216 COMPREHENSIVE PRACTICAL CHEMISTRY—XII

2Al(s) + 2KOH(aq) + 6H2O(l) ⎯→ 2KAl(OH)4(aq) + 3H2(g)

Potassium aluminate solution on treatment with dil. sulphuric acid first gives precipitate
of Al(OH)3, which dissolves on addition of small excess of H2SO4 and heating.
2KAl(OH)4(aq) + H2SO4(aq) ⎯→ 2Al(OH)3(s) + K2SO4(aq) + 2H2O(l)
Δ
2Al(OH)3(s) + 3H2SO4(aq) ⎯→ Al2(SO4)3(aq) + 6H2O(l)
The resulting solution is concentrated to near saturation and cooled. On cooling crystals
of potash alum crystallize out.
K2SO4(aq) + Al2(SO4)3(aq) + 24H2O(l) ⎯→ K2SO4 . Al2(SO4)3 . 24H2O(s)

PROCEDURE
1. Clean a small piece of scrap aluminium with steel wool and cut it into very small
pieces. Aluminium foil may be taken instead of scrap aluminium.
2. Put the small pieces of scrap aluminium or aluminium foil (about 1.00 g) into a coni-
cal flask and add about 50 ml of 4 M KOH solution to dissolve the aluminium. The
flask may be heated gently in order to facilitate dissolution. Since during this step
hydrogen gas is evolved, this step must be done in a well-ventilated area. Continue
heating until all of the aluminium reacts. Filter the solution to remove any insoluble
impurities and reduce the volume to about 25 ml by heating.
3. Allow the filtrate to cool. Now add slowly 6 M H2SO4 until insoluble Al(OH)3 just
forms in the solution.
4. Gently heat the mixture until the Al(OH)3 precipitate dissolves. Cool the resulting
solution in an ice-bath for about 30 minutes whereby alum crystals separate out. For
better results the solution may be left overnight for the crystallisation to continue. In
case the crystals do not form the solution may be further concentrated and cooled
again.
5. Filter the crystals from the solution using a vacuum pump, wash the crystals with
50/50 ethanol-water mixture. Continue applying the vacuum until the crystals appear
dry.
6. Determine the mass of the alum crystals.

OBSERVATIONS
Mass of aluminium metal = ............ g
Mass of potash alum = ............ g
Theoretical yield of potash alum = ............ g
Percent yield = ............ %

9. STUDY OF THE EFFECT OF METAL COUPLING ON THE

RUSTING OF IRON

INTRODUCTION
Metals and alloys undergo rusting and corrosion. The process by which some metals when
exposed to atmospheric conditions i.e., moist air, carbon dioxide form undesirable compounds
on the surface is known as corrosion. The compounds formed are usually oxides. Rusting is
INVESTIGATORY PROJECTS 217

also a type of corrosion but the term is restricted to iron or products made from it. Iron is easily
prone to rusting making its surface rough. Chemically, rust is a hydrated ferric oxide
Fe2O3.nH2O. Rusting may be explained by an electrochemical mechanism. In the presence of
moist air containing dissolved oxygen or carbon dioxide, the commercial iron behaves as if
composed of small electrical cells. At anode of cell, iron passes into solution as ferrous ions.
Fe ⎯→ Fe2+ + 2e–
The electrons from the above reaction move towards the cathode and form hydroxyl ions
H2O + (O) + 2e– ⎯→ 2OH–
Under the influence of dissolved oxygen the ferrous ions and hydroxyl ions interact to
form rust, i.e., hydrated ferric oxide.
2Fe2+ + H2O + (O) ⎯→ 2Fe3+ + 2OH–
2Fe3+ + 6OH– ⎯→ Fe2O3.3H2O or 2Fe(OH)3
(Rust)
If supply of oxygen is limited the corrosion product may be black anhydrous magnetite,
Fe3O4.
Methods of Prevention of Corrosion and Rusting
Some of the methods used to prevent corrosion and rusting are:
1. Barrier Protection. In this method, a barrier film is introduced between iron sur-
face and atmospheric air. The film is obtained by painting, varnishing, etc.
2. Galvanization. The metallic iron is covered by a layer of more active metal such as
zinc. The active metal loses electrons in preference to iron.
Zn ⎯→ Zn2+ + 2e–
Thus, protecting iron from rusting and corrosion.

