Formal Lab Report

CHEM 1002

Reduction-Oxidation Titration
Name: Nizar Ismail
Partners Name: Adam Hughes
Group: Wednesday AM, group C
Date of experiment: January 28th, 2015
Purpose:

Page | 1

In the reduction-oxidation titration experiment, standardized potassium permanganate solution

(KMnO4) to study and analyze an unknown sample of iron (ii), (Fe2+).

Theory:
A redox reaction is the transfer of electrons from one species to another. The specie which gains
electrons is said to be reduced (oxidizing agent), and the specie losing electrons is said to be
oxidized. The cation iron (ii), (Fe2+), is said to be oxidized due to its loss of electrons. Potassium
permanganate is the oxidizing agent in this experiment, as it gains electrons. The iron (ii), (Fe2+)
cation loses one more electron to be iron (iii), (Fe3+) cation. The ratio of the number of moles of
Fe2+ oxidized per mole of oxidizing agent can be determined by a balanced stoichiometric
reaction equation.
There are four main essential conditions needed to analyse the titration using redox reaction in
the same way of analyzing an acid-base reaction which are:

The reaction must be spontaneous. Which means it should goes in the forward direction.
There has to be a sufficient indicator.

The reaction needs to be fast in order to give instant results.

There shouldnt be any side reactions occurring.

Redox titration of Fe2+ with KMnO4:

1. The following are half reactions for this redox reaction:
Oxidation of Fe2+:

Nizar Ismail - 100988902

CHEM 1002-A4

Fe2+

Fe3+ + 1e-

Formal Lab Report

(1.1)

Page | 2

Reduction of MnO4-:

MnO4- + 8H3O+ + 5e- +

Mn2+ + 12H2O

In order to cancel all electrons, the oxidation reaction is multiplied by five, therefore:

MnO4- + 8H3O+ + 5Fe2+

5Fe3+ + Mn2+ + 4H2O

2. The titration is carried out in an acidic medium by adding excess H2SO4 and a high

temperature to increase the rate of the reaction.

3. The end point must be read quickly, as it fades quickly in an acidic medium due to the reaction of
MnO4- with Mn2+.
4. Phosphoric acid is added because the orange colour of Fe3 - can cause the endpoint to be unclear.
Therefore, Phosphoric acid forms a colourless complex with Fe 2+.
5. The following equation:

2MnO4- + 3Mn2+ + 6H2O

5MnO2 + 4H3O+

Is a side reaction that could occur if the solution isnt acidic enough.

Standardization of KMnO4 solution with Na2C2O4;

1. The following are the half reactions for the standardization reaction:

Oxidation of C2O42-:

C2O42-

Reduction of MnO4-:

MnO4- + 8H3O+ + 5e-

2CO2 + 2e-

Mn2+ + 12H2O

(In order to cancel all electrons, both reactions are multiplied by a factor of five)

16H3O+ + 5C2O42- + 2MnO4-

2Mn2+ + 10CO2 + 24H2O

2. The presence of MnO2 in KMnO4 will alter the standardization reaction.

3. KMnO4 needs to be filtered in order to remove the MnO2 which is insoluble.
4. Titration is held and begun at room temperature, because hot sodium oxalate decomposes
producing peroxide and water if left open to the air with the presence of acid.
5. 1.0 M H2SO4 needs to be titrated as blank in order to make sure of its purity. If the blank took
more than one drop of KMnO4 to turn to pink, then it must be from the titrated volume in
order to correct the titration for the endpoint.

Observations:

Nizar Ismail - 100988902

CHEM 1002-A4

Formal Lab Report

Page | 3

1. The iron sample #222 used was a white coloured powder.

2. During the standardization of KMnO4, the colour of the titration solution changed to light
pale pink.
3. During the titration of Fe2+, the colour of the titration solution changed to light pale pink.

Data:
Table 1.Unknown Fe2+ information:
Accepted value of % Fe2+
1.2%

Sample Number
222

Table 2.Weights of Sodium Oxalate (Na2C2O4):

Trial 1
Trial 2
Trial 3

Mass, Initial(g)
0.0000 0.0001
0.0000 0.0001
0.0000 0.0001

Mass, Leftover (g)

-0.2552 0.0001
-0.2644 0.0001
-0.2837 0.0001

Mass, Sample (g)

0.2552 0.0002
0.2644 0.0002
0.2837 0.0002

Table3. KMnO4Titration Volumes from the Buret in standardization of KMnO4:

Trial 1
Trial 2
Trial 3

Volume, Initial (mL)

34.30 0.05
36.10 0.05
38.12 0.05

Volume, Final (mL)

37.50 0.05
36.80 0.05
40.98 0.05

Volume, Used (mL)

3.20 0.10
0.70 0.10
2.86 0.10

Table 4.Weights of iron ore samples (Fe2+):

Trial 1
Trial 2

Mass,Initial(g)
0.0000 0.0001
0.0000 0.0001

Mass, Leftover (g)

-1.5780 0.0001
-1.5208 0.0001

Mass, Sample (g)

1.5780 0.0002
1.5208 0.0002

Table 5.KMnO4Titration Volumes from the Buret in titrations of the Fe2+ sample:

Trial 1

Volume, Initial (mL)

21.60 0.05

Nizar Ismail - 100988902

CHEM 1002-A4

Volume, Final (mL)

