XII-

Chemistry

Practical

Procedure
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 2022-2023
Surface Chemistry
EX.NO:1
PREPARATION OF COLLOIDAL SOLUTION OF STARCH
(Lyophilic Sol)
Aim:
To prepare a colloidal solution of starch.
Materials required:
Apparatus:
Beakers, Glass Rod, Pestle and Mortar, Tripod Stand, Wire Gauze, Filter
paper and Burner.
Chemicals:
Soluble Starch and Distilled Water.
Theory:
Starch forms a lyophilic sol when water is used as dispersion medium.
The formation of sol is accelerated by heating. The starch sol can be
prepared by heating starch and water at about 100 0C.It is quite stable
and is not affected by the presence of any electrolytic impurity.
Procedure:
1) Take 500 mg of starch in a mortar and add few ml of distilled water.
2) Grind the starch to make a thin paste and transfer this paste to a 50
ml beaker.
3) Take about 100 ml of distilled water in a 250 ml beaker and heat the
beaker so that water starts boiling.
4) Pour the paste slowly with stirring into boiling water in the beaker.
5) Continue boiling for about 10 minutes and then allow the beaker to
cool.
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 6) Filter the contents of the beaker through a filter paper, fixed in a
funnel. The filtrate is called as ‘Starch Sol’.
Result:
A colloidal solution of Starch was prepared.
Precaution:
1) The apparatus used for preparing sol should be properly cleaned.
2) Distilled water should be used for preparing sols in water.
3) Constant stirring of contents is necessary during the preparation of
sol.

EX.NO:2
PREPARATION OF FERRIC HYDROXIDE SOL
(Lyophobic Sol)
Aim:
To prepare a colloidal sol of Ferric hydroxide.
Materials required:
Apparatus:
Water, Beakers, Glass Rod, Test tube, Tripod Stand, Wire Gauge,
Burner.
Chemicals:
FeCl3 and Distilled Water.
Theory:
Ferric Hydroxide is a lyophobic sol. It can be prepared by the hydrolysis
of Ferric Chloride with boiling water as per the reaction.
FeCl3(aq) + 3 H2O(l) → Fe(OH)3(s) + 3 HCl(aq)
The hydrolysis reaction produces insoluble ferric hydroxide particles
which undergoes ‘agglomerisation’ i.e., cluster formation to yield bigger
particles of colloidal size. These particles adsorb Fe 3+ ions preferentially
from the solution to result in positively charged sol. The stability of the
sol is due to the adsorption of this positive charge on the sol particles.
HCl which is produced during the preparation process tries to
destabilize the sol and so must be removed by dialysis process, otherwise
sol will not be stable. The sol is represented as Fe(OH) 3.
Procedure:
1) Prepare 2% solution Ferric chloride by dissolving 2g of pure FeCl 3 in
100ml distilled water.
2) Take 100ml of distilled water in a 250ml beaker and keep it for
boiling.
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 3) To the boiling water add the 2% solution of Ferric chloride drop wise
using a dropper.
4) Continue heating till deep red brown solution of Fe(OH) 3 is obtained.
Replace the water lost by evaporation during boiling at regular
intervals.
5) Keep the contents of the beaker undisturbed for some time, Ferric
hydroxide sol is obtained.
Result:
A colloidal sol of Ferric hydroxide was prepared.
Precaution:
1) Ferric hydroxide sol is affected by impurities, hence the apparatus
should be thoroughly cleaned.
2) Ferric chloride solution should be added drop wise.
3) Heating is to be continued till the sol is obtained.
4) HCl formed as a result of hydrolysis of Ferric chloride is to be
removed by dialysis otherwise it would destabilize the sol.

EX.NO:3
PURIFICATION OF COLLOIDAL SOLUTION OF STARCH
(Dialysis of Lyophilic Sol)
Aim:
To purify colloidal solution of Starch containing sodium chloride as
impurity.
Materials required:
Apparatus:
Cellophane or Parchment paper, Beaker, Clamp stand, Rubber Band,
Test tube and Dropper.
Chemicals:
Distilled Water, Starch sol having Sodium chloride as impurity, Silver
nitrate Solution and Iodine Solution.
Theory:
Dialysis: The separation of the particles of an electrolyte from the
colloidal sol by diffusion through semipermeable membrane is called
dialysis.
Cellophane or Parchment paper allows only the passage of sodium
chloride through it and not starch. These papers thus can be used to
purify starch or other sol.
Procedure:
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 1.Take a long stem funnel. Attach with a parchment or cellophane
paper with the help of rubber band.
2.Pour Starch solution that contains NaCl into the funnel until the
parchment bag is three-fourth full.
3.Immerse the bag in distilled water and keep immersed for about half
an hour.
4.Withdraw 1ml of water from the beaker in a test tube and add to it
iodine solution. If no blue colour is produced, starch not diffused out
through parchment paper.
5.Add Silver nitrate to a little water taken from the beaker in a
separate test tube. If white precipitate of AgCl is formed, it indicated
the presence of chloride ions.
6.Repeat the above step unit the water in beaker stops showing
precipitate with Silver nitrate.
7.On complete removal of chloride ions, remove the bag out of
beaker.
Precautions to be taken during the experiment:
 The apparatus used for this experiment should be washed with
distilled water and dried.
 Change the water continuously from the beaker.
 Use distilled water for dialysis.

EX.NO:4
STUDY OF THE ROLE OF EMULSIFYING AGENTS IN STABILIZING
THE EMULSION OF DIFFERENT OILS
Aim:
To study the role of emulsifying agents to stabilize the emulsions of
different oils.
Materials required:
Apparatus:
Test tube, Glass rod, Stopwatch, Droppers.
Chemicals:
Soap or detergent, Mustard oil, Coconut oil, Castor oil and Olive oil.
Theory:
An emulsion is a colloid where both the dispersion medium and the
dispersed phase are in liquid form. Here it has been differentiated based on
their relative proportions. The dispersed phase is in a smaller quantity and
the dispersion medium is present in a larger proportion.

