II PU Chemistry Lab Manual (Part - A+B) Final - 10!09!22 (File)

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II PU CHEMISTRY LAB MANUAL
Experiment No. 1 Date:

(Note: To be written on ruled side)
Aim: Preparation of Lyophilic and Lyophobic sols
Principle: The lyophilic sols are directly formed by mixing and shaking the substance with a
suitable liquid. Lyophobic sols cannot be prepared by direct mixing and shaking. Special methods
are employed to prepare lyophobic sols.
Chemical required
1. Egg albumin
2. Sodium chloride solution (5g in 100 ml water)
3. Ferric chloride solution (2g in 100 ml water)
4. Aluminium chloride solution (2g in 100 ml water)
5. Starch/gum – 500 mg
6. Arsenious oxide (0.2g in 100 ml water)
Procedure
A. Preparation of Lyophilic Sol
I. Egg Albumin Sol
(i) Prepare 100 mL of 5% (w/v) solution of NaCl in water in a 250 mL beaker.
(ii) Break one egg in a porcelain dish and pipette out the albumin and pour it in sodium
chloride solution. Stir well to ensure that the sol is well prepared.
II. Starch/gum Sol
(i) Take 100 mL of distilled water in a 250 mL beaker and boil it.
(ii) Make a paste of 500 mg starch or gum in hot water and transfer this paste in 100 mL of
boiling water constant stirring. Keep water boiling and stirring for 10 minutes, cool, ensure
that the sol is well prepared.
B. Preparation of Lyophobic Sol
I. Ferric hydroxide/Aluminium hydroxide

Page 1
(i) Take 100 mL of distilled water in a 250 mL beaker and boil it.
ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

Add 2g of ferric chloride / aluminium chloride powder to boiling water and stir it well.
(ii) Take 100 mL of distilled water in another 250 mL beaker and boil it.
(iii) Pour 10 mL of ferric chloride/aluminium chloride solution prepared in step (ii) and transfer
it into the boiling water with constant stirring. Keep the water boiling till brown/white sol is
obtained.
II. Arsenious sulphide Sol
(i) Take 100 mL of distilled water in a 250 mL beaker.
(ii) Add 0.2 g of arsenious oxide to it and boil the contents of the beaker.
(iii) Cool and filter the solution.
(iv) Pass hydrogen sulphide ( H2S ) gas through the filtered solution till it attains the smell of
H 2 S . (Use Kipp’s apparatus to pass hydrogen sulphide gas).
(v) Expel H2S gas from the sol by slow heating and filter it.
(vi) Label the filtrate as arsenious sulphide sol.
(Note: Diagram to be drawn on un-ruled side)
Page 2

Aim: Purification of sol by dialysis
Chemical required
1. Colloidal dispersion of egg albumin
2. Parchment/cellophane paper
3. Uranyl zinc sulphate
4. Silver nitrate
Procedure: A square sheet of Parchment/cellophane paper is soaked in water and folded into a
conical shape. Colloidal solution is poured into cellophane paper and thread is tied tightly. It is
suspended in a trough containing distilled water. Distilled water in the trough is changed every half
an hour till it is free from impurities of Na+ and Cl − ions. Presence of Na+ ion is tested using uranyl
zinc sulphate (gives yellow ppt) and Cl − ion is tested using AgNO3 solution (gives white ppt).
Time required for the purification of colloidal dispersion is noted.
Page 3

Aim: To study the role of emulsifying agent in stabilizing the emulsions of different oils.
An emulsion contains liquid dispersed phase and liquid dispersion medium.
• Soap solution is prepared by dissolving 1g of soap powder in 10 mL water.
• 10 drops each of mustard oil, linseed oil, castor seed oil and machine oil are taken in four
separate test tubes labeled as A, B, C & D and 15 mL of distilled water is added into each
test tube.
• The solutions in the test tubes are shaken well and left for settling to get the emulsion. The
time taken for the formation of separate layers in each test tube is recorded using a stop
clock.
• Soap solution is added in drops into each test tube and shaken well for about 5 minutes. The
time taken for the formation of separate layer is recorded using a stop clock.
(Note: To be written on un-ruled side)
Tabulation
Test Tube Oil taken Time taken for the formation of separate layers
Without Soap solution With soap solution
A Mustard oil
B Linseed oil
C Castor seed oil
D Machine oil
Page 4

Effect of concentration on rate of reaction
Aim: To study the effect of concentration on the rate of reaction between sodium thiosulphate and
hydrochloric acid.
Principle: Sodium thiosulphate solution reacts with dilute hydrochloric acid and forms a sulphur
precipitate of sulphur. The time taken for a certain amount of sulphur to forms a sulphur precipitate
of sulphur. The time taken for a certain amount of sulphur to form can be used to indicate the rate
of reaction.
Apparatus and Chemicals required: 100 mL Conical flask, 50 mL measuring cylinder,

thermometer and a stopwatch. 0.1 M sodium thiosulphate solution, 1 M hydrochloric acid.
Procedure
1. Five 100 mL clean conical flasks are taken and labeled as 1, 2, 3, 4 and 5.
2. 10 ml of 0.05 M sodium thiosulphate solution is taken in the conical flask labeled 1.
3. 10 mL of dilute hydrochloric acid is added and immediately stop clock is started.
4. The flask is swirled to mix the solution and placed on paper marked with a cross.
5. Marked cross is observed from the top. When the cross is just invisible, time is noted.
6. Experiment is repeated by adding 10 ml of 1 M HCl to the conical flask 2, 3, 4, 5

containing 10 ml of different concentrations of sodium thiosulphate solution as tabulated
below.
(Different concentration of sodium thiosulphate solution are made by mixing different volumes
of the sodium thiosulphate solution with water as shown in the table)
Result: Rate of reaction between sodium thiosulphate and hydrochloric acid decreases with the
decrease in the concentration of sodium thiosulphate.
Equation
Na2S2O3 ( aq ) + 2HCl ( aq ) ⎯⎯
→S ( s )  +2NaCl ( aq ) + H2O (l ) + SO2 ( g )
Flask Volume of Volume of Total volume Conc. Of Time taken for

