EXPERIMENT 2A

“VOLUMETRIC ANALYSIS”
INORGANIC LAB
FIRST-YEAR LABORATORY

NAME : LING YEN HWA

MATRIX NUMBER : SEC 080025

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GROUP :N

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DATE : 10th MARCH 2009

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LECTURER : PROFESSOR DR. SHARIFAH
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BEE
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TUTOR : LEE SEE MU

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LABORATORY : INORGANIC CHEMISTRY 1st

YEAR
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 EXPERIMENT 2A: VOLUMETRIC ANALYSIS

NAME: LING YEN HWA

GROUP: N
DATE OF EXPERIMENT: 10th MARCH 2009
MATRIX NO.: SEC 080025
LECTURER: PROFESSOR DR. SHARIFAH BEE
TUTOR: LEE SEE MU

Objective:
The objective of the experiment is to determine the concentration of potassium permanganate
solution and nitrite solution.

Introduction:
Volumetric analysis is a quantitative analysis process whereby volumes are measured. A

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volume of reagent known as the standard solution of known concentration is chemically

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reacted with a solution of unknown concentration in order to determine the concentration of

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the unknown. The solution that is used as standard is called the titrant which is delivered from

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a burette and is added until the reaction is completed. The end point of the titration is noted

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by observing the change of colour of an indicator. In a direct titration, the titrant is added to
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analyte until the end point is observed whereas in a back titration, a known excess of a
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standard reagent is added to the analyte. A second standard reagent is then used to titrate the
excess of the first reagent. All the calculations in determining the molarity and average
concentration for all equations involve the formula:
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MAVA = a
MBVB b
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The equation for the standardization experiment is given in the ionic form as:
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5C2O42- + 2MnO4- + 16H+ → 10CO2 + 2Mn2+ + 8H2O

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The back titration is explained by the equations:

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5NO2- + 2MnO4- + 6H+ → 5NO3- + 2Mn2+ + 3H2O

2MnO4- + 10Fe2+ + 16H+ → 10Fe3+ + 2Mn2+ + 8H2O

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Method:
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1. About 0.3g sodium oxalate (formula weight = 134) is weighed and is transferred into a
100-mL volumetric flask. 20mL distilled water is added followed by 50mL dilute
sulphuric acid (2.5M) and then is topped up to the calibration mark with distilled water.
2. Potassium permanganate is weighed between 0.8 to 1.0g and then it is transferred into a
250-mL volumetric flask. 50mL distilled water is added to the flask and is shaken to
dissolve the solid, then the calibration mark is topped up with distilled water. Some of the
solution is placed in the burette.
3. 25mL of the sodium oxalate solution is pipette into a 250-mL conical flask. The solution is
heated to 80°C, and the hot solution is titrated with the potassium permanganate solution.
Two more times are repeated.
4. The molarity of the potassium permanganate solution is calculated.

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 5. 10mL of the potassium permanganate solution is ran into a 400-mL beaker and dilute
sulphuric acid (1:5) is added to the 100-mL mark.
6. The beaker is warmed to 40°C, and then 8mL of the nitrite solution is added from a
burette. The tip of the burette must be below the surface of the solution. The tip of the
burette is rinsed with distilled water. The solution is cooled to room temperature.
7. The standard iron(II)ammonium sulfate solution is placed in a burette and is titrated
against nitrite solution. Two more times are repeated.
8. The molarity of the nitrite solution is calculated.

Results and calculations:

Sodium oxalate
Table 1: Table of weight of weighing bottle and weight of weighing bottle with sodium
oxalate
Reading Weight of weighing bottle (g) Weight of weighing bottle
with sodium oxalate (g)
1 21.3259 21.6258

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2 21.3258 21.6259
3 21.3258 21.6258

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Average 21.3258 21.6258

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Weight of weighing bottle + sodium oxalate = 21.6258 g
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Weight of sodium oxalate, Na2C2O4 = 21.6258 g – 21.3258 g
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= 0.3000 g

Potassium permanganate
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Table 2: Table of weight of weighing bottle and weight of weighing bottle with potassium
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permanganate
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Reading Weight of weighing bottle (g) Weight of weighing bottle

with potassium
permanganate
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1 28.70 29.50
2 28.69 29.50
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3 28.70 29.49
Average 28.70 29.50
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Weight of weighing bottle + potassium permanganate = 29.50 g

Weight of potassium permanganate, KMnO4 = 29.50 g – 28.70 g
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= 0.80 g

Table 3: Table of volume of potassium permanganate used against sodium oxalate

Reading Initial volume (mL) Final volume (mL) Volume used (mL)
1 0.40 12.10 11.70
2 12.10 23.75 11.65
3 23.75 35.35 11.60
Average (mL) 11.65

Relative molecular mass of Na2C2O4 = 134

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 Number of mol of C2O42- = 0.3000
134
= 2.24 x 10-3 mol

Molarity of C2O42- = 2.24 x 10-3

100
1000
= 2.24 x 10-2
= 0.0224 M

From the equation,

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

Molarity of KMnO4
MC O VC O
2 4
2-
2 4
2-
=5

m
MMnO VMnO 2

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- -
4 4

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(2.24 x 10-2)(24.9984) = 5

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x(11.65) 2

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x = 0.0192 M
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 The molarity of KMnO4 = 0.0192 M
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Table 4: Table of volume of iron(II)ammonium sulphate used against nitrite solution

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Reading Initial volume (mL) Final volume (mL) Volume used (mL)
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1 0.50 8.50 8.00

2 8.50 16.40 7.90
3 16.40 24.50 8.10
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Average 8.00
From the reaction equation between MnO4- and Fe2+:
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2MnO4- + 10Fe2+ + 16H+ → 10Fe3+ + 2Mn2+ + 8H2O

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MMnO VMnO 4
-
4
-
=2
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MFe VFe 2+ 2+
10

0.0192x = 2
0.0107 x 8.00 10

x = 0.89 mL

Volume of KMnO4 react with NO2-

10.00 – 0.89 = 9.11 mL

From the reaction equation,

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 5NO2- + 2MnO4- + 6H+ → 5NO3- + 2Mn2+ + 3H2O

MNO VNO 2
-
2
-
=5
MMnO VMnO4
-
4
-
2

x8 = 5
(0.0192)(9.11) 2

x = 0.0547 M (molarity of nitrite solution)

Discussion:
The potassium permanganate solution becomes the standard solution after it has been
standardized against sodium oxalate. In preparation of sodium oxalate, make sure that sodium
oxalate is completely dissolved so that the solution produced can react with potassium
permanganate completely. Therefore, a better measurement of volume used (KMnO 4) can be
obtained. In other words, the molarity is known exactly. In enhancing the precision of

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molarity (KMnO4), the calibration mark must be reached exactly on the mark, neither more

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nor less. Back titration is used when the end point of the back titration is clearer than the end

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point of the direct titration of when excess of the first reagent is required. From this, we know

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the volume of KMnO4 that is in excess which is reacting with NO 2-. Therefore, back titration

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is useful in calculating excess volume of certain solution.
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This experiment is also an oxidation-reduction reaction. Potassium permanganate solution
acts as an oxidising agent while iron(II)ammonium sulphate solution and nitrite solution act
as reducing agent. In this reaction, the titrant, which is potassium permanganate acts as its
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own indicator with very deep purple colour. Solutions are titrated with standard MnO 4-are
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usually coloured until the end point, which it turns pink when there are no reducing species
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left to react. In this reaction, the temperature of sodium oxalate solution must reached 80°C to
enable clearer outcome of the reaction to be obtained that is the solution changes colour from
colourless to pink. This is also one of the precaution steps that we should take when
conducting the experiment. Nitrite solution is a very volatile liquid. That is why is has to be
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added into the warmed potassium permanganate solution with the tip of the burette
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submerged into the solution to prevent the vapourisation of nitrite solution occur. Titrating
nitrite solution with potassium permanganate solution will not give an accurate reading due to
vapourisation. The tip of the burette was rinsed to prevent the contamination of the solution.
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The heated solution must be cooled to the room temperature before titrated so that Fe 2+ will
not be oxidised to Fe3+ as this will affect the outcomes of the experiment.
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Conclusions:
In conclusion, the concentration of potassium manganate solution is 0.0192 M and the
concentration of nitrite solution is 0.0547 M.

References:
1. Inorganic Chemistry First-Year Laboratory Manual, University of Malaya
2. Atkin’s Inorganic Chemistry, Oxford University Press

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