OBJECTIVE OF PROJECT
In this project the aim is to investigate effect of metal coupling on the rusting of iron. Metal
coupling affects the rusting of iron. If the iron nail is coupled with a more electro-positive metal
like zinc, magnesium or aluminium rusting is prevented but if on the other hand, it is coupled
with less electro-positive metal like copper, the rusting is facilitated.

EXPERIMENT 1

To study the effect of metal coupling on rusting of iron.

REQUIREMENTS
Two petridishes, four test tubes, four iron nails, beaker, sand paper, wire gauge. Gelatin, copper,
zinc and magnesium strips, potassium ferricyanide solution, phenolphthalein.

PROCEDURE
1. Clean the surface of iron nails with the help of sand paper. Wash them with carbon
tetrachloride and dry on filter paper.
2. Wind a clean zinc strip around one nail, a clean copper wire around the second and
clean magnesium strip around the third nail. Put all these three and a fourth nail in
petridishes so that they are not in contact with each other.
218 COMPREHENSIVE PRACTICAL CHEMISTRY—XII

3. Preparation of agar agar solution. Heat about 3 g of agar agar in 100 ml of water
taken in a beaker until solution becomes clear. Add about 1 ml of 0.1 M potassium
ferricyanide solution, 1 ml of phenolphthalein solution and stir well the contents.

Iron Zinc Copper Magnesium

nail strip wire ribbon

Fig. P-9.1

Iron Agar — agar Fe — Zn

nail Fe — Cu solution couple
couple Fe — Mg
couple

Fig. P-9.2. Study of effect of metal coupling on rusting of iron.

4. Fill the petridishes with hot agar agar solution in such a way that only lower half of
the nails are covered with the liquids.
5. Keep the covered petridishes undisturbed for one day or so.
6. The liquid sets to a gel on cooling. Two types of patches are observed around the
rusted nail, one is blue and the other pink. Blue patch is due to the reaction between
Ferrous ions and potassium ferricyanide to form potassium ferroferricyanide,
KFe[Fe(CN)6] whereas pink patch is due to the formation of hydroxyl ions which
turns colourless phenolphthalein to pink.

OBSERVATIONS

S. No. Metal pair Colour of the patch Nail rusts or not

1. Iron-Zinc
2. Iron-Magnesium
3. Iron-Copper
4. Iron-Nail
INVESTIGATORY PROJECTS 219

CONCLUSION
It may be concluded that coupling of iron with more electropositive metal such as zinc and
magnesium resists corrosion and rusting of iron. Coupling of iron with less electropositive
metal such as copper increases rusting.

10. PREPARATION OF RAYON THREAD FROM FILTER PAPER

INTRODUCTION
Natural fibres are the chief raw materials for the preparation of rayon. The term rayon includes
all synthetic fibres obtained from cellulose and are used commercially in fibre manufacturing.
Cellulose can be converted into cupra silk, acetate rayon and viscose rayon depending upon the
mode of treatment it undergoes while preparing rayon. Among these, viscose rayon is the most
common.
Cellulose is an insoluble material which is first converted into a soluble derivative called
viscose. The viscose is then forced through fine orifices into some reagent (usually dilute sul-
phuric acid) and the resulting thread is kept under tension to form the fibres of required tensile
strength. Rayon, also called artificial silk, is used for manufacturing of fabrics like stockings,
shirts, sarees, etc.

OBJECTIVE OF PROJECT
This project is aimed at preparation of rayon thread from filter paper employing cuprammonium
process.

EXPERIMENT 1

To prepare rayon threads from filter papers using cuprammonium process.

REQUIREMENTS
Beakers, conical flasks, filtration flasks, vacuum pump, bent tube, glass rod, 50% ammonia
solution, dil. NaOH solution, dil. H2SO4, filter paper or waste paper.

PROCEDURE
The cellulose is dissolved in cuprammonium hydroxide [Cu(NH3)4](OH)2 and the procedure to
be followed is given below:
1. To Prepare Cuprammonium Hydroxide Solution. Weigh about 20.0 g of crystal-
line copper sulphate in a clean watch glass. Dissolve it in 100 ml of water taken in a beaker.
Add dilute NaOH solution to this solution slowly with stirring and note the separation of
precipitate of Cu(OH)2. Filter the precipitate on water pump and wash the precipitate thoroughly
with water so that a portion of filtrate does not indicate the presence of sulphate ions on testing
with BaCl2 solution. Now transfer the precipitate to a 250 ml beaker add 50 ml of liquor ammonia.
The precipitate will dissolve resulting in a deep blue solution of cuprammonium hydroxide
(Schweitzer’s solution). This is the solvent for dissolving cellulose.