2019 DHS Year 5

Practical 1–1: [Volumetric Analysis]

To determine the amount of iron(II) present by titration with potassium manganate(VII) in the presence
of dilute acid

[modified from 9255/Nov 2001/P5]

Aim of Perform a titration to determine the amount of iron (II) present by titration with
Experiment: potassium manganate(VII) in the presence of dilute acid.

Skills: After this experiment, you should be able to:

 read a burette and use a pipette;
 carry out a titration experiment;
 record your titration results in an appropriate manner

Description: FA 1 is a solution prepared by dissolving iron wire in dilute sulfuric acid. Some of
the iron present in FA 1 is in the form of iron(III) ions, Fe3+, the remainder as
iron(II) ions, Fe2+.

FA 2 is a solution of potassium manganate(VII) containing 3.16 g dm−3 of KMnO4.

The iron(II) present may be determined by titration with potassium
manganate(VII) in the presence of dilute acid.

You are required to view the A Level Chemistry LabSkills module under the
Section on Quantitative Analysis  Titrations  Common Experiments 
Iron(II)/ manganate(VII) titrations and answer the following questions before
this practical lesson.

Pre–Lab Q1) What is the colour change at end–point?

Assignment: Pale yellow to pale orange
Q2) What is the mole ratio between Fe2+ and MnO4−?

Equation: 5Fe2+ + MnO4− + 8H+ + 5e–  5Fe3+ + Mn2+ + 4H2O

MnO4−  5Fe2+

Chemicals & You are provided with

Apparatus:
FA 1 is a mixture of iron(III) ions, Fe3+ and iron(II) ions, Fe2+.

FA 2 is a solution of potassium manganate(VII) containing 3.16 g dm−3 of

KMnO4.

1 mol dm−3 sulfuric acid

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 2019 DHS Year 5

S/N Apparatus Quantity per student

1 50 cm3 burette 1
2 25 cm3 measuring cylinder 1
3 stand and burette clamp 1
4 25 cm3 pipette 1
5 pipette filler 1
6 funnel 1
7 250 cm3 beaker 1
8 100 cm3 beaker 1
9 250 cm3 conical flasks 2
10 wash bottle containing distilled water 1
11 white tile 1
12 droppers 2

(a) Titration of FA 1 with FA 2

Method
 Fill the burette with FA 2.
 Pipette 25.0 cm3 of FA 1 into the conical flask.
 Using the measuring cylinder to add about 25.0 cm3 of 1 mol dm−3 sulfuric acid the flask.
 Titrate with FA 2 until the appearance of the first permanent pale orange colour.

Results

 You should perform a rough titration.

 Carry out as many accurate titrations as you think necessary to obtain consistent results.
 Make certain any recorded results show the precision of your practical work.
 Record, in an appropriate form below, all your burette readings and the volume of FA 2
added in each accurate titration.

Rough 1 2
Final burette reading / cm 3
Initial burette reading / cm 3
Volume of FA 2 / cm3

For titration readings

Table drawn with headings and units [1];
2 d.p.[1];
Obtained 2 values that are within  0.10 cm3 of each other [1];
Tick pair of data used, award [1]

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 2019 DHS Year 5

Obtain from your titration results a suitable mean titre. Show clearly the titres used in calculating
the mean.

Working for the calculation of mean titres must be clearly shown with 2 dp [1]

mean titre = 23.00 cm3 of FA 2

[5]

(b) Iron can also be oxidised in air in the presence of water.

Explain why the iron wire was dissolved in dilute sulfuric acid rather than water to form Fe2+.

Iron reacts with acid to form Fe2+ as iron is not soluble in water. [1]

OR

Acidic medium helps to stabilise the +2 oxidation state of iron. Iron in water will be oxidised
to Fe3+.

OR

It is more difficult for iron(II) in acidic medium to undergo oxidation in air than in aqueous
neutral medium.

[1]

(c) Explain why it is unnecessary to measure the volume of the sulfuric acid more accurately than
by using a measuring cylinder in (a).

Sulfuric acid used in (a) merely provides an acidic medium for the titration and moreover, it will
be used in excess. [1]

Hence, the exact amount of it used is not important and measurement of the acid need not be
accurately made.

[1]

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 2019 DHS Year 5

(d)(i) Calculate the concentration, in mol dm−3, of KMnO4 in FA 2.

[Ar: K, 39.1; Mn, 54.9; O, 16.0.]

Relative formula mass of KMnO4 = 158.0 [1]

Concentration of KMnO4 in FA 2 = 3.16/158 = 0.0200 mol dm−3 [1]

[2]

(ii) Calculate how many moles of MnO4− ions are run from the burette into the titration flask.

Moles of MnO4− ions in 23.00 cm3 = (0.0200)(0.0230) = 4.60 x 10−4 mol [1]

[1]

(iii) Calculate how many moles of Fe2+ ions were present in the titration flask.

Moles of Fe2+ ions present in the titration flask = 5 x (4.6 x 10−4)

= 2.30 x 10−3 mol [1]

[1]

(iv) Calculate the mass of iron(II) ions, in 1 dm3 of FA 1.

[Ar: Fe, 55.8]

Moles of Fe2+ ions present in 1 dm3 = (1000/25.0) x (2.30 x 10−3)

= 0.0920 mol [1]

Mass of Fe2+ ions present in 1 dm3 = 0.0920 x 55.8 = 5.13 g [1]

[2]

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 2019 DHS Year 5

Planning 1-2: [Gravimetry Analysis]

To determine that the crystalline solid given is a heptahydrated salt

The aqueous iron(II) ions used in Practical 1-1 are prepared from iron(II) sulfate heptahydrate solid,
FeSO4.7H2O. Describe how you can show by experiment that the crystallised solid is a heptahydrated
salt. You can assume all the apparatus and reagents normally found in a school laboratory are
available. You should include the measurements you would take and explain how you would use your
results to confirm that it is a heptahydrated solid.
[Ar: Fe, 55.8; S, 32.1; O,16.0]

[5]
[Total: 18]

Upon heating,
FeSO4.7H2O  FeSO4 + 7H2O
Procedure:
1. Weigh accurately mass of empty boiling tube using a weighing balance.
2. Weigh accurately mass of hydrated iron(II) sulfate placed in a boiling tube.
3. Record all mass readings.
4. Heat the contents gently initially, followed by strong heating using a Bunsen burner for
about 5 minutes.
5. Allow to cool to room temperature and reweigh the contents and boiling tube.
6. Repeat heat, cool & weighing (repeat steps 4–4) till a constant mass is obtained.
7. Record the final mass of the contents and boiling tube.
[2]
Tabulation of results:

Mass of empty boiling tube = z g

Mass of sample of hydrated iron(II) sulfate + boiling tube = x g

After 1st heating After 2nd heating After 3rd heating [1]
Mass of contents + boiling w y y
tube after heating /g

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 2019 DHS Year 5

Treatment of results:

Mass of water driven out = x – y g

Moles of water driven out = (x–y)/18.0 mol [1]

Moles of FeSO4 = (y– z)/151.9 mol

If sample is heptahydrated solid, FeSO4.7H2O,

(x  y ) [1]
Moles of water driven out
 18.0  7
Moles of FeSO4 ( y  z)
151.9

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