SAFETY AND BASIC LABORATORY TECHNIQUES

(SIC1011)
INORGANIC CHEMISTRY

NAME: DAYANA SYAZANA BINTI MOHD NOOR

MATRIC NUMBER: U2103536
EXPERIMENT: VOLUMETRIC ANALYSIS.
LECTURE NAME: DR. MUGGUNDHA RAOOV A/L
RAMECHANDRAN
OCCURANCE: 4
TITLE: VOLUMETRIC ANALYSIS.

OBJECTIVES:
1. To understand the concept of volumetric analysis.
2. To determine the unknown solution concentration via titration.

RESULTS:
PART A
Table 1: Table of volume of potassium permanganate used against sodium oxalate.
Burette reading (mL) Gross 1 2
Initial volume (mL) 0.00 9.50 18.30
Final volume (mL) 9.50 18.30 27.10
Volume used (mL) 9.50 8.8 8.8
Average volume used (mL) 9.03

Mass of sodium oxalate, 𝑁𝑎2 𝐶2 𝑂4 = 0.2948g

Mass of potassium permanganate, 𝐾𝑀𝑛𝑂4 = 0.9986g
Relative molecular mass of sodium oxalate, 𝑁𝑎2 𝐶2 𝑂4 = 133.99 g/mol
0.2948g
Number of moles of 𝐶2 𝑂4 2− =
133.99 g/mol

= 2.200× 10−3 mol

2.200×10−3 mol
Molarity of 𝐶2 𝑂4 2−= 100
(1000)𝐿

= 0.0220 M
From the equation,

5 𝐶2 𝑂4 2− + 2 𝑀𝑛𝑂4 − + 16 𝐻 + → 10 CO2 + 2 𝑀𝑛2+ + 8 𝐻2 𝑂

Molarity of 𝐾𝑀𝑛𝑂4 :
𝐌𝐶 𝑂 2− 𝐕𝐶 𝑂 2− 5
2 4 2 4
= =
𝐌𝑀𝑛𝑂4 − 𝐕𝑀𝑛𝑂4− 2

(0.0220 M)(25.00) 5
= =
𝑥(9.03) 2
𝑥 = 0.0244 M
 The molarity of potassium permanganate, 𝐾𝑀𝑛𝑂4 = 0.0244 M
 Table 2: Table of volume of iron(II)ammonium sulphate used against nitrite solution

Burette reading (mL) Gross 1 2

Initial volume (mL) 0.00 0.00 0.00
Final volume (mL) 41.50 41.40 41.30
Volume used (mL) 41.50 41.40 41.30
Average volume used (mL) 41.40

From the reaction equation between 𝑀𝑛𝑂4 − and 𝐹𝑒 2+ :

2 𝑀𝑛𝑂4 − + 10 𝐹𝑒 2+ + 16 𝐻 + → 10 𝐹𝑒 3+ + 2 𝑀𝑛2+ + 8 𝐻2 𝑂

Volume of 𝑀𝑛𝑂4 − :
𝐌𝑀𝑛𝑂4 − 𝐕𝑀𝑛𝑂4 − 2
= =
𝐌 𝐹𝑒2+ 𝐕 𝐹𝑒2+ 10
(0.0244 M)𝑥 2
= =
(0.0106 M )(41.40mL) 10
𝑥 = 3.60 mL

Volume of react 𝐾𝑀𝑛𝑂4 with 𝑁𝑂2 − = 10.00 mL - 3.60 mL

= 6.40 mL

From the reaction equation,

5 𝑁𝑂2 − + 2 𝑀𝑛𝑂4 − + 6 𝐻 + → 5 𝑁𝑂3 − + 2 𝑀𝑛2+ + 3 𝐻2 𝑂
𝐌𝑁𝑂2 − 𝐕𝑁𝑂2 − 5
= =
𝐌𝑀𝑛𝑂4 − 𝐕𝑀𝑛𝑂4 − 2

𝑥(8.00 mL) 5
= =
(0.0244 M)(6.40 mL) 2
𝑥 = 0.0488 M
The molarity of nitrite solution = 0.0488 M
PART B
Mass of potassium iodate (step 2) = 0.1940g

Mass of potassium iodate (step 3) = 1.0172g

Table 3a: Table of volume of sodium thiosulphate used against potassium iodate solution

Burette reading (mL) 1 2

Initial volume (mL) 0.00 11.70
Volume after the color of 11.10 22.80
mixture is pale yellow (mL)
Volume after add distilled water 11.70 23.30
and starch solution (mL)
Volume used (mL) 11.70 11.60
Average volume used (mL) 11.65

