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NAME: NOR FATIHAH BINTI AHMAD

CLASS: M12H
TITLE: PRACTICAL 22: ANALYSIS OF THE IRON CONTENT IN IRON WOOL BY
REDOX TITRATION

DATA COLLECTION
Qualitative:
1. Iron wool is grey in color.
2. Potassium permanganate (VII) solution, KMnO
4(aq)
, is blue-black in color.
3. 2M sulphuric acid and 0.5M sulphuric acid are clear colorless solutions.
4. When iron wool is heated with 2M sulphuric acid, the clear colorless solution gradually
turns grey.
5. At the end of heating, only small residue of iron wool is left in 2M sulphuric acid.
6. After filtering, the resulting iron (II) sulphate solution, FeSO4
(aq)
is clear colorless
solution.
7. When FeSO4
(aq)
that is added with 0.5M sulphuric acid, is titrated with KMnO
4(aq)
, the
clear solution gradually turns into faint red in color.
Quantitative:
1) Mass of iron wool
= 0.9958g 0.0001g

2) Volume of 2M sulphuric acid, H
2
SO
4(aq)

= 50ml 5ml

3) Volume of KMnO
4(aq)
used
Trial Volume of KMnO
4(aq)
used

(
Start of experiment End of experiment
1 0ml 19ml
2 20ml 37ml
3 37ml 55ml
4 56ml 72ml
5 73ml 99ml
Table 1: Volume of KMnO
4(aq)
used during start and end of experiment

DATA PROCESSING
1) Volume of KMnO
4(aq)
used to titrate FeSO4
(aq)

Trial Volume of KMnO
4(aq)
used

(
Example calculation for
volume of KMnO
4(aq)
used to
titrate FeSO4
(aq)

Volume of
KMnO
4(aq)
used used to
titrate
FeSO4
(aq)

(
Start of
experiment
End of
experiment
1 0ml 19ml
=


For trial 2:
= 37-20
=
19ml
2 20ml 37ml 17ml
3 37ml 55ml 18ml
4 56ml 72ml 16ml
5 73ml 99ml 16ml
Table 2: Volume of KMnO
4(aq)
used used to titrate FeSO4
(aq)
(

2) Average volume of KMnO
4(aq)
used in titration in order to reach endpoint

=


= 17.2ml

3) Equation for redox reaction

Oxidation:
Fe
(s)

Fe
2+
(aq)
+ 2e
Fe
2+
(aq)

Fe
3+
(aq)
+ e

Reduction:
MnO4
-
(aq)
+ 8H
+
(aq)
+ 5e Mn
2+(
aq)
+ H
2
O
(l)

Redox:
5Fe
2+
(aq)

+ MnO4
-
(aq)
+ 8H
+
(aq)
5Fe
3+
(aq)
+ Mn
2+
(aq)
+ H
2
O
(l)


4) Number of moles of MnO
4
-

=


= 0.00344 moles
=0.003 moles

The volume of FeSO
4(aq)
prepared is 250ml, but only

of the volume is used, which is


25ml. Hence , the equations needs to be multiplied by 10.

In short,
25ml : 0.000344 moles
250ml : 0.00344 moles

5) Number of moles of Fe
3+
(aq)
:
1 mole of MnO4
-
reacts with 5 moles of Fe
3+
, thus number of moles of Fe
3+

is
= 0.00344 x 5
= 0.0172 moles

6) Mass of Fe
3+
(aq)

= number of moles x relative atomic mass of Fe
1

= 0.0172 x 55.85
= 0.96062g

7) Uncertainties in mass of Fe
3+
(aq)

(



)
(

)
= 0.061g

8) Absolute error
=


= 6.35%

1
http://chemistry.about.com/library/blperiodictable.htm
9) Amount of iron in the iron wool
=
(

x 100%
=


x 100%
= 96.5%

10) Percentage error
=


x 100%
=

x 100%
= 0.52%


CONCLUSION
The theoretical value of iron content in iron wool is 96%, whereas the experimental value
only exceeds 0.5% from the former value. Although the error is not huge, there are still
limitations in the experiment that draws the line between the book value and the empirical value.

EVALUATION
Limitations Suggestions
Overshooting during titration Produce a reference solution and record the
volume of KMnO
4
needed to end up with such
result. For the subsequent trials, carefully
titrate KMnO
4
drop by drop when the reading
is approaching the one recorded for the
reference solution.


From the experiment, the relative molecular mass(RMM) obtained for amidosulphuric acid,
H
3
NSO
3
is 98.9, yet the calculation from book value points that the supposed RMM for
amidosulphuric acid, H
3
NSO
3
is 97.10. There is a difference of 1.8 between those two values and
as the calculation above indicates, 1.80% percentage error since a few errors occurred during the
experiment.
Firstly, end point of neutralization might be exceeded. During titration, overshoot might occur,
causing excessive amount of sodium hydroxide solution to be titrated with amidosulphuric acid
solution. This can be prevented by starting the titration with a trial experiment to obtain the right
end point the moment NaH
2
NSO
3
suddenly turns yellowish orange . When the end point has
been acquired, for the next few readings, make sure when the volume of sodium hydroxide
solution in burette is approaching end point, titrate the alkaline solution drop by drop. Besides,
the sample of NaH
2
NSO
3
from the trial experiment can be kept aside to be referred in the next
readings. On top of that, our eyes should focus on the reading of sodium hydroxide solution in
burette to keep track of the end point.
Secondly, systematic error could have happened since there might be foreign substances from
previous experiments inside burette and pipette. In order to improve the accuracy of this
experiment, rinse burette with sodium hydroxide solution and pipette with amidosulphuric acid
solution beforehand. The contaminants will be removed after rinsing.

There are a few steps should be taken to minimize errors during conducting experiment.
Start the experiment by weighing 2.5g of solid amidosulphuric acid. The windows of electronic
balance must be tightly closed to prevent mass of air affecting the readings later on. Ensure the
electronic balance is at 0.0000g before weighing by pressing the tare button. Weigh the mass
of the container first, followed by the mass of container + solid amidosulphuric acid. After that,
subtract the latter with former to obtain the mass of solid amidosulphuric acid.
Next, while dissolving solid amidosulphuric acid, stir the solution to increase the rate of reaction.
If the solid amidosulphuric acid cannot be dissolved after a few moments, add more water and
keep stirring. Stop stirring when there is no more solute left.
After amidosulphuric acid solution has been transferred into volumetric flask, ensure our eyes
are on the meniscus level while making up the solution to the 250cm
3
mark to avoid random
error. If the meniscus level is exceeded, the experiment has to be repeated all over again or the
solution has to be measured to 250cm
3
by using measuring cylinder, hence increasing the
percentage uncertainty.
During the uptake of 25cm
3
of amidosulphuric acid solution, do not hold the protruding part of
pipette because the part is thinner and slight pressure from our hand can break the pipette, thus
forcing us to find a new pipette and repeat the step to obtain 25cm
3
of amidosulphuric acid
solution.
Then, the titration process must be conducted by one person only to avoid random error. While
titrating, use one hand to control the stopcock of burette whereas the other hand swirls the
conical flask containing amidosulphuric acid solution mixed with methyl orange. Repeat the
experiment a few times to obtain consistent readings.