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NIOS CLASS 12TH Chemistry (313)


Written by Manish Verma
Solved Practical
Where every problem is solved of nios.

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CERTIFICATE

This is to certify that ……………………… a student of class 12th has


successfully completed the research on the below practical under the
guidance of ………………………… (teacher name) during the year
.................. in partial fulfilment of Chemistry practical exam conducted by
NIOS, new Delhi,

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ACKNOWLEDGEMENT

I Would like to convey my heartfelt thanks to……………..., who always


gave valuable suggestion and guidance for completion of my practical.
she/he helped me and to understand and remember important details of
the project. She/he helped me and gave her/his guidance in completing
of my practical successfully.

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Index
1. To Determine Cut and bend glass rods/tubes.

2. To determine the melting point of the given solid substance.

3. To prepare a sol of

a) Starch
b) Ferric hydroxide
c) Aluminium hydroxide

4. To prepare crystals of

a) Ferrous ammonium sulphate (Mohr salt), FeSO4.(NH4)2SO4.6H2O.


b) Potash alum K2SO4.Al2(SO4)3.24H2O
c) Potassium ferric oxalate K3[Fe(C2O4)3].3H2O.

5. Preparations of

a) Iodoform
b) Acetanilide

6. To study the variation of cell potential in Zn/Zn2+ || Cu2+/Cu with change in


concentration of electrolytes (CuSO4 or ZnSO4) at room temperature.

7. To find out the Molarity of given NaOH solution by titrating against M/10 solution of
oxalic acid. Both the solutions to be provided.

8. To identify the cationic radicals present in an inorganic mixture of salts by


performing various tests.

9. Anions To identify the anionic radicals present in an inorganic mixture of salts by


performing various tests.

10. (a) To Identify the Functional Groups present in the given organic compounds
and perform:

10.(b) To identify the presence of a phenolic functional group in a given organic


compound.

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Experiment - 1

Objective

 Basic laboratory Techniques

 Cut and bend glass rods/tubes

 Bore rubber cork

 Perform simple laboratory operations such as filtration, crystallisation and


distillation

Aim
To Determine Cut and bend glass rods/tubes.

Materials Required
Glass tube / rod, ruler, small triangular file, gas burner/ spirit lamp.

Diagram

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Procedure

 Place the rod or glass tube on the table.

 Mark the glass tube or rod with triangular file keeping.

 Keep the triangular file perpendicular to the rod or tube and pull it towards you so
that a single deep scratch is made.

 Hold the glass rod or tube with the help of your thumbs.

 Now apply pressure in the direction away from you and try breaking the glass rod
or tube.

 If you see any jagged edge, Trim it by striking with a wire gauge.

Precautions

 The file should be moved always in backward down direction.


 If difficulty is experienced in breaking the glass tube or rod, put another scratch on the
point.

Aim
To Determine Bore rubber cork.

Material Required
Glass tube, burner, file, and asbestos sheet.

Diagram

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Procedure

 Hold the tube with both the hands horizontally, in flame from the Bunsen burner.
 Get the point of bending of the glass with flame.
 Keep rotating the glass tube with the help of thumbs and fingers while heating so
that the tube is heated and softened uniformly.
 Determine in which direction you want to bend the glass tube.
 Continuously keep the glass tube in the flame till it becomes red hot.

Precautions

Do not touch the bent portion of the tube with fingers until it is cooled.

Filtration

Aim
In filtration, insoluble small solid particles/dust/ impurities etc. are separated from
liquids by passing the mixture through filter paper.

Materials Required
Funnel, glass rod, beaker, filter paper, sugar solution with small amount of sand.

Diagram

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Precautions

 Do not transfer all the mixture to the filter funnel at one time,
 The filter paper should be smaller in size than funnel.
 The mixture level should never be above 3/4th of the height of the filter paper,
 The lower end of the funnel should just touch the inside wall of the beaker.

DISTILLATION

Aim
Distillation is used to purify liquids such as water and organic solvents, and/or
recycling used solvents.

Materials Required
Conical flask / round bottomed flask, condenser, thermometer, beaker, heating mantle and
oil bath.

Diagram

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Precautions

 Slowly increase heating rate.


 Do not open the round bottom flask during heating
 Stop distillation when a small amount of liquid is still left in the flask. Do not
evaporate to dryness.
 Punice stones should be added in the beginning itself.

Crystallization

Aim
Crystallization is a process of obtaining crystals of a pure substance from a solution
which may contain some impurities.

Materials Required
50 mL capacity Beaker, filtration unit, watch glass, kerosene burner and CuSO4.5H20

Diagram

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Procedure

 To this solution add 2 drops of H2SO4.


 Heat the solution for a while and filter it using a filtration unit.
 Transfer the solution from the filtration unit to another beaker and allow it to cool
down to room temperature.
 Formation of the crystals is witnessed.
 Filter and wash these crystals and allow them to dry.

Precautions

 Avoid overheating of the solution.

 The filtrate should be evaporated slowly by gentle heating of the solution.

 The solution should be cooled slowly and do not use any rapid cooling
procedures.

Viva Questions

1. Define the term ‘crystallisation’.

Ans. The substances when present in well-defined geometrical shapes are called
crystals. These are formed when a hot saturated solution of the salt is allowed to
cool slowly and undisturbed. This process is termed as crystallisation.

2. What is solubility ?

Ans. It is the amount of the solute which when dissolved in 100 gms of the solvent
provides a saturated solution.

3. Why is crystallisation done?


Ans. Crystallisation enables to prepare a substance in state of highest purity.

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4. What is Kipp’s waste?


Ans. It is a’ mixture left behind after production of H2S gas by reaction between FeS
and dilute H2S04. It mainly contains FeS04 and unreacted dilute H2S04.

