AP Chemistry Laboratory Experiments

6 Volumetric Analysis by Redox Titration

Volumetric analysis is a quantitative technique based on the mole

relationships, or stoichiometry, in a chemical reaction. The procedure
Background involves titration. This method determines the volume of one solution,
which will react with an accurately measured volume of another solution.

In this experiment, the titration examines a redox reaction between a

reducing agent, iron (II) and a standardized solution of an oxidizing agent,
potassium permanganate, KMnO4. Each redox reaction involves two ion-
electron equations, called half-reactions. One half-reaction is an oxidation
reaction. In this case, it is,

Fe2+ Fe3+ + e- (oxidation)

The electrons produced by the oxidation reaction are transferred to the other
half-reaction, the reduction reaction, which in this experiment is,

MnO4- + 8H+ + 5e ⟶ Mn2+ + 4H2O (reduction)

In each half reaction there has been a change in the oxidation number of
the reacting species. In the oxidation reaction, the iron has increased from
+2 to +3. In the reduction reaction, the manganese has reduced from +7 to
+2. In order to balance the redox reaction, the number of electrons
produced by the iron(II) must be the same as the number received by the
permanganate ion. Once this is done, the balanced chemical reaction may
be obtained by adding the oxidation and reduction reactions together.

5Fe2+ 5Fe3+ + 5e (oxidation)

MnO4- + 8H+ + 5e Mn2+ + 4H2O (reduction)

Thus, the balanced chemical reaction is,

5Fe2+ + MnO4- + 8H+ 5Fe3+ + Mn2+ + 4H2O (redox)

5x moles x moles

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Thus, x moles of MnO4- react completely with 5x moles of Fe2+.

Since both reactants are in solution, the number of moles, n, of each solute
is related to the volume, V, and the molarity, M, of each solution by the
equation,

volume  molarity V(cm 3

)  M(mol/L)
n = =
1,000 1,000 …6.1
From the balanced equation,

nA : nB = 5:1

where, nA = number of moles of iron(II) ions, Fe2+(aq)

nB = number of moles of permanganate ions, MnO4-(aq)

Thus,
VA  M A V  MB
: B = 5:1
1,000 1,000
or
(VA × MA) = 5(VB × MB) ……………………….….6.2
where, VA = volume of Fe2+solution (mL)
VB = volume of MnO4-(aq) solution (mL)
MA = molarity of Fe2+solution (mol/litre)
MA = molarity of MnO4-(aq) solution (mol/litre)

When using potassium permanganate as a titrant, it acts as its own indicator.

The permanganate ion, MnO4-, is deep purple in color, while the
manganese(II) is almost colorless. Thus, the endpoint is reached at the first
sign of a permanent pink tinge to the solution. The iron(II) solution is a very
pale green color, but it does not interfere with experimental observations.

In this experiment, you will weigh, accurately, a small quantity, m, of iron(II)

sulfate heptahydrate, FeSO4•7H2O. It is dissolved in distilled water and
standardized to 100mL in a standard flask. From this solution, 10mL aliquots
are titrated against a standard solution of potassium permanganate, 0.0200
M KMnO4 and the molarity of the iron (II) solution, MA, is determined. This
is compared to the molarity of the prepared solution and the purity of the
iron salt evaluated

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The students must be able to

• To introduce the techniques involved in volumetric analysis and
Objectives titration.
• To learn how to identify the oxidation and reduction reactions
taking place in a redox titration.
• To learn how to balance a redox reaction
• To determine the concentration of iron (II) in an iron(II) sulfate
solution by titration with a standard solution of acidified potassium
permanganate.
• To determine the purity of the iron (II) sulfate heptahydrate.

beakers (100 mL) (2) white paper square

burette (50 mL) tissue paper
Materials burette clamp paper towels
retort stand small funnel
conical flasks (125 mL) (3) concentrated H2SO4
magnetic stirrer (+ bar) 0.0200 M potassium
burette marker permanganate solution
plastic burette funnel FeSO4•7H2O
pipette (10 mL) distilled water
pipette pump (10 mL) wash-bottle
o ring
analytical balance
volumetric flask (+ stopper) (100mL)
weighing dish
microspatula

• Standard personal protection equipment must be worn at all times.

• Potassium permanganate is a very powerful oxidizing agent. It must
Safety
not come into contact with the skin or eyes. Safety glasses,
disposable rubber gloves and lab coat must be worn, when handling
this substance.
• Concentrated sulfuric acid, H2SO4 is a corrosive solution. It must not
come into contact with the skin or eyes. Safety glasses, disposable
rubber gloves, lab coat must be worn. It is advisable to use the
fume hood while handling this substance.

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Preparation of the Iron (II) Sulfate Heptahydrate Stock Solution

Method 1. Using the analytical balance, measure out accurately about 2.5 g of the
iron (II) sulfate heptahydrate in the weighing dish. Record the actual
mass in the Data Section
2. Place the small filter funnel (if available) on the standard flask (100-mL
volumetric flask) and carefully wash the iron (II) sulfate into it using
distilled water from the wash-bottle until 2/3 from the mark. Swirl the
flask until all the solid is dissolved.
Alternately, the weighing dish can be folded to one corner and carefully
transfer the solid into the mouth of the flask.
3. Fill the flask with enough distilled water until the mark is reached.
4. Replace the cap of the volumetric flask. Hold the cap with the forefinger
while the other fingers are holding the neck of the flask. Turn the flask
upside down and back until the solution is homogenized.

