EXPERIMENT NO.

1
Aim: To prepare colloidal solution (sol) of starch.
Theory: Starch forms a lyophilic sol when water is used as the dispersion medium. The
formation of sol is accelerated by heating. The starch sol can be prepared by heating starch and
water at about 100°C. It is quite stable and is not affected by the presence of any electrolytic
impurity.

Materials Required:

Apparatus: Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar,
tripod stand, wire-gauze and burner.

Chemicals: Soluble starch (500 mg) and distilled water.

Diagram:

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 (Figure).
5) Continue boiling for about 10 minutes and then allow the beaker to cool.
6) Filter the contents of the beaker through a filter-paper, fixed in a funnel.
7) Label the filtrate ‘Starch Sol’.

Precautions: 1) The apparatus used for preparing sol should be properly cleaned.
2) Distilled water should be used for preparing sols in water.
3) Starch should be converted into a fine paste before adding to boiling water.
4) Starch paste should be added in a thin stream to boiling water.
5) Constant stirring of the contents is necessary during the preparation of the sol.
 EXPERIMENT NO. 2

Aim: To prepare ferric hydroxide sol.

Theory: Ferric hydroxide (Fe(OH)3) has the ability to form a lyophobic sol. Sulphides or metal
hydroxides which form colloidal solution, when treated with water, are termed as lyophobic
colloids. Fe(OH)3 sol is obtained by hydrolysis of ferric chloride with boiling distilled water.
The reaction is as follows:
FeCl3(aq) + 3H2O(l)  Fe(OH)3(s) +3HCl(aq)
The hydrochloric acid formed during the hydrolysis destabilizes the ferric hydroxide sol and
therefore must be removed through the process of dialysis.

Materials required:

Apparatus: Glass rod, round bottom flask, boiling tube, conical flask of 250 ml, tripod stand,
funnel, beaker of 250 ml, burette, wire gauze, dropper, burner, iron stand with clamp, boiling
tube.

Chemicals: Distilled water, solution of ferric chloride.

Diagram:
Procedure:
1. Take a conical flask of volume 250 mL and steam clean it.
2. To clean the conical flask by steaming out process, take the help of the given figure.
3. Prepare 2% solution of ferric chloride by taking 2 g of pure ferric chloride in 100mL of
distilled water.
4. Take the conical flask cleaned by steaming out process and add 100mL of distilled water.
5. Boil the water on a wire gauze.
6. Drop by drop pour 10 mL of ferric chloride solution with the help of a dropper or burette.
7. Constantly keep stirring the boiling water mixture while adding ferric chloride solution.
8. Heat the conical flask containing a mixture of distilled water and ferric chloride solution until
you see a brown or deep red coloured ferric hydroxide solution.
9. Allow the mixture in the conical flask to settle at room temperature.
10. Label the flask containing mixture as ferric hydroxide sol.

Precautions:

 Fe(OH)3 sol gets affected due to the presence of impurities. Therefore, to avoid this,
conical flask is cleaned by steaming out process.
 The FeCl3 solution is added drop wise.
 Heat the mixture of distilled water and ferric chloride solution until brown or deep red
colour is obtained.
 The hydrochloric acid (HCl) formed is removed by the process of dialysis to avoid
destabilization of sol.
 EXPERIMENT NO. 3

Aim: To purify lyophilic and lyophobic sol by dialysis.

Theory: The purification of lyophilic and lyophobic sols is carried out through a process called
dialysis where the colloidal particles cannot pass through a parchment or cellophane membrane
but the ions of an electrolyte can.

Materials required:
Apparatus: Beaker of volume 400 mL, parchment/cellophane membrane, test tubes, funnel
with long stem, iron stand, dropper.

Chemicals: Starch sol mixed with iodine solution, silver nitrate and sodium chloride

Diagram:

Procedure:
1. Take a square parchment/ cellophane paper whose size is 30 cm × 30 cm.
2. Dip the sheet in water and make it into a conical shape.
3. Add starch sol colloidal dispersion in the cellophane/parchment paper cone.
4. Make use of a thread to tie the cone and hang it in a channel filled with distilled water.
5. After 30 minutes, check the channel water for the presence of ions.
6. For every 30 minutes keep changing the water from the channel till it separates Na+ and
Cl– ions.
7. You can determine the presence of Na+ and Cl– ions by the simple test:
8. Take two test tubes
9. Add channel water in both the tubes.
 10. Add uranyl zinc acetate in one test tube and silver nitrate solution in the other tube.
11. If a yellow precipitate with uranyl zinc acetate is formed then it means sodium ions are
still present.
12. If a white precipitate with silver nitrate is formed then it means Cl– ions are still present.
13. Make a note of the time required to purify colloidal dispersion.

Precautions:

 During the process of dialysis create airtight parchment bag to ensure that water does not
get inside the bag.
 Remember to keep the neck of the parchment bag just above the water surface.
 For every 30 minutes change the water from channels during the process of dialysis.
 EXPERIMENT NO. 4

Aim: To study the role of emulsifying agents to stabilize the emulsions of different oils.

Theory: A colloid where the dispersion medium, as well as dispersed phase, are in liquid form
it is called an emulsion. Here they are differentiated based on their relative amounts. Dispersed
phase is present in smaller quantity whereas the dispersion medium is present in large
proportion.
Mix oil and water and shake the mixture. You can see a slight milky solution. It is unstable and
is known as an emulsion of oil in water. When allowed standing, two layers are formed
separating oil and water.
To increase the stability of oil and water emulsion soap solution can be added. Soap solution is
an emulsifying agent. The carboxyl polar group decreases the interfacial surface tension
between the two layers. Optimum concentration is the soap concentration essential to
complete emulsification process. Effective stabilization is not achieved if the amount is greater
or less than optimum concentration.

Materials required:
Apparatus: One test tube stand, stopwatch, one glass rod, five droppers, six test tubes.
Chemicals: Kerosene oil, mustard oil, coconut oil, castor oil (10 ml each).

Procedure:

1. Take a test tube with 10 mL of distilled water and dissolve 1 g of detergent in it. Shake
the test tube vigorously and label it as ‘A’.
2. Take four test tubes and label them B, C, D and E. Add 5 mL distilled water in each test
tube. Pour 10 drops of mustard oil in B, 10 drops of kerosene oil in C, 10 drops of castor
oil in D and 10 drops of coconut oil in E.
3. Take test tube B in your hand and shake it vigorously (for 5 minutes) and keep it in the
test tube stand. Start the stopwatch to record the time taken to separate two layers.
4. Follow the same procedure with the rest of the test tube’s viz, C, D and E.
5. Add two drops of detergent or soap solution prepared in test tube A into each test tube.
Shake the test tubes for 5 minutes each and record the time of separation.
6. Record the results in the table below.

Specification of test Oil used for Without soap or With soap or

tube emulsification detergent detergent

B Mustard oil 14 seconds 20 seconds

C Kerosene oil 4 seconds 6 seconds

 D Castor oil 6 seconds 10 seconds

E Coconut oil 12 seconds 15 seconds

Result: It is clear from the observations that mustard oil takes longest time to get separated
from its emulsion and is rated 1 and kerosene oil takes the minimum time and is rated 4.

Precautions:

 Add equal amount of detergent solution to all the five test tubes.
 Shake all five test tubes for an identical time span to minimize the time recording error.
 Stop the stopwatch immediately when you see the layers separated and start it as soon as
the shaking stops.
 EXPERIMENT NO. 5

Part A:

Aim: To study the effect of concentration on the rate of reaction between hydrochloric acid and
sodium thiosulphate.

Theory: According to the law of mass action, rate of a chemical reaction is directly
proportional to the product of the molar concentrations of the reactants. In other words, the rate
of reaction increases with increase in the concentration of the reactants. The effect of
concentration of reactants can be studied easily by the reaction between sodium thiosulphate
and hydrochloric acid.
The reaction occurs as follows:
Na2S2O3 (aq) + 2HCl (aq) → 2NaCl (aq) + H2O(l) + SO2 (g) + S(s)
The above reaction when written in its ionic form:
S2O3-2 (aq) + 2H+ (aq) → H2O (l) + SO2 (g) + S(s)
As the concentration of reacting species increases the rate of precipitation of sulphur also
increases. As the concentration increases, molecular collisions per unit time of the reacting
species increase which can result in increased chances of product formation. This results in an
increase in the rate of precipitation of sulphur. The insoluble sulphur, formed during the
reaction, gives 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:
Apparatus: 5 flasks, burette of volume 50 ml, pipette, burette stand, stopwatch.
Chemicals: Sodium thiosulphate, 1M hydrochloric acid.

Procedure:
The effect of concentration on the rate of reaction:

1. Take five conical flasks, rinse them with water, and label them 1, 2, 3, 4, 5.
2. Add 45 mL of sodium thiosulphate solution in flask 1, 35 mL of sodium thiosulphate
solution in flask 2, 25 mL of sodium thiosulphate solution in flask 3, 15 mL of sodium
thiosulphate solution in flask 4, and 5 mL of sodium thiosulphate solution in flask 5.
3. Add 10 mL of distilled water in the flask 2, 20 mL of distilled water in the flask 3, 30 mL
of distilled water in flask 4, 40 mL of distilled water in flask 5.
4. Add 1M HCl of volume 5 mL in flask 1 with the help of a burette.This is done to adjust
the volume of solution in flask 1 to 50 mL.
5. Start the stopwatch immediately.
6. Take a white tile and draw a cross mark on it.
 7. Add half of the HCl in the flask 1 and shake it well and start the stop-watch.
8. Observe the flask and start the stop-watch as soon as the cross mark becomes invisible.
Record the time taken for the process.
9. Repeat the experiment by adding 5 mL HCl in flask 2, 3, 4, 5 and record the time for
each.

Diagram:

Observations:
Stock solutions:

Sodium thiosulphate: 0.25 mol/L

Hydrochloric acid: 1mol/L

Volume of Volume of Volume of Total Concentration Time for X Rate (1/t)
Na2S2O3 water (ml) HCl (ml) Volume of Na2S2O3 to
(ml) (ml) after mixing disappear s-1
(mol/l) (s)
45 0 5 50 0.225 44 0.0227
35 10 5 50 0.175 58 0.0172
25 20 5 50 0.125 83 0.0120
15 30 5 50 0.075 125 0.008
5 40 5 50 0.025 333 0.003

Plotting of graph: Plot a graph by taking 1/t along y – axis and concentration of sodium
thiosulphate along x-axis. It should be a straight line passing through origin
.

Result: From the graph, it is clear that 1/t is directly proportional to the concentration of
sodium thiosulphate.

Precautions:

 Thoroughly wash the apparatus.

 The solutions taken for this experiment should be measured accurately.
 Use the same tile for all the observations.
 Stay alert while you start and stop the stop-watch.
Part B:

Aim: To study the effect of temperature variation on the rate of reaction between hydrochloric
acid and sodium thiosulphate.

Theory: The rate of chemical reaction is directly proportional to the temperature. As the
temperature increases, the reaction rate also increases. With the increase in temperature the
kinetic energy of the molecules also increases. Usually, it is observed that for every 10
increase in temperature, the rate of reaction is doubled. Therefore, the rate of reaction of
hydrochloric acid and sodium thiosulphate also increases with rise in temperature.

Materials required:
Apparatus: Conical flask of volume 250 ml, stop watch, tripod stand, measuring cylinder,
stopwatch, burner, thermometer, wire gauze.
Chemicals: 0.1M sodium thiosulphate solution, Concentrated nitric acid, Distilled water, 1M
hydrochloric acid.

Procedure:
The effect of temperature on the rate of reaction:

1. Take a conical flask of volume 100 mL.

2. Add 50 mL of 0.1M sodium thiosulphate solution to it.
3. With the help of a thermometer, measure the temperature of solution added to the flask.
4. Take 1M HCl of volume 10 mL with the help of a burette and add it to the conical flask
containing sodium thiosulphate.
5. Start the stopwatch as soon as you have poured half of hydrochloric acid in the flask
containing sodium thiosulphate solution.
6. Take a white tile and draw a cross mark on it.
7. Shake the conical flask and place it on the tile.
8. Observe the flask and start the stop-watch as soon as the cross mark becomes invisible.
9. Empty the flask and wash it with concentrated nitric acid first and later with distilled
water.
10. Take the washed flask add 50 mL of 0.1M sodium thiosulphate solution and heat it to (T+
10) .
11. Continue the steps from point 4.
12. Repeat the experiment for (T+ 20) , (T+ 30) , (T+ 40) and record the results.
13. Record the time taken for the process.

Observations:

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

Volume of 1 M HCl added each time = 10 ml

 Trials Temperature (T) Time taken for cross to become 1/t
just invisible (t)

1 T = 30 38 seconds 0.026 sec-1

2 (T+ 10)° = 40 30 seconds 0.033 sec-1

3 (T+ 20)° = 50 22 seconds 0.045 sec-1

4 (T+ 30)° = 60 15 seconds 0.066 sec-1

5 (T+ 40)° = 70 10 seconds 0.1 sec-1

Plotting of graph: Plot a graph by taking 1/t along y – axis and temperature along x-axis.

Result: The rate of reaction between sodium thiosulphate and hydrochloric acid increases with
increase in the temperature.

Precautions:
 Thoroughly wash the apparatus with concentrated nitric acid and distilled water.
 Take the exact quantity of solutions needed for this experiment.
 Complete the experiment in one go to avoid temperature variations.
 Use same tile for all the observations.
 Stay alert while you start and stop the stop-watch.
 EXPERIMENT NO. 6

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: Hydrogen peroxide oxidizes iodide ions to iodine in acidic medium
H2O2 + 2I– + 2H+ —–> 2H2O + I2
The reaction is monitored by adding a known volume of sodium thiosulphate solution and
starch solution to the reaction mixture. Iodine liberated at once reacts with sodium
thiosulphate solution and is reduced to iodide ions
I2+ 2S2O32- —fast—> S8O62- + 2I–
When thiosulphate ions are completely consumed, the liberated iodine reacts with starch
solution and gives blue colour
I2 + Starch ——-> Blue complex
The time elapsed before the appearance of blue colour, gives an idea about the rate of the
reaction.

Apparatus: 4 Conical flasks (250 ml), measuring cylinder, burette, pipette (25 ml), stop-watch.

Chemicals: 0.1 M KI solution, 2.5 M H2SO4, starch solution, ‘3%’ H2O2 solution, 0.05 M
sodium thiosulphate solution.

Procedure: 1) Take four 250 ml conical flasks 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 flasks A, B, C and D
respectively.
3) Add 10 ml of to each flask.
4) Add water to make the volume of solution 100 ml in each flask.
5) Add 5 ml starch solution to each flask.
6) Add 10 ml of 0.05 M sodium thiosulphate solution to each flask.
7) Add 5 ml of 3% hydrogen peroxide solution to flask A with the help of a 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 step 7 with the solutions in flasks B, C and D.

Observations:
Time required for the blue colour to first appear in :
Flask A — 265 s
Flask B — 138 s
Flask C — 96 s
Flask D — 74 s

Result: The rate of the reaction increases with increase in concentration of iodide ions.

Precautions: 1) Always use a freshly prepared solution of sodium thiosulphate.

2) Concentration of KI solution should be higher than the concentration of sodium thiosulphate
solution.
3) Use freshly prepared starch solution.
 EXPERIMENT NO. 7

Aim: To determine the enthalpy of dissolution of given copper sulphate at room temperature
using water as reaction medium.

Theory: In thermochemical measurements generally, aqueous solutions are mixed therefore,

water in the reaction medium and the temperature changes result due to the chemical reactions
taking place in solution.
According to law of conservation of energy, the sum of enthalpy changes taking place in the
calorimeter (loss and gain of energy) must be zero. Thus, we can write the following equation-
ΔH1 + ΔH2 + ΔH3 + ΔH4 = 0
(∆H1) Heat gained by calorimeter, thermometer and stirrer.
(∆H2) Enthalpy change of solution/water in calorimeter.
(∆H3) Enthalpy change of added solution/ water in calorimeter.
(∆H4) Enthalpy change of reaction.
In these reactions we take the product of density and heat capacity of solutions, dCp , to be
4.184 J.mL–1.K–1, nearly the same as that of pure water.* (* Density of the solutions is 4 to 6%
higher than that of pure water and heat capacity is about 4 to 8% less than pure water so the
product of density and heat capacity (dCp ) is nearly the same as the product of pure water.)

Solution formation often accompanies heat changes. Enthalpy of solution is the amount of heat
liberated or absorbed when one mole of a solute (solid/liquid) is dissolved in such a large
quantity of solvent (usually water) that further dilution does not make any heat changes.

Materials Required:

Apparatus: Beakers, thermometer, glass rod, weight box, physical balance, stirrer, measuring
cylinder, small wooden block, small piece of cardboard, filler, cotton wool.

Chemicals: Hydrated copper sulphate, distilled water.

Reaction: Cu2SO4.5H2O(s) + H2O(l) →Cu2SO4 (aq)

Apparatus Setup:
Procedure: 1) Put 200 ml of distilled water into the polythene bottle.
2) Now fit a cork with two holes into the mouth of the polythene bottle. Insert a thermometer
into one hole with its bulb about 1 cm above the bottom of the bottle. Put the stirrer into the
second hole.
3) Note down the temperature (t1).
4) Take a 0.5g of finely powdered hydrated copper sulphate.
5) Transfer the finely powdered hydrated copper sulphate quickly into the polythene bottle by
removing the rubber cork and putting it back into its position without any loss of time.
6) Stir it with the help of a stirrer till hydrated copper sulphate is dissolved. However, the rate of
stirring should he kept as low as efficiency permits to minimise the energy introduced by
stirring (vigorous stirring does cause some increase in temperature).
7) Note down the temperature (t2) when the substance just dissolves.

Observations
Weight of the hydrated copper sulphate dissolved =0.5 g
Volume of water taken into the bottle = 25 ml
Temperature of water =25°C
Temperature of water after dissolving hydrated copper sulphate = 27°C
Change in temperature = 27°C - 25°C = 2°C
Specific heat capacity of water = 4.184 J/g

Calculations:
Heat released (Q) for dissolution of 0.5g of copper sulphate = m.s.∆t
where,
m = mass of solution = mass of solute + mass of solvent = 0.5g + 25g = 25.5g
s = specific heat capacity of water = 4.184 J/g
∆t = change in temperature = 27°C - 25°C = 2°C
Q = m.s.∆t = 25.5 x 4.184 x 2 = 213.38 J

Result: The enthalpy of dissolution of given copper sulphate at room temperature is 10669
J/mole.

Precautions: 1) To dissolve the solid and record the temperature, stir the solution well. Avoid
too much stirring because due to friction it can produce heat.
2) Carefully weigh copper sulphate as it is naturally hygroscopic.
3) Use a 0.1°C thermometer to record the water temperature.
 EXPERIMENT NO. 8

Aim: To study the variation of cell potential in Zn/Zn2+ || Cu2+/Cu with change in concentration
of electrolytes (CuSO4 or ZnSO4) at room temperature.

Theory on variation of cell potential in Zn-Cu Cell:

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.

 Electrochemical reaction – The chemical reaction which takes place in a cell like Daniel
cell.
 Electrochemical cell – The cell in which chemical energy is converted into electrical
energy.
 Electrolytic cells – Electrical energy is consumed to bring about a chemical reaction or a
chemical change.
 Galvanic cells – Also called voltaic cells where chemical energy is converted into
electrical energy.
In daniel cell current flows from copper electrode to the zinc electrode. 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)
———————————————————————————————
→ When Emf < 1.1V
Electrons flow from Zn rod to Cu rod and hence current flows from Cu to Zn electrode. Zinc
dissolves at anode and copper deposits at cathode.
→ When Emf = 1.1V
The reaction stops altogether and there is no flow of electrons or current in the circuit. There is
no chemical reactions at the electrode.
→ When Emf > 1.1V
The current flows in opposite direction and the reaction proceeds in the opposite direction.
Electrons flow from Cu to Zn and current flows from Zn to Cu.

Materials Required:

Apparatus: Zinc electrode, copper electrode, beakers, voltmeter or potentiometer, salt bridge,
connecting wires.

Chemicals: 1M zinc sulphate solution, 1M copper sulphate solution.

Apparatus Setup:

Procedure:

Preparation of Salt Bridge:

 In a U-shaped tube heat 20gm of agar-agar gel and 5gm of potassium chloride in a
beaker.
 Suck the molten mixtures into U-shaped tube.
  Allow it to cool.

1. Prepare 1M of zinc sulfate solution and 1M of copper sulfate solution in separate beakers.
2. Connect a salt bridge in such a manner that its one end dips in zinc sulfate and the other
dips in copper sulfate solution.
3. Now connect the zinc plate to negative terminal of voltmeter and copper plate to positive
terminal of voltmeter.
4. Note down the reading of voltmeter in observation table.
5. Take 10ml of 1M zinc sulfate and add water to make its volume up to 20ml. The resultant
molarity will be 0.5M. Now dip zinc rod in 0.5M zinc sulfate solution and copper rod in
1M copper sulfate solution and note the readings.
6. Take 10ml of 1M zinc sulfate and add water to make its volume up to 100ml. The
resultant molarity will be 0.1M. Now dip zinc rod in 0.1M zinc sulfate solution and
copper rod in 1M copper sulfate solution and note the readings.
7. Repeat the same for 0.01M and 0.025M of zinc sulfate solution.
8. Note down the reading in voltmeter.
9. Repeat this procedure for other solutions of copper sulfate solutions.
10. Record electrode potentials values of copper electrodes for different concentrations.
11. Plot a graph for the variation of cell potential with concentration.
12. Calculate Ecell in each case and write down in the observation table.

Observation and Inference:

S.No Concentration of zinc Concentration of copper Ecell/V

sulphate sulphate

1 1M 1M 1.1

2 1M 0.5M 1.091

3 1M 0.025M 1.052

4 1M 0.0125M 1.043

5 0.5M 1M 1.108
By substituting all the values we can measure Ecell at different concentration of electrolyte.

Result and Discussion:

1. The Ecell decreases with increase in molar concentration of [Zn 2+]. (Zinc sulfate solution)
2. The Ecell increases with increase in molar concentration of [Cu 2+]. (Copper sulfate
solution)

Precautions:

1. Immediately after use, place the salt bridge in distilled water.

2. Very carefully dilute the solution to another concentration.
3. Always clean strips of copper and zinc with sandpaper and connect the wires before use.
4. Choose appropriate graph plot scales.
 EXPERIMENT NO. 9
AIM:- To separate the pigments or coloured components present in given leaves, flowers or
grass juice by paper chromatography and compare their Rf values.

THEORY: The juice of the flowers, spinach leaves or grass contains a number of coloured
compounds mostly green, yellow, orange or red. These can be separated by paper
chromatography. A spot of the juice is made near the starting line on the filter paper strip. It is
suspended in a jar containing a suitable solvent (acetone, benzene, toluence or petroleum ether)
so that the lower end of the strip dips in the solvent. The solvent moves up by capillary action
and carries the pigments along with it. As the pigments travel with different speeds, they get
separated and form separated spots. These can be separated by cutting the filter paper strip.

REQUIREMENTS: Glass jar having arrangement for suspending the filter paper strip.
Whatmann filter paper, fine capillary tube, scale and pencil, mortar and pestle, flower petals,
spinach leaves of grass leaves, ethyl alcohol, or mixture of acetone and petroleum ether (40:60).

PROCEDURE:
1. Crush fresh flowers, spinach leaves or grass separately in mortar with the help of a pestle
and extract the juice separately with acetone.
2. Draw a line with pencil at about 3 cm from one end on filter paper strip (18 x 5 cm). With
the help of fine capillary, put one spot of flower juice on this line. Dry the spot in the air.
Repeat it 2-3 times by putting the drop on the same spot. Mark this spot as X.
3. Similarly put a spot of spinach extract or grass juice, at least one cm away from spot X
using a fine capillary tube. Mark it as spot Y.
4. Suspend the paper in the glass jar containing acetone + petroleum ether (40-60) so that
lower end is dipping about 2 cm in the solvent.
5. Allow it to stand so that the solvent rises about 15 cm on the paper strip.
6. Take out the chromatographic paper, dry it and mark the position of the solvent front.
7. Mark the number of components present in flower extract and in spinach leaves or grass
juice.
8. Measure the distance of each coloured spot and solvent front from the original line and
calculate the Rf value as explained earlier.

Diagram
Observation table

Sr. Name of the Colour of the Distance Distance Rf value

No. Extract spot travelled by spot travelled by
from the original solvent from
line the original
line
1 Flower extract Yellow 7.4 cm 7.4 cm 1
2 Leaf extract Yellow 7.2 cm 7.4 cm 0.97
3 Leaf extract Green 1.8 cm 7.4 cm 0.24

Calculations:

Result: 1) Rf value of yellow spot of flower extract is 1.

2) Rf value of yellow spot of leaf extract is 0.97.
3) Rf value of green spot of leaf extract is 0.24.
 EXPERIMENT NO. 10
AIM: To separate Cd2+ and Pb2+ ions present in the given mixture by using ascending paper
chromatography and determine their Rf values.
REQUIREMNETS: Glass jar, glass rod, filter paper strip, whatmann filter paper, gas cover,
fine capillary tube, mixture of cadmium and lead ions, acetone, concentrated aqueous ammonia,
rubeanic acid spray reagent.
PROCEDURE: 1) Use a mixture of acetone (90%), concentrated hydrochloric acid (5%) and
water (5%) as an eluent.
2) After elusion and drying place the paper in a large, dry, covered beaker containing small
amount of concentrated ammonia.
3) After about 2 minutes remove the paper and spray it on both sides with rubeanic acid reagent.
Allow it to dry.
4) Cadmium ions become blue purple whereas lead ions become yellow orange.
5) Evaluate Rf values of these ions.
Diagram

OBSERVATION TABLE

Colour of the spot Distance travelled by Distance travelled by

different components solvent
Cd2+ (Yellow) 9.9 cm 11.5 cm
Pb2+ (Black) 8.7 cm 11.5 cm
CALCULATIONS:
Distance travelled by Cd2+from base line 9.9
Rf value of Cd2+ = = = 0.86
Distance travelled by solvent from base line 11.5

Distance travelled by Pb2+from base line 8.7

Rf value of Pb2+ = = = 0.75
Distance travelled by solvent from base line 11.5

RESULT: 1) Rf value of Cd2+ is 0.86.

2) Rf value of Pb2+ is 0.75.
 EXPERIMENT No. 11

Aim: To prepare Mohr’s salt: ferrous ammonium sulphate from ferrous sulphate and
ammonium sulphate in the presence of acid.

Theory: The formula for ferrous ammonium sulphate is FeSO4.(NH4)2SO4.6H2O. It is prepared

by dissolving equimolar mixture of hydrated ferrous sulphate and ammonium sulphate in water
containing a little sulfuric acid. The solution is subjected to crystallization, ferrous ammonium
sulphate separates out from the solution.
The chemical reaction is given below.
FeSO4 + (NH4)2SO4 + 6H2O → FeSO4.(NH4)2SO4.6H2O (Mohr’s salt)
The addition of sulphuric acid in this experiment prevents the hydrolysis of this salt. Ferrous
ammonium sulphate is a pale green crystalline compound which does not effloresce like ferrous
sulphate. It is less readily oxidised than FeSO4 and therefore, a better volumetric reagent in
preference to ferrous sulphate.
Mohr’s salt is also called as double salt which contain more than one simple salt. It undergoes
complete dissociation in aqueous solutions. Mohr’s salt dissociates into Fe2+, NH4+, SO42- ions
and give their individual chemical test.
Mohr’s salt is light green transparent octahedral crystals. It is soluble in water giving acidic
solution which turns blue litmus paper red and gives effervescence with sodium bicarbonate
evolving carbon dioxide.
Preparation of Mohr’s Salt:
Ferrous Ammonium Sulphate also called Mohr’s salt is prepared by dissolving equimolar
mixture of hydrated ferrous sulphate and ammonium sulphate in water containing a little
sulphuric acid. The solution is subjected to crystallization.

Materials Required:

1. Conical flask
2. Tripod stand
3. Burner
4. Funnel
5. Watch glass
6. Glass rod
7. Filter paper
8. Wire gauze
9. China dish
10. Ferrous sulphate
11. Ammonium sulphate
12. Dilute sulphuric acid
Apparatus Setup:

Laboratory Preparation of Ferrous Ammonium Sulphate – Mohr’s Salt

Procedure:

1. Weigh 7g of ferrous sulphate and 3.5g of ammonium sulphate separately.

2. Mix ferrous sulphate and ammonium sulphate in water in a beaker containing dilute
sulphuric acid.
3. Gently warm the solution in order to get a clear solution.
4. Filter the solution in order to remove suspended impurities and concentrate the clear
filtrate by heating it china dish over a sand bath till the crystallization point is reached.
5. Stir the solution occasionally during heating.
6. Keep the solution undisturbed for slow cooling. After some time crystal of ferrous
ammonium sulphate will get separated from the solution.
7. Separate the crystals by decantation from the mother liquor and wash the crystals with
cold water.
8. Dry the crystals between the folds of filter paper or by spreading on a porous plate.

Observations:

Colour of the crystal Light green

Shape of the crystal Octahedral

Solubility in water Soluble

Action of blue litmus paper Blue litmus turns red

Result:
Pure light green crystals of ferrous ammonium sulphate or Mohr’s salt were obtained.
Precautions:
 Allow slow cooling and do not disturb the solution during cooling in order to get good
quality crystals.
 During the process heating of the solution should be done in a short time only. Because
prolonged heating forms ferric ions along with ferrous ammonium sulphate.
 Suppose if the solution is yellow instead of green the experiment should be repeated.
 EXPERIMENT NO. 12

Aim: To prepare the pure samples of crystals of potassium ferric oxalate from oxalic acid
dihydrate, potassium oxalate monohydrate and ferric chloride.

Theory: Potassium ferric oxalate is prepared when freshly prepared ferric hydroxide is
dissolved in a solution of oxalic acid, yellow precipitate of ferrous oxalate will be formed. It is
further treated with potassium oxalate monohydrate, a green precipitate of Potassium Ferric
Oxalate is formed. Potassium ferric oxalate is a complex compound with the formula
K3[Fe(C2O4)3].3H2O.
The chemical reactions are given below.
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
(Potassium Ferric Oxalate)
Oxalic acid is added in excess so that ferric hydroxide dissolves and the soluble complex is
formed. Alcohol is added to the solution to precipitate the complex iron salt as it is less soluble
in alcohol than water.
Other names – Potassium Trioxalatoferrate (III), Potassium ferrioxalate, Potassium iron (+3)
oxalate, Potassium tris (oxalato) ferrate (III).

Materials Required:

1. Oxalic acid hydrate

2. Ferric chloride
3. Potassium oxalate
4. Potassium hydroxide
5. Beaker
6. Conical flask
7. Tripod stand
8. Glass rod
9. Wire gauze
10. Filter paper
11. China dish
12. Funnel
Apparatus Setup:

1. Ferric oxalate solution – Fe2(C2O4)3

2. Potassium Ferric Oxalate – K3[Fe(C2O4)3].3H2O

Procedure:

1. In a beaker dissolve 3.5g of freshly prepared ferric chloride in 10 ml of water.

2. Take another beaker and dissolve 4g of potassium hydroxide in 50ml of water.
3. Add the potassium hydroxide solution slowly to ferric chloride solution with constant
stirring. A brown colour ferric hydroxide precipitate is formed
4. Filter the precipitate of ferric hydroxide through the funnel and wash the precipitate with
hot water.
5. In another beaker take 4g of oxalic acid and 5.5g of potassium oxalate. Add 100ml water
and stir well to get a clear solution of potassium oxalate.
6. Add the freshly prepared ferric hydroxide precipitate to potassium oxalate solution
gradually with constant stirring so that precipitate dissolves completely and green colour
solution is formed.
7. Filter the solution in order to remove any insoluble impurities.
8. Transfer the green coloured solution in a china dish and concentrate the solution till
the crystallization point is achieved.
9. Place the china dish in cold water and allow cooling for an hour.
10. Green crystals of potassium ferric oxalate is formed. Remove the crystals from the
mother liquor
 11. Wash the crystals with ethyl alcohol and dry them between the folds of filter paper.
12. Weigh the crystals in order to know the yield.

Observations:

Colour of the crystals Green colour

Shape of the crystals Octahedral

Melting point 230oC

Expected Yield 10 gm

Result:
Pure green crystals of potassium ferric oxalate were obtained.

Precautions:

1. Do not concentrate the solution too much

2. Do not disturb the solution during crystallization in order to get big crystals.
3. While washing the crystals wash it with hot water in order to dissolve unwanted salt.
 EXPERIMENT NO. 13

Aim: To prepare 2-Naphthol Aniline Dye from aniline, sodium nitrite, hydrochloric acid and
alkaline solution of β-napthol also called 2-naphthol.

Theory: 2- Naphthol aniline dye is a scarlet dye can be prepared by coupling reaction.
Aniline reacts with sodium nitrite in the presence of hydrochloric acid forms benzene
diazonium chloride. Further benzene diazonium chloride reacts with 2-naphthol forms a bright
orange colour 2-naphthol aniline dye.

Azo compounds are prepared by the reaction of diazonium salts with phenol under alkaline
conditions. Primary aromatic amines react with nitrous acid at 0oC to give a diazonium salt.
Nitrous acid is in turn formed by the reaction of sodium nitrite with hydrochloric acid. The
active reagent is nitrous anhydride or dinitrogen trioxide. Nitrous anhydride reacts with aniline
to give nitroamine derivative which is unstable and isomerizes to form a diacetic acid which in
turn converted to a diazonium salt. Finally, this diazonium salt reacts with 2-naphthol in the
presence of sodium hydroxide to give 2-naphthol aniline which is an aniline dye.

Materials Required:

Apparatus: Beaker, test tube, Buchner funnel, pipette, capillary tube, thermometer, distilled
water , hot air oven, ice bath.

Chemicals: Aniline, sodium nitrite, hydrochloric acid, 2 – Naphthol, sodium hydroxide

solution.
Apparatus Setup:

Procedure:

1. Dissolve 5ml of aniline in a mixture of concentrated hydrochloric acid and water.

2. Cool the solution in ice bath between 0-5oC.
3. Add a solution of 4gm sodium nitrite in 15ml of water drop wise with continuous shaking
and controlling the temperature below 5oC.
4. Take another flask to dissolve 8gm of 2-naphthol in a solution of 5 gm sodium
hydroxide solution in 50ml of water.
5. Cool the solution in the ice bath to 0-5oC.
6. Now mix the two cold solutions slowly drop wise with constant stirring.
7. Continue the stirring at least half an hour without allowing the temperature to rise above
10oC.
8. An orange colour azo dye called 2-naphthol aniline separates out.
9. Filter the crude sample and wash it with cold water.
10. Dry and recrystallize it from ethyl alcohol or glacial acetic acid.

Observations:

Colour of the crystals Orange crystals

Yield 5 gm

Melting Point 131oC

Result: Pure orange crystals of of 2- Naphthol aniline dye were obtained.

Precautions:

1. The solution must be cooled to 5oC. Do not raise the temperature.

2. Not to touch the dye otherwise it will stick to hands.
3. Not to touch the concentrated acids otherwise it will cause irritation.
4. Wash the crude sample repeatedly with cold water in order to remove soluble impurities.
5. Maintain the pH between 4-5.
 EXPERIMENT No. 14

Aim: To study the different tests for the functional groups present in organic compounds:
Unsaturation, alcoholic, phenolic, aldehydic, ketonic, carboxylic and amino (Primary) groups.

Tests for Unsaturation

There are two tests for detecting unsaturation in organic compound:
1. Bromine Test.
2. Alkaline KMnO4 Test.
1. Bromine Test
In this test, the orange-red colour of bromine solution disappears when it is added to the
unsaturated hydrocarbon to form colourless addition products.

Procedure
(i) When the compound is soluble in water. Dissolve a part of the given compound (solid or
liquid) in about 2 ml of distilled water in a test-tube and add a drop of bromine water and shake.
Disappearance of orange-red. colour of bromine indicates unsaturation. Continue the addition of
bromine water drop wise with constant shaking. The disappearance of orange- red colour
continues so long as there are unsaturated bonds. When all the pi-bonds are broken, the orange-
red colour shall persist. Bring a rod dipped in NH4OH near the mouth of the test-tube.
Absence of white fumes confirms unsaturation.
(ii) When the compound is insoluble in water. Dissolve a small amount of the given compound
in 1 ml of CCl4 in a test tube and add 2% solution of bromine in CCl4. Shake the mixture.
Disappearance of orange-red colour indicates unsaturation. Continue the drop wise addition of
Br2 with constant shaking until the brown colour persists. Bring a rod dipped in NH4OH near
the mouth of the test-tube. Absence of white fumes confirms unsaturation.
(iii) When the compound is a gas. Add 1-2 ml of bromine solution into a gaseous compound
taken in a jar and shake. Disappearance of orange-red colour of bromine indicates unsaturation.
Note: No HBr is evolved in bromine test for unsaturation. However, some compounds such as
aniline form substituted products with bromine and evolve HBr.
Caution
Handle bromine solution carefully. Avoid its context with skin.
2. Alkaline KMnO4, Test (Baeyer’s Test)
In this test, the pink colour of KMnO4 disappears, when an alkaline KMnO4 is added to an
unsaturated hydrocarbon. The disappearance of pink colour may take place with or without the
formation of brown precipitate of MnO2.

Procedure
Dissolve a little of the given organic compound in about 2 ml of water or acetone in a test-tube.
Add 1-2 drops of alkaline solution of KMnO4 (1%) and shake the mixture. Decolourization of
pink colour of KMnO4 indicates unsaturation.
Preparation of Reagents:
1. Bromine water. Add 2 ml of liquid bromine in 100 ml of distilled water and shake. Decant
off the clear liquid.
2. Bromine in CCl4. Shake 2 ml of liquid bromine in 100 ml of CCl4 and stopper the bottle.
3. Alkaline KMnO4 (1%). Dissolve 1 g of KMnO4 (solid) in 100 ml of distilled water. Now add
10 g of anhydrous Na2C03. Shake to dissolve and stopper the bottle.

Tests for the Alcoholic [R-OH] Group

The alcoholic group can be detected by any of the following tests:
1. Sodium metal test.
2. Ester test.
3. Ceric ammonium nitrate test.
4. Acetyl chloride test.
5. Iodoform test for alcohols containing the

1. Sodium metal test

This test is based on the appearance of effervescence due to liberation of hydrogen gas when the
alcohol is reacted with active metals like sodium.
Procedure
Take about 1 ml of the given pure liquid in a dry test-tube, add about 1 gram of anhydrous
calcium sulphate and shake well to remove water. Filter or decant off the liquid to another clean
dry test tube and add a small piece of sodium metal.
A brisk effervescence due to the evolution of hydrogen gas indicates an alcoholic group.
Note: 1. The alcohol should be dry as water also reacts with sodium metal to evolve hydrogen
gas.
2. Do not throw unreacted sodium metal into the sink or waste bin. Add more alcohol to the
unreacted sodium to complete the reaction.

2. Ester test
Alcohols react with carboxylic acids to form sweet smelling esters. The reaction between an
alcoholic group and a carboxylic acid group is called esterification. This is a slow and reversible
reaction and is catalysed by an acid such as conc. sulphuric acid.

Procedure:
Take 1 ml of the given liquid in a clean dry test-tube, add 1 ml of glacial acetic acid and 2-3
drops of cone, sulphuric acid. Warm the mixture on a water bath for about 10 minutes. Pour it
into about 20 ml of cold water taken in a beaker and smell. A fruity smell indicates the presence
of an alcoholic group.

3. Ceric ammonium nitrate test

Place about 1 ml of the given compound in a clean dry test-tube, add a few drops of ceric
ammonium nitrate reagent and shake well. Appearance of pink or red colour indicates the
presence of an alcoholic group.
4. Acetyl chloride test
Alcohols react with acid halides to form esters and give out hydrogen chloride gas. The
hydrogen chloride formed gives white fumes of ammonium chloride with ammonium
hydroxide.

Procedure
Take about 2 ml of the given compound in a clean dry test-tube, add 1 g of anhydrous calcium
sulphate and shake well. Filter, and to the filtrate, add 2 or 3 drops of acetyl chloride, shake and
bring a glass rod dipped in ammonium hydroxide solution near the mouth of the test -tube.
Formation of white fumes indicates the presence of alcoholic group.

5. Iodoform test

Procedure
Take 1 ml of the given compound in a clean dry test-tube and add about 1 ml of 1% iodine
solution. Then add dilute sodium hydroxide solution drop wise until the brown colour of iodine
is discharged. Warm gently on a water bath.
Formation of yellow precipitate of iodoform indicates ethanol, acetaldehyde, sec-methyl alcohol
or methyl ketone.

Distinction Between Primary, Secondary and Tertiary Alcohols

Lucas Test
This test is based upon relative reactivities of various alcohols towards HCl in the presence of
ZnCl2. In this test, the alcohol is treated with Lucas reagent which is equimolar mixture of HCl
and ZnCl2. Alcohols are soluble in Lucas reagent, so a clear solution is obtained. On reaction,
alkyl chlorides are formed which being insoluble result in cloudiness in the solution.

Procedure
Take about 1 ml of dry alcohol in a clean dry test-tube and add 8-10 drops of Lucas reagent.
Shake the mixture well. Note down the appearance of cloudiness.

1. If cloudiness appears immediately, tertiary alcohol is indicated.

2. If cloudiness appears within five minutes, secondary alcohol is indicated.
3. If cloudiness appears only upon heating, primary alcohol is indicated.

Preparation of Reagents
1. Ceric ammonium nitrate. Ce(NO3)4. 2NH4NO3. Dissolve 20 g of orange crystals of ceric
ammonium nitrate in 200 ml of warm dilute nitric acid (2N).
2. Iodine solution. Dissolve 2 g of solid potassium iodide in about 40 ml water, add 1 g solid
iodine, shake well and dilute to 100 ml.
3. 5% sodium hydroxide solution. Dissolve 5 g of solid sodium hydroxide in about 50 ml water
and then make up the volume to 100 ml.
4. Lucas reagent. Dissolve 135 g of anhydrous zinc chloride in 100 ml of concentrated
hydrochloric acid. Shake well and cool.

Tests for Phenolic [Ar—OH] Group

The phenolic group can be detected by the following tests:

1. Litmus test.
2. Ferric chloride test.
3. Liebermann’s test.
4. Phthalein Dye Test

1. Litmus Test
Procedure
Place a drop of the given liquid or a crystal if solid on moist blue litmus paper. If the colour
changes to red, phenolic group may be present.
Note. Carboxylic acids also give this test. But as phenol is not as strong an acid as carboxylic
acid, it does not give an effervescence with aqueous solution of sodium carbonate.

2. Ferric Chloride Test

Phenols react with ferric ions to form coloured complexes. Many other types of organic
compounds also react with ferric chloride solution.
Procedure:
Take 1 ml of neutral ferric chloride solution in a clean test-tube and 2-3 drops of the liquid
compound (or 1 crystal of solid). A change in colour indicates the phenolic group. Phenol
produces violet colouration.

Note:
1. o, m, p-cresol, resorcinol give violet or blue colouration.
2. β-Naphthol gives a green colouration.
3. α-Naphthol gives pink colouration.
4. Formic acid and acetic acid give deep red colouration.
Preparation of neutral ferric chloride. Place 1 ml of 1% ferric chloride solution in a clean test -
tube and add ammonia solution until a brown precipitate just appears. Now add the original
ferric chloride solution drop wise until the precipitate just disappears.

4. Liebermann’s Test
Most of the phenols give this test. Red or brown colouration is produced when a nitrite is
added to a phenol dissolved in conc. sulphuric acid. The colour changes to blue or green
by the addition of a strong alkali.
 Procedure:
Place 2-3 crystals of sodium nitrite in a clean dry test-tube and add about 1 g of phenol. Heat
very gently for half a minute and allow it to cool. Then add about 1 ml of conc. sulphuric
acid and shake the tube to mix the contents. A deep blue or deep green colouration develops.
Add water carefully, the colour turns red. Now add an excess of sodium hydroxide solution,
the blue or green colour appears.
Note:
1. Nitrophenols and p-substituted phenols do not give this test.
2. Among the dihydroxyphenols, only resorcinol gives positive test.

4. Phthalein Dye Test

Take 0.1 g of organic compound and 0.1 g of phthalic anhydride in a clean dry test tube 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 into a beaker containing 15 mL of dilute sodium hydroxide solution.
Appearance of pink, blue, green, red etc. colours indicate the presence of phenolic —OH group
in the compound.

Tests for Aldehydic and Ketonic [—CHO and —CO—] Groups

1. 2, 4-Dinitrophenyl hydrazine Test (2, 4—DNP Test)

Take 0.5 ml or 0.5 g of the given compound in a clean dry test-tube, add rectified spirit until the
compound just dissolves. Now add a few drops of 2, 4-dinitrophenyl hydrazine solution. Cork
the test-tube, shake the mixture and allow it to stand for 5 minutes.

Formation of yellow or orange crystals indicate the presence of carbonyl group.

2. Sodium bisulphite Test
Take 2 ml of a saturated solution of sodium bisulphite in a clean test-tube , and add 1 ml or 1 g
of the given compound. Cork the test- tube , shake and leave it for 15-20 minutes.
Formations of crystalline precipitate confirms carbonyl group.
Note:

1. Formaldehyde, acetaldehyde, benzaldehyde, acetone, methyl ethyl ketone and

diethyl ketone give position tests.
2. Aqueous solutions of formaldehyde and acetaldehyde form addition products but as
they are highly soluble , precipitates are rarely formed.
3. Acetophenone and benzophenone do not give this test.

Differentiating Tests for Aldehydes

The following tests are given by aldehydes but not by ketones:
1. Schiff’s Test
Dissolve about 0.5 ml or 0.5 g of the given compound in alcohol in a clean test-tube and add 1
ml of Schiff’s reagent. Shake and note the change in colour.
Appearance of pink, red or magenta colour confirms the presence of aldehydic group.

Note: 1) The Schiff’s reagent should not be warmed.

2) The Schiff’s reagent should not be treated with alkalies. Otherwise the pink colour develops
even in the absence of aldehydes.
3) With benzaldehyde the pink colour develops slowly.

2. Tollen’s Test (Silver mirror test)

Procedure
Place 1 ml of silver nitrate solution in a clean test-tube and add 2-3 ml of dilute NaOH solution.
A brown 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 0.1 g if
solid) and warm the test-tube on a water-bath for about 5 minutes.

A shining mirror confirms the presence of the aldehyde group.

Note:

1. Many other types of compounds give positive silver mirror test but they do not give
2,4-dinitro phenyl hydrazine test.
2. Formic acid, tartaric acid and many carbohydrates like glucose give silver mirror
test.

3. Fehling’s Test
Procedure
Take 1 ml each of Fehling’s solution A and B in a test-tube. Add 4-5 drops (or 0.2 g) of the
given organic compound and warm the test-tube in hot water bath for 4-5 minutes.
Note:
1. Benzaldehyde may or may not give this test as the reaction is very slow.
2. Formic acid also gives this test.

Differentiating Tests for Ketones

The following tests are given by ketones but not by aldehydes:
1. m-Dinitrobenzene test
Place 0.5 ml of the given liquid (or 0.5 g of solid) in a clean test-tube and add about 0.1 g of
finely powdered m-dinitrobenzene. Now add about 1 ml of dilute sodium hydroxide solution
and shake.
Appearance of violet colour which slowly fades confirms ketonic group.
Note: Benzophenone does not give this test.

2. Sodium nitroprusside test

The anion of the ketone formed by an alkali reacts with nitroprusside ion to form coloured ion.

Procedure:
Dissolve a crystal of sodium nitroprusside in about 1 ml of distilled water in a clean test -tube
and then add 0.5 ml (or 0.5 g) of the given compound. Shake and add sodium hydroxide
solution drop wise.
A red colouration indicates the ketonic group.
Note:
1. Benzaldehyde also gives red colour,
2. Benzophenone does not give this test.

Preparation of Reagents
1. 2, 4-Dinitro phenylhydrazine (2, 4-DNP). Dissolve 1 g of 2, 4-dinitrophenyl hydrazine in 50
ml methanol to which 2 ml of concentrated sulphuric acid is added. Filter, if necessary.
2. Sodium bisulphite, NaHSO3. Dissolve about 30 g sodium bisulphite in 100 ml of distilled
water.
3. Schiff’s reagent. Dissolve 0.1 g p-rosa aniline hydrochloride in 100 ml water and pass
sulphur dioxide gas until its red colour is discharged. Filter and use the filtrate.
4. Fehling’s solution A. Dissolve 35 g of crystalline copper sulphate in 500 ml water and add 2
ml cone. H2S04
5. Fehling’s solution B. Dissolve 173 g of Rochelle salt (sodium potassium tartrate) and 60 g
sodium hydroxide in 500 ml water.
Tests for Carboxylic Group [—COOH]
Carboxylic acids can be identified by the following tests:
1. Litmus test.
2. Sodium bicarbonate test.
3. Ester test.

1. Litmus Test
The carboxylic acids turn blue litmus red. The hydroxyl group in —COOH is far more acidic
than in alcohol.

Procedure
Place a drop of the given liquid (or a crystal of the solid) on a moist blue litmus paper and note
the change in colour.
If the colour changes to red, carboxylic group or phenolic group is present.
Note: Phenols also give this test.

2. Sodium Hydrogencarbonate Test

Carboxylic acids react with sodium hydrogen carbonate to give carbon dioxide gas which is
identified by the effervescence produced. This test is used to distinguish carboxylic acids from
phenols.

Procedure
To 1 ml of organic liquid in a test-tube, add a pinch of sodium bicarbonate (NaHC03).
A brisk effervescence indicates the presence of carboxylic group in the organic compound.

3. Ester Test
A carboxylic acid reacts with an alcohol in presence of a little sulphuric acid to form an ester
which is recognized by its fruity smell.

Procedure
Take about 0.1 g of the organic compound, 1 ml of ethyl alcohol and 1-2 drops of cone.
H2S04 in a test tube. Heat the reaction mixture on a water bath for about five minutes. Pour the
reaction mixture in a beaker containing water. A fruity smell indicates the presence of
carboxylic group in the compound.

Tests for Amino Group [—NH2]

1. Solubility Test
Amines are the organic compounds that have appreciable basicity and so they dissolve in
mineral acids.

Procedure
Take a small amount of the given compound in a clean test-tube and add 2-3 ml of dilute
hydrochloric acid. Shake and note the solubility.
If the compound is soluble, it may be an amine.
2. Litmus Test
Amines have appreciable basicity and turn red litmus blue.

Procedure
Place a drop of the given liquid (or pinch of the solid) on the moist red litmus paper and note
the change in colour.
If the colour changes to blue, it may be an amine.
3. Carbylamine
This test is given-by both aliphatic and aromatic primary amines.
Secondary and tertiary amines do not give this test.
Procedure
Take about 0.2 g of solid potassium hydroxide in a clean dry test-tube and add 2 ml of ethanol.
Warm the test-tube until the pallets dissolve. To this add a few drops of chloroform, small
amount of the given compound and warm gently.

Caution
1. Carbylamine (isocyanide) is highly poisonous so do not inhale its vapours.
2. Destroy carbylamine with conc. HCl after the test and then throw into sink.
Nitrous Acid Test

Procedure
Make a solution of about 1 g sodium nitrite in about 5 ml water in a test-tube and cool in ice
bath. In a separate test-tube, dissolve a few drops or few crystals of the given compound in
about 1 ml conc. hydrochloric acid and cool this also in ice bath. Mix both the solutions and
observe that what happens.
(а) Bubbles of nitrogen gas is seen if the compound is a primary aliphatic amine.
(b) A yellow oily layer is formed if the compound is a secondary amine.
(c) No visible change in the reaction mixture if the compound is a tertiary amine.
5. Azo-Dye Test
This test is given by primary aromatic amines. Primary amines on reaction with nitrous acid
give diazonium salts. These diazonium salts can undergo coupling reaction with phenols
resulting in the formation of coloured compounds.
Procedure
Take three test tubes A, B and C. In test tube A, dissolve about 0.2 g of the compound in 2 ml
of dilute hydrochloric acid. In test tube B, prepare an aqueous solution of sodium nitrite, In test
tube C, dissolve 0.2 g of β-naphthol in dilute sodium hydroxide. Place all the three test tubes in
the ice bath.
Now add sodium nitrite solution to test tube A and the resulting solution is added to the test
tube C.
Formation of a red or orange dye confirms the presence of primary aromatic amino (Ar-NH2)
group.
Distinguishing Test for Primary, Secondary and Tertiary Amines
1. Hinsberg Test
The given amine is shaken with benzene sulphonyl chloride.

1. A clear solution of NaOH solution which on acidification gives insoluble material

indicates primary amine.
2. A precipitate (insoluble compound) which is insoluble in NaOH solution indicates
secondary amine.
3. Tertiary amines do not react with benzene sulphonyl chloride. An insoluble
compound in NaOH solution which dissolves by the addition of acid indicates
tertiary amine.

Procedure
Place 0.5 ml of the given amine in a clean test-tube, add about 2 ml of 25% NaOH, 2 ml of
water and 1 ml of benzene sulphonyl chloride. Shake the mixture for about 10 minutes and then
cool under tap water and note the formation of a precipitate. Treat the precipitate, if any, with 2
ml of conc. HCl.
1. Tertiary amine. Precipitate in the test-tube. It dissolves in conc. HCl.
2. Secondary amine. Precipitate in the test-tube. It does not dissolve in conc. HCl.
3. Primary amine. No precipitate (clear solution). On addition of conc. HCl, insoluble
material is seen.
 EXPERIMENT NO. 15
AIM :- To study some simple tests of oils and fats.

REQUIREMENTS :- Chloroform, furfural solution, ethyl alcohol, KHSO4 crystal,

Huble’s reagent, desi ghee, vegetable ghee and refined oil.

PROCEDURE :-
(a) Solubility Test – This test is based on the fact that oils and fats are soluble in organic
solvent like chloroform, alcohol etc. but are insoluble in water. Shake a small amount of given
sample with 5 ml each of water, alcohol and chloroform in test test tube and observe the
solubility and draw inferences.
(b) Translucent Spot Test – Press a little of the substance in folds of filter paper. On unfolding
the filter paper, the appearance of translucent or greasy spot on the filter paper indicates the
presence of fat or oil.
(c) Acrolein Test – Heat a little of the sample with some crystals of KHSO4 in a test tube. A
pungent irritating odour of acrolein confirms fat or oil presence.

(d) Baudouin Test – Substance + concentrated hydrochloric acid + few drops of furfural
solution in alcohol. Rose red colour develops on standing indicates presence of oil or fat.
(e) Huble’s Test – This test is applied to know degree of unsaturation in the given sample of oil
or fat. Take two test tubes and label them as I and II. Put in each test tube 3 ml chloroform. Add
3-4 drops of cotton seed oil in test tube no. I and linseed oil in test tube II. Shake and add 3
drops of Huble’s reagent in each test tube and observe the fading of violet colour in test tubes.
Violet colour fades in II not I, thus indicating that liquid linseed oil is more unsaturated than
cotton seed oil. Mix equal volume of 5 to 7% HgCl2 in alcohol with 5% solution of iodine in
96% alcohol to prepare Huble’s solution.
AIM: To study simple tests of carbohydrates.
REQUIREMENT:- Glucose, sucrose, lactose, starch, Molisch’s reagent, Fehling’s solution,
Benedict’s solution and iodine solution.
PROCEDURE :- (a) Molisch’s Test
All carbohydrates give this test. Take 1-2 ml of aqueous solution of carbohydrate and add few
drops of Molisch’s reagent. Put one ml of concentrated H2SO4 slowly along the side of the test
tube. A red violet ring is produced at the junction of two layers. It indicates the presen ce of
lactose, glucose, sucrose and starch.
Carbohydrate + conc. H2SO4 Purple/ Violet/ Deep blue

Alpha naphthol

(b) Fehling’s Test

Take 2 ml of aqueous solution of carbohydrate (nearly 5%) and add 1—2 ml each of Fehling’s
solution A and Fehling’s solution B. Keep the test tube in boiling water bath. Reddish
precipitate indicates the presence of a reducing sugar (lactose and glucose).

Preparation of Fehling’s Solution

Fehling’s Solution A. Dissolve 17.5 g of CuSO4 in 250 ml of distilled water containing few
drops of H2SO4.
Fehling’s Solution B. Dissolve 86.5 g of sodium potassium tartarate and 30 g NaOH in 250 ml
of distilled water.
(c) Benedict’s Test
To 1-2 ml of aqueous solution of carbohydrate in a test-tube add 1-2 ml of Benedict’s reagent.
Keep the test-tube in a boiling water bath. Reddish precipitate indicates the presence of
reducing sugar (lactose and glucose).
Preparation of Benedict’s Reagent
Dissolve 17.3 g of sodium citrate and 10 g of anhydrous Na2CO3 in about 80 ml of distilled
water.
Heat if necessary. Dissolve 1.73 g of CuSO4 in 10 ml of water. Mix the two and make the
volume 100 ml by adding water. Note. Chemistry of this test is the same as that of Fehling’s
test. Here citrate ions are used as complexing agent.

(d)
Tollen’s
Test
Take 2-3 ml of aqueous solution of carbohydrate in a test tube. Add to it 2-3 ml of Tollen’s
reagent. Keep the test tube in a boiling water bath for 10 minutes. A shining silver mirror
indicates the presence of reducing carbohydrate.

Preparation of Tollen’s Reagent

Add NaOH solution to AgNO3 solution. Then add NH4OH solution drop wise till the ppt. just
dissolve. The clear solution obtained is Tollen’s reagent. Chemistry of the test.
AgNO3 + NH4OH NH4NO3 + AgOH

(e) Iodine Test (For starch only)

To the aqueous suspension of the sample, add 1-2 drops of iodine solution.
Appearance of blue colour indicates the presence of starch.
Iodine + starch Intense blue – black colour due to formation of I3- in the coils of
starch

I2 + I- I3-

OBSERVATIONS:
Sr No. Test Glucose Lactose Sucrose Starch
1 Taste Sweet Sweet Sweet Tasteless
2 Solubility Soluble Soluble Soluble Insoluble
3 Molisch’s Purple Purple ring Purple ring Purple ring
Test ring
4 Fehling’s Test Red ppt Red ppt Negative Negative
5 Benedict’s Red ppt Red ppt Negative Negative
Test
6 Iodine Test Negative Negative Negative Blue colour
AIM:- To study some simple tests of proteins.
REQUIREMENTS:- Egg albumin dispersion, gelatin dispersion, Millon’s reagent and
Ninhydrin reagent.
PROCEDURE:-
1. Biuret Test - To the dispersion of the substance to be tested (say 5% solution of egg
albumin) add about 2 ml of NaOH solution. Now add 4-5 drops of 1% CuSO4 solution. Warm
the mixture for about five minutes. Bluish violet colour indicates the presence of protein.
Protein + CuSO4 + OH- ∆ Bluish violet complex formed
(With peptide linkage)

2. Xanthoproteic Test - Take about 2 ml of egg albumin dispersion in a test-tube and add a few
drops of cone. HNO3 and heat. A yellow colour indicates the presence of proteins.
Protein + HNO3 ∆ Bluish violet complex formed
(With peptide linkage) (concentrated)

3. Ninhydrin Test - Take about 2 ml of egg albumin dispersion in a test-tube and add 3-4 drops
of Ninhydrin solution. Boil the contents. Intense blue colour confirms the presence of proteins.
Ninhydrin solution is prepared by dissolving 0.1 g of ninhydrin in about 100 ml of distilled
water. This solution is unstable and can be kept only for two days.
Amino acid/Protein + Ninhydrin ∆ Intense blue colouration
Boil
4. Millon’s Test - This test is given by proteins containing phenolic amino acids. Gelatin does
not give this test. To 1-2 ml of egg albumin dispersion add 2 drops of Millon’s reagent. White
precipitate which changes to brick red on boiling, confirms the presence of proteins. Millon’s
reagent is prepared by dissolving 5 g each of HgNO3 and Hg(NO3)2 in 100 ml of dil. HNO3.

Dil. HNO3 Brick red precipitate

Hg
 EXPERIMENT NO. 16
AIM:- To prepare M/50 solution of oxalic acid and with its help determine the molarity and
strength of given solution of KMnO4.
REQUIREMENTS: Watch glass, analytic balance weight box, fractional weight box, glass rod,
wash bottle, conical flask, burette, pipette, oxalic acid crystals and distilled water.
PROCEDURE:-
1) Weigh 0.63 g of oxalic acid crystals and dissolve them in water to prepare 250 ml
of M/50 oxalic acid solution.
2) Rinse the pipette with M/50 oxalic acid solution and pipette out 10ml of it in a
washed conical flask.
3) Add half test tube (~10ml) full of dilute H2SO4 to solution in conical flask. Then
heat the solution to about 60 ℃ to 70 ℃ on a wire gauze, since the reaction is very
slow at room temperature.
4) Rinse and fill the burette with KMnO4 solution.
5) Note the initial reading of burette.
6) Now add KMnO4 solution from the burette till a permanent pink colour is formed in
the conical flask.
7) Note final reading of burette.
8) Repeat the procedure till the concordant readings are obtained.
 Diagram:

CHEMICAL EQUATION:-
Molecular Equation
2KMnO4 + 3H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5 [ O ]
{ (COOH)2 . 2H2O + [ O ] 60 -70 ℃ 2CO2 + 3H2O } x 5
2KMnO4 + 3H2SO4 + 5 (COOH)2 . 2H2O K2SO4 + 2MnSO4 + 18H2O + 10CO2
Ionic Equation
{ MnO4- + 8H+ + 5e- Mn2+ + 4H2O } x 2 (reduction)
{C2O42- 2CO2 + 2e-} x 5 (oxidation)
2MnO4- + 16 H+ + 5C2O42- 2Mn2+ + 8H2O(l) + 10 CO2 (g) (redox reaction)
INDICATOR :- KMnO4 is a self indicator
END POINT :- Colourless to permanent pink
Observation table:

Concordant reading: 8.4 ml of KMnO4

Calculations:

M1 x V1/M2V2 = 2/5
M KMnO4 x 8.4/10 x 1/50 = 2/5
M KMnO4 = 2/5 x 1/8.4 x 5 = 0.4 (0.02) = 0.0095 M
Strength: M x Molar mass = 0.0095 x 158
= 1.5010 g/L

Result:
1. Molarity of KMnO4 solution= 0.0095 mol/l
2. Strength of KMnO4 = 1.5 g/L

Precautions:

1. Do not overheat the solution in flask.

2. Potassium permanganate is dark, so always read the upper meniscus.
3. Rinse the pipette and burette before use.
4. Use dilute sulphuric acid for acidifying the potassium permanganate.
5. Clean all the apparatus with distilled water before starting the experiment and then
rinse with the solution to be taken in them.
6. Take accurate readings once it reaches the endpoint and doesn’t go with average
readings.
.
 EXPERIMENT No. 17
Aim: To prepare M/20 solution of ferrous ammonium sulphate and with its help determine the
molarity and strength of given solution of KMnO4.

Theory: Potassium permanganate is a strong oxidant in the presence of sulfuric acid. Mohr salt
is a double salt forming a single crystalline structure having the formula
(NH4)2SO4.FeSO4.6H2O. The chemical name for Mohr’s salt is ferrous ammonium sulphate.
In this titration Mohr salt acts as a reducing agent and potassium permanganate acts as an
oxidising agent. So, the reaction between Mohr’s salt and potassium permanganate is a redox
reaction. In this redox reaction, ferrous ion from Mohr’s salt gets oxidised and pink colour of
manganese present in potassium permanganate, which is in the +7 oxidation state gets reduced
to colourless Mn2+ state.
The chemical reaction and the molecular chemical equation is given below:
Reduction half reaction –
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O] 1)
Oxidation half reaction –
[2FeSO4.(NH4)2SO4.6H2O + H2SO4 + [O] → Fe2(SO4)3 + 2(NH4)2SO4 + 13H2O] x 5
10FeSO4.(NH4)2SO4.6H2O +5H2SO4 + 5[O] → 5Fe2(SO4)3 + 10(NH4)2SO4 +
65H2O 2)
Overall reaction – Adding equation 1) and 2)
2KMnO4 + 10FeSO4(NH4)2SO4.6H2O+ 8H2SO4 → K2SO4+ 2MnSO4+
5Fe2(SO4)3+ 10(NH4)2SO4+
68H2O
The ionic equation involved in the process is given below.
Oxidation half reaction – [Fe2+ → Fe3+ + e–] x 5
Reduction half reaction – MnO4– + 8H+ + 5e– → Mn2+ + 4H2O
Overall ionic equation – MnO4– + 8H+ + 5Fe2+ → Mn2+ + 5Fe3+ + 4H2O
This titration is based upon oxidation-reduction titrations. When ferrous ammonium sulfate
solution is titrated against potassium permanganate in the presence of acidic medium by sulfuric
acid. Acidic medium is necessary in order
to prevent precipitation of manganese oxide. Here KMnO4 acts as a self indicator and this
titration is called permanganate titration.

Materials Required:

1. Mohr’s salt (ferrous ammonium sulfate)

2. Potassium permanganate solution
3. Dilute sulfuric acid
4. Chemical balance
5. Burette
6. Burette stand
7. Pipette
8. Conical flask
9. Funnel
10. Measuring flask
11. Weighing cylinder
12. White tile
13. Burner
14. Wire gauze

Apparatus Setup:
1. In burette – KMnO4 solution
2. In Conical flask – 10ml of Ferrous Ammonium Sulfate (Mohr’s salt) + Sulfuric acid
3. Indicator – Self indicator (KMnO4)
4. End Point – Colourless to permanent pale pink colour.
(b) Titration of potassium permanganate solution against standard
ferrous ammonium sulphate (Mohr’s salt) solution:
1. Wash and rinse the burette and pipette with distilled water and then rinse
with the corresponding solution to be filled in them.
2. Rinse the burette with the potassium permanganate solution and fill the
burette with potassium permanganate solution.
3. Fix the burette in the burette stand and place the white tile below the
burette in order to find the endpoint correctly.
4. Rinse the pipette and conical flask with standard ferrous sulphate solution.
5. Pipette out 10ml of 0.05M standard Mohr’s salt solution into the conical
flask.
6. Add a half test tube of sulphuric acid in order to prevent oxidation of
manganese to form manganese dioxide.
7. Note down the initial reading in the burette before starting the titration.
8. Now start the titration, titrate against potassium permanganate solution and
simultaneously swirl the solution in the flask gently.
9. Initially, the purple colour of KMnO4 is discharged with ferrous
ammonium sulphate. The appearance of a permanent pink colour reveals the
endpoint.
10. Repeat the above steps till the concordant readings are obtained.
11. Note down the upper meniscus on the burette readings.
12. Record the reading in the observation table given below in order to
calculate the molarity of KMnO4 given.
 Observation table:

Concordant reading: 9.8 ml of KMnO4

Calculations:
MKMnO4 x VKMnO4 / MMohr’s salt = MKMnO4 x 9.8/ 0.05x 10 = 2/10
MKMnO4 = 0.01 M
Strength g/L = MKMnO4 x mol. Mass
= 0.01x 158
= 1.58 g/L
Preparation of M/20 Mohr’s salt solution:
Strength g/L = Molarity x Molar mass x Volume (L)
= 1/20 X 392 X 250/1000
= 4.9 gm in 250 ml of water
Result:
1. Molarity of KMnO4 solution = 0.01 M
2. Strength of KMnO4 solution = 1.58 g/L
Precautions:
1. Potassium permanganate is dark, so always read the upper meniscus.
2. Rinse the pipette and burette before use.
3. Use dilute sulphuric acid for acidifying the potassium permanganate
 EXPERIMENT NO. 18
AIM:-To analyse the given salt for acidic and basic radicals.

Requirements:
Apparatus: Small conical funnel, small beakers, small test tubes with test tube stand, test tube
holder, evaporating dish.
Chemicals: Given salt, common laboratory reagents.

Procedure:

Experiment Observation Inference

1. Preliminary tests for
cations:
(a) Noted the colour of the White Cu2+, Fe2+, Fe3+, Ni2+,
given salt. Mn2+, Co2+ absent.
Al3+, Ba2+, Sr2+, Ca2+,
NH4+, Zn2+, Mg2+, Pb2+
may be present.

(b) Mixture + water a) Crystalline (water Nitrates, sulphates and

soluble) halides of NH4+, Al3+,Cu2+
etc. may be present.

b) Amorphous (Insoluble Water insoluble salts like

in water) sulphides, carbonates etc.
may be present.

c) Hygroscopic Chlorides or nitrates of

(Deliquescent) (Salts Cu2+, Ni2+, Co2+, Mg2+,
absorbing moisture from Ca2+, Zn2+, Fe3+, may be
atmosphere) present.
Dry tests for cations:
2. Dry heating test:
Heated a pinch of the salt a) White sublimate NH4+ may be present.
in a dry test tube and
noted the following b) Decripitation Pb(NO3)2 may be present.
observations: (crackling sound)

c) White residue Pb2+, Al3+, Zn2+, Ca2+,

Sr2+, Ba2+, Mg2+ may be
present.

d) Coloured residue Cu2+, Co2+, Ni2+, Mn2+,

Fe3+ may be present.
 e) Residue yellow when Zn2+may be present.
hot and white when cold.

f) Evolution of gas
1) gas with NH3 smell NH4+ may be present.

2) yellowish green gas Salts of chloride may be

present.
3) brown gas Salts of bromide, nitrate,
nitrite may be present.
4) violet gas Salts of iodide may be
present.
3. Charcoal cavity test:
Mixed a pinch of the salt a) Red scales. Cu2+ may be present.
with double the quantity
of Na2CO3 on a piece of b) Incrustation
paper. Place it in a i) Yellow incrustation Pb2+ may be present.
charcoal cavity and add a forming metallic bond.
drop of water to it. Heat it ii) white fumes and NH4+ may be present.
in a yellow reducing white incrustation.
flame using a blow pipe c) Decripitation Pb2+ may be present.
(for 1-2 minutes). d) Residue
Observe the changes. i) yellow when hot and Zn2+ may be present.
white when cold.
ii) Coloured residue Cu2+, Co2+, Ni2+, Mn2+,
Fe3+ may be present.

iii) white infusible

residue. (Do not throw Al3+, Ca2+, Sr2+, Ba2+,
the charcoal and use it Mg2+ may be present.
to perform cobalt
nitrate test)

4. Cobalt nitrate test:

If white residue is a) Blue residue Al3+ may be present.
obtained in charcoal b) Pink residue Mg2+ may be present.
cavity test, add 2 drops of c) Green residue Zn2+ may be present.
cobalt nitrate solution to d) Grey residue Ca2+,Ba2+ may be present.
the white residue and heat e) Black or any other Al3+, Mg2+, Zn2+ may be
it in blue flame using coloured residue present.
blow pipe. Observe the
colour of residue.
5. Flame test: a) Bluish green Cu2+ may be present.
Clean a platinum wire b) Apple green Ba2+ may be present.
with concentrated HCl. c) Brick red Ca2+ may be present.
Moisten a small quantity d) Crimson Sr2+may be present.
of a mixture with e) Bluish white Pb2+ may be present.
concentrated HCl on a f) No distinct colour Cu2+ , Ba2+ , Ca2+ , Sr2+ ,
watch glass. Dip the Pb2+ may be present.
cleaned platinum wire in
it and heat it in oxidising
(blue) flame. Observe the
colour of the flame.
6. NaOH test for NH4+:
a) Mixture + 1 ml NaOH. Smell of NH3, vapours NH4+ may be present.
Shake and warm. Smell turning moist turmeric
carefully. paper brown.
b) Mixture + 1 ml NaOH.
Shake well and warm.
Hold moist turmeric paper
over the mouth of the test
tube. Papers turn brown. NH4+ may be present.
Wet tests and
confirmatory tests for
cations:
7. Preparation of
original solution (O.S.):
Shake a pinch of the salt Solution obtained Labelled it as original
with water. solution (O.S.)
8. To a part of the O.S. Group I present. (Pb2+
added 1-2 ml of dilute White ppt. formed. present)
hydrochloric acid.
9. Confirmatory test for
Lead ion (Pb2+):
Filtered the above white
ppt + water, boil till ppt
dissolves
a) Solution + KI Yellow ppt Pb2+ confirmed
b) Solution + K2CrO4 Yellow ppt Pb2+ confirmed
c) Solution + dil.
H2SO4. Yellow ppt Pb2+ confirmed

10. Through a part of the a) Black ppt. formed. Group II present – Pb2+ or
above solution (in point Cu2+ may be present
8), passed H2S gas. b) Yellow ppt. formed. Group II present – As3+
may be present.
11. Confirmatory test
for Arsenic ion (As3+):
a) Filtered the above
yellow ppt + water +
ammonium molybdate +
heat. Yellow ppt not formed. As3+ absent.
b) Solution + NH4OH till
alkaline + magnesia
mixture. White ppt not formed. As3+ absent.

12. To the remaining

solution, added a pinch of
solid ammoniumchloride. a) Reddish brown ppt Group IIIA present – Fe3+
Boiled the solution, may be present.
cooled it and added b) White gelatinous ppt Group IIIA present – Al3+
excess of ammonium may be present.
hydroxide
(NH4OH)solution
13. Through a part of a) White ppt Group IIIB present – Zn2+
above solution (in point may be present.
10), passed H2S gas. b) Black ppt Group IIIB present – Ni2+
or Co2+ may be present.
c) Buff Group IIIB present –
Mn2+ may be present.
14. Confirmatory test
for Zinc ion (Zn2+):
Dissolve the white ppt I
dilute HCl. Boil the
solution to expel H2S gas.
Use thus solution for
confirmatory test of zinc
ion:
a) Solution + NaOH White ppt soluble in Zn2+ confirmed.
excess of NaOH but
reprecipitated by H2S gas.

b) Solution + K4Fe(CN)6. White or bluish white ppt. Zn2+ confirmed.

15. To the remaining

ammoniacal solution (in Group IV present.
point 10) added White ppt. formed. (Ca2+, Ba2+, Sr2+ may be
ammonium carbonate present)
{(NH4)2CO3}solution.
16. Confirmatory test
for Barium ion:
Filtered the above white
ppt.
Dissolved the ppt. in hot
dilute acetic acid.
(a) Solution + dilute
sulphuric acid. White ppt. Ba2+ confirmed.
(b) Solution + ammonium
acetate. White ppt. Ba2+ confirmed.
17. Confirmatory test
for Calcium ion:
Solution + NH4OH + White ppt Ca2+ confirmed
(NH4)2C2O4

18. To the remaining

ammoniacal solution (in
point 10) added disodium White ppt. formed. Group V present.
hydrogen phosphate (Mg2+ may be
solution. present)
19. Confirmatory test
for Magnesium ion
(Mg2+):
Solution + hypoiodide
reagent (Hypoiodide
reagent: NaOH + equal Reddish brown ppt. Mg2+ confirmed.
volume of KI + iodine
solution dropwise till the
solution becomes just
yellow)
20. Dissolve 0.5g of the Evolution of NH3 gas NH4+ present.
mixture in 5 ml of water turning moist turmeric
in small beaker + NaOH. paper brown.
Heat and test with moist
turmeric paper.
Confirmatory test for
Ammonium ion (NH4+):
a) Dissolve 0.5g of the
mixture in 5 ml of water
in small beaker +
Nessler’s reagent. Brown ppt. NH4+ confirmed.
b) Dissolve 0.5g of the
mixture in 5 ml of water
in small beaker + picric Brown ppt. NH4+ confirmed.
acid.
20. Preliminary tests for
anions:
a) Nature Crystalline NO3-,Cl-, Br-, I-, CH3COO-
,CO32-, NO2-, SO42-, NO3-
may be present.
b) Solubility in water Soluble in water NO3-, Cl-, Br-, I-, CO32-,
SO42- may be present.

c) Heating in a dry test

tube: Take a small i) Odourless, colourless, CO32-, C2O42- may be
quantity of a mixture in a gas turns which tuns lime present.
clean, dry test tube and water milky.
heat it in an oxidising ii) Coloured gases
flame for 2-3 minutes. evolved:
Observe the gas evolved. a) Reddish brown gas NO3-, NO2- may be
which turns ferrous present.
sulphate solution dark
brown.
b) Greenish yellow gas
which bleaches moist Cl- may be present.
litmus paper.
c) Reddish brown fumes
which turns starch Br- may be present.
solution orange yellow.
d) Dark violet fumes and
turns starch iodide I- may be present.
solution blue.
iii) Colourless gas with
odour:
a) Vinegar smell CH3COO- may be present.

b) Suffocating smell
turning acidified SO32- may be present.
potassium dichromate
solution green.

c) Smell of rotten egg

which turns lead acetate S2- may be present.
solution black.
Dry tests for anions:
21. Dilute sulphuric acid a) Brisk effervescence
test: Treat a pinch of the with colourless gas (CO2)
salt with dil. H2SO4, and which turns lime water CO32-may be present.
warmed. milky.
b) Colourless gas with
smell of rotten eggs(H2S) S2- may be present.
which turns lead acetate
solution black.
c) Reddish brown gas
(NO2) which turns ferrous NO2- may be present.
sulphate solution black.

d) Colourless gas (SO2)

having suffocating smell SO32- may be present.
which turns acidified
potassium dichromate
solution green.
22. Concentrated
sulphuric acid test:
Heated a pinch of the salt a) A reddish brown gas
with concentrated evolved which turned NO3- may be present.
sulphuric acid FeSO4, solution black.

b) Greenish yellow gas

which turns blue litmus Cl- may be present.
paper red and then
bleaches it.

c) Reddish brown gas

which turns starch paper Br- may be present.
orange yellow.

d) Deep violet vapours I- may be present.

e) Colourless vapours
with smell of vinegar and CH3COO- may be present.
turns blue litmus red.

f) Colourless gas which

turns lime water milky C2O42- may be present.
(due to evolution of CO2
+ CO)
Wet tests for anions:
23.Dissolve given mixture
in water to prepare
original solution.

a) Original solution + a) White ppt soluble in

AgNO3 dilute HNO3 with CO32- present.
effervescence.

b) Curdy white ppt

soluble in NH4OH. Cl- present.

c) Pale yellow ppt

sparingly soluble in Br- present.
NH4OH.

d) Yellow ppt insoluble in I- present.

NH4OH.

e) Black ppt soluble in

dilute HNO3 with smell of S2- present.
rotten eggs.

b) Distinction between
Cl- , Br- , I- :
(Perform only if Cl- , Br-
, I- are detected in
previous test) a) Colourless layer of Cl- present.(if detected
Original solution + dilute chloroform. earlier)
sulphuric acid till solution
becomes acidic + b) Yellow layer of Br- present. (if detected
chloroform + chlorine chloroform. earlier)
water. Shake vigorously
and observe the lower c) Violet layer of I- present. (if detected
layer of chloroform. chloroform. earlier)

24. Confirmatory test

for nitrate ion (NO3-):
(a) Copper chips test:
Heated a pinch of the salt Reddish brown gas NO3- confirmed.
with concentrated evolved.
sulphuric acid and a few
copper chips.
(b) Ring test: To 2-3 ml of
the salt solution, added
freshly prepared FeSO4 A dark brown ring formed NO3- confirmed.
solution. Now add at the junction of the two
concentrated sulphuric liquids.
acid along the sides of the
test tube.
25. Confirmatory test for
carbonate ion (CO32-):
(a) Given mixture + water Effervescence of CO2
+ dil. HCl. which turns lime water CO32- confirmed.
milky.
(b) Given mixture + water
+ MgSO4 White ppt CO32- confirmed.

c) Given mixture + water

+ Phenolphthalein Pink colouration. CO32- confirmed.
indicator

26. Confirmatory test

for chloride ion (Cl-):
a) Given mixture + White ppt soluble in Cl- confirmed
water + AgNO3 NH4OH

b) Given mixture + Yellowish green gas Cl- confirmed

water + MnO2 + which turns moist starch
concentrated H2SO4 iodide paper blue.

c) Chromyl chloride
test: Dry mixture + Red vapours or red liquid Cl- confirmed
crystals of K2Cr2O7
(potassium
dichromate) +
concentrated H2SO4
+ heat.

d) Given mixture + White ppt soluble in hot Cl- confirmed

water + lead acetate water
27.Confirmatory test for
sulphide ion (S2-):
(a) Given mixture + water Purple or violet
+ sodium nitroprusside colouration. S2- confirmed.
solution
(b) Given mixture + water
+ CH3COOH + lead Black ppt S2- confirmed.
acetate

c) Given mixture + water Yellow ppt S2- confirmed.

+ cadmium nitrate in
water
28. Mixture + dil. HCl + White ppt insoluble in SO42- present.
boil + filter. Filtrate + concentrated HCl.
BaCl2 solution.
Confirmatory test for
sulphate ion (SO42-):
(a) Given mixture + acetic
acid + lead acetate White ppt SO42- confirmed.

29. Acidifying a small Bright yellow precipitate

amount of the sample with layer of ammonium PO4 3-confirmed
concentrated nitric acid phosphomolybdate
Adding a little ammonium
molybdate

RESULT: The following acidic and basic radicals were found in the given mixtures:
Acidic radicals: NO3-, Cl-, SO42- , S2- and CO32- .
Basic radicals: Ba2+, Ca2+, NH4+, Zn2+ and Pb2+.