5. What is meant by the term, ‘water of crystallisation’?


Ans. Water of crystallisation is the definite number of water molecules that is present
in lose combination with one formula unit of the compound.

6. Explain the term—saturated solution.


Ans. A solution in which no more of solute can be dissolved at a particular
temperature is known as saturated solution.

7. Why glass does not possess a sharp melting point?

Glass is an amorphous solid crystalline structure having tightly packed molecules.


Hence Glass does not possess a sharp melting point.

8. Why is it required to round off the freshly cut edges of the glass tube or the
glass rod?

The jagged edges might cause injury while handling, hence for safety and to give
good look with a smooth finish, the edges of the glass tube or rod are rounded off.

9. Why is a glass tube rotated while heating on a burner?

To ensure the uniform heating glass tube is rotated while heating.

10. Which type of glass softens easily?

Soda-lime glass

11. Mention the various steps which are involved in the cutting of a glass tube.

 Scratching

 Breaking

 Heating the cut edges

 Cooling

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Experiment – 2

Aim
To determine the melting point of the given solid substance.

Materials required
Beaker (100 mL). Thermometer, Glass capillary tube (5-6 cm long), Burner, Iron
stand, Clamp and boss, Tripod-stand, Wire gauze, Stirrer, Spatula. Glass tube (25-
30 cm), Watch glass, Cork with one bore.

Diagram

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Procedure

 Take a glass capillary tube of about 5-6 cm in length and seal one end of it. This
is done by heating the tip of tube with the side of the flame of the Bunsen burner.
The end of the capillary tube melts and seals itself. It is indicated by the formation
of a small glass bead at the tip.
 Take a small quantity of a solid (about 50 mg) in watch glass, powder it by
crushing it with the help of a spatula.
 Fill the powdered substance in the capillary tube up to about 1 cm height. This is
done by pushing the open-end of the capillary tube into the heap of powdered
substance kept in a watch glass.
 Take a beaker of 100mL capacity. Fill it nearly half with paraffin oil. Place this
beaker (paraffin bath) over a wire gauze kept on a tripod stand.
 Heat the paraffin bath slowly with a burner and keep stirring the oil so as to
maintain a uniform temperature.
 Remove the burner and allow the temperature to come down. Note the
temperature (t2 ) at which the solid just reappears.
 The average of the readings (t1+ t2 ) is the correct melting point.

Observations
Temperature at which the substance begins to melt (t 1) = 80°C

Temperature at which the substance resolidifies (t 2) = 80°C

Melting point ( ) = 80°C

Melting Points of Some Organic Compounds

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Precautions
 Use dry and powdered sample for the determination of melting point.
 Keep the lower end of the capillary tube and the thermometer at the same level.
 Packing of the powder should be uniform without any big air gaps in between the
solid particles.
 Heating should be gradual and the bath should be stirred regularly to maintain
uniform temperature.
 The bulb of the thermometer and the capillary sticking to it should not touch the
side or the bottom of the beaker.

Conclusion
 The melting point of the given substance is 80°C.
 The melting point of the substance is sharp / not sharp. Hence the substance is
of a pure / impure quality.

Viva Questions
1. Define melting point.
Ans. It is defined as the constant temperature at which the solid and the liquid
phases of substance coexist.

2. How is the determination of melting point useful?


Ans. It helps us to :
(i) identify unknown substances ;
(ii) know whether a compound is pure or not.
3. How does the determination of melting point help us know about the purity
of the compound?
Ans. Melting point indicates the purity of a substance. If a substance contains
moisture or some other impurity, then its melting point is usually lowered. A sharp
melting point indicates a pure substance.
4. What is sharp melting point?
Ans. Melting point of a solid is said to be sharp if it melts completely within a range of
1°C.

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5. Why do pure solids possess sharp melting point?


Ans. A pure solid has same force of attraction between particles at different places
and hence melts at a constant temperature.
6. What is the effect of impurities on the melting point of solids?
Ans. Impurities lower the melting point of a solid.
7. Can we heat the capillary tube directly for the determination of melting
point?
Ans. No, because direct heating would result in uneven and fast heating.
8. Can any other liquid be used in place of liquid paraffin to determine the
melting point?
Ans. Yes, concentrated H2S04 or silicone oils can be used to determine the melting
point.
9. Why is the melting point of benzamide more than that of acetamide?
Ans. Benzamide and acetamide contain same functional group, but the molecular
mass of benzamide is more than that of acetamide. As a result benzamide has
stronger intermolecular forces and hence has higher melting point.
10. Why different solids have different melting points?
Ans. Melting point depends upon intermolecular forces existing in the solid state.
Since different solids have intermolecular forces of different strength, their melting
points are different.

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Experiment – 3

Aim

To prepare a sol of

a) Starch
b) Ferric hydroxide
c) Aluminium hydroxide

Materials required
Apparatus Required

Tripod stand, Burner, Beaker, Glass rod, a round bottomed flask, funnel, 250 ml.
conical flask, glass tubing, rubber stoppers, clamp stand, burner, wire gauge, tripod
stand, a boiling tube.

Chemical Required

Starch (about 1 g), Ferric chloride, 2% AlCl3 solution and distilled water.

Procedure Starch

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Procedure Ferric Hydroxide

Procedure Aluminium Hydroxide

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Precautions

 The starch powder should not be added directly to boiling water. Instead, a thin
paste should be prepared and added.
 The contents of the beaker should be cooled down to room temperature before
filtration.
 The apparatus must be cleaned before use.
 The separation of HCl (dialysis) must be carried out immediately after the
preparation of the colloidal sol.
 FeCl3 solution should be added dropwise into the boiling water.
 After the addition is complete, stir the mixture for at least five minutes more,
 Allow the solution in the beaker to cool ‘down to room temperature and then filter,
the filtrate is the sol. of gum.
 Test the sol by throwing beam of light from a torch or an electric bulb with a slit
placed in front of it. The path of the beam of light is visible.