No. 0.1M distilled water of the Na2S2O3 the printing to
Na2S2O3 Soln (ml) solution (ml) become
Soln
Page 5
invisible (in sec)

(ml)

1 10.00 40.00 50 0.02 M
2 20.00 30.00 50 0.04 M
3 30.00 20.00 50 0.06 M
4 40.00 10.00 50 0.08 M
5 50.00 0.00 50 0.1 M
A graph is plotted between the concentration of sodium thiosulphate and the time taken for the
marked cross to become just invisible.
It is clear from the graph that rate of reaction between Na2 S2O3 and HCl decreases with the
decrease in concentration of sodium thiosulphate.
Page 6


Effect of temperature on rate of reaction
Aim: To study the effect of temperature on rate of reaction between sodium thiosulphate and
hydrochloric acid.
Principle: The rate of reaction depends upon the temperature of the reactants. Generally rate of
reaction increases with increase in temperature. Rate of reaction between sodium thiosulphate and
hydrochloric acid is studied by measuring the time taken for precipitation of sulphur.
Equation
Na2S2O3 ( aq ) + 2HCl ⎯⎯
→S ( s )  +2NaCl ( aq ) + H2O(l ) + SO2 ( g )
Apparatus and Chemicals required: 100 mL Conical flask, 25 mL and 10 mL measuring

cylinders, wire gauze, tripod stand, thermometer and a stopwatch. 0.1 M sodium thiosulphate
solution and 1 M hydrochloric acid.
Procedure
1. 50 ml of 0.1 M sodium thiosulphate solution is taken in a clean 100 ml conical flask and kept
in a thermostat of 30 C .
2. 10 ml of 1 M hydrochlorice acid is added and immediately stop clock is started.
3. The flask is swirled to mix the solution and placed on paper marked with a cross.
4. Marked cross is observed from the top. When the cross is just invisible, time is noted.
5. Again, 50 ml of 1M sodium thiosulphate solution is taken in another clean 100 ml conical

flask. The flask is kept in a thermostat at a temperature of 40 C . Temperature of the solution
is noted after placing it on a piece of printed paper. Immediately 10 ml of 1 M HCl is added
and a stop watch is started. The time taken for the precipitate of sulphur enough to make
printing on the paper just invisible is noted.
6. The same experiment is repeated at 50 C and 60 C and using fresh sodium thiosulphate
solution and HCl each time taken for paper mark to become just invisible is noted.
Page 7

Result: Rate of reaction between sodium thiosulphate and hydrochloric acid increases with the
increase in temperature.
Observation: Volume of 0.1 M sodium thiosulphate solution taken each time = 50 ml
Volume of 1 M HCl added each time = 10 ml
Sl. No. Temperature in  C Time taken for the printing to become invisible (in sec)
A graph between the time vs temperature is plotted and from shape of the curve.
Page 8


Air: To study the effect of concentration of iodide ions on the rate of reaction between
KI and H2O2 (Hydrogen peroxide)
Apparatus and Chemicals required:

2.5 M H2SO4, 0.1M KI, 0.04 M Na2S2O3 and 3% H2O2. five conical flasks (250 mL).
Hydrogen peroxide is an oxidizing agent which will oxidize KI into I 2 in acidic medium.
2KI + H2O2 + H2SO4 → K 2SO4 + 2H2O + I2
The reaction mixture is treated with sodium thiosulphate and starch solution. The I2 liberated in the
solution will oxidize sodium thiosulphate into sodium tetrathionate. When the oxidation is over then
the excess of I2 present in the solution combines with starch forming a deep blue coloured complex
compound. The time taken to combine with fixed amount of sodium thiosulphate will be known
from the time of appearance of blue colour.
I2 + 2Na2S2O3 → 2NaI + Na2S4O6
I2 + starch → Deep blue solution
Sodium thiosulphate Sodium tetrathionate
Procedure:
25 mL of H2O2 is mixed with 25 mL H2SO4 and 5 mL starch solution in ‘A’ labeled conical flask and
is kept in a water bath to attain constant room temperature.
A mixture of 10 mL Na2S2O3 + 10 mL KI + 80mL distilled water is taken in ‘B’ labeled conical

flask and is kept in a water bath to attain constant temperature.
A mixture of 10 mL Na2S2O3 + 20 mL KI + 70mL distilled water is taken in ‘C’ labeled conical

flask and is then kept in a water bath to attain constant temperature.
A mixture of 10 mL Na2S2O3 + 30 mL KI + 60mL distilled water is taken in ‘D’ labeled conical

flask and is kept in a water bath to attain constant temperature.
25 mL of ‘A’ flask solution is mixed with 25 mL of ‘B’ flask in a separate conical flask with constant
shaking. After adding half of the solution a stop clock is started and the time taken for the
appearance of blue colour is recorded.
The procedure is repeated for ‘C’ and ‘D’ flask solution and the time taken for the appearance of
blue colour to the solution is recorded. The whole experiment is repeated twice and the average
time of appearance of blue colour is found.
Page 9

Tabulation:
Time taken for the appearance

Sl. No. Composition of mixture of blue colour Average time
I II
1 25 mL ‘A’ + 25 mL ‘B’ flask solution
2 25 mL ‘A’ + 25 mL ‘C’ flask solution
3 25 mL ‘A’ + 25 mL ‘D’ flask solution
Result:
Rate of reaction increases as concentration of one of the reactant increases.
Page 10


Aim: To study the rate of reaction between potassium iodate (KIO3) and sodium
sulphite (Na2SO3)
Apparatus and Chemicals required:

2 M H2SO4, 5% starch solution, 6% KIO3 and 6% Na2SO3, five conical flasks (250 mL).
When potassium iodate and sodium sulphite solution are mixed the following reaction takes place.
Equation:
KIO3 + 3Na2SO3 → KI + 3Na2SO4
5KI + KIO3 + 3H2SO4 → 3K 2SO4 + 3H2O + 3I2
The iodine liberated produces blue colour with the starch solution.
Procedure:
25 mL of KIO3 is mixed with 25 mL of 2M H2SO4 and 50 mL distilled water in ‘a’ labeled conical
flask and is then kept in a water bath to attain constant temperature.
20 mL Na2SO3 + 5mL starch + 75 mL distilled water is taken in ‘B’ labeled conical flask and is then
kept in a water bath to attain constant temperature.
15 mL Na2SO + 5mL starch + 80 mL distilled water is taken in ‘C’ labeled conical flask and is then
kept in water bath to attain constant temperature.
10 mL Na2SO3 + 5mL starch + 90 mL distilled water is taken in ‘E’ labeled conical flask and is then
5 mL Na2SO3 + 5mL starch + 90 mL distilled water is taken in ‘E’ labeled conical flask and is then
25 mL of ‘A’ and 25 mL of ‘B’ conical flask solutions are mixed together in a separate conical flask.
A stop clock is started after adding half of ‘A’ flask solution. The time taken for the appearance of
blue colour is recorded. The above procedure is repeated for solutions of ‘C’, ‘D’ and ‘E’ flask and
the time for the appearance of blue colour to the solution is record.
The whole experiment is repeated twice and the average time for the appearance of blue colour is
found.
Page 11

Tabulation
Time taken for the appearance

Sl. No. Composition of mixture of blue colour Average time
I II
1 25 mL ‘A’ + 25 mL ‘B’
2 25 mL ‘A’ + 25 mL ‘C’
3 25 mL ‘A’ + 25 mL ‘D’
4 25 mL ‘A’ + 25 mL ‘E’
Conclusion: The rate of reaction decreases on decreasing the concentration of one of the
reactants.
Page 12

Determination of enthalpy of solution
Aim: To determine the enthalpy of solution of potassium nitrate crystals or copper sulphate.
Principle: A known amount of potassium nitrate is dissolved in water. The heat absorbed or
evolved is experimentally determined. Amount of heat absorbed or evolved when one mole of
potassium nitrate is dissolved in excess of the solvent at a given temperature is calculated. It gives
the enthalpy of solution.
Reaction
KNO3 ( s ) + aq ⎯⎯
→ KNO3 ( aq )
OR
CuSO4 ( s ) + aq ⎯⎯
→CuSO4 ( aq )
Apparatus and Chemicals required: Polythene bottle fitted with thermometer and stirrer.
Potassium nitrate or copper sulphate crystals.
Procedure: 100 cm3 of water is taken in a polythene bottle fitted with thermometer and stirrer.
About of 2 – 3 g of KNO3 or CuSO4 crystals are powered and weighed accurately. Initial
temperature of water is noted. Powered Potassium nitrate is quickly added to polythene bottle
containing water and the bottle is immediately stoppered and solution is stirred well. The minimum
temperature attained is noted. Enthalpy of solution is then calculated.
Result: Enthalpy of solution of potassium nitrate =  s H = ............kJ mol −1 .
Observation and calculation
Initial temperature = T1 K =
Final temperature = T2 K =
Page 13
Change in temperature = ( T1 − T2 ) K =
Mass of KNO3 taken = Wg
Molecular mass of KNO3 = 101.1 g mol −1
Volume of the solution = 100 cm3

Mass of the solution = 100 g = 0.1 kg
Specific heat of solution = 4200 J Kg K
Heat absorbed during the

process mass x sp. Heat x
change in temperature = 0.1 4200  ( T1 − T2 )

= 0.1  4200  _______
= ______ _______ J
Amount of heat absorbed

when one mole of potassium
______ _______ 101.1
nitrate is dissolved in water = =
w
= _______________ J
Page 14

Determination of enthalpy of neutralization
Aim: To determine the enthalpy of neutralization of strong acid ( HCl ) with a strong base
( NaOH ) .
Principle: A known amount of acid is neutralized by an equivalent amount of base. The heat
evolved is experimentally determined. Amount of heat liberated per gram equivalent of an acid
neutralized is calculated. It gives the enthalpy of neutralization.
Reaction:
HCl ( aq ) + NaOH ( aq ) ⎯⎯
→ NaCl ( aq ) + H2O
Apparatus and Chemicals required: Polythene bottle fitted with thermometer and stirrer. 1 N
HCl, 1 N NaOH.
Procedure: 100 cm3 of 1 N HCl is taken in a polythene bottle fitted with thermometer and
stirrer. 100 cm3 of 1N NaOH is taken in a 250 cm3 of beaker. Both the solution are kept in a water
bath for 15 minutes to attain the temperature of water bath. When both the solutions attain steady
temperature, initial temperature is noted. Let it be T1 K .
Sodium hydroxide solution is quickly added to polythene bottle containing HCl solution and the
bottle is shaken well. The maximum temperature attained is noted. Let it be T2 K .
Result: Enthalpy of neutralization of HCl with NaOH,  n H = __________ kJ equ −1 .