Preparation of the Analyte in the Flask

1. Collect about 50 mL of the Iron (II) sulfate solution in a 100-mL beaker.
2. Using the volumetric pipet, transfer 10 mL of the solution to each of the
three 125-mL Erlenmeyer flask.
3. Record the volume of the solution used in the Data Section.
4. Add about 10 drops of concentrated sulfuric acid (this must be done
under the fume hood!) to each of the analyte solutions in the
flasks. Your teacher may ask you to add more to ensure that
the solution remains acidic.

Preparation of the Buret

1. Collect 80.0 mL of the 0.0200 M KMnO4 solution in a 100 mL beaker and
add a small amount of the liquid in the buret (with the tap in OFF position)
2. Record the actual concentration of the KMnO4 solution as indicated in the
label of the container.
3. Set the buret horizontally and rotate to coat the insides of the buret with
the titrant solution and discard the liquid to the chemical waste bin.

Preparation of the Titrant in the Buret

1. Fill the buret with the 0.0200 M KMnO4 solution collected earlier,
ensuring that the stopcock is closed.
2. Expel the trapped air by allowing the liquid to flow out onto a receiving
container.
3. Refill the buret with the solution to the desired initial volume reading.

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Titration Proper
1. Set up the apparatus illustrated in diagram 6.1, below.

2. Using the burette marker, read the initial volume of the KMnO4 solution
from the bottom of the meniscus. Record this value in the column,
headed “Rough Titer”, in Table 6.2.
[Note: The burette may be read to 0.05 mL only.]
3. Open the burette stopcock and run about 1mL of the KMnO4 into the
flask. Close the stopcock. Initially, a purple color will be seen, but it will
soon disappear.
4. Continue adding the KMnO4 solution, about 1mL at a time, until the pink
color remains. Do not add any more KMnO4 solution.
5. Read the final volume of the KMnO4 solution. Record this value in the
column marked “Rough Titer” in Table 6.2. Calculate the volume of
KMnO4 added to the conical flask.
[Note: This is only an approximate volume of KMnO4 needed to oxidize
completely the iron (II) solution and will not be used in any calculation.]

Note: You may need to refill the burette with KMnO4 solution

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6. For Titer 1, open the burette stopcock and run the KMnO4 solution to a
volume about 2mL less than the rough Titer into the conical flask. Close
the stopcock.
7. From now until the endpoint is reached, add only 1-2 drops of KMnO4 at
a time. Close the stopcock, when the first permanent pink color is
reached. Record the final volume of the KMnO4 solution into the
column, headed “Titer 1”, Table 6.2. Calculate the volume of KMnO4
added to the flask.
8. Switch off and unplug the magnetic stirrer.

Note: You may need to refill the burette with KMnO4 solution
9. For Titer 2, open the burette stopcock and run the KMnO4 solution to a
volume about 2mL less than the titer 1 into the conical flask. Close the
stopcock.
10. From now until the endpoint is reached, add only 1-2 drops of KMnO4 at
a time. Close the stopcock, when the first permanent pink color is
reached. Record the final volume of the KMnO4 solution into the
column, headed “Titer 2”, Table 6.2. Calculate the volume of KMnO4
added to the flask.
11. Switch off and unplug the magnetic stirrer.

Housekeeping
12. Return any surplus KMnO4 solutions to the stock bottle on the Teacher’s
bench.
13. Empty the remains of the iron (II) solution down the sink with plenty of
cold, running tap water. Rinse the standard flask with a small amount of
distilled water.
14. Dismantle the apparatus. Wash out the burette, pipette, beakers and
conical flasks with distilled water, and dry with paper towels.
15. Once you have completed your housekeeping duties, answer all the
questions in the Analysis Section.

1. Fill in the information needed for the Pre-Lab Worksheet

2. Read the Post Lab Guide to writing a Full Lab Report
Results and
Analysis

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Reference

• Iron (II) sulfate heptahydrate has a formula FeSO4•7H2O has a molar mass of 278.02
g/mol
• The percent purity of FeSO4•7H2O can be calculated using the formula below

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑡ℎ𝑒 𝑖𝑟𝑜𝑛 (𝐼𝐼)𝑠𝑢𝑙𝑓𝑎𝑡𝑒 ℎ𝑒𝑝𝑡𝑎ℎ𝑦𝑑𝑟𝑎𝑡𝑒

% 𝑃𝑢𝑟𝑖𝑡𝑦 = × 100%
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑖𝑚𝑝𝑢𝑟𝑒 𝑠𝑎𝑚𝑝𝑙𝑒

• The percentage error for the purity can be calculated as follows

|𝐸𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑉𝑎𝑙𝑢𝑒 − 𝐴𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑉𝑎𝑙𝑢𝑒|

% 𝑒𝑟𝑟𝑜𝑟 = × 100%
𝐴𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑉𝑎𝑙𝑢𝑒

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 AP Chemistry Laboratory Experiments
Curriculum Correlation
Essential Knowledge
• Volumetric relationships can be used to
find the unknown concentration of a
substance by reacting it with a
substance of known concentration.
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Learning Objectives Science Practice
4.3-4.4, 5.1, 6.1
• To perform a volumetric 4.3 The student can collect data to
analysis on a redox answer a particular scientific
reaction question
• To determine the purity
of an impure sample 4.4 The student can evaluate
sources of data to answer a
particular scientific question
5.1 The student can analyze data to
identify a pattern or a relationship
6.1 The student can justify claims
with evidence