Illinois Central College

CHEMISTRY 132 Name:___________________________

Laboratory Section: _______
Redox Titration
Equipment
1-25.00 mL burette 0.100 N KMnO
4
solution
2-50 mL beakers KHSO
3
solution of unknown Normality
Objectives
The objectives of this experiment are to develop an understanding of oxidation-reduction
titration and the use of the "eqivalent" concept as applied to oxidizing and reducing agents.
Background
Oxidation Reduction reactions are chemical reactions in which substances undergo changes in
oxidation state.
Oxidation is defined as the loss of electrons (or an increase in oxidation state) and
reduction as the gain of electrons (or a decrease in oxidation state).
In acid base titrations, equivalent amounts of acid and base must be used for exact neutralization
at the titration endpoint. In oxidation-reduction reactions, there is a similar equivalence between
oxidizing and reducing agents.
In acid base reactions, one "equivalent" corresponded to 1 mole of H
+1
(for an acid) or 1 mole of
OH
-1
(for a base). In oxidation-reduction reactions, one "equivalent" refers to 1 mole of
electrons either provided (by a reducing agent) or taken (by an oxidizing agent). So, just as
with acids and bases, one equivalent of a reducing agent will reduce one equivalent of an
oxidizing agent.
At the endpoint of a redox titration;

number of equivalents of oxidizing agent = number of equivalents of reducing agent.
Oxidizing Agent: the substance which takes up electrons
Reducing Agent: the substance which gives up electrons
Alternatively, we can write:
"milliequivalents" of oxidizing agent = "milliequivalents" of reducing agent
where a "milliequivalent is 1/1000 of an equivalent.
Exercise 8 Page 1
Consider the reaction of potassium permanganate with oxalic acid in the presence of sulfuric
acid. The balanced chemical equation and net ionic equations are;
2 KMnO
4
+ 5 H
2
C
2
O
4
+ 3 H
2
SO
4
10 CO
2
+ 2 MnSO
4
+ 8 H
2
O
2 MnO
4
-1
+ 5 H
2
C
2
O
4
+ 6 H
+1
10 CO
2
+ 2 Mn
+2
+ 8 H
2
O
The molecular mass of KMnO
4
is 158.0 g/mol
Since one mole of KMnO
4
actually removes 5 moles of electrons in this redox reaction, we can
say that 1 mol KMnO
4
=5 equivalents of KMnO
4
(at least, in this particular reaction).
This allows us to define the "equivalent weight" of a compound, that is, the mass which would
provide 1 equivalent of oxidizing power. For KMnO
4
, that would be;
The molecular mass of oxalic acid is 90.0 grams. Since one mole of oxalic acid actually provides
2 moles of electrons in this redox reaction, we can say that 1 mol H
2
C
2
O
4
=2 equivalents of
H
2
C
2
O
4
(again, in this particular reaction).
So, the equivalent weight of this reducing agent can also be calculated, that is, the mass of
ocxalic acid that would provide 1 equivalent of reducing power. For oxalic acid, that would be;
This leads us to the logical end of defing the "Normality" of oxidizing and reducing agents just
as we did with acids and bases. Since different oxidizing and reducing agents can provide
various numbers of equivalents, we simply redefine the strength of an oxidizing or reducing
agent as
"the number of equivalents per liter" (or milliequivalents per milliliter) ,or Normality.
Since the endpoint of a redox titration demands that the equivalents of oxidizing agent equal the
equivalents of reducing agent, then;
Exercise 8 Page 2
(
158.0 grams KMnO
4
1 mol KMnO
4
)x(
1 mol KMnO
4
5 equivalents
) = 31.60 grams/equivalent
(
90.0 grams H
2
C
2
O
4
1 mol H
2
C
2
O
4
)x(
1 mol H
2
C
2
O
4
2 equivalents
) = 45.0 grams/equivalent
N
oxidizing agent
=
milliequivalents of oxidizing agent
milliliter
N
reducing agent
=
milliequivalents of reducing agent
milliliter
(reduction: gain of 5 e
-1
) x 2 = 10 e
-1
(oxidation: loss of 2 e
-1
) x 5 = 10 e
-1
N
oxidizing agent
x mL
oxidizing agent
= N
reducing agent
x mL
reducing agent
Safety Precautions
Safety goggles must be worn in the lab at all times. Any skin contacted by chemicals should be
washed immediately.
Procedure
In this experiment, you will determine the normality of the reducing agent, potassium
bisulfite (KHSO
3
) by titrating with a standard 0.100 N KMnO
4
solution.
1. Set up a 25.00 mL burrette and fill it with your unknown concentration of reducing agent
(KHSO
3
). Be sure to record the letter of your unknown on your Report Sheet.
2. Draw 15-25 mL of the 0.100 N KMnO
4
solution (from the dispensing table) into a clean,
dry 50 mL beaker. Carefully read the burette to the nearest 0.01 mL before and after the
withdrawal and record these values on your Report Sheet.
3. Add approximately 5 mL of concentrated (12 M) H
2
SO
4
to your permanganate solution. If
the solution turns brown during the titration with your reducing agent, add additional acid..
4. Dispense the reducing agent into your permanganate solution while stirring drop by drop as
the endpoint is approached, until one drop of the reducing agent completely decolorizes
the permanganate. (White paper or some other white background makes the color change
more discernable.) Record your final burette reading on your Report Sheet.
5. Starting with a different volume of permanganate, repeat the titration for Trial 2.
6. Calculate the Normality of the KHSO
3
and record it on your Report Sheet.
7. Report the average Normality on your Report Sheet.
8. Write a balanced oxidation-reduction equation for the reaction of KMnO
4
with KHSO
3
. The
unbalanced equation is:
KMnO
4
+ KHSO
3
+ H
2
SO
4
MnSO
4
+ KHSO
4
+ K
2
SO
4
+ H
2
O
9. Based on their Normalities, calculate the weights of KMnO
4
and KHSO
3
present in one liter
of each solution and record these values on your Report Sheet.
Exercise 8 Page 3
Exercise 8 Page 4
Illinois Central College
CHEMISTRY 132 Name:___________________________
Laboratory Section: _______
REPORT SHEET
Redox Titration
Unknown Number ___________
Oxidizing Agent: KMnO
4
Final burette reading
Initial burette reading
Volume used
Normality of KMnO
4
0.100 N 0.100 N
Reducing Agent: KHSO
3
Final burette reading
Initial burette reading
Volume used
Normality of KHSO
3
Average Normality
1. Write the balanced redox equation for the reaction of KMnO
4
with KHSO
3
.
(over)
Exercise 8 Page 5
2. Mass of KMnO
4
per liter in a 0.100 N solution. ______________________g/L
3. Mass of KHSO
3
per liter ______________________g/L
(based on your experimental normality)
Show All Calculations Below:
Exercise 8 Page 6
Illinois Central College
CHEMISTRY 132 Name:________________________
Laboratory Section ________
PRELAB: Exp. 8 Redox Titration
1. Balance the following Redox reactions.
a) _____Zn + _____AgNO
3
_____Zn(NO
3
)
2
+ _____Ag
b) _____Sn + _____HNO
3
_____SnO
2
+ _____NO
2
+ _____H
2
O
c) _____MnO +_____PbO
2
+____HNO
3
____HMnO
4
+____Pb(NO
3
)
2
+____H
2
O
d) _____Zn +_____NaNO
3
+_____NaOH _____Na
2
ZnO
2
+_____NH
3
+____H
2
O

e) ___K
2
Cr
2
O
7
+___H
2
S +___H
2
SO
4
__K
2
SO
4
+__Cr
2
(SO
4
)
3
+___S +____H
2
O
f) ___MnCl
2
+___PbO
2
+ ___HNO
3
___HMnO
4
+___Cl
2
+___Pb(NO
3
)
2
+___H
2
O
Exercise 8 Page 7
Exercise 8 Page 8