Observation and calculation
Initial temperature = T1 K =
Final temperature = T2 K =
( T2 − T1 ) K =
Page 15
Rise in temperature =

Total volume of the solution = 200 cm3

Mass of the solution = 200 g = 0.2 kg
Specific of heat of soluiton = 4200 J kg K
Heat liberated during the process = Q = mass x sp. Heat x change in temperature
(i.e. when 0.1 gram eq. wt of HCl is neutralized)
Q = 0.2  4200  ( T2 − T1 )
Q = 0.2  4200  _______
Q = _____________J
Amount of heat liberated when one gram

Q
Equivalent mass of HCl is neutralized =
0.1
= _____________ J
Page 16

Determination of enthalpy change on mixing chloroform and acetone
i. Transfer 8.14 ml of chloroform (0.1 mol) into the insulated boiling tube.
ii. Record the temperature of chloroform. Let it be t1 C .
iii. Transfer 7.34 ml of acetone ( 0.1 mol ) into a clean measuring cylinder.
iv. Record the temperature of acetone. Let it be t 2 C .
v. Pour acetone form the measuring cylinder into the chloroform contained in the insulated
boiling tube.
vi. Stir gently the mixture of chloroform and acetone with the help of a stirrer.
vii. Record the temperature of the mixture of chloroform and acetone. Let it be T2 C .
Report: Enthalpy of solution Acetone and chloroform is = − ve J.
Hence this binary solution shows negative deviation from Raoult’s law.
Calculation
1. Initial temperature of chloroform = t1  C
2. Initial temperature of acetone = t 2  C
t1 + t2
3. Average temperature = T1 = = 
C.
2
4. Temperature of mixture of chloroform and Acetone = T2 C
5. Rise in temperature t = ( T2 − T1 )
6. Water equivalent of calorimeter = w,
1.47 g cm3
Page 17
7. Density of chloroform =

8. Density of acetone = 0.787 g cm3
9. Specific heat of chloroform = s1 = 0.96 J g
10. Specific heat of Acetone = S2 = 2.18 J g
Enthalpy of solution = W  specific heat  t
=  ( 8.141.47  S1 ) + ( 7.34  0.79  S2 )   t
(Because W = Volume  Density)
Page 18


Aim: To study the variation is cell Zn / Zn2+ Cu2+ / Cu with change in concentration of
electrolytes (CuSO4/ ZnSO4) at room temperature.
Theory:
The Daniel Cell is symbolically represented as
Zn(s) / Zn2+(aq ) Cu2+(aq ) / Cu(s)
If the concentration of Zn2+ (aq ) and Cu2+(aq ) is 1 M each.
Then the E0cell = E0Cu − E0Zn = +0.34 − ( −0.76) = 1.1V

On changing the concentration of metal ions in solution, the ‘E’ cell values also changes. In this
experiment keeping the concentration of Zn2+ ion as constant, changing only the concentration of
Cu2+ ion, the emf of the cell is calculated using Nernst equation.
0 2.303RT Cu2+  0 0.059 Cu2+ 

Ecell = E cell + log or Ecell = E cell + log at 298 K
nF Zn2+  2 Zn2+ 
Materials required:
A strip of copper, a strip of zinc, a large beaker, porous pot, a plastic tube, cotton, 40 mL of 1M
CuSO4, 40 mL of 1 M ZnSO4, distilled water, a voltmeter with oscillator clips.
Procedure:
About 100 mL of 1 M CuSO4 solution is taken in a porous pot. Copper metal strip is dipped into it.
About 100 mL of 1 M ZnSO4 solution is taken in a large beaker. A zinc metal strip is dipped into it.
A sat bridge of KCl is used to connect the two solutions. Thus the Daniel Cell is formed.
The copper plate with +ve terminal and zinc plate with the –ve terminal are connected to the
voltameter as shown in the figure.
As soon as the circuit is completed, electric current will begin to flow and then the voltmeter reading
is noted which indicates the e.m.f. of the cell. This is reading Number (1).
The above procedure is repeated with 1 M ZnSO4 solution and 0.2M, 0.1M, 0.05M CuSO4 solution.
The corresponding readings are record as 2, 3 and 4.
Electrodes reactions are
At anode: Zn → Zn2+ + 2e− ( oxidation )
At cathode: Cu2+ + 2e− → Cu ( reduction)
In the cell: Zn + Cu2+ → Zn2+ + Cu ( overall reaction )
E.m.f of the cell can be calculated using Nernst equation
2.303  8.314  T
Ecell = 1.1 + log Cu2+(aq ) 
2  96500  
Page 19
The graph is obtained by plotting cell potential on y-axis and log Cu2+ (aq )  on x-axis


LHS and Calculation: Study of variation of emf with respect of concentration
Reading Concentration of CuSO4 Observed EMF of the cell Calculated EMF of the cell
No. Solution (volt) from Nernst equation (volt)
1
Conclusion: Increase in Cu2+  increases the emf of the cell.
Increase in Zn2+  decreases the emf of the cell.
Voltmeter
V
Cl– K+
Zinc anode Salt bridge Copper cathode
So2– 4
Cu2+
2+
Zn So42–
Page 20


Aim: To separate the pigments present in leaves and flowers by ascending paper
chromatography and determination of Rf value (Retardation factor)
Principle:
The components of the pigment are separated by paper chromatography. The R f value of each
component is calculated.
Distance travelled by the substance from the reference line in cm
Rf =
Distance travelled by the solvent front from the reference line in cm
Procedure:
Preparation of green pigment from leaves and colour pigments from flowers.
1. Grind the flowers and the leaves separately in a mortar and transfer the paste into separate test
tubes.
2. Small amount of methanol or acetone is added to the paste and shaken well. The mixture is
filtered and the filtrate is collected with a test tube and corked.
A special adsorbent paper like whatman filter paper No.1 of size 4 cm x 17 cm is taken. A line at
about 3 cm from one end of the filter paper with a pencil is marked. Using a capillary tube drops of
the prepared pigments are kept on the points a and b marked on the line of filter paper (as shown in
front cover page) and allowed to dry. This is repeated till the spots a and b are rich with the
pigments. The dry filter paper is hanged in a closed jar so that the bottom end of the filter paper just
dips into a solution containing 19 ml of ether and 1 ml of acetone or chloroform (eluent)
The solvent slowly moves upwards to reach the top due to capillary action. The pigment spots also
move to different distances along with the mobile phases when the solvent raises to about 15 cm on
the filter paper, it is removed from the jar. The distance travelled by the solvent is marked with a
pencil. This is called solvent front. Similarly the distances travelled by the pigment from the
reference points a and b are also measured. The Rf values for the components of the pigment can
Page 21
be calculated from using the formula.