Observations
1. Colloidal sol of starch is formed.
2. Colloidal sol of ferric hydroxide is formed.
3. Colloidal sol of aluminium hydroxide is formed.

Conclusion
Starch forms a stable hydrophilic sol. Ferric hydroxide and aluminium hydroxide forms a
hydrophobic sol.

Viva Questions
1. What is starch mixed with?

Ans Distilled water.

2. The starch and distilled water are heated to what temperature?

Ans: 100° C.

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3. How much amount of distilled water is taken to prepare 500 mg of starch


sol?

Ans: 100 mL

4. Pour the paste into cold distilled water before boiling. True or false?

Ans: False.

5. Constantly keep stirring the water in the beaker while adding the paste. True
or false?

Ans: True.

6. How to prepare 2% Aluminium chloride solution?

Ans: Mix 2 g of Aluminium chloride in 100 mL of distilled water.

7. Why is it important to clean the apparatus by steaming out the process?

Ans: Aluminium hydroxide sol gets affected due to the presence of ionic impurities.
Therefore, the apparatus is steam cleaned before performing the experiment.

8. Boil the mixture of Aluminium chloride solution and distilled water until it
attains _______ colour.

Ans: White colour.

9. Hydrolysis of Aluminium chloride results in ________.

Ans: Hydrochloric acid.

10. What is the quantity of Aluminium chloride solution added to 100 mL


distilled water?

Ans: 10 mL.

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Experiment – 4

Aim

To prepare crystals of

a) Ferrous ammonium sulphate (Mohr salt), FeSO 4.(NH4)2SO4.6H2O.


b) Potash alum K2SO4.Al2(SO4)3.24H2O
c) Potassium ferric oxalate K3[Fe(C2O4)3].3H2O.

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)

Potash alum is a double salt of assium sulphate and aluminium sulphate, hence it is
prepared by taking the amount of K2SO4 and Al2(SO4)3.18H2O in the ratio of their
molecular masses, preparing their concentrated solutions.

K2SO4 + Al2(SO4)3.18H2O + 6H2O → K2SO4.Al2(SO4)3.24H2O

Potassium ferric oxalate is an inorganic complex which dissociates in a suitable solvent to


give simple potassium (K+) and the complex ferric oxalate, [Fe(C2O4)3] 3– ions.

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Materials Required

Conical flask, Tripod stand, Burner, Funnel, watch glass, Glass rod, Filter paper,
Wire gauze, China dish, Ferrous sulphate, Ammonium sulphate, Dilute sulphuric
acid, Oxalic acid hydrate, Ferric chloride, Potassium oxalate, Potassium hydroxide.

Procedure

(a) Preparation of crystals of Ferrous ammonium sulphate (Mohr salt),


FeSO4.(NH4)2SO4.6H2O.

 Weigh 10 g of ferrous sulphate crystals and 5 g of ammonium sulphate crystals


on two separate pieces of paper on a rough balance.
 Transfer the amounts thus weighed into a 250 ml beaker.
 Boil about 20-30 ml of distilled water in the second beaker for about 5 minutes to
remove the dissolved air (as otherwise, it may oxidize ferrous sulphate to ferric
sulphate in presence of sulphuric acid),

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(b) Preparation of crystals of Potash alum K2SO4. Al2(SO4)3.24H2O

 Take about 3 g of potassium sulphate crystals in a 250 ml beaker. Add about 25


ml of distilled water. Stir with a glass rod to dis-solve the salt. Heat if necessary.
 Take about 12 g of aluminium sulphate crystals in another beaker. Add about 25
ml of distilled water and a few drops of dil. sulphuric acid (to prevent the
hydrolysis of aluminium sulphate). Stir with a glass rod to dissolve the salt. Heat if
necessary. Filter if the solution is not clear.
 Mix the two solutions by transferring them into a China dish. Heat the China dish
gently on a water bath to concentrate the solution up to the crystallization point

(c) Preparation of crystals of Potassium ferric oxalate K3[Fe(C2O4)3].3H2O.


Preparation of ferrous oxalate, Fe(C2O4).2H2O

 Dissolve 5.5 g of Mohr’s salt (ferrous ammonium sulphate),


Fe(NH4)2(SO4)26H2O, in 17 ml of warm water in 250 ml.
 Add a few drops of (4 M) sulphuric acid to the solution necessary for complete
dissolution of Mohr’s salt to avoid hydrolysis of ferrous ion in water.
 In another 250 ml beaker dissolve about 3g of oxalic acid in 30 ml of water to
prepare 30 ml of oxalic acid solution.
 Add 30 ml of oxalic acid solution to the ferrous sulphate solution.
 Heat the mixed solution to boiling with ion continuous stirring.

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Precautions

 To avoid oxidation of fer-n sulphate boiled water (containing no dis-solved air)


should be used to make the solution.

 Dilute sulphuric acid must be added immediately after adding water into the
mixture of the salts. Sulphuric acid prevents hydrolysis of FeSO 4

 The solution should not be heated beyond the crystallization point otherwise a
solid mass will be formed.

 The solution should not be disturbed while being cooled for crystallization. A
slight disturbance may curie change in the shape and yield of the crystals.

 Cover the China dish while cooling the concentrated solution.

 The solution should be kept undisturbed for crystallization.

 The solution should not be concentrated beyond the crystallization point.

