cl + 8 NH3 + H2O2 ---> 2 [Co(NH3)5(H2O)]Cl3 +

12 H2O

[Co(NH3)5(H2O)]Cl3 ----> [Co(NH3)5Cl]Cl2 + H2O

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

2.4878 g
No. of mole of cobalt (II) chloride 6-hydrate used =
237.93 g/mol

= 0.0105 mol

1.2504 g
No. of mole of ammonium chloride =
53.49 g/mol

= 0.0234 mol

2 CoCl2.6H2O + 2 NH4Cl + 8 NH3 + H2O2 ---> 2 [Co(NH3)5(H2O)]Cl3 +

12 H2O

[Co(NH3)5(H2O)]Cl3 ----> [Co(NH3)5Cl]Cl2 + H2O

Cobalt (II) chloride 6-hydrate is the limiting agent in this experiment as

ammonium chloride was added in excess.

2 moles CoCl2.6H2O produce 2 moles [Co(NH3)5(H2O)]Cl3.

0.0105 mole CoCl2.6H2O produce 0.0105 mole [Co(NH3)5(H2O)]Cl3.

1 mole [Co(NH3)5(H2O)]Cl3 produces 1 mole [Co(NH3)5Cl]Cl2.

 0.0105 mol
Hence, no. of mole of [Co(NH3)5Cl]Cl2 produced = = 0.00525
2

mol

Molar mass of product, [Co(NH3)5Cl]Cl2 = 250.44 g/mol

Theoretical mass of product, [Co(NH3)5Cl]Cl2 = 250.44 g/mol x 0.00525

mol

= 1.3148 g