Distance travelled by the green pigment

Rf value of the green pigment =
Distance travelled by the solvent front
Distance travelled by the coloured pigment

Rf value of the colour pigment =
Distance travelled by the solvent front
Page 22


Aim: To separate the constituents of a mixture of compounds containing Pb2+ and Cd2+
ions using ascending paper chromatography and to calculate the Rf (retardation factor)
values.
Principle:
The cations Pb2+ and Cd2+ are separated by chromatography and they are coloured using the
developer ammonium sulphide. By measuring distances moved by these ions on the filter paper
their Rf values are calculated.
Procedure:
The experiment is repeated as in experiment 5.1 using the solvent mixture ethanol, conc. HNO 3 and
distilled water in the ratio 8 : 1 : 1 (eluent) when the solvent front moves on the filter paper carries
the ions also to the different heights. When the solvent front moves about 15 cm on the filter paper
it is removed dried and the spots of the ions are coloured by spraying ammonium sulphide
(Aq. NH3 + H2S). PbS gives black spot whereas CdS gives yellow spot. The distances of these spots
moved from the reference line are measured. The distance travelled by the solvent front is also
measured. There by Rf values of both Pb2+ and Cd2+ ions can be calculated.
Distance travelled by Pb2+ ions in cm

Rf value of Pb 2+
ion =
Distance travelled by the solvent front in cm
Distance travelled by Cd 2+ ions in cm

Rf value of Cd2+ ion =
Distance travelled by the solvent front in cm
Page 23

To determine the concentration / molarity of KMnO4 solution by titrating it against

0.1 M standard solution of ferrous ammonium sulphate
Principle:
A known volume of standard ferrous ammonium sulphate solution (Mohr’s salt solution) is titrated
against potassium permanganate solution in acid medium.
In the reaction, ferrous sulphate gets oxidized to ferric sulphate and KMnO4 gets reduced to
colourless manganous sulphate.
2 KMnO4 + 8 H2SO4 + 10 FeSO4 → K2SO4 + 2 MnSO4 + 8 H2O + 5Fe2 ( SO4 )3
(a1 ) (a2 )
By knowing the volume of KMnO4 solution required to oxidize ferrous sulphate from the titration,
the molarity of KMnO4 solution, is calculated.
Procedure:
A 10 cm3 pipette is washed with water, and then rinsed with the given FAS solution. A burette is
washed with water, and then rinsed with KMnO4 solution. It is filled with KMnO4 solution and
fixed to a stand. Initial burette reading is noted to the upper meniscus (coloured solution).
10 cm3 of FAS solution is pipette out into a clean conical flask. One test tube full of dilute sulphuric
acid is added. The solution is titrated against the KMnO4 solution till the solution taken in the
burette turns permanent pale pink colour. Final burette reading is noted. Titrations are repeated for
concordant values. In this titration KMnO4 acts as self indicator.
Report:
Molarity of KMnO4 = .................... M

Page 24

Observations and calculations:

Burette KMnO4 solution
Conical flask 10 cm3 of FAS solution + 1 test tube full of dil  H 2SO4
Indicator KMnO4 itself (self indicator)
End point Colourless to permanent pale pink
Tabular column:
Trial numbers I II III
Final burette reading
Initial burette reading
Volume of KMnO4 solution added in cm3
VKMnO4 = ............cm3
Calculations
 M 1V 1  M V 
  =  2 2
 a1 KMnO4  a 2 FAS
Where a1 and a 2 are the stoichiometric co-efficient of KMnO4 and FeSO4 in the balanced
chemical equations. (a1 = 2 and a2 = 10)

aKMnO4  M FAS  VFAS
 M KMnO4 =
aFAS  VKMnO4
2  0.1  10
= = ...........M
10  ............
Page 25


To determine the concentration / molarity of potassium permanganate solution by
titrating it against 0.1 M standard solution of oxalic acid.
Principle:
A known volume of standard oxalic acid solution is titrated against potassium permanganate
solution in acid medium and in hot condition.
In the reaction, oxalic acid gets oxidized to CO2 and H2O  KMnO4 gets reduced to colourless
manganous sulphate.
2 KMnO4 + 3H2SO4 + 5H2 C2O4 → K2SO4 + 2 MnSO4 + 8H2O + 10CO2 
(a1 ) (a2 )
By knowing the volume of KMnO4 solution, the molarity of KMnO4 solution can be calculated.
Procedure:
A 10 cm3 pipette is washed with water and then rinsed with the given oxalic acid solution.
A burette is washed with water, and then rinsed with KMnO4 solution. It is filled with KMnO4
solution and fixed to a stand.
10 cm3 of oxalic acid solution is pipetted out into a clean conical flask. One test tube full of dilute
sulphuric acid is added. The solution is heated nearly to boiling. The hot solution is titrated against
the potassium permanganate solution taken in a burette till the solution turns permanent pale pink
colour. Final burette reading is noted. Titrations are repeated for concordant values.
Result:
Molarity of KMnO4 solution = ................M

Observations and calculations:
Page 26

Burette KMnO4 solution

Conical flask 10 cm3 of oxalic acid + one test tube full of dilute H2SO4
Indicator KMnO4 itself (self indicator)
End point Colourless to pale pink
Tabular column:
Trial numbers I II III
Final burette reading
Initial burette reading
Volume of KMnO4 solution added in cm3
Volume of KMnO4 = ............cm

3
Calculations
 M 1V 1  M V 
  = 2 2
 a1 KMnO4  a 2 H 2C 2O4
Where a1 and a 2 are the stoichiometric co-efficient of KMnO4 and oxalic acid in the balanced
chemical equations. (a1 = 2 and a2 = 5)

aKMnO4  MOxacid  VOxacid
M KMnO4 =
aOxacid  VKMnO4
2  0.1  10
= = ...........M
5  ............
Page 27


