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Lower 6 Lab #4 to be done in pairs

Skill assessed: AI
Title: Redox Titration
Aim: To determine the concentration of (NH4)2Fe(SO4)26H2O using a redox titration
Apparatus (per pair): 250ml beakers (2), 100ml beaker, 25 ml pipette, pipette filler, 50ml burette,
retort stand and clamp, white tile, funnel, conical flasks (3), 10ml measuring cylinder, 0.02M
KMnO4 (150ml), (NH4)2Fe(SO4)26H2O solution (120ml), 1M H2SO4 (60ml)
1. Rinse all apparatus thoroughly
2. Clamp the burette to the retort stand
3. Using a funnel, fill the burette with potassium permanganate solution ensuring that the tip
is filled
4. Record the initial burette reading.
5. Using the pipette, transfer 25ml of the (NH4)2Fe(SO4)26H2O solution to the conical flask.
6. Using the measuring cylinder, add 10ml of sulphuric acid to the conical flask.
7. Titrate the iron (II) solution against the potassium permanganate until the first permanent
pink color remains.
8. Record the final burette reading.
9. Repeat steps 3 8 to obtain concordant titre values

Final burette
Initial burette
Volume of KMnO4

Write the balanced equation for the reaction taking place

Calculate the average volume of potassium permanganate used
Calculate the number of moles in the average volume of KMnO4 used
From 1 and 3, deduce the number of moles of (NH4)2Fe(SO4)26H2O present in the 25ml
aliquot used
5. Calculate the concentration of (NH4)2Fe(SO4)26H2O in mol/dm3

Titration is a common laboratory method of qualitative chemical analysis that can be used to
determine the unknown concentration of a solution (analyte). The basis of this process is the
reaction between the analyte and a solution of unknown concentration (standard solution). The
analyte is taken in a conical flask using a pipette and the solution of known concentration is take in a
calibrated burette (titrant). The endpoint of a titration is the point at which the reaction between the
titrant and the analyte becomes complete. Generally the endpoint of a titration is determined using
indicators. In some cases, either the reactant or the product can serve as the indicator. A best
example is the redox titration using potassium permanganate where MnO 4- ions acts as the self
indicator. Redox titration is based on oxidation and reduction reaction between the titrant and
analyte. It is a process used to determine the concentration of an ion in an unknown solution by
reacting it with another ion in a solution having a known concentration. The equivalence point is
reached when the total number of electrons lost in the oxidation reaction is equal to the total number
of electrons gained in the reduction reaction. Oxidation is the process of the addition of oxygen or
removal of hydrogen/electron and reduction involves the process of addition of hydrogen/electrons
or removal of oxygen. Oxidizing agents are substances that gain one or more electrons and are
reduced. Reducing agents are substances that lose one or more electrons and are oxidized. That is,
oxidizing agents are electron acceptors, and reducing agents are electron donors. In this titration,
potassium permanganate is the oxidizing agent since it gets reduced in the presence of acid
[MnO4-(aq) + 8H+(aq) + 5e- Mn2+(aq) + 4H2O(l)]. Mohrs salt is the reducing agent since
it gets oxidized, [Fe2+ Fe3+(aq) + e-]. Mohrs salt is a double salt of ferrous sulphate and ammonium
sulphate and its composition is FeSO4.(NH4)2SO4.6H2O. Due to the reduction of purple
permanganate ion to the colorless Mn2+ ion, the solution turn from dark purple to a faint pink color at
the equivalence point.

Acidic conditions are necessary for this titration, because in neutral or alkaline conditions
Mn+7 is reduced only as far as Mn+4. So, the pipetted Fe 2+ solution was acidified by addition of
about 10 cm3 of dilute sulfuric acid before commencement of the titration. Also, it was added to
to increase the concentration of hydrogen ions in the solution, to convert the oxygen from the
oxidizing agent into water molecules. It also prevented hydrolysis and provided charge
balancing. Hydrochloric acid would not have been suitable as it would react with the KMnO4,
and chlorine gas would be evolved. Also, nitric acid would not have been suitable as it is itself a
very powerful oxidizing agent - the NO3- ion is readily reduced and the accuracy of the titration
would have been reduced. No indicator was needed, as the manganate(VII) ions are decolourised
in the reaction until the end-point, when a pale pink colour persists.
Iron(II) is very susceptible to air oxidation, forming iron(III), under neutral or alkaline
conditions but this oxidation is inhibited in the presence of acids. The ammonium
iron(II) sulfate solution is made up in dilute acid solution to make it stable towards
air oxidation.

Your discussion should include but is not limited to:

Deduce the oxidation states of each element before and after the reaction
Deduce what type of redox reaction took place

Include possible sources of error