PUC1 PRACTICAL PROCEDURE

1. Preparation of potash alum

2. Acid –Base Titrations :
a. Sodi um hydroxide Vs hydrochloric acid
b. Sodium carbonate Vs hydrochloric acid
3. Redox titrations:
c. Potassium permanganate Vs oxalic acid
d. Potassium permanganate Vs Mohr’s salt (ferrous
ferrous ammonium sulphate
sulphate)

1. Preparation of potash alum.

Aim: To prepare potash alum (K2SO4*Al2 (SO4)3*24H2O)
Principle:

Potash
otash alum is prepared by dissolving an equimolar mixture of aluminium
sulphate and potassium sulphate in minimum amount of water containing a
little amount of sulphuric acid and then subjecting
subject the solution to
crystallization; octahedral crystals of potash alum separate out.

Apparatus required:

Beaker (250 mL), Trough, Funnel,

Funne Wire gauze, Glass rod, Tripod stand

Chemicals required:

Aluminium sulphate : 5 g
Water : 20 mL
Potassium sulphate : 1.4 g
Dilute sulphuric acid : 0.5 mL
Alcohol + water mixture: 2 cc
Procedure:

a. Take 20 mL of distilled water in a 250 mL beaker and heat it to about 40°c. Add
about 0.5 mL of dilute sulphuric acid, warm this and dissolve 5 g of aluminium
sulphate adding small amounts at a time.
b. Weigh 1.4 g of powdered potassium sulphate and add it to the above solution
stir well.
c. Heat the solution with constant stirring till potassium sulphate dissolves
completely and to concentrate to the crystallization point on water bath.
d. Allow the solution to cool to room temperature.
e. On cooling, white crystals of potash alum separate out.
f. Decant the mother liquor carefully and shake gently with a mixture of
(1 cc alcohol + 1 cc water) to the crystals mixture..
g. Filter the crystals, dry these between the folds of a filter paper and note the
yield.

Results:

Weight of crystals obtained = ………………… g

Color of the crystals = ………………….

The crystals of potash alum are octahedral in shape.

Precautions:

a. Cool the solution slowly to get good crystals. Avoid rapid cooling.
b. Do not disturb the solution while cooling.

Answer the following question:

1. Why do we take equimolar quantities of reacting compounds in the

preparation of Alum?
 Volumetric analysis – I
NaOH vs. HCl
Aim: - Calculate strength of sodium hydroxide (NaOH) solution. Using standard
0.1 M hydrochloric acid (HCl) solution.

Chemical equation: - NaOH + HCl ⟶ NaCl + H2O

Indicator: - Phenolphthalein

End point: - Pale pink to colorless

Apparatus used: - Burette, Pipette, Conical flask (Titration flask), Standard flask
and glazed tile.

Procedure:-

 Burette is washed with water and rinsed with given HCl solution.
 Fill the burette with given HCl solution up to the mark and fix it to the
stand.
 First given NaOH is standardized by using standard flask with the help of
water up to the mark.
 Pipette is taken and rinsed with the standard NaOH solution and pipette
out 20ml of the solution in to the conical flask.
 1 – 2 drops of phenolphthalein indicator are added to the conical flask. The
solution becomes pink in color.
 The flask is placed on the glazed tile under the burette and the initial
reading in burette is noted.
 The HCl solution in the burette is released slowly and drop wise with
continuous shaking of conical flask until the end point is reached i.e. the
pink color is just disappeared.
 At the end point pink color of the solution disappears.
 The final reading in the burette is noted.
  Wash the conical flask; Repeat the experiment till to get two concurrent
readings.
 The readings are tabulated in the following table.

Observations:-

S.No. Pipette volume Initial reading of Final reading of Volume of acid

(NaOH) (ml) the burette (ml) the burette (ml) (HCl) used. (ml)
(a) (b) (b-a)
1
2
3
4

HCl solution:

Molarity of given HCl = M1 = 0.1 M

Volume of acid (HCl) consumed = V1 ml =

Soichiometric coefficient of HCl in balanced equation = n1 = 1

NaOH Solution:

Molarity of NaOH taken = M2 =?