(Note: To be written on both sides of record)
Tests for functional groups in organic compounds
1. Functional group tests for alcohols
(i) Ceric ammonium nitrate test: It is used to detect alcohols
Experiment Observation Inference
Organic compound + few drops of Pink or red colour appears Indicates the presence of
ceric ammonium nitrate solution. alcoholic − OH group.
Shake well
(ii) Lucas reagent test:

Lucas reagent is mixture of anhydrous zinc chloride and concentrated hydrochloric acid.
Lucas reagent test is used to distinguish between primary, secondary and tertiary alcohols.
Organic compound + Lucas reagent a) White turbidity Indicates the presence of

ZnCl2 appears immediately tertiary alcohol
(Anhyd. + Conc. HCl )
b) White turbidity Indicates the presence of
appears after 5 – 10 secondary alcohol
minutes
c) No turbidity at room Indicates the presence of
temperature or white primary alcohol
turbidity appears
only on heating.
2. Functional group tests for phenols

(i) Neutral Ferric chloride test: It is used to detect phenolic −OH group.
Organic compound + few drops of Voilet colour is obtained Indicates the presence of
neutral FeCl3 solution. phenolic −OH group.
(ii) Phthalein fusion test: It is used to detect phenol.

Organic compound + Phthaleic Pink colour is obtained Indicates the presence of

anhydride + few drops of phenol
concentrated H 2 SO4 , Heat, pour
into NaOH solution.
3. Functional group tests for aldehydes and ketones
(i) 2, 4-DNP test: It is a general test for aldehydes and ketones.
Organic compound + 2, 4-DNP Orange crystalline Confirms the presence

solution (2,4-dinitrophenyl precipitate is obtained carbonyl group (aldehyde
Page 28
hydrazine) or ketone)

(ii) Tollen’s reagent test or silver mirror test: It is used to detect aldehydic group.
Organic compound + Tollen’s Silver mirror is obtained Aldehyde group is

reagent, Heat on water bath, for or Black ppt of silver is present.
about 5 min. obtained.
4. Functional group tests for carboxylic acids

(i) Litmus paper test: It is used to detect −COOH group.
Organic compound + blue litmus Blue litmus paper turns Indicates the presence of
paper. red. carboxylic acid group
( −COOH ) .
(ii) Sodium bicarbonate test: It is used to detect −COOH group.

Organic compound + NaHCO3 Brisk effervescence Indicates the presence of

takes place carboxylic acid group
( − COOH ) .
(iii) Esterification test: It is a confirmatory test for carboxylic acids.
Organic compound + few drops of A fruity smell is The carboxylic acid group
ethyl alchol + 2-3 drops of conc. obtained. is confirmed.
H2SO4 , heat and pour into
Na2CO3 solution.
5. Functional group tests for primary amines

(i) Carbylamine test: It is used to detect primary amines.
Foul smell or unpleasant Primary amine is

Organic compound + CHCl3 + alc.
smell is obtained confirmed
KOH, Heat (aliphatic/aromatic)
(ii) Azo dye test or Diazotisation test: It is used to detect −COOH group.
Organic compound + sodium nitrite Orange red dye is Primary aromatic amine is
+ dil HCl , cool, add  − naphthol obtained confirmed.
in NaOH solution.
Page 29

Preparation of Ferrous ammonium sulphate crystals (Mohr’s salt)

Aim: To prepare crystals of ferrous ammonium sulphate or Mohr’s salt.
Theory: Mohr’s salt i.e., ferrous ammonium sulphate ( FeSO  ( NH )

4 4 2 )
SO4  6H2O is a double
salt. It can be prepared by mixing equal volume of equimolar solutions of FeSO4  7 H 2O and
( NH4 )2 SO4 . On concentration and cooling crystals of Mohr’s salt are formed.
Reactions: FeSO4  7H2O + ( NH4 )2 SO4 ⎯⎯→ FeSO4  ( NH4 )2 SO4  6H2O + H2O
Apparatus and Chemicals required: Two 25 ml beakers, a glass rod, china dish, funnel stand
wire gauze, tripod stand and filter paper. Ferrous sulphate, ammonium sulphate, dilute sulphuric
acid and ethanol.
Procedure:
1. 14 g of ferrous sulphate and 6.5 g of ammonium sulphate are taken in a clean beaker.
2. About 50 ml of distilled water is boiled in another beaker for about 5 minutes to expel
dissolved air.
3. About 2 ml of dilute sulphuric acid is added to the above water and it is poured into the first
beaker containing FeSO4 and ( NH4 )2 SO4 . The mixture is stirred with a glass rod to
dissolve the salts.
4. The solution is filtered to remove any suspended impurities.
5. The filtrate is collected in a clean china dish and concentrated on a low flame until the
crystallization point is reached.
6. The china dish is covered with a watch glass and kept in an undisturbed place for cooling.
Well defined crystals will be obtained after some time.
7. The mother liquor is removed and the crystals in the china dish are washed with a small
quantity of ethanol.
8. The crystals are dried by pressing between the folds of rough filter paper and weighed. The
colour and shapes of crystals are observed.
Result: Colour of the crystals = Light green
Shape of the crystals = Monoclinic
Yield (mass of the crystals obtained) = ………. g