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Observations
Yield 12g

Theoretical value 12g

Conclusion
Crystals of Ferrous ammonium sulphate (Mohr salt), FeSO 4.(NH4)2SO4.6H2O =
12.5g

Crystals of Potash alum K2SO4.Al2(SO4)3.24H2O = 12g

Crystals of Potassium ferric oxalate = 11.8g

Viva Questions
1. What are double salts? Give two examples.

Ans A combination of two different salts taken together as a single substance in a


definite molecular proportion is known as double salt.

Eg:- Mohr’s salt and potash alum.

2. What is the oxidation state of Fe in Mohr’s salt?

Ans Iron has a +2-oxidation state in Mohr’s salt.

3. If a saturated solution is evaporated quickly then what will happen?

Ans We will not get pure and good crystals.

4. What will happen when concentrated sulphuric acid is added instead of


dilute sulphuric acid?

Ans Concentrated sulphuric acid will oxidize Fe2+ to Fe3+

5. What is the difference between double salt and complex salt?

Ans Double salt is simple salt which dissociates in aqueous solutions. Complex salt
may or may not be simple but does not dissociate in aqueous solution.

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6. What is the colour of Potassium ferric oxalate and what is its melting point?

Ans The colour of Potassium ferric oxalate is green and its melting point is 230 oC.

7. Write the chemical reaction for the reaction of ferric chloride with potassium
hydroxide.

Ans FeCl3 + 3KOH → Fe(OH)3 + 3KCl

8. Define crystallisation?

Ans Crystallisation is the process through which a solid form is formed, where the
atoms or molecules are highly organised into a structure called a crystal.

9. What is called “seeding”?

Ans In some cases, crystallisation does not occur, if the crystal of the same
substance is added to the saturated solution, then it induces crystallisation. This is
called seeding.

10. Give the relation between specific conductivity and resistance of a


solution?

Ans The relation is, Specific conductance = Cell constant x (1/Resistance)

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Experiment – 5

Aim

Preparations of

a) Iodoform
b) Acetanilide

Materials required

Distilled water, round bottom flask, Beaker, Pipette, Reflux condenser, Funnel,
Stirrer, Bunsen Burner, Filter paper, electronic balance.

Chemicals required

Propanol or ethanol, Iodine, Sodium hydroxide, Aniline, Glacial acetic acid, Acetic
anhydride, Zinc dust.

Theory

Iodoform (CHI3) is the iodine analogue of chloroform. It is a pale yellow crystalline solid
(m.p.119°C), having a characteristic odour. It is used as a mild antiseptic and
disinfectant. It is also used in the preparation of many medicinal ointments used as
pain-relievers.

iodoform can be prepared by treating any organic compound containing CH 3CH(OH)-


group (e.g., ethanol, 2-propanol, 2-butanol) or CH3CO– group (e.g., propanone, 2-
butanone) with iodine in presence of sodium hydroxide. In the laboratory, it is usually
prepared from either ethanol or propanone. The chemical reactions involved are:

(a) With ethanol

2NaOH + I2 → NaOI + NaI + H2O

CH3CH2OH + NaOI → CH3CHO + NaI + H2O

CH3CHO + 3NaOI → I3CCHO + 3NaOH

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I3CCHO + NaOH → CHI3 + HCOONa

(b) With Propane

CH3COCH + 3NaOI → CH3COCI3 + 3NaOH

CH3COCI3 + NaOH → CHI3 + CH3COONa

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.

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Diagram

Procedure
Preparation of iodoform

 Dissolve 5 g of iodine in 5 ml propane or ethanol in a 100 ml conical flask or round


bottomed (R.B.) flask.
 Add 5% NaOH solution in small portions while continuously shaking the flask. Cool
the flask from time to time under tap water. The addition of NaOH solution is further
continued till the brown colour of iodine just disappears.
 Allow the flask to stand for 5-10 minutes.
 Decant off the clear supernatant liquid.
 Filter the iodoform, wash with little cold water and then dry on a filter paper.

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Crystallization of iodoform

 Place the crude iodoform in a 100 ml conical flask.


 Add small amount of rectified spirit and heat it on a water bath.
 Add more rectified spirit slowly till the iodoform dissolves.

Preparation of acetanilide

 Take a 100 ml clean and dry R.B. flask and pour 5 ml of aniline into it followed by
5 ml of acetic anhydride and 5 ml of glacial acetic acid. Also add about 0.1 g of
zinc dust and a few boiling chips.
 Attach a reflux condenser to the flask and heat the reaction mixture gently on a
sand bath for about.
 Remove the flask and pour the hot liquid in a thin stream into 125 ml of cold
water with continuous stirring.
 Cool the flask in ice and filter the crude acetanilide at the suction pump using a
Buchner funnel.
 Wash the crude solid with little cold water and dry upon filter paper in the air.

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Observations

Yield of Iodoform 5g

Yield of acetanilide 14.5g

Conclusion
Pale Yellow coloured 5g crystals of iodoform is prepared.

Colourless crystals coloured 14.5g crystals of acetanilide is prepared.

Precautions

 Handle acetic anhydride carefully as it causes irritation to the eyes.


 If aniline sample is too much coloured, distil. it before carrying out the
 experiment, because yield is lowered with impure aniline.
 Use perfectly dry apparatus.
 Wash the solid 2-3 times with cold water till the filtrate is neutral to litmus.

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Experiment No. 6

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.

 Electrochemical reaction – The chemical reaction which takes place in a cell


like Daniel cell.

 Electrochemical cell – Electrochemical reaction carried out in a specially


designed set up.

 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)

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 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

When 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
 1M zinc sulphate solution
 Copper sulphate solution
 Zinc electrode
 copper electrode
 Beakers
 Voltmeter (or) Potentiometer
 Salt bridge
 Connecting wires

Diagram

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Procedure
Preparation of Salt Bridge

1. Prepare 1M of zinc sulphate solution and 1M of copper sulphate solution in


separate beakers.
2. Connect a salt bridge in such a manner that its one end dips in zinc sulphate and
the other dips in copper sulphate 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 sulphate and add water to make its volume up to 100ml.
The resultant molarity will be 0.1M.
6. Now dip zinc rod in 0.1M zinc sulphate solution and copper rod in 1M copper
sulphate solution and note the readings.
7. Repeat the same for 0.1M and 0.01M of zinc sulphate solution.
8. Note down the reading in voltmeter.
9. Repeat this procedure for other solutions of copper sulphate solutions.
10. Record electrode potentials values of copper electrodes for different
concentrations.

Observation

S.No [Cu2+(aq)]/mol L-1 log [Cu2+(aq)]/mol L-1 Ecell/V E(Cu2+/Cu)

Experimental value

1 0.2 1.3010 1.068 0.298

2 0.1 1.0000 1.062 0.292

3 0.05 2.6990 1.054 0.284

4 0.025 2..3679 1.044 0.274

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Calculations

ECell = EoCell – log [(Zn2+)/(Cu2+)]


EoCell = Eo(cathode) – Eo(anode)
R = 8.314
T = 298K
F = 96500C
n = 2 (number of electrons lost or gained)
By substituting all the values
ECell = EoCell – log [(Zn2+)/(Cu2+)]
We can measure ECell at different concentration of electrolyte.

Results and Discussions


 The Ecell decreases with increase in molar concentration of [Zn2+]. (Zinc sulphate
solution)
 The Ecell increases with increase in molar concentration of [Cu2+]. (Copper
sulphate solution)

Precautions
 Immediately after use, place the salt bridge in distilled water.
 Very carefully dilute the solution to another concentration.
 Always clean strips of copper and zinc with sandpaper and connect the wires
before use.
 Choose appropriate graph plot scales.

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Viva Questions

1. What is electrochemical cell?

Ans: An electrochemical cell is a device producing electrical energy from a


spontaneous redox reaction. This type of cell includes the cell named after Luigi
Galvani and Alessandro Volta, which is galvanic or voltaic.

2. Mention the names of anode and cathode of a Daniel cell?

Ans: The names of anode and cathode of a Daniel cell is, Anode – Zinc electrode,
Cathode – Copper electrode

3. What is salt bridge?

Ans: A laboratory device used to connect half-cells of a galvanic cell, a type of


electrochemical cell, with oxidation and reduction. It maintains electrical neutrality
within the internal circuit, preventing the cell’s reaction to equilibrium from running
rapidly.

4. What is the direction of flow of electrons in an electrochemical cell?

Ans: Electrons flow through an external wire from the anode into the cathode. The
Daniel cell is a common galvanic cell.

5. Define the term EMF?

Ans: Electromotive force (emf) is an energy measurement that causes the flow of
current through a circuit. It can also be defined as the possible charge difference
between two points in a circuit. Also known as voltage, electromotive force is
measured in volts.

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Experiment No. 7

Aim

(b) To find out the Molarity of given NaOH solution by titrating against M/10 solution
of oxalic acid. Both the solutions to be provided.

Apparatus Burette, pipette, clamp stand, white tile or paper, conical flask, wash
bottle, beaker.

Chemicals required M/10 oxalic acid solution, phenolphthalein, sodium


hydroxide solution.

Theory

This estimation involves titration of a weak acid that is oxalic acid against a strong
base sodium hydroxide and phenolphthalein is the indicator of choice. The reaction
between oxalic acid and sodium hydroxide is

(COOH)2 + 2NaOH → (COONa)2 + 2H2O

Since sodium hydroxide is not a primary standard a standard solution of oxalic acid
is prepared and used for standardisation of sodium hydroxide.

Diagram

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Procedure
Preparation of 0.1M Standard Oxalic Acid Solution

1. Take a watch glass, wash it with distilled water and dry it.
2. Weigh the exact amount of clean and dried watch glass and record its weight in
the notebook.
3. Weigh 3.15 g of oxalic acid on the watch glass correctly and record this weight in
the notebook.
4. Using a funnel, transfer oxalic acid softly and carefully from the watch glass into
a clean and dry measuring flask.
5. Wash the watch glass with distilled water to move the particles that stick to it
into the foam with the assistance of a wash bottle.
6. For this purpose, the volume of distilled water should not exceed 50 ml.
7. Wash the funnel several times with distilled water to move the sticking particles
into the measuring flask using a wash bottle. Add water in tiny quantities while
washing the funnel. The distilled water quantity used for this purpose should not
exceed 50 mL.
8. Using a wash bottle, wash the funnel carefully with distilled water to pass the
solution attached to the funnel into the measuring flask
9. Turn the flask of measurement until the oxalic acid dissolves.

Titration of Sodium Hydroxide and Oxalic Acid Solution

1. Rinse the burette with the standard oxalic acid solution.


2. Take 10cm3 of oxalic acid solution in a titration flask. Fill the burette with sodium
hydroxide solution.
3. Remove the air gap if any, from the burette by running the solution forcefully from
the burette nozzle and note the initial reading
4. Pipette out 20ml of NaOH solution is a conical flask. Add 2-3 drops of
phenolphthalein indicator to it.
5. Titrate the base with oxalic acid solution until the pink colour disappears.
6. Repeat the titration till three concordant readings are obtained.

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Observations

1. Molarity of oxalic acid solution =

2. Molarity of sodium hydroxide solution = x


3. Volume of oxalic acid solution = 10cm3
4. Indicator = Phenolphthalein
5. End point = Light pink colour

S.No Initial Reading of Final Reading of Volume of NaOH Concordant


the Burette the Burette solution used Reading

1 0 cm3 8.7 cm3 8.7 cm3 8.7 cm3

2 0 cm3 8.7 cm3 8.7 cm3 8.7 cm3

3 0 cm3 8.7 cm3 8.7 cm3 8.7 cm3

Calculations
Mass of oxalic acid dissolved in 100ml of standard solution = 4.9 g

𝑆𝑡𝑟𝑒𝑛𝑔𝑡ℎ of oxalic acid = 4.9𝑔 × 10𝑔/𝐿

10
𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦(𝑁) of standard oxalic acid = 𝑆𝑡𝑟𝑒𝑛𝑔𝑡ℎ/𝐸𝑞. 𝑤𝑡 = 4.9 × =𝑁
63.04

Normality (N1) of sodium hydroxide solution

𝑁 ×𝑉 =𝑁×𝑉

Therefore,

𝑉
𝑁 =𝑁×
𝑉

Normality (N2) of given oxalic acid solution

𝑁 ×𝑉 =𝑁 ×𝑉

𝑉
𝑁 =𝑁 ×
𝑉

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Strength of given oxalic acid = N2 x 63.04 g/L

Results and Discussion

The strength of the given sodium hydroxide solution is 8.7 g/L.

Precautions

1. Weighing of oxalic acid crystals need weights of 2g + 1g + 100mg + 50mg.


2. While weighing, do not spill the substance on the balance pan.
3. Rotate the knob of balance gently.
4. Keep the weights in the weights box at the proper places after weighing
5. Wash the watch glass carefully so that even a single crystal is not left on the
watch glass.
6. Bring the watch glass close to the funnel while transferring weighed substance
and transfer it gently. Wash it repeatedly with distilled water.
7. Wash the burette with water after titration is over.
8. The last few drops should be added using a pipette to avoid extra addition of
distilled water above the mark on the neck of the measuring cylinder.

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Experiment No. 8

Aim
To identify the cationic radicals, present in an inorganic mixture of salts by
performing various tests.

Theory

The qualitative analysis of an inorganic mixture is started by first carrying out some
preliminary tests. The Preliminary tests for cations are

 Borax bead test


 Flame test

1. Group I Cations (Ag+, Hg22+ and Pb2+ – insoluble chlorides):

Among the common metallic cations only three cations form insoluble chlorides with
hydrochloric acid. When 6M of HCl is added to the solution, white precipitates of
AgCl, Hg2Cl2 and PbCl2 are formed. Other metallic cations remain in solution.

2. Group V Cations (Mg2+, Na+, K+ and NH4+):

None of the cations in this group form precipitates in the separation processes of
group 1-4 cations and thus remain in the final solution.

Classification of Cations

Group Cations Group Reagents

Zero NH4+, K+ Tested using the mixture.

I Ag+, Hg22+, Pb2+ HCl

II A Hg2+, Pb2+, Cu2+, Bi3+, Cd2+

B As3+, Sb3+, Sn2+ H2S in the presence of HCl

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Materials Required

1. Test tubes
2. Boiling tubes
3. Test tube holder
4. Test tube stand
5. Corks
6. Filter paper
7. Delivery tube
8. Reagents
9. Measuring cylinder

Procedure

(i) Preliminary Test of Cations

Colour Inference

Blue or bluish green Copper or Nickel salts

Light green Ferrous salts

Dark green Chromium salts

(iii) Borax Bead Test

This test is used for the detection of cations in coloured mixtures which may contain
copper, nickel, iron or manganese. The borax bead reacts with these metal oxides to
form metabolites which have characteristic colour. Some metaborates when heated
in reducing flame form lower metaborates or even metals thus causing a change in
the colour of bead.

Na2B4O7.10H2O → Na2B4O7(White porous mass) → NaBO2 + B2O3

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B2O3 + CuSO4 → Cu(BO2)2(blue green cupric metaborate) + SO3↑

2Cu(BO2)2 + C → 2CuBO2(colourless coprous metaborate) + B2O3 + CO↑

2CuBO2 + C → 2Cu (red) + B2O3 + CO↑

Procedure for Borax Bead Test

 Make a small loop at the end of the platinum wire.

 Heat the loop in a Bunsen flame until it is red hot.

 Dip it into powdered borax placed on a watch glass and heat again. The borax
will first swell up and will fuse giving a colourless, transparent glass like bead.

 Touch the hot bead with conc.HCl and touch it with the given mixture or salt.
Heat it in an oxidising (non-luminous) and reducing (luminous) flame. Observe
the colour of the bead and draw inferences.

(iv) Flame Test


Certain cations like fifth group radicals Ba2+, Sr2+ and Ca2+ in the form of their
chlorides impart characteristic colours to the non-luminous flame. The chlorides of
these cations are thermally ionised. The ions so formed absorb heat energy and get
excited. The extra energy is released in the form of light of the characteristic colour
in the visible part of spectrum. Since different metal ions emit light energy of different
wavelengths, the colours imparted by the different cations to the flame are also
different.

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Procedure for Flame Test

 Take a platinum wire and dip it in conc.HCl taken on a watch glass and heat it
strongly in the flame. Repeat this process until the wire does not impart any
colour to the flame.

 Dip platinum wire in con.HCl and then touch it with a given salt and heat it in
the flame of the Bunsen burner. Observe the colour of the flame and draw
inferences.

Observation and Inference

(ii) Borax Bead Test

S.No Colour of the Bead in Colour of the Bead in Inference


Oxidising Flame Reducing Flame

Hot Cold Hot Cold

1 Green Blue Reddish or Reddish or Copper


Colourless Colourless

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2 Yellow Yellow Green Green Iron

3 Brown Brown Grey or Black Grey or Black Nickel

(iii) Flame Test

S.No Colour of the Flame Inference

With Naked Eye Through Blue Glass

1 Golden Yellow Nil Sodium (Na+)

2 Violet Pink Potassium (K+)

3 Crimson red Purple or crimson Strontium (Sr2+)

Results

The given salt contains ion is confirmed (NH4+, K+, Ag+, Hg22+, Pb2+) cation.

Precautions

1. Read the label carefully on the bottle before using any reagent or chemicals.
Never use a reagent that is unlabeled.
2. Always use an apron, an eye protector and hand gloves in the chemical
laboratory.
3. In smelling chemicals or vapours, be careful. Always gently fan the vapours to
your nose
4. Do not unnecessarily mix chemicals with reagents. Do not taste chemicals at all.
5. For dilution, always pour acid into water. Never add acid to water.

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Viva Questions

1. What is qualitative analysis?


Ans. The type of analysis that deals with the methods which are used to determine
the constituents of a compound.
2. What is a radical?
Ans. A radical may be defined as an atom or group of atoms which carries charge
and behaves as a single unit in chemical reactions.
3. What are acidic and basic radicals?
Ans. Radicals carrying positive charge are called basic radicals and those carrying
negative charge are called acidic radicals.
4. What type of bond is present in an inorganic salt?
Ans. Electrovalent bond.

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Experiment No. 9

AimCa
Anions To identify the anionic radicals present in an inorganic mixture of salts by
performing various tests.

Theory
Qualitative analysis involves the detection and identification of acidic and basic
radicals present in inorganic salts. Inorganic salts are formed by the reaction of acids
and bases or acidic oxides with a base or basic oxides.

Some of the examples of the reaction of acids and bases or acidic oxides with a
base or basic oxides are

NaOH + HCl → NaCl + H2O

CO2 + 2NaOH → Na2CO3 + H2O

KOH + HNO3 → KNO3 + H2O

2NaOH + H2SO4 → Na2SO4 + 2H2O

Most of the organic compounds are crystalline solids as they have defined
geometrical shapes. Usually, they consist of oppositely charged particles or ions
called radicals.

In the salt analysis, two fundamental principles are of great use

1. Solubility Product
2. Common Ion Effect

1. Solubility Product

Solubility product is defined as a product of ion concentrations elevated to a power


equal to the number of occurrences of ions in an equation representing electrolyte
dissociation at a given temperature when the solution is saturated. Under all
conditions, the solubility product is not the ionic product, but only if the solution is

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saturated.

Materials Required

1. Test tubes
2. Boiling tubes
3. Test tube holder
4. Test tube stand
5. Corks
6. Filter paper
7. Delivery tube
8. Reagents

Diagram

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Procedure

S.No. Experiment Observation Inference

4 Action of dilute.H2SO4: Brisk effervescence is Anion is


obtained from colourless, Carbonate
Add 1 or 2ccs of dilute
odourless gas that turns CO32-
H2SO4 to a small portion of
lime water.
the salt in a test tube and
warm it gently.
Colourless gas with an Sulphide
odour of rotten eggs is anion is
obtained, turning lead present.
acetate black paper.

Colourless gas with the Sulphate


odour of burning sulphur anion is
that turns acidified present.
dichromate green.

Reddish brown gas is Nitrate


obtained with a fishy odour anion is
that turns acidified brown present.
ferrous sulphate.

Colourless vinegar- May be


flavoured gas is obtained. acetate
anion.

No characteristic Absence of
observation. above-
mentioned
anions.

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Sodium Carbonate Extract:

Confirmatory Tests for CO32-, S2– anions:

Confirmatory anion testing is carried out using water extract when salt is water-
soluble and using sodium carbonate extract when salt is water-insoluble.
Confirmation of CO32– is done using aqueous salt solution or using solid salt as such,
as carbonate ions are contained in the sodium carbonate extract. Extract of water is
produced by dissolving salt in water.

Observations

S.No Anions Observation

1 CO32‒ CO2 gas is evolved with brisk effervescence with


dilute sulphuric acid, which turns lime water milky.
(Carbonate anion)

2 S2‒ (Sulphide anion) Add a drop of solution for sodium nitroprusside.


Appears purple or violet colouring.

Results:

1. The given salt contains ions confirmed (CO32‒, S2‒) anion.

Precautions

1. Read the label carefully on the bottle before using any reagent or chemicals.
Never use a reagent that is unlabeled.
2. Always use an apron, an eye protector and hand gloves in the chemical
laboratory.
3. In smelling chemicals or vapors, be careful. Always gently fan the vapors to your
nose
4. Do not unnecessarily mix chemicals with reagents. Do not taste chemicals at all.
5. For dilution, always pour acid into water. Never add acid to water.

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Viva Questions

1. How will you test the presence of carbonate ion?

Ans:- A dilute acid is used to detect carbonate ions, CO32- Bubbles are released
when an acid is added to the test compound, usually diluted hydrochloric acid.
Carbon dioxide causes the bubbles using Limewater and the gas is carbon dioxide.

2. What do you understand by the term common ion effect?

Ans:- The common ion effect describes the effect on balance that occurs when
adding to a solution a common ion an ion that is already contained in the solution.
Generally, the common ion effect decreases a solvent’s solubility.

3. Why does iodine give a blue colour with starch solution?

Ans:- The iodine test is used to test for starch presence. Starch becomes an intense
“blue-black” colour due to the formation of an intermolecular load-transfer complex
by adding aqueous solutions of the triiodide anion.

4. How do you test the presence of sulphide ion?

Ans:- Rotten egg smell of H2S is observed when adding dilute sulphuric acid to the
salt. The confirmatory test is the black spot of Ag 2S is observed when adding S2-ion
to silver foil.

5. Describe the layer test for bromide and iodide ions.

Ans:- In the presence of diluted hydrochloric acid, the layer test is performed by
adding Carbon Disulphide to the solution. It will give an orange layer in the case of
bromine, whereas in the case of iodine it will give a violet layer.

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Experiment No. 10 (a)

Aim

To Identify the Functional Groups, present in the given organic compounds and
perform:

a. Test for unsaturation.


b. Test for carboxylic, phenolic, aldehydic and ketonic groups.

Theory:

1. Unsaturated Hydrocarbons
In organic compounds unsaturation is due to the presence of double and triple
bonds. The aliphatic hydrocarbons that contain a double bond between the two
carbon atoms are called alkenes and the hydrocarbons that contain triple
bonds between two carbon atoms are called alkynes.

There are two methods for detecting the unsaturation in an organic compound.

1. Alkaline potassium permanganate test (Baeyer’s test)


2. Bromine test

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1. Alkaline potassium permanganate test (Baeyer’s test):

In this test the pink colour potassium permanganate disappears when an alkaline
potassium permanganate is added to an unsaturated hydrocarbon. The
disappearance of pink colour may take place with or without the formation of brown
precipitate of manganese oxide.

The chemical reaction is given below.

2KMnO4 + H2O → 2KOH + 2MnO2 + 3[O]

-C=C- + H2O → -C(OH)-C(OH)- + KOH

(Colourless)

2. Bromine Test
Bromine solution is brown. In this test when bromine solution is added to the
unsaturated hydrocarbon the brown colour disappears if the hydrocarbon is
unsaturated. Bromine forms an addition product with the unsaturated hydrocarbon.

The chemical reaction is given below.

-C=C- + Br2 → -C(Br)-C(Br)- (colourless)

Materials Required:

1. Potassium hydroxide solution


2. Bromine water solution/ Bromine in CCl4 or chloroform
3. Carbon tetrachloride/chloroform
4. Potassium permanganate solution
5. Sample compound to be tested
6. Distilled water
7. Test tubes
8. Test tube holder

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Diagram

Procedure:

(a) Alkaline potassium permanganate test (Baeyer’s test):

1. Take a little of the given organic compound to be tested in a test tube.


2. Dissolve the organic compound in 2ml of water or acetone in the test tube.
3. Add 1% alkaline potassium permanganate solution dropwise and shake the
mixture.
4. Observe the solution, if pink colour persists then it is saturated compound. If the
pink colour disappears then the given organic compound is unsaturated.

(b) Bromine test

(i) Water-soluble Compounds:

1. The organic compound to be tested is taken in a test tube.


2. Dissolve it in 2ml of distilled water.
3. Add bromine water drop wise with constant shaking.

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4. If the orange red colour of bromine disappears then the given organic
compound is unsaturated. When all the pi bonds are broken then the colour
persists.
5. If the colour of bromine persists then the given organic compound is saturated.

Observations:

Alkaline potassium Either disappearance of pink colour or pink


permanganate test colour persists.

Bromine test Either disappearance of orange -red colour or


orange -red colour persists.

Results

1. Baeyer’s test:

The given organic compound is unsaturated compound.

2. Bromine test:

The given organic compound is unsaturated compound.

Precautions:

1. The bromine solution should be handled carefully.


2. Do not inhale the vapours of bromine and chloroform.
3. The test should be carried out at room temperature.
4. Avoid bromine solution in contact with skin.

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Viva Questions

1. If the given organic compound is aldehyde, then what test is performed to


find the unsaturation?

Ans: Aldehydes decolourise potassium permanganate solution due to its oxidation to


carboxylic acid. Bromine water test can be carried out in this case to find out
unsaturation.

2. What is Baeyer’s reagent?

Ans: Baeyer’s reagent is a cold potassium permanganate alkaline solution, which is


a powerful oxidant that makes it a redox reaction.

3.Why does phenol decolourise bromine water?

Ans: Phenol is not an unsaturated compound also decolourizes bromine water. This
is due to the substitution reaction forming bromine substituted phenol.

4.What type of reaction takes place between alkenes and bromine water?

Ans: The double bond breaks when alkenes react with bromine, and each carbon is
attached to a bromine atom. It gives a colourless liquid, the bromine loses its original
red-brown colour.

5.If the compound is insoluble in water, what reagent is used to find saturation
or unsaturation?

Ans: If the compound is insoluble in water bromine in 100ml of carbon tetrachloride


is used to test its unsaturation.

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Experiment no. 10 (b) (i)

Aim
To identify the presence of a phenolic functional group in a given organic compound.

Theory
Any of the following tests can be carried out to detect the phenolic functional group.

1. Libermann’s test
2. Bromine water test

(c) Libermann’s Test:

Phenol reacts with concentrated sulfuric acid and sodium nitrite forms a yellow
colour quinone monoxime complex. With excess of phenol and sulfuric acid a deep
blue indophenol complex is formed. On dilution a red colour indophenol is formed
which turns to deep blue colour sodium salt solution of indophenol on treatment with
sodium hydroxide.

(d) Bromine Water Test:

Phenol undergoes electrophilic substitution reaction with bromine. When bromine


water is added to aqueous solution of phenol the brown colour of bromine
disappears and a white precipitate of tribromophenol is formed.

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Materials Required

1. Blue litmus paper, Ferric chloride solution, Sodium nitrite, Concentrated sulfuric
acid, Sodium hydroxide, Bromine water, Phthalic anhydride, Organic compound
to be tested, Test tubes,Test tube holder
2. Dropper