Volume of NaOH taken for each titration (Pipette volume) = V2 ml =

Soichiometric coefficient of NaOH in balanced equation = n2 = 1

Calculations:-

M1V1/n1 = M2V2/n2

M2 = [M1V1/n1] x [n2/ V2]

Molarity of NaOH taken = M2 = -------- M (or) mol/liter

 Strength of sodium hydroxide (NaOH) solution = M2 x GMW
Molar mass of NaOH = GMW = 40 g/mol

Strength of sodium carbonate (NaOH) solution = -------- g/liter

Volumetric analysis – II
Na2CO3 vs. HCl
Aim: - Calculate strength of sodium carbonate (Na2CO3) solution. Using standard
0.2 M hydrochloric acid (HCl) solution.

Chemical equation: - Na2CO3 + 2 HCl ⟶ 2 NaCl + H2O + CO2

Indicator: - Methyl orange

End point: - Pale yellow to Pale pink

Apparatus used: - Burette, Pipette, Conical flask (Titration flask), Standard flask
and glazed tile.

Procedure:-

 Burette is washed with water and rinsed with given HCl solution.
 Fill the burette with given HCl solution up to the mark and fix it to the
stand.
 First given Na2CO3 is standardized by using standard flask with the help of
water up to the mark.
 Pipette is taken and rinsed with the standard Na2CO3 solution and pipette
out 20ml of the solution in to the conical flask.
 1 – 2 drops of methyl orange indicator are added to the conical flask. The
solution becomes pale yellow.
  The flask is placed on the glazed tile under the burette and the initial
reading in burette is noted.
 The HCl solution in the burette is released slowly and drop wise with
continuous shaking of conical flask until the end point is reached i.e. the
pale yellow color is changed to pale pink.
 At the end point pale yellow color is changed to pale pink.
 The final reading in the burette is noted.
 Wash the conical flask; Repeat the experiment till to get two concurrent
readings.
 The readings are tabulated in the following table.

Observations:-

S.No. Pipette volume Initial reading of Final reading of Volume of acid

(Na2CO3) (ml) the burette (ml) the burette (ml) (HCl) used. (ml)
(a) (b) (b-a)
1
2
3
4

HCl solution:

Molarity of given HCl = M1 = 0.2 M

Volume of acid (HCl) consumed = V1 ml =

Soichiometric coefficient of HCl in balanced equation = n1 = 2

Na2CO3 Solution:

Molarity of Na2CO3 taken = M2 =?

Volume of Na2CO3 taken for each titration (Pipette volume) = V2 ml =

Soichiometric coefficient of Na2CO3 in balanced equation = n2 = 1

Calculations:-

M1V1/n1 = M2V2/n2

M2 = [M1V1/n1] x [n2/ V2]

Molarity of Na2CO3 taken = M2 = -------- M (or) mol/liter

Strength of sodium carbonate (Na2CO3) solution = M2 x GMW

Molar mass of Na2CO3 = GMW = 106 g/mol

Strength of sodium carbonate (Na2CO3) solution = -------- g/liter

Questions:
1. What is indicator?
Solution:
Indicator is a chemical substance which changes colour at the end point.

2. What is end point?

Solution:
The stage during titration at which the reaction is just complete is known as
the end point of titration.

3. Why a titration flask should not be rinsed with the reacting solution?
Solution:
This is because during rinsing some liquid will remain sticking to the titration
flask, therefore the pipette volume taken in the titration flask increases.

4. Burette and pipette must be rinsed with the solution with which they are
filled, why?
Solution:
 The burette and pipette are rinsed with the solution with which they are filled
in order to remove any substance sticking to their sides, which otherwise
would decrease the volume of the liquids to be taken in them.

Volumetric analysis – III

KMnO4 vs. Mohr’s salt
Aim: - Calculate strength of Mohr’s salt solution. Using standard 0.02 M
potassium permanganate (KMnO4) solution.

Mohr’s salt formula = FeSO4* (NH4)2SO4*6H2O

Chemical equation: -

2 KMnO4 + 8 H2SO4 + 10 FeSO4  2 MnSO4 + K2SO4 + 8 H2O + 5 Fe2 (SO4)3

2 mole KMnO4 = 10 mole FeSO4

Indicator: - No indicator is needed. KMnO4 acts as self indicator.

End point: - Colorless to Pale pink

Apparatus used: - Burette, Pipette, Conical flask (Titration flask), Standard flask
and glazed tile.

Procedure:-

 Burette is washed with water and rinsed with given KMnO4 solution.
 Fill the burette with given KMnO4 solution up to the mark and fix it to the
stand.
 First given Mohr’s salt solution is standardized by using standard flask
with the help of water up to the mark.
 Pipette is taken and rinsed with the Mohr’s salt solution and pipette out 20
ml of the solution in to the conical flask and add 10 ml of dil.H2SO4 to the
conical flask.
  The flask is placed on the glazed tile under the burette and the initial
reading in burette is noted.
 The KMnO4 solution in the burette is released slowly and drop wise with
continuous shaking of conical flask until the end point is reached i.e. the
colorless solution turns into pale pink.
 At the end point colorless solution turns into pale pink.
 The final reading in the burette is noted.
 Wash the conical flask; Repeat the experiment till to get two concurrent
readings.
 The readings are tabulated in the following table.

Observations:-

S.No. Pipette volume Initial reading of Final reading of Volume of KMnO4

Mohr’s salt the burette (ml) the burette (ml) used. (ml)
(ml) (a) (b) (b-a)
1
2
3
4

KMnO4 solution:

Molarity of given KMnO4 = M1 = 0.1 M

Volume of KMnO4 consumed = V1 ml =

Soichiometric coefficient of KMnO4 in balanced equation = n1 = 2

Mohr’s salt Solution:

Molarity of Mohr’s salt taken = M2 =?

Volume of Mohr’s salt taken (Pipette volume) = V2 ml =

Soichiometric coefficient of Mohr’s salt in balanced equation = n2 = 10

Calculations:-
 M1V1/n1 = M2V2/n2

M2 = [M1V1/n1] x [n2/ V2]

Molarity of Mohr’s salt taken = M2 = -------- M (or) mol/liter

Strength of Mohr’s salt solution = M2 x GMW

Molar mass of Mohr’s salt = GMW = 392 g/mol

Strength of Mohr’s salt solution = -------- g/liter

Volumetric analysis – IV
KMnO4 vs. C2H2O4
Aim: - Calculate strength of oxalic acid (C2H2O4) solution. Using standard 0.02 M
potassium permanganate (KMnO4) solution.

Chemical equation: -

2 KMnO4 + 3 H2SO4 + 5 C2H2O4  2 MnSO4 + K2SO4 + 8 H2O + 10 CO2

Indicator: - No indicator is needed. KMnO4 acts as self indicator.

End point: - Colorless to Pale pink

Apparatus used: - Burette, Pipette, Conical flask (Titration flask), Standard flask
and glazed tile.

Procedure:-

 Burette is washed with water and rinsed with given KMnO4 solution.
 Fill the burette with given KMnO4 solution up to the mark and fix it to the
stand.
 First given oxalic acid (C2H2O4) is standardized by using standard flask with
the help of water up to the mark.
 Pipette is taken and rinsed with the oxalic acid solution and pipette out
20ml of the solution in to the conical flask.
 Add 10 ml of dil.H2SO4 to the conical flask and heat the solution up to 600c.
 The flask is placed on the glazed tile under the burette and the initial
reading in burette is noted.
 The KMnO4 solution in the burette is released slowly and drop wise with
continuous shaking of conical flask until the end point is reached i.e. the
colorless solution turns into pale pink.
 At the end point colorless solution turns into pale pink.
 The final reading in the burette is noted.
 Wash the conical flask; Repeat the experiment till to get two concurrent
readings.
 The readings are tabulated in the following table.

Observations:-

S.No. Pipette volume Initial reading of Final reading of Volume of KMnO4

oxalic acid the burette (ml) the burette (ml) used. (ml)
(C2H2O4) (ml) (a) (b) (b-a)
1
2
3
4
KMnO4 solution:

Molarity of given KMnO4 = M1 = 0.1 M

Volume of KMnO4 consumed = V1 ml =

Soichiometric coefficient of KMnO4 in balanced equation = n1 = 2

C2H2O4 Solution:

Molarity of C2H2O4 taken = M2 =?

Volume of C2H2O4 taken (Pipette volume) = V2 ml =

Soichiometric coefficient of C2H2O4 in balanced equation = n2 = 5

Calculations:-

M1V1/n1 = M2V2/n2

M2 = [M1V1/n1] x [n2/ V2]

Molarity of C2H2O4 taken = M2 = -------- M (or) mol/liter

Strength of oxalic acid (C2H2O4) solution = M2 x GMW

Molar mass of C2H2O4 * 2 H2O = GMW = 126 g/mol

Strength of oxalic acid (C2H2O4) solution = -------- g/liter