Table 3b: Table of colour of sodium thiosulphate used against potassium iodate solution
Reading 1 2
Initial colour Brownish Brownish
Colour after titrated liberated iodine Pale yellow Pale yellow
with thiosulphate solution
Colour after add distilled water and Dark blue Dark blue
starch solution
Final colour colourless Colourless

Relative molecular mass of potassium iodate, 𝐾𝐼𝑂3 :

= 39.098 + 126.90 +(3×15.999)

=213.995 g/mol
0.1940g
Number of moles of 𝐾𝐼𝑂3 =
213.995 g/mol

= 9.0656 × 10−4mol
9.0656 ×10−4 mol
Molarity of 𝐾𝐼𝑂3 solution = 100
(1000)𝐿

= 9.0656 × 10−3 M

Overall reaction between,

𝐼𝑂3 − + 5 𝐼 − + 6 𝐻 + → 3 I2 + 3 𝐻2 𝑂

𝟐 𝑺𝟐 𝑶𝟑 𝟐− + 𝑰𝟐 → 𝑺𝟐 𝑶𝟔 𝟐− + 2 𝑰− ( × 𝟑)

:𝐼𝑂3 − + 5 𝐼 − + 6 𝐻 + → 3 𝐈𝟐 + 3 𝐻2 𝑂

: 6 𝑆2 𝑂3 2− + 3 𝑰𝟐 → 3 𝑆2 𝑂6 2− + 6 𝐼 −

= 𝐼𝑂3 − + 6 𝑆2 𝑂3 2−+ 6 𝐻 + → 3 𝐻2 𝑂 + 3 𝑆2 𝑂6 2− + 𝐼 −
 𝐌𝐼𝑂3 − 𝐕𝐼𝑂3− 1
= =
𝐌𝑆 𝑂 2− 𝐕𝑆 𝑂 2−
2 3 2 3
6

(9.0656 ×10−3 M)(11.65mL) 1

= =
𝑥(25.00 mL) 6
𝑥 = 0.0253 M
The molarity of thiosulphate solution = 0.0253 M

Table 4: Table of volume of sodium thiosulphate used against chlorox

Burette reading (mL) 1 2

Initial volume (mL) 0.00 8.40
Final volume (mL) 8.40 17.30
Volume used (mL) 8.40 9.10
Average volume used (mL) 8.75

Overall reaction between,

:2 𝑆2 𝑂3 2− + 𝐼2 → 𝑆2 𝑂6 2− + 2 𝐼 −

: 𝐶𝑙𝑂− + 2 𝐼 − + 2 𝐻 + → 𝐼2 + 𝐶𝑙 − + 𝐻2 𝑂

= 2 𝑆2 𝑂3 2− + 𝐶𝑙𝑂− + 2 𝐻 + → 𝑆2 𝑂6 2− + 𝐶𝑙 − + 𝐻2 𝑂

𝐌𝐶𝑙𝑂− 𝐕𝐶𝑙𝑂− 1
= =
𝐌𝑆 𝑂 2− 𝐕𝑆 𝑂 2−
2 3 2 3
2

𝑥(10.00mL) 1
= =
(0.0253 M)(8.75 mL) 2
𝑥 = 0.0111 M
The molarity of 𝐶𝑙𝑂− = 0.0111 M
In % 𝑪𝒍𝟐 :
𝐶𝑙𝑂− + 4 𝐻 + + 3𝑒 − → 𝐶𝑙2 + 2 𝐻2 𝑂

: 2 moles of 𝐶𝑙𝑂− produces 1 mole of 𝐶𝑙2

Therefore, in 1 𝑑𝑚3 of solution,

: 0.0111 M of 𝐶𝑙𝑂− will produce 5.55 × 10−3 M of 𝐶𝑙2

Number of moles of 𝐶𝑙2 = molarity × volume
10
= 5.55 × 10−3 M × L
1000

= 5.55 × 10−5 mol

Mass of 𝐶𝑙2 = mol × molar mass 𝐶𝑙2

= 5.55 × 10−5 mol × (35.453×2)

= 3.9353× 10−3g

𝐌𝐚𝐬𝐬 𝐨𝐟 𝑪𝒍𝟐
Percentage of 𝑪𝒍𝟐 = × 𝟏𝟎𝟎%
𝑴𝒂𝒔𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏

3.9353×10−3
= × 100%
1000

= 3.9353× 𝟏𝟎−𝟒 %
ANALYSIS AND DISCUSSION:
Part A

In this experiment, the potassium permanganate solution becomes the standard solution after
it has been standardized against sodium oxalate. In preparation, solid sodium oxalate and solid
potassium permanganate had to be completely dissolved so that the standard sodium oxalate solution
and potassium permanganate solution can be obtained. These standard solutions will affect the
volume obtained in the titration of potassium permanganate against sodium oxalate. The end point of
the back titration is much clearer than that of the direct titration. Therefore, back titration is useful in
calculating excess volume of certain solution.
This experiment is an oxidation-reduction reaction. The deep purple colour potassium
permanganate solution acts as an oxidising agent while iron(II)ammonium sulphate solution and
nitrite solution act as reducing agent. The equation is shown as:

5 𝐶2 𝑂4 2− + 2 𝑀𝑛𝑂4 − + 16 𝐻 + → 10 CO2 + 2 𝑀𝑛2+ + 8 𝐻2 𝑂

(PURPLE) (COLOURLESS)

2 𝑀𝑛𝑂4 − + 10 𝐹𝑒 2+ + 16 𝐻 + → 10 𝐹𝑒 3+ + 2 𝑀𝑛2+ + 8 𝐻2 𝑂
(PURPLE) (COLOURLESS)
In this reaction, the temperature of sodium oxalate solution must reach 80°C to enable clearer
outcome of the reaction to be obtained that is the solution changes colour from colourless to pale pink.
Then, the sodium oxalate solutions are titrated with potassium permanganate solution until the end
point, which it turns to pale pink when there are no reducing species left to react.
Nitrite solution is a very volatile liquid. When the nitrite solution is added into the potassium
permanganate solution that has been heated, the precaution step had to be taken which is the tip of the
burette must be below the surface of the solution. It is to prevent vaporization of the nitrite solution.
The tip of burette is rinsed with distilled water first to avoid the result of titration affecting by the
contamination of the solution. The solution must be cooled down to the room temperature before
titration to prevent the oxidation of Fe2+ ions to Fe3+ ions.

Part B

This experiment is also a redox reaction. 𝑙2 is oxidizing agent while 𝑆2 𝑂3 2− is reducing

agent. After the titration between the liberated iodine and thiosulphate solution, the solution
becomes pale yellow. The freshly prepared starch solution is used to test for the presence of
iodine in solution as it can form a complex with Iodine which is dark blue solution. The
freshly prepared starch also act as an indicator so that in the end point, it can be seen clearly
from dark blue to colourless when titrating with sodium thiosulphate solution.
Next, the standardized sodium thiosulphate solution is used to determine the amount of
chlorine in chlorox. The oxidizing power of ‘chlorox’ will be lost when it is exposed to heat,
sunlight or when left uncovered causing a deviation from the actual percentage of chlorine.
The hypochlorite ion oxidizes the iodide ion to molecular ion as shown as the equation below:
𝐶𝑙𝑂− + 2 𝐼 − + 2 𝐻 + → 𝐼2 + 𝐶𝑙 − + 𝐻2 𝑂

The average concentration of hypochlorite in the chlorox is 3.9353× 10−4 %.

QUESTION AND ANSWER:

1. What is an acid base indicator and how it is been used for?

= Acid-base indicators are chemicals used to determine whether an aqueous solution

is acidic, neutral, or alkaline. Because acidity and alkalinity relate to pH, they may
also be known as pH indicators. Acid-base indicators widely used in applications that
involve pH changes, such as titrations, pH testing, and science demonstrations.

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

= In titration, when the colour of the solution is change, it is considered as

equivalence point.

SUMMARY:

The concept of volumetric analysis is understood and the unknown solution concentration via titration
is determined. The molarity of potassium permanganate, 𝐾𝑀𝑛𝑂4 is 0.0244 M. The molarity of nitrite
solution is 0.0488 M. The average molarity of thiosulphate solution is 0.0253 M. The average
concentration of hypochlorite ion, 𝐶𝑙𝑂− is 0.0111 M. The average concentration of hypochlorite in
the chlorox is 3.9353× 10−4 %.

REFERENCES:
Anne Marie.H. (2020, January 27). Equivalence Point Definition: Equivalence Point in Titrations.
Retrieved from https://www.thoughtco.com/definition-of-equivalence-point-605101

Bruce Wilson. (2107, November). Acid-Base Indicator. Retrieved from

https://www.carolina.com/teacher-resources/Interactive/acid-base-indicators/tr10647.tr

StuDocu. (n.d). Retrieved from https://www.studocu.com/my/document/universiti-malaya/inorganic-

chemistry-1/inorganic-1-labreport-u2004-818-exp1/13452514

Inorganic Chemistry First-Year Laboratory Manual, University of Malaya