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 If you mix oil and water, after shaking the mixture you will notice a
slightly milky solution that is soluble, is unstable and is known as an
emulsion of oil in water. It will form two layers, separating water and oil.
If you want to increase the stability of the emulsion of oil and water soap
solution can be added. Since it acts as an emulsifying agent. The interfacial
surface tension between the two layers is decreased by the carboxyl polar
group.
Soap concentration is the optimum concentration required to complete
the emulsification process. To get an effective stabilization the amount
should not be more or less than optimum concentration.
Procedure:
1.Take 4 test tubes and label them as A, B, C and D. Add 5ml distilled
water in each test tube. Put 10 drops of Mustard oil in the test tube A, 10
drops of Coconut oil in B, 10 drops of Castor oil in C, and 10 drops of
Olive oil in test tube D.
2.Take the test tube A in your hand and shake it vigorously for 5 minutes
and keep it aside in a test tube Stand. Start your stopwatch to record the
time required to separate the two layers.
3.Follow the same process with other test tubes B, C and D.
4.Take a test tube. Put 10ml of distilled water and dissolve 1g of
detergent in it. Vigorously shake the test tube and label the test tube as
“E”.
5.Add two drops of soap solution or detergent which were prepared in the
test tube E into each test tube. Shake each test tube for 5 minutes. And
record the time taken to separate two layers.
Observations:
Specification Name of the Time taken for the
of test tube Oil used for separation of layers
emulsion (in
Sec)
With Without
soap or soap or
detergen detergen
t t
A Mustard oil
B Coconut oil
C Castor oil
D Olive oil
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 Result:
It is clear from the above observations that,
1. -------------- oil takes longest time to get separated from its emulsion
and is rated as 1.
2. ---------------oil takes the minimum time and is rated as 4.
3. The decreasing order of effectiveness is----------------.
Precautions to Be Taken During the Experiment:
 First thing is to add to all the test tubes an equal amount of soap or
detergent solution.
 To minimize the error in recording the time, shake all the test tubes for
an identical time span.
 Start your stopwatch as soon as you stop shaking the test tubes and
stop it immediately when you notice the layers are separated.

CHEMICAL KINETICS
EX.NO:5
EFFECT OF CONCENTRATION ON THE RATE OF REACTION BETWEEN
SODIUM THIOSULPHATE AND HYDROCHLORIC ACID
Aim:
To study the effect of concentration on the rate of reaction between
sodium thiosulphate and hydrochloric acid
Theory:
According to the law of mass action, rate of a chemical reaction is directly
proportional to the product of molar concentrations of the reactants, in other
words, the rate of reaction increases with the increases in concentration of
the reactants. The effect of concentration of reactants on rate of a reaction
can be studied easily by the reaction sodium thiosulphate and hydrochloric
acid.
Na2S2O3(aq) + 2HCl → S(s) + 2NaCl(aq) + SO2(g) + H2O(l)
The insoluble sulphur, formed during the reaction, gives a milky
appearance and makes the solution opaque. Therefore, rate of reaction can
be studied by measuring the time taken to produce enough sulphur to make
some mark invisible on a paper kept under the conical flask in which the
reaction is carried out.
Materials required:

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 Apparatus:
Conical flasks, Beakers, Measuring cylinder and Stop watch.
Chemicals:
0.1M Na2S2O3 solution and 1M HCl solution.
Procedure:
1) Wash the conical flasks with water and label them as 1,2,3,4, and 5
respectively.
2) Using a measuring cylinder, add 10, 20, 30, 40 and 50 ml of 0.1M
Na2S2O3 solution to the flasks 1,2,3,4 and 5 respectively.
3) Now add 40, 30, 20 and 10ml of distilled water to the flask 1, 2, 3 and 4
respectively so that volume of solution in each flask is 50ml.
4) Take 10ml of 1M HCl solution in a test tube using a measuring cylinder.
5) Add 10ml of 1 M HCl taken in a test tube to the conical flask No.1
containing 10ml of 0.1M Na2S2O3 solution and 40 ml of distilled water and
start the stop watch. When half of the HCl solution has been added. Shake
the contents of the conical flask and place it on the tile (or paper) with a
cross-mark.
6) Go on observing from top to downwards in the flask and stop the stop-
watch when the cross mark just becomes invisible. Note down the time.
7) Repeat the experiment by adding 10ml of 1M HCl to flask 2,3,4 and 5
and record the time taken in each case for the cross mark to become just
invisible.
8) Plot a graph between 1/t (in s) and concentration of 0.1M Na 2S2O3
solution.

Observations:

Flask Volume Volum Total Volume Time

Concentration

No. of e of volume of Na2S2O3 of 1M taken for

Na2S2O3 water of solution HCl cross to
solutio become
solutio
n just
n
invisible t
(ml (ml) (s) (s-1)
(ml (ml) (M)
)
)
1. 10 40 50 0.02 10

2. 20 30 50 0.04 10

3. 30 20 50 0.06 10

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4. 40 10 50 0.08 10

5. 50 0 50 0.10 10

Result:
From the graph,
It is clear that 1/t is directly proportional to the concentration
ofNa2S2O3 solution. But 1/t is a direct measure of the reaction, therefore
rate of the reaction between Na 2S2O3 and HCl is directly proportional to
the concentration of Na2S2O3 solution taken. Hence, rate of this reaction
is directly proportional to the concentration of Na 2S2O3, which is one of
the reactants.
Precautions:
The apparatus must be thoroughly clean. If the same conical flask is to
be used again and again, it should be thoroughly washed with conc. HNO 3
and then with water.
Measure the volumes of Sodium thiosulphate solution, hydrochloric acid
and distilled water very accurately.
Use the same tile (or paper) with the same cross-mark for all
observation.
Complete the experiment at one time only so that there is not much
temperature variation.
Start the stop-watch immediately when half of the hydrochloric acid
solution has been added to Sodium thiosulphate solution.
View the cross-mark through the reaction mixture from top to bottom
from same height for all observations.

EX.NO:6
EFFECT OF CHANGE IN TEMPERATURE ON THE RATE OF REACTION
BETWEEN SODIUM THIOSULPHATE AND HYDROCHLORIC ACID
Aim:
To study the effect of change in temperature on the rate of reaction
between sodium thiosulphate and hydrochloric acid.
Materials required:
Apparatus:
Conical flasks, Beakers, Measuring cylinder (50ml and 5ml), Stop watch,
Thermometer, Tripod stand, Wire gauge and Burner.
Chemicals:
0.1M Na2S2O3 solution, 1M HCl solution, Distilled water and Conc. HNO 3.
Procedure:
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 1) Take 50ml of 0.1M Na2S2O3 solution in a 100ml conical flask and note
its temperature with the help of a thermometer.
2) Add 10ml of 1M HCl to it and start the stop watch immediately when
half of the hydrochloric acid solution has been added.
3) Shake the contents of the flask gently and place it on the tile with a
cross-mark.
4) Observe the cross-mark from the top and note the time taken for the
mark to become just invisible.
5) Empty the flask and clean it thoroughly with Conc. HNO 3 and then with
water.
6) Take again 50ml of 0.1M Na2S2O3 solution in a 100ml conical flask and
ₒ
heat it so that the temperature of the solution becomes (T+10) C.
7) Remove the flask from tripod stand and add 10ml of HCl to it and start
the stop-watch.
8) Shake the contents gently and place it on the tile having cross-mark.
9) Note the time taken for the mark to become just invisible.
ₒ ₒ ₒ
10) Repeat the experiment at (T+20) C,(T+30) C and (T+40) C
temperatures and record the observations.
11) Plot a graph by taking 1/t along the ordinate (vertical axis) and
temperature along the abscissa (horizontal axis).
Observations:
Volume of 0.1M Na2S2O3 solution taken each time = 50ml
Volume of 1MHCl added each time = 10ml
S Te Ti
. m m (s-1)
N pe e
O ra ta
. tu k
re e
n
(in fo
ₒ
C) r
th
e
cr
os
s
m
ar
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success
 k
to
b
ec
o
m
e
ju
st
in
vi
si
bl
e(
t)
(i
n
s)
1
.
2
.
3
.
4
.
5
.

Result:
Rate of reaction between Sodium thiosulphate and hydrochloric acid
increases with the increase in temperature.
Precautions:
The apparatus must be thoroughly clean. If the same conical flask is to
be used again and again, it should be thoroughly washed with conc. HNO 3
and then with water.
Measure the volumes of Sodium thiosulphate solution, hydrochloric acid
and distilled water very accurately.

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success
 Use the same tile (or paper) with the same cross-mark for all
observation.
Complete the experiment at one time only so that there is not much
temperature variation.
Start the stop-watch immediately when half of the hydrochloric acid
solution has been added to sodium thiosulphate solution.
View the cross-mark through the reaction mixture from top to bottom
from same height for all observations.

EX.NO:7
STUDY OF REACTION RATES OF REACTION OF IODIDE ION WITH
HYDROGEN PEROXIDE AT ROOM TEMPERATURE USING DIFFERENT
CONCENTRATIONS OF IODIDE IONS
Aim:
To study the effect of variation in concentration of iodide ions in the
reaction rate between iodide ions and hydrogen peroxide at room
temperature.
Theory:
The reaction of iodide ions and hydrogen peroxide takes place in an
acidic medium. It is represented as follows:
H2O2 + 2I- +2H+ → 2H2O + I2
In the above reaction, iodide ions are oxidised to molecular iodine by
hydrogen peroxide. When Sodium thiosulphate is added in the presence of
starch solution to the above reaction mixture, the iodine liberated, reacts
with thiosulphate ions immediately after it is formed and is reduced back to
iodide ions as long as all the thiosulphate ions oxidise to tetrathionate ions.
Fast
I2(g) + 2S2O32–(aq) → S4O62–(aq) + 2I–(aq)
I2 + Starch → Starch-I2 complex
(Colourless) (Blue Colour)

Once all the thiosulphate ions are consumed, the concentration of

liberated iodine increases swiftly to a point where an intense blue complex
is formed. The time for the colour to appear is recorded, therefore, the
reaction is sometimes known as a clock reaction.
Materials required:
Apparatus:

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success
 Four conical flask of volume 250 ml, Burette, Pipette, Stop-watch and
Measuring cylinder.
Chemicals:
Starch solution, 0.1 M Potassium Iodide solution, 2.5 M Sulphuric acid
solution, 0.05M Sodium thiosulphate solution and 3% Hydrogen peroxide
solution.
Procedure:
1.Take four conical flask of volume 250 ml and label them as A, B, C and
D.
2.Add 10 ml, 20 ml, 40 ml and 60 ml of 0.1 M KI solution to the flask A, B,
C and D respectively.
3.Add 10 ml of 2.5 M H2SO4 solution to each flask.
4.Add water to make the volume of solution to 100 ml in each flask.
5.Add 5 ml of starch solution to each flask.
6.Add 10 ml of 0.05M Sodium thiosulphate solution to each flask with the
help of burette.
7.Add 5 ml of 3% Hydrogen peroxide solution to flask A with the help of
pipette and start the stop watch immediately. Stir the mixture and watch
for the blue colour to appear. Note the time when the blue colour just
appears.
8.Repeat the above step with the solutions in flask B, C and D.
9.Record the observations in tabular form.

Observations:

Flas 0.1 M KI 2.5 M Water Starch 0.05 M 3%

k solution H2SO4 (ml solution(m Sodium Hydroge
(ml (ml) ) l) thiosulphat n
) e solution peroxide
(ml) solution
(ml)
A 10 10 80 5 10 5
B 20 10 70 5 10 5
C 40 10 50 5 10 5
D 60 10 30 5 10 5

Time required for the blue colour to first appear in:

Flask A - ----------s
Flask B - ----------s

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success
 Flask C - ----------s
Flask D - ----------s

Result:
The rate of reaction increases with increase in concentration of iodide
ions.
Precautions:
Keep the concentration of Na2S2O3 solution less than that of KI solution.
Use starch solution which is freshly prepared.
Use Na2S2O3 solution which is freshly prepared.
Use fresh samples of KI (potassium iodide) and hydrogen peroxide
(H2O2).
Do not suck hydrogen peroxide solution with mouth but use a pipette.
Record the time immediately once the blue colour appears.

Thermochemistry
EX.NO:8
Enthalpy of neutralization of strong acid (hydrochloric acid) and
strong base (sodium hydroxide)
Aim:
To determine the enthalpy of neutralization of strong acid (hydrochloric
acid) and strong base (sodium hydroxide).

Theory:
Heat is evolved during neutralization of an acid with alkali.
The neutralization reaction of a strong acid with a strong base is essentially
the combination of one equivalent of hydrogen ions with one equivalent of
hydroxyl ions. Known volumes of standard solutions of an acid and alkali
are mixed and the change in temperature is observed and from this,
enthalpy of neutralisation is calculated.
Enthalpy of neutralization is the heat evolved when one gram equivalent
of the acid is completely neutralized by a base in dilute solution.
The chemical reaction is given below.
HCl(aq) + NaOH(aq) → NaCl (aq) +H2O(l) ∆H=-57.3KJ

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 H+(aq) + Cl–(aq) + Na+(aq) + OH–(aq) → Na+(aq) + Cl–(aq) + H2O
Materials Required:
Apparatus:
A wide-mouthed polythene bottle, Rubber cork, Thermometer, Stirrer
fitted with a cork and Measuring cylinder.
Chemicals:
1 M Hydrochloric acid and 1 M Sodium hydroxide solution.
Procedure:
1. Calculate the water equivalent of the calorimeter.
2. Place 100 ml of 1 M Hydrochloric acid solution in clean and dry
polythene bottle.
3. Now record the temperature of the acid solution.
4. Take another separate vessel and place 100 ml of 1 M Sodium
hydroxide solution in it.
5. Note down the initial temperature of sodium hydroxide taken.
6. Wait till both the solution attains the same temperature.
7. Now transfer 100 ml of Sodium hydroxide solution into the
Hydrochloric acid quickly.
8. Fit the cork immediately which has a thermometer and a stirrer in the
mouth.
9. Stir well the solution and note down the temperature after small
intervals of time.
10. Keep noting down the temperature till the temperature becomes
constant.
11. Record the highest temperature reached.

Observation:
Initial temperature of the acid and base (t1) =------- oC
Final temperature after neutralization (t 2) =------- oC
Change in temperature (Δt= t1- t2) =------- oC
Mass of the mixture solution after neutralization= 200 g
Water equivalent of calorimeter (W) = -------g
Calculations:
1.Enthalpy change during neutralization of 100 ml of 1 M HCl
= (200+W) x Δt x 4.184 = ------------J
2.Therefore, the enthalpy change during neutralization of 1000 ml of 1M
HCl = (200+W) x Δt x 4.184 x =
-------------J
3.Enthalpy of neutralization
= =---------kJ
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 Results:
The enthalpy of neutralization of HCl with NaOH =--------- kJ.
Precautions:
1.Due to radiation, some heat is lost to the environment.
2.The solution density is supposed to be 1g / ml.
3. Hydrochloric acid and sodium hydroxide ionization is assumed to be 100 %.
4.The solution’s specific heat is taken as 4.184J/g
5.The mixture of HCl and NaOH should be stirred well.
6.Water equivalent calorimeter or beaker should be calculated
accurately.

EX.NO:9
Variation of cell potential in Zn/Zn2+|| Cu2+/Cu with change in
concentration of electrolytes (CuSO4 or ZnSO4) at room
temperature.
Aim:
To study the variation of cell potential in Zn/Zn 2+ || Cu2+/Cu with change
in concentration of electrolytes (CuSO 4 or ZnSO4) at room temperature.
Theory:
Electrochemistry deals with the interconversion of other forms of energy
into electrical energy or vice versa. Potential difference is called cell
potential or emf of the cell between the two electrodes. It is always
measured in volts.
The reaction between copper sulphate solution and zinc metal forms the
basis of Daniel cell. When this reaction is carried out in a test tube then no
electricity is produced. If the same reaction is carried out in Daniel cell
electricity is produced.
In Daniel cell, Under Standard condition, it generates an emf of 1.1V.
The reaction taking place in Daniel cell are
Zinc electrode : Zn(s) → Zn2+(aq) + 2e–
Copper electrode: Cu2+(aq) + 2e– → Cu(s)
———————————————————————————————
Net reaction : Zn(s) + Cu2+(aq) → Zn2+(aq) + Cu(s)
———————————————————————————————
The emf of Daniel Cell is given by the following Nernst Equation:
E=E0 - log

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success
 Materials Required:
Apparatus:
Beaker, Voltmeter, A porous pot, Connecting wires, Zinc strip and Copper
strip.
Chemicals:
1M zinc sulphate solution and Copper sulphate solution.
Apparatus Setup:

Procedure:
1.Take Copper sulphate solution in a clean beaker.
2.Take Copper strip and dip it into Copper sulphate solution.
3.Take Zinc sulphate into porous pot.
4.Take Zinc strip and dip it into Zinc sulphate solution.
5.Keep the porous pot in the beaker.
6.Connect the Copper strip with positive terminal and Zinc strip with
negative terminal of a Voltmeter.
7.Note down the reading of voltmeter in observation table.
8.Repeat the experiment by taking different concentrations of Zinc
sulphate and Copper sulphate solutions.

Observations:

S.N Conc. Of ZnSO4 Conc. Of CuSO4 EMF of the

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 O solution (M) solution (M) cell
(V)

1. 1 1

2. 1 0.5

3. 1 0.025

4. 1 0.0125

5. 0.5 1
Results:
The EMF of the cell increases with decrease in concentration of
electrolyte around anode and increase in concentration of the electrolyte
around cathode.
Precautions:
1.The porous pot should not be completely dipped into Copper sulphate
solution.
2.Very carefully dilute the solution to another concentration.
3.Always clean strips of copper with positive terminal of Voltmeter and
zinc with negative terminal of Voltmeter.
4.Note the reading only when the pointer becomes stable.
EX.NO:10
Separation of pigments from extracts of leaves and flowers by
paper chromatography and determination of Rf values.
Aim:
To separate the pigments present in leaves and flowers by paper
chromatography and determine their Rf values.
Theory:
Paper chromatography is essentially a partition chromatography. In paper
chromatography the stationary phase is paper. Paper contains 22% of
water molecules absorbed on about 78% of cellulose.
The separation of the components of the mixture takes place by
partitioning of the components between the stationary phase and mobile
phase. The mobile phase travels through the paper by capillary action.
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 Based upon the ways the solvent travels on the paper there are three types
of chromatography.
1. Ascending Paper Chromatography
2. Descending Paper Chromatography
3. Circular Paper Chromatography
The distribution occurs in a definite ratio which represents the
characteristic distribution coefficient of the solution.
The Rf coefficient ratio is given by
Rf =
Different substances possess different Rf values. Rf depends upon a
number of factors.
They are
 Nature of the substance
 Nature of the solvent
 Temperature
 Presence of impurities
 Quality of the filter paper
If the compound is coloured, it can be easily located on the
chromatographic paper. If the substance is colourless, however, a reagent
may be used to treat it, which gives it a characteristic colour. The
name developer is given to this reagent. Iodine is the most frequently used
paper chromatography developer.
Materials Required:
Apparatus:
Whatman filter paper, Extract of leaves and extract of flowers, Rubber
cork fixed with hook in the centre, Glass jar, Rubber cork fixed with hook in
the centre, Test tubes and Distilled water.
Chemicals:
Acetone, Dil.HCl and Distilled water.

Apparatus Setup:

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 Procedure:
1.Measure the height of the glass jar with an ordinary scale. Cut the
strips of Whatman filter paper NO.1 equivalent to the height of glass jar
and around 5 cm wide.
2.Take the Whatman filter paper and draw a line with the help of a pencil
above 3 cm from one end.
3.Grind the leaves and flowers in a motor and transfer the paste into a
test tube.
4.This crushed material add acetone, shake well and filter the mixture.
5.The filtrate is collected in a test tube for performing experiments.
6.Using a capillary put one drop of the filtrate on the filter paper on the
line marked with a pencil and allow it to dry.
7.Pour the mobile phase(a mixture of 5 ml acetone + 1 ml dil.HCl + 5 ml
water) into the jar upto a height of 2 cm and suspend the paper strip with
the help of hook such that the paper touch the side of the jar and stands
vertical.
8.Keep this jar till the mobile phase rises up to 2/3th of the length of the
paper.
9.Remove the filter paper from the jar mark the position of solvent.
10. Outline the spots with the help of pencil and make the filter paper to
dry.
11. Measure the distance between the position of solvent and the centre
of different spots in relation to the reference line as indicated.
12. Determine the number of pigments in the leaves and flowers
extract.
13. Using the expression, calculate the R f value of different spots.

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 Observations:
S.N Name Colour Distance Distance Rf Value
O of the of the travelled travelled s
extrac spot by the by the
t spot solvent
from the from the
original original
line line
(cm) (cm)
1.
2.
3.
4.

Results:
1. The Rf value of the components of leaves are ________.
2. The Rf value of the components of flowers are ________.
Precautions:
1. Always make use of a fine capillary tube.
2. Do not allow spots to spread while spotting the test solution on the
paper.
3. Use the capillary finely drawn to place the spot on the paper.
4. Do not disturb the jar once the experiment is set as long as the
chromatogram is developed.
5. Before developing the spots, make the paper strip perfectly dry.
6. Carefully handle organic solvents.

EX.NO:11
SEPARATION OF CONSTITUENTS PRESENT IN AN INORGANIC
MIXTURE CONTAINING TWO CATIONS ONLY
Aim:
To separate the constituents present in an inorganic mixture containing
two cations (Pb2+ and Cd2+) only and the constituents should have large
difference in Rf values.
Theory:

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 Chromatography is a modern and sensitive technique used to analyse
and separate components from a mixture and purify compounds quickly
and efficiently.
The characteristic rate of movement of each substance on the
chromatography paper can be determined at a given temperature and for a
given solvent as the moving phase moves. This is represented by
the Rf value of the relative front or retardation factor.
Although the mobile phase (solvent) is the same, the R f values of
different compounds are different. In addition, a compound’s R f value may
differ in different solvents. Using the following expression, R f values can be
calculated.
Rf =
In this experiment the two cations to be separated in this case are
colourless. A developer is therefore needed. In this case, ammonium
sulphide (NH4)2S may be used to locate these ions in chromatographic
paper or plate position.
Materials Required:
Apparatus:
Whatman filter paper, Glass jar, Rubber cork fixed with hook in the
centre, Test tube and Capillary tubes.
Chemicals:
1-2% of Lead nitrate solution, 1-2% of Cadmium nitrate solution,
Ammonium sulphide, Ethanol, 3 M Nitric acid, Petroleum ether and Distilled
water.
Apparatus Setup:

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 Procedure:
1.Mark a line at a distance of 3 cm from one end of Whatman filter paper
with the help of a pencil.
2.Use a fine capillary to place a spot of the mixture on the marked line.
3.In a jar containing a mixture of Ethanol, 3 M HNO 3 and distilled water,
hang the filter paper in the ratio 4:0.5:0.5.
4.Keep the jar as such until the paper length rises to two-thirds of the
mobile phase (solvent).
5.Now remove the filter paper and mark the position of solvent.
6.Spray ammonium sulphide solution to obtain yellow and black spots on
the chromatography paper.
7.Mark with a pencil the position of the spots and let the paper dry.
8.Measure the distance to the reference line moved by the position of
solvent and the cations.
9.The distance between the reference line and the centre of different
spots is the shortest distance.
10. Record in tabular form the observations and calculate the R f value for
each cation.

Observations:

S.NO Colour of Distance Distance Rf value

the spot travelled by travelled
different by the
components solvents
from from
reference reference
line (cm) line (cm)
1.
2.
3.
Results:
1.The Rf values of Cd2+ ions is _________.
2.The Rf values of Pb2+ ions is _________.
Precautions:
1.Always make use of a fine capillary tube.
2.Use the capillary finely drawn to place the spot on the paper.
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 3.Do not allow spots to spread while spotting the test solution on the
paper.
4.Do not disturb the jar once the experiment is set as long as the
chromatogram is developed.
5.Carefully handle organic solvents.
6.Before developing the spots, make the paper strip perfectly dry.
EX.NO:12
PREPARATION OF FERROUS AMMONIUM SULPHATE
(INORGANIC COMPOUND)
Aim:
To prepare a pure sample of Ferrous ammonium sulphate (Mohr’s salt)
[FeSO4.(NH4)2SO4.6H2O]
Theory:
Mohr’s salt is prepared by dissolving an equimolar mixture of hydrated
Ferrous sulphate and Ammonium sulphate in water containing a little of
sulphuric acid, and then subjecting the resulting solution to crystallization
when light green crystals of Ferrous ammonium sulphate separates out.

FeSO4.7H2O + (NH4)2SO4 → FeSO4.(NH4)2SO4.6H2O + H2O

(Ferrous sulphate) (Ammonium sulphate) (Ferrous ammonium sulphate)
Materials Required:
Apparatus:
Two beakers (250ml), china dish, funnel, funnel-stand, glass-rod, wash-
bottle, tripod stand and wire-gauze.
Chemicals:
Ferrous sulphate crystals, Ammonium sulphate crystals, dilute sulphuric
acid and ethyl alcohol.
Procedure:
1) Take a 250ml beaker and wash it with water. Transfer 3.0g Ferrous
sulphate and 1.5g of Ammonium sulphate crystals to it. Add about 2-3ml
of dilute sulphuric acid to prevent the hydrolysis of Ferrous sulphate.
2) In another beaker boil about 20 ml water for about 5 minutes to expel
dissolved air.
3) Add the boiling water to the contents in the first beaker in small
installments at a time. Stir with a glass rod until the salts have
completely dissolved.
4) Filter the solution to remove undissolved impurities and transfer the
filtrate to a china-dish.
5) Heat the solution in the china-dish for some time to concentrate it to
the crystallization point.
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 6) Place the china-dish containing saturated solution over a beaker full of
cold-water. On cooling crystals of Mohr’s salt separate out.
7) Decant off the mother liquor quickly. Wash the crystals in the china-
dish with a small quantity of alcohol to remove any sulphuric acid sticking
to the crystals.
8) Dry the crystals by placing them between filter paper pads.

Observations:
1.Colour of the crystals - Light Green
2.Shape of the crystals - Monoclinic
3.Solubility in water - Soluble
Precautions:
1) Cool the solution slowly to get good crystals.
2) Do not disturb the solution while it is being cooled.
3) Do not heat the solution for a long time as it may oxidize Ferrous ions
to Ferric ions.

Result:
Weight of the crystals obtained = ------g.

EX.NO:13
PREPARATION OF POTASSIUM FERRIC OXALATE
(INORGANIC COMPOUND)
Aim:
To prepare the pure Potassium Ferric Oxalate from three chemicals such
as Potassium monohydrate, oxalic acid, and Ferric chloride dihydrate.
Theory:
When a freshly prepared ferric hydroxide is treated with an oxalic acid
solution, Ferrous oxalate in the form of a yellow precipitate will be formed.
When dissolved further with Potassium oxalate monohydrate, Potassium
Ferric Oxalate is formed in the form of a green precipitate. Potassium ferric
oxalate is considered a complex compound with the chemical formula of
K3 Fe(C₂O₄)3Fe(C₂O₄)3.3H₂O.
The chemical reactions,
FeCl₃ + 3KOH → Fe(OH)₃ + 3KCl
2Fe(OH)₃ + 3(COOH)2.2H₂O → Fe2(C₂O₄)3 + 12H₂O
Fe₂(C₂O₄)3 + 3(COOK)2.H₂O → 2K₃[Fe(C₂O₄)₃].3H₂O
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 (Potassium Ferric Oxalate)
Ferric hydroxide gets dissolved and the soluble complex is formed when
the oxalic acid is added excessively. To precipitate the complex iron salt
alcohol is added to the solution, as it is less soluble in alcohol than water.

Materials Required:
Apparatus:
Beakers, Conical flask, Tripod stand, Glass rod, Wire gauze, Filter paper,
China dish and Funnel.
Chemicals:
Oxalic acid hydrate, Ferric chloride, Potassium oxalate and Potassium
hydroxide.
Procedure:
1.Dissolve 3.5g of freshly prepared Ferric chloride in 50 ml of water in a
beaker.
2.Dissolve 4g of Potassium hydroxide in another beaker with 50ml of
water.
3.With constant stirring, slowly add the Potassium hydroxide solution to
the Ferric chloride solution to form a brown colour Ferric hydroxide
precipitate.
4.Through the funnel, filter the Ferric hydroxide precipitate and wash it
with hot water.
5.Take 4g of hydrated Oxalic acid and 5.5g of hydrated Potassium
oxalate in another beaker. Add 100ml of water and stir it well to get a
clear Potassium oxalate solution.
6.To potassium oxalate solution, gradually add the freshly prepared
ferric hydroxide precipitate by stirring it constantly so that precipitate
dissolves completely and the green colour solution is formed.
7.Remove the insoluble impurities by filtering the solution.
8.Take a china dish and transfer the green-coloured solution into it and
concentrate the solution till the crystallization point is reached.
9.In cold water, place the china dish and let it cool for an hour.
10. Green crystals of potassium ferric oxalate are formed. From the
mother, liquor removes all the crystals.
11. With ethyl alcohol, wash the crystals and dry them between the
folds of filter paper.
12. To know the yield, weigh the crystals.

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 Observations:
1. Colour of the crystals - Green colour
2. Shape of the crystals - Octahedral
Results:
Weight of the crystal formed=------g.
Precautions:
1.Do not concentrate too much on the solution.
2.To get big crystals during crystallization, do not disturb the solution.
3.To dissolve unwanted salt, wash the crystals with hot water.

EX.NO:14
Preparation of Acetanilide
(ORGANIC COMPOUND)
Aim:
To prepare the organic compound acetanilide from aniline, glacial acetic
acid/acetic anhydride and zinc dust.
Theory:
Acetanilide is prepared from aniline when it reacts with acetic
anhydride/glacial acetic acid in the presence of zinc dust. A mixture of
aniline, glacial acetic acid, acetic anhydride and zinc dust is refluxed under
anhydrous condition and then poured the mixture into ice cold water to get
acetic anhydride precipitate. The crude precipitate of acetic anhydride is
recrystallized to get pure crystals of acetanilide.
The chemical reaction is given below.

Zinc is used to prevent the oxidation of aniline during the chemical

reaction. Acetanilide is medicinally important and it is used as febrifuge.
Acetanilide can also be prepared by acetylating aniline with acetic
anhydride in the presence of concentrated hydrochloric acid. Dissolve
aniline in hydrochloric acid and add acetic anhydride stir well. Pour the

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 mixture to sodium acetate in water. Acetanilide is formed which can be
separated and recrystallized by ethyl alcohol.
Materials Required:
Apparatus:
Round bottom flask, Beaker, Pipette, Reflux condenser, Funnel, Stirrer,
Bunsen burner, Filter paper and Electronic balance.
Chemicals:
Aniline, Glacial acetic acid, Acetic anhydride, Zinc dust and Distilled
water.
Apparatus Setup:

Procedure:
1.Wash all the apparatus with distilled water before starting the
experiment.
2.Take a round bottom flask in that add 10ml of aniline and 20ml of
acetic anhydride and glacial acetic acid mixture and add zinc dust.
3.Fix the reflux condenser with the round bottom flask.
4.Heat the mixture gently for about 15-20 minutes on sand bath.
5.Pour the hot mixture in a beaker containing ice-cold water with
constant stirring.
6.Stir the mixture vigorously to hydrolyse excess of acetic anhydride.
7.Once all the acetanilide is precipitated collect and filter in Buchner
funnel.
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 8.The precipitate obtained is a crude sample of acetanilide.
9.Transfer the crude sample into a beaker containing 20ml water and
heat gently. If the solution is coloured then add a small amount
of activated carbon. Filter the hot solution with a funnel. Cool the mixture
for 30 minutes so that white shiny crystals of acetanilide separates out.
Filter off the crystals, wash them with water and dry the precipitates with
the help of filter paper.
10. Note the weight of product and determine melting point of the
compound.
Observations:
1.Colour of the crystals – White flaky crystals.
2.Shape of the crystals – Plate shaped
Results:
1.Melting point of acetanilide = -------0C
2.The yield of Acetanilide = --------g.
Precautions:
1.Do not inhale the fumes of acetic anhydride.
2.Always carry out experiments in fuming chamber or near the window.
3.Use the water condenser for refluxing the reaction mixture.
4.Dry the crystals of acetanilide before finding the weight and its melting
point.

EX.NO:15
TEST FOR THE FUNCTIONAL GROUPS PRESENT IN ORGANIC COMPOUNDS
SAMPLE A- TEST FOR UNSATURATION
S.N EXPERIMENT OBSERVATION INFERENCE
O
1 KMnO4 Test:
Take small amount of the organic Pink colour Presence of
compound in a test tube Add 2 ml of is unsaturation
distilled water to dissolve it. To this decolourised
solution add few drops of very dilute
alkaline KMnO4 solution and shake it well.
2. Bromine Test.
Dissolve a little of the given organic Disappear Compound
compound in about 2 ml of distilled water ance of is
in a test tube and add few drops of orange- Unsaturated.
bromine water to it and shake well. red colour
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 of
bromine.
SAMPLE B- TEST FOR ALCOHOL
S.N EXPERIMENT OBSERVATIO INFERENCE
O N
1. CERRIC AMMONIUM NITRATE TEST:
Place about 1ml of the given compound in a Appearance Presence of
dry clean test-tube, add few drops of Cerric of red alcohol
ammonium nitrate reagent and shake well. colour
2. ESTER TEST:
Take 1ml of the given liquid in a clean dry Fruity smell Presence of
test-tube, add 1ml of Acetic acid and 2to 3 alcohol
drops of Conc. Sulphuric acid. Warm the
mixture on a water bath for about
10minutes. Pour it into about 20ml of cold
water taken in a beaker and smell.

RESULT:
1. Sample A is Unsaturated
2. Sample B is Alcohol.

EX.NO:16
TESTS FOR THE FUNCTIONAL GROUPS PRESENT IN ORGANIC
COMPOUNDS
SAMPLE A -TEST FOR PHENOL
S.NO EXPERIMENT OBSERVATION INFERENCE
1 NEUTRAL FERRIC CHLORIDE TEST:
. Take 1ml of neutral Ferric chloride solution Violet colour Presence
in a clean test-tube and 2-3 drops of the of Phenol
liquid compound (or 1 crystal if solid).
2 PHTHALEIN DYE TEST:
. Take pinch of organic compound and pinch Pink colour Presence
of Phthalic anhydride in a clean dry test tube of Phenol
and add 1-2 drops of Conc. H2SO4. Heat the
test tube for about 1 minute in an oil bath.
Cool and pour the reaction mixture carefully
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 into a beaker containing 15 ml of dilute
sodium hydroxide solution.
SAMPLE B-TEST FOR ALDEHYDE
S.NO EXPERIMENT OBSERVATION INFERENCE
1. FEHLING’S TEST:
Take 1ml each of Fehling’s A and B in a test tube. Add Appearance of Presence of
4-5 drops (or pinch) of the given compound and warm red precipitate aldehyde
the test tube in hot water bath for 4-5 minutes.
2. TOLLEN’S REAGENT TEST:
Take 1ml of silver nitrate solution in a clean test tube A shining mirror Presence of
and add 2-3 ml of dilute NaOH solution. A brown appears aldehyde
precipitate forms. Now add dilute ammonia solution
drop wise until the brown precipitate of silver oxide just
dissolves. To this add 3-4 drops of the given liquid (or
pinch of solid) and warm the test tube on a water bath
for about 5minutes.
RESULT:
1. Sample A is Phenol
2. Sample B is Aldehyde.

EX.NO:17
TESTS FOR THE FUNCTIONAL GROUPS PRESENT IN ORGANIC COMPOUNDS
SAMPLE A-TEST FOR KETONES
S.N EXPERIMENT OBSERVATION INFERENCE
O
1. SODIUM NITROPRUSSIDE TEST:
Dissolve a crystal of Sodium nitroprusside in about Red colouration Presence of
1ml of distilled water in a clean test tube and then add ketone
0.5ml (or pinch) of the given compound. Shake and
add Sodium hydroxide solution dropwise.
2. SODIUM BISULPHITE TEST:
Take 2ml of a saturated solution of Sodium Crystalline Presence of
bisulphite in a clean test-tube, and add 1ml or 1g of white precipitate ketone
the given compound. Cork the test tube, shake and is formed
leave it for 15-20 minutes.
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 SAMPLE B- TEST FOR AMINES
1. ODOUR:
The odour of the compound is noted. Fishy smell May be
amine
2. DYE TEST:
Take A small amount of an organic substance in a Scarlet red dye Presence of
clean test tube, add 2 ml of Conc. HCl to dissolve it. is an aromatic
Add few crystals of NaNO2 , and cool the mixture in obtained primary
ice bath . Then add 2 ml of ice cold solution of β- amine
naphtholin NaOH.
SAMPLE C-TEST FOR CARBOXYLIC ACID
EXPERIMENT OBSERVATION INFERENCE
1. SODIUM BICARBONATE TEST:
To 1ml of the organic liquid in a test tube, add a Brisk Presence of
pinch of sodium bicarbonate. effervescence carboxylic
acid
2. ESTER TEST:
Take 1ml of the given liquid in a clean dry test- A fruity smell Presence of
tube, add 1ml of Ethyl alcohol and 2 to 3 drops of carboxylic acid
Conc. Sulphuric acid. Warm the mixture on a
water bath for about 10minutes. Pour it into about
20ml of cold water taken in a beaker and smell.

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 Result:
1.Sample A is Ketone
2.Sample B is amine
3.Sample C is Carboxylic acid
EX.NO:18
Test for carbohydrates in pure samples and their detection in
given foodstuffs.
S.N Experiment Observation Inference
o
1. Molisch’s Test:
Take a little aqueous A reddish-purple Presence of
solution of ring is formed at Carbohydrate
carbohydrates in a test the junction of
tube. Add 2 drops 1% α- two layers.
Naphthol and then add
Conc.H2SO4 along the
sides of the test tube.
2. Benedict’s Test:
Take 2 ml aqueous Red precipitate Presence of
solution of carbohydrate is obtained Carbohydrate
and add 1-2 ml of
Benedict’s reagent. Heat
the test tube in a boiling
water bath.
3. Iodine Test:(Test for
Starch) Deep blue Presence of
Take 2 ml aqueous colour is Carbohydrate
solution of carbohydrate obtained
and add few drops of
iodine solution.
Result:
The give food sample is Carbohydrate.

EX.NO:19

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success
 Test for fats in pure samples and their detection in given
foodstuffs.

S.N Experiment Observation Inference

o
1. Spot Test:
Put a small amount of Appearance of Presence of fat
the given substance on translucent
a filter paper. Fold the spot on
paper and press it unfolding the
tightly. paper.
2. Solubility Test:
Take few drops of the Sample forms Presence of fat
given substance add lower layer,
alcohol which dissolve
on heating
3. Acrolein Test:
Heat a little of the A pungent Presence of fat
sample with few drops irritating odour
of Potassium bisulphide of acrolein
in a test tube.
Result:
The give food sample is Fat.
EX.NO:20
Test for proteins in pure samples and their detection in given
foodstuffs.

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success
 S.N Experiment Observation Inference
o
1. Biuret Test:
Put a small amount of Appearance of Presence of
the given substance in bluish violet protein
a test tube. Add NaOH colour.
solution and 4-5 drops
of 1% CuSO4 solution.
Warm the mixture for
about five minutes.
2. Xanthoproteic Test:
Take few drops of the Appearance of Presence of
given substance and yellow colour. protein
add few drop of
Conc.HNO3 and heat it.
3. Ninhydrin Test:
Heat a little of the Intense blue Presence of
sample with few drops colouration protein
of Ninhydrin solution
and boil the contents.
Result:
The give food sample is Protein.

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Result:
1. Sample A is Ketone
2. Sample B is Amine
3. Sample C is Carboxylic acid.

EX.NO:

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 37 | P a g e Self-belief and hard work will always earn you
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