Page 30

Preparation of potash alum
Aim: To prepare crystals of Potash alum.
Theory: Potash alum, a double salt, commonly known as fitkari has the formula
K2SO4  Al2 ( SO4 )3  24H2O . It can be prepared by the crystallization of a mixture of equal volume
of equimolar solutions of Al2 ( SO4 )3  18H2O and K2SO4
Reactions: K2SO4 + Al2 ( SO4 )3  18H2O + 6H2O ⎯⎯→ K2SO4 Al2 ( SO4 )3 24H2O
Apparatus and Chemicals required: Two 25 ml beakers, a glass rod, china dish, funnel stand,
wire gauze, tripod stand and filter paper. Potassium sulphate, aluminium sulphate and conc.
Sulphuric acid.
Procedure:
1. 7 g of potassium sulphate is taken in a clean beaker. It is dissolved in a minimum amount of

distilled water with gentle heating.
2. 26.5 g of aluminium sulphate is taken in another beaker. About 3 – 4 drops of concentrated
sulphuric acid are added. About 30 ml of distilled water is added to the beaker and heated
on a wire gauze with occasional stirring. The solution is thus filtered to remove the turbidity.
3. The two clear solutions are mixed in a china dish. The dish heated gently on a wire gauze
and the solution is concentrated to the crystallization point.
4. The crystals formed are separated by decanting the another liquor. Crystals are washed with
very small quality of ice cold water.
5. The crystals are then dried between the folds of filter paper and weighed. The colours and
shapes of the crystals are observed and noted.
Result: Colour of the crystals = colourless
Shape of the crystals = Octahedral
Yield (weight of the crystals obtained) = ………. g

Page 31


Aim: Preparation of potassium trioxalato ferrate (III)
Chemicals required: 3g of oxalic acid, 3.8 g of KOH, 2.5g of FeCl3
Procedure:
1. 3g oxalic acid is dissolved in 15 mL of hot distilled water and 3.8g KOH are dissolved in a
beaker with constant stirring.
2. 2.5 g FeCl3 are added into the above solution with constant stirring. The solution is then boiled
and cooled to get white crystals of potassium trioxalatoferrate (III). The crystals are separated
by filtration and dried between the folds of filter paper.
Reaction: FeC 3
heat
+ 6KOH + 3H2C2O4 ⎯⎯⎯ → K4 Fe (C2O4 )6  + 3KC + 6H2O
Result:
Yield of potassium trioxalatoferrate (III) = …………..g.
Page 32


Aim: To prepare acetanilide from aniline.
Apparatus and Chemicals Required: Aniline (5 mL), Acetic anhydride (5 mL), Glacial acetic
acid (5 m), Ethanol, funnel, RB flask (100 mL), beaker (250 mL).
It can be prepared by heating aniline with acetic anhydride.
Procedure:
1. 5 mL of aniline is dissolved in 5 mL acetic anhydride and 5 mL glacial acetic acid and with
constant shaking in a round bottomed flask.
2. The mixture is reflexed on a sand bath for about 15 minutes. Aniline reacts with acetic
anhydride giving acetanilide.
3. The reaction mixture is poured into a beaker containing 100 mL of ice water. Acetanilide
precipitates from the solution as white solid. It is separated by filtration and purified by
recrystallization from hot water containing little alcohol.
NH2 NH CO CH3
Glacial acetic acid
+ (CH3CO)2O + CH3COOH
Aniline Acetanilide Acetic acid
Page 33

Preparation of dibenzal acetone
Aim: To prepare a pure sample of dibenzal acetone.
Apparatus and chemicals required: 250 ml conical flask with cork, measuring cylinder, funnel,
filter paper. Benzaldehyde, acetone, sodium hydroxide, ice and rectified spirit.
Procedure:
1. 25 ml of rectified spirit is taken in a clean conical flask.

2. 5.0 ml of benzaldehyde and 2.0 ml of pure acetone are added it.
3. 2.5 ml of 4% aqueous NaOH solution is added to the above mixture.
4. The conical flask is fitted with a cork and is shaken vigorously for 10 mins, releasing the pressure by
removing the cork from time to time.
5. The contents are allowed to stand for about 30 mins and cooled in an ice cold water.
6. Pale yellow crystals of dibenzal acetone precipitates. It is filtered, dried and crystalised using rectified
spirit.

Chemical reaction
CHO CH = CH - CO - CH = CH
dil. NaOH
2 + CH3COCH3 + 2H2O
Dibenzal acetone
Benzaldehyde Acetone
Page 34

Preparation of p–nitroacetanilide from acetanilide
Aim: To prepare a pure sample of p − nitroacetanilide from acetanilide.
Apparatus and Chemicals required: 25 ml round bottomed flask, ice bath, beaker, measuring
cylinder, funnel and filter paper. Acetanilide, conc. Nitric acid, conc. Sulphuric acid, glacial acetic
acid and rectified spirit.
Procedure:
1. 10 g of powdered acetanilide is placed in a 250 ml of round bottomed flask and 10 ml of

glacial acetic acid is added.
2. The mixture is stirred well and 20 ml of conc. Sulphuric acid is added to it.
3. The flask is placed an ice bath and cooled.
4. 4 ml of cold conc. Nitric acid is added drop by drop with constant stirring.
5. The flask is removed from the ice bath and allowed to stand for about 45 mins at room
temperature.
6. The reaction mixture is poured on a crushed ice contained in a beaker and allowed to stand
for 15 mins.
7. The precipitates of p − nitro acetanilide is separated by filtration, washed with cold water
and with ethyl alcohol.
Chemical reaction:
Page 35

Preparation of phenyl-azo-  -naphthol (an azo dye)
Aim: To prepare phenyl-azo-  − napthol.
Apparatus and Chemicals required: Conical flask, beaker, funnel, measuring cylinder, ice bath.
Aniline,  − naphthol, sodium nitrite, conc. HCl , sodium hydroxide, glacial acetic acid and spirit.
Procedure:
1. 2.5 ml of pure aniline, 8 ml of conc. HCl and 8 ml of water are mixed in a beaker.
2. The solution is cooled to 0 − 5 C in an ice bath.
3. To the cold solution, a solution of sodium nitrite is slowly added. Benzene diazonium
chloride solution is formed.
4. 22.5 ml of 10% NaOH solution is taken in a beaker and 4.0 g of pure  naphthol is added.
5. The cold benzene diazonium chloride solution is added with constant stirring to the  −
naphthol −NaOH mixture.

6. The mixture is allowed to stand for 10 mins and an orange – red dye is filtered.
7. The product is recrystalised using glacial acetic acid.
Chemical reaction
Page 36

(Note: To be written on both sides of record)

Tests for Carbohydrates, Fats and Proteins
A. Tests for Carbohydrates.
1) Molisch test (carbohydrates general test)
Aqueous solution of the A deep violet ring is formed at Carbohydrate is present

compound + alcoholic solution the junction of two layers
of α – naphthol + Conc  H2SO4
is added carefully along the sides
of the test tube.
General test for reducing sugars:
2) Benedict’s reagent test: A red precipitate Carbohydrate is reducing
Solution of the compound + sugar
Benedict’s reagent. The test
tube is heated on a water
bath.
3) Fehling’s solution test: A red precipitate Carbohydrate is reducing

Solution of the compound + sugar
Fehling’s solution. The test
tube is heated on a water
bath.
4) Tollen’s reagent test: A black precipitate of silver or a Carbohydrate is reducing

Solution of the compound + shining silver mirror is observed sugar
Tollen’s reagent. The test tube
is heated on a water bath.
Test to distinguish monosaccharide from disaccharide

5) Barfoed’s test: Solution of Orange red precipitate. Carbohydrate is a
the compound + Barfoed’s monosaccharide.
reagent. The test tube heated No orange red precipitate Carbohydrate is a
on a water bath. disaccharide
Test to distinguish Ketose from aldose
6) Seliwanoff’s test: Solution Red colour or precipitate Carbohydrate is ketohexoses
Page 37
of the compound +
Blue green colour Carbohydrate is ketopentose
Seliwanoff’s reagent. The test

tube is heated on water bath. No colour or precipitate Carbohydrate is aldose
Test to polysaccharides (Starch)

7) Iodine test: Solution of the A blue colour Starch is confirmed
compound (starch) + few
drops of iodine solution
B. Test for oils and fats

8) Acrolein test: 3 drops of A pungent smell due to the Oil or fat is present
the oil or melted fat + few
formation of acrolein
crystals of potassium hydrogen
sulphate. The mixture is
heated gently
C. Tests for Proteins

9) Biuret test (For peptide A violet colour is observed Protein is present
bonds) Protein solution (egg
albumin or casein) + 2 mL of
10% NaOH + few drops of
CuSO4 solution, warm the
mixture
10) Ninhydrin test: Protein A blue colour is observed Protein is present

solution + Ninhydrin solution
heated & cooled.
11) Xanthoproteic test: Protein Yellow colour observed which Protein is present
solution + few drops
turns to orange red on adding (Test for proteins containing
conc  HNO3 warmed the
NaOH solution benzene ring)
mixture.
Page 38

II PU Chemistry Lab Manual (Part - A+B) Final - 10!09!22 (File)

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CONTENTS

Sl. Expt. Pg.

Experiment No. 1 Date:

Aim: Preparation of Lyophilic and Lyophobic sols

2. Sodium chloride solution (5g in 100 ml water)

3. Ferric chloride solution (2g in 100 ml water)

4. Aluminium chloride solution (2g in 100 ml water)

6. Arsenious oxide (0.2g in 100 ml water)

A. Preparation of Lyophilic Sol

I. Egg Albumin Sol

(i) Prepare 100 mL of 5% (w/v) solution of NaCl in water in a 250 mL beaker.

II. Starch/gum Sol

B. Preparation of Lyophobic Sol

I. Ferric hydroxide/Aluminium hydroxide

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

II. Arsenious sulphide Sol

(i) Take 100 mL of distilled water in a 250 mL beaker.

(iii) Cool and filter the solution.

(vi) Label the filtrate as arsenious sulphide sol.

(Note: Diagram to be drawn on un-ruled side)

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

Experiment No. 2 Date:

(Note: To be written on ruled side)

Aim: Purification of sol by dialysis

1. Colloidal dispersion of egg albumin

3. Uranyl zinc sulphate

Time required for the purification of colloidal dispersion is noted.

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

Experiment No. 3 Date:

(Note: To be written on ruled side)

An emulsion contains liquid dispersed phase and liquid dispersion medium.

• Soap solution is prepared by dissolving 1g of soap powder in 10 mL water.

(Note: To be written on un-ruled side)

Without Soap solution With soap solution

C Castor seed oil

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

Experiment No. 4 Date:

Effect of concentration on rate of reaction

(Note: To be written on ruled side)

Apparatus and Chemicals required: 100 mL Conical flask, 50 mL measuring cylinder,

6. Experiment is repeated by adding 10 ml of 1 M HCl to the conical flask 2, 3, 4, 5

(Note: To be written on un-ruled side)

Flask Volume of Volume of Total volume Conc. Of Time taken for

invisible (in sec)

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

1 10.00 40.00 50 0.02 M

2 20.00 30.00 50 0.04 M

3 30.00 20.00 50 0.06 M

4 40.00 10.00 50 0.08 M

5 50.00 0.00 50 0.1 M

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

Experiment No. 5 Date:

(Note: To be written on ruled side)

Apparatus and Chemicals required: 100 mL Conical flask, 25 mL and 10 mL measuring

2. 10 ml of 1 M hydrochlorice acid is added and immediately stop clock is started.

5. Again, 50 ml of 1M sodium thiosulphate solution is taken in another clean 100 ml conical

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

(Note: To be written on un-ruled side)

Observation: Volume of 0.1 M sodium thiosulphate solution taken each time = 50 ml

Volume of 1 M HCl added each time = 10 ml

ASC INDEPENDENT PU COLLEGE, RAJAJINAGAR, BANGALORE – 10

Experiment No. 6 Date: