FACULTY OF SCIENCE

DEPARTMENT OF CHEMISTRY

SIC 1011 INORGANIC CHEMISTRY

LAB REPORT

NAME: NISHANTHINI A/P SIVA KUMAR

MATRIC NO: 24005025
EXPERIMENT TITLE: VOLUMETRIC ANALYSIS
OCCURANCE: 4
LAB INSTRUCTOR: DR.WOI PENG MENG
DATE OF EXPERIMENT: 10/12/2024
Objective:

1. To understand the concept of the volumetric analysis

2. To determine the unknown solution concentration by using the standard solution via
titration.

Experimental procedure
Part A:

0.3124 g of sodium oxalate is weighed and transferred to a volumetric flask. 20 mL

distilled water and 50 mL dilute sulfuric acid is added into the flask. The distilled water is
added to a calibration mark.

0.9434 g of potassium permanganate is weighed and transferred to a 250 mL volumetric

25 mL50
flask. ofmLthedistilled
sodiumwater
oxalate solution
is added toisdissolve
pipettedtheinto a 250
salt, andmL
thenconical
moreflask. Thewater
distilled solution
is
is heated
added to 80°C
to the and titrated
calibration mark.with
Somethe
ofpotassium
the solutionpermanganate
is placed in a solution.
burette. The procedure
is repeated 2 times. The molarity of the potassium permanganate solution is calculated.
The beaker is warmed to 40°C and 8 mL of nitrite solution is added. The tip of the burette
The
muststandard
be belowiron the(II) ammonium
surface of the sulphate
solution. solution
The tip ofis burette
placed in a burettewith
is distilled anddistilled
is titrated
against
water. thesolution
The nitrite solution.
is cooled The procedure
to room is repeated 2 times. The molarity of the nitrite
temperature.
10 mL
solutionof the potassium
is calculated. permanganate solution is added into a 400 mL beaker and
The beaker is warmed to 40°C and 8 mL of nitrite solution is added. The tip of the burette
diluted sulfuric acid (1:5) is added to the 100 mL mark.
must be below the surface of the solution. The tip of burette is distilled with distilled
water. The solution is cooled to room temperature.

Part B:

The burette is filled with sodium thiosulphate solution. 0.2134g of potassium iodate solution is
weighed and dissolved with distilled water in a 100 mL volumetric flask.

25 mL of the potassium iodate solution is pipetted into a 250 mL conical flask. 1 g of potassium
iodide solution is added followed by 5 mL of sulphuric acid (1M).

The liberated iodine is titrated with the thiosulphate solution immediately. When the colour of
the mixture turned to pale yellow, 100 mL distilled water is added followed by 1-2 mL of starch
solution

The titration is continued until the solution is colourless. The titration is repeated one more time
and the average molarity of the thiosulphate solution is calculated.

10 mL of the Clorox solution is pipetted into a conical flask. 40 mL of distilled water is added
followed by 1 g of potassium iodide and 10 mL of sulphuric acid (1 M). 8. The liberated iodine is
titrated with standard sodium thiosulphate solution.
 The titration is repeated, and the average concentration of hypochlorite in the Clorox is
calculated (expressed in % Cl2)

Result and analysis

Part A:
Titrate Na2C2O4 solution with KMnO4 solution:

Burette Conical flask A Conical flask B Conical flask C Colour change

reading(mL)

Initial reading 12.30 23.00 26.50

Final reading 23.00 33.60 36.80 Colourless to

pale pink

Volume used 10.70 10.60 10.30

Average volume 10.50

Part A:
 2−¿¿ −¿¿ 2 +¿8 H 2 O ¿

5 C2 O4 + 2 Mn O4 + 16 H +¿→ 10 C O +2 Mn
2 ¿

Molarity of KMnO4:
mass
Moles of Na2C2O4:
molar mass
0.3124 g
¿ −1
133.99 g mol
−3
¿ 2.33 ×10 mol

mole
Molarity of Na2 C 2 O 4 , M :
volume

−3
2.33× 10
= −3
100× 10

¿ 0.0233 M

M aV a a
Molarity of KMnO4 ,M : =
M bV b b

−3
( M a )(10.50× 10 )
2
: −3
=
(0.0233)(25 ×10 ) 5

= 0.02219 M

Titrate (KMnO4 solution + nitrite solution) with the iron (II) ammonium sulphate solution:

Molarity of iron (II) ammonium sulphate: 0.01034

Burette reading (mL) 1st reading 2nd reading Colour change

Initial reading 16.90 17.20

Final reading 50.00 49.30 Purple colour to

colourless
Volume used 33.10 32.10

Average volume 32.60

5 NO 2−+ 2 MnO 4 →5 NO 3−+2 Mn 2+ +3 H 2 O
2 MnO 4−+10 Fe 2++16 H +→10 Fe 3++2 Mn 2++8 H 2O
2+¿ +8 H O¿
2
3+¿+ 2Mn ¿
2+ ¿+ 16H +¿ → 10 Fe ¿
¿
−¿+10 Fe ¿
overall equation :2 Mn O 4

M aV a a
Molarity of nitrile solution: =
M bV b b

(0.02219)(V a) 2
: −3
=
( 0.01034 ) (32.60× 10 ) 10

:3.0382 ×10−3 mL

Volume of KMnO4 that reacts with Fe2 +¿¿ = (10 – 3.0382 )×10−3 mL
−3
¿ 6.9618 ×10 mL

Molarity of Nitrite solution: ¿ ¿

−3
: (0.02213)(6.9618 × 10 )
¿¿

: 0.04815 M

Part B:
Titrate (KIO3 solution +KI solid + H2SO4 solution) with Na2S2O4 solution:

Burette reading 1st reading 2nd reading 3rd reading Colour change
(mL)
Initial reading 15.10 9.50 21.30

Final reading 31.50 25.70 37.80 Dark brown to

pale pink
Volume used 16.40 16.20 16.50

Average volume 16.35

Molarity of thiosulphate solution:
Conical A:
mass
Moles of potassium iodate, KIO3 =
molar mass
0.2134
=
214
= 9.972 ×10−4 mol
−4
9.972 ×10
Molarity of KIO3=
0.1
= 9.972 ×10−3 M

Given,
+ ¿→ 3I +3H O ¿
2 2

−¿+5 I −¿+ 6 H ¿
¿
IO 3
−¿ ¿
2−¿+6 I ¿
¿
6 S2 O2−¿+3
3
I 2 →3 S 4 O6

Overall equation:
−¿ +3I +3H O ¿
2 2
2−¿+ 6I ¿
2−¿ →3S O ¿
+ ¿+6 S O 4 6 ¿
2 3
−¿+ 6 H ¿
−¿+5 I ¿
I O3

2−¿¿

From the equation above: 1 mol of I O−¿≡6

3
mol of S 4 O6 ¿

M 1V 1 6
= =
M 2V 2 1
−3
(M 1)(16.35 ×10 ) 6
= −3 −3
=
(9.972 ×10 )(25× 10 ) 1

Molarity of thiosulphate = 0.09148 M

Titrate (Clorox solution +KI solution+ H2SO4 solution) with the Na2S2O4 solution:

Burette reading (mL) 1st reading 2nd reading Colour change

Initial reading 11.60 21.30

Final reading 28.00 38.10 Dark brown to

colourless
Volume used 16.40 16.80
 Average volume 16.60
used

Ionic equations:
−¿+ H O¿
2
−¿+ 2H + → I2 + Cl ¿

Cl O−¿+2 I ¿

−¿ ¿
2−¿+ 2 I ¿
¿
2 S 2 O2−¿+
3
I →S2 4 O6

Overall equation:
2−¿ +H O ¿
2
−¿+ S O ¿
4 6
2−¿+ 2 H+ ¿→ C l ¿
¿
−¿+2 S2 O3 ¿
Cl O

2−¿¿

From the equation, 1 mole of ClO−¿≡2 mole of S O 2 3 ¿

M 1V 1 1
By using formula: =
M 2V 2 2
−3
M 1(10 ×10 ) 1
= −3
=
(0.09148)(16.6 × 10 ) 2

Molarity of hypochlorite = 0.07593 M

Mole of ClO−¿=molarity × volume ¿

= 0.07593 × 0.01
= 7.593×10−4 mol

+¿ → I +2 H O+C l ¿
2 2 2
−¿+4 H ¿

2 ClO−¿+2 I ¿

To calculate the percentage of Cl 2 :

2 moles of ClO−¿≡1 mole of C l ¿ 2

7.593×10−4 mol ≡ 3.7965×10−4 mol

Mass of Cl 2
mass , n × molar mass
= 3.7965×10−4 mol ×70.90 g mol−1

= 0.02692 g

Percentage of active Cl 2:
0.0269
×100=2.69 %
1.0000

Conclusion:
1. The molarity of the potassium permanganate solution is 0.02219M.
2. The molarity of nitrite solution is 0.04815 M
3. The molarity of the thiosulphate solution is 0.09148 M
4. The concentration of hypochlorite in the Chlorox (expressed in % C l 2 ¿ is 2.69 %

Question:
1. What is an acid base indicator and how it is been used for?
An acid base indicator is a chemical substance that changes colour with pH, it is
used to determine whether an aqueous solution is acidic, neutral or alkaline .

2. How to determine the equivalence point of a titration?

The equivalence point is the point in a neutralization reaction where the number of
moles of hydrogen ions are equal to the number of moles of hydroxide ions.