18.60 0.05

Volume, Used (mL)

3.00 0.10

Formal Lab Report

Page | 4

Trial 2

21.60 0.05

18.40 0.05

2.80 0.10

Calculations:
1. Calculation of 90% of KMnO4 added during standardization of KMnO4:
90% of KMnO4 in mL =

MNa 2 C 2O 4
2 mol
1

0.9 1000
( MWNa
)
2C 2 O 4 5 mol 0.02

Trail 1:
90% of KMnO4 in mL =

0.002 g 2
1
)
0.9 1000
( 0.2552
133.9985 g /mol 5 0.02

= 34.28 mL 34.28 mL
Trial 2:
90% of KMnO4 in mL =

0.002 g 2
1
)
0.9 1000
( 0.2644
133.9985 g/mol 5 0.02

= 35.51 mL 35.51 mL
Trial 3:
90% of KMnO4 in mL =

0.002 g 2
1
)
0.9 1000
( 0.2837
133.9985 g/mol 5 0.02

= 38.109 mL 38.12 mL
2. Calculation of [KMnO4]:

[KMnO4] =

Nizar Ismail - 100988902

CHEM 1002-A4

2C2O 4 2
1
)(
( MNa
MWNaC 2 O 4 5 Volume ( Litres) KMnO 4 )

Formal Lab Report

Page | 5

Trial 1:
[KMnO4] =

0.2552 g
2
1
)(
( 133.9985
g /mol 5 0.0375 L )

= 0.0203 mol/L
Trial 2:
[KMnO4] =

0.2644 g
2
1
)(
( 133.9985
g /mol 5 0.0368 L )

= 0.0214 mol/L
Trial 3:
[KMnO4] =

0.2837 g
2
1

( 133.9985
g /mol 5 )( 0.04098 L )

= 0.0207 mol/L

Average of the two successful trials=

0.0203
Average =

mol
mol
mol
+0.0214
+0.0207
L
L
L
3

of values
number of values

= 0.0208 mol/ L

3. Calculation of Percentage Uncertainty:

Nizar Ismail - 100988902

CHEM 1002-A4

Formal Lab Report

Page | 6

Percentage Uncertainty =

volume error
100 )+ (
100 )
( masserror
mass
volume

Trial 1
Percent uncertainty =

0.1
100 )+ (
100 )
( 0.0002
0.2552
3.2

= 3.20%

Trial 2
Percent uncertainty =

0.1
100 ) +(
100 )
( 0.0002
0.2644
0.7

= 14.36%

0.1
100 )+ (
100 )
( 0.0002
0.2827
2.86

= 4.20%

Trial 3
Percent uncertainty =

Average Percentage Uncertainty

=

3.20 +14.36 + 4.20

3

= 7.25%

4. Calculation of the relative spread:

Relative spread =

Relative spread =

difference betweenextreme results

1000
average value

0.0214 mol/ L0.0203 mol/ L

1000
0.0208 mol /L

= 52.88 ppt 52.9 ppt

Nizar Ismail - 100988902

CHEM 1002-A4

Formal Lab Report

Page | 7

5. Calculation of % Fe2+ in the unknown sample:

2+

% Fe =

[ KMnO 4 ] VKMnO 4 5 55.845

MFe 2+ sample

100

Trial 1:
% Fe2+ =

0.0208 0.003 5 55.845

100
1.5780

% Fe2+ =

0.0208 0.0028 5 55.845

100
1.5208

= 1.10%

Trial 2

Average =

= 1.07%

1.10 +1.07
2

= 1.085% 1.1%

Percent Error =

1.085 1.2
100
1.2

= -9.58 %
6. Calculation of Percentage Uncertainty:

Trial 1:
Percent uncertainty=

0.1
100 )+ (
100 )
( 0.0002
1.5780
3.0

= 2.35%

Trial 2

Nizar Ismail - 100988902

CHEM 1002-A4

Formal Lab Report

Page | 8

Percent uncertainty=

7.

0.1
100 )+ (
100 )
( 0.0002
1.5208
2.8

Average =

8.

Relative spread =

2.35+ 3.58
2

= 3.58%

= 2.965%

3.58 2.35
1000 = 415 ppt
2.965

Discussion:
The objective of this experiment was to determine the percentage of iron (ii) in an unknown
sample by redox titration. The accepted value for the percentage of iron (ii) in the unknown
sample is 1.2%, the calculated experimental value was calculated to be 1.1%. The experimental
value was slightly less than the accepted value; therefore the experiment was carried out
precisely and accurately. However, the factors that may have affected this slight difference could
be:
1. The addition of a few more KMnO4 drops after reaching the end point.
2. The further oxidation of iron (ii) to iron (iii). This happens due to the contact of air with
the experiment.

Conclusion:
In conclusion, the accepted value of the sample given (sample #222) was 1.2%, and the
experimental value was calculated to be 1.1%. The percentage uncertainty of the standardization
was calculated to be 7.25%, and the relative spread as 52.9 ppt. However, the percentage
uncertainty of the%Fe2+ was calculated to be 2.965%, and the relative spread as 415 ppt.

Nizar Ismail - 100988902

CHEM 1002-A4

Formal Lab Report

Page | 9

Nizar Ismail - 100988902

CHEM 1002-A4

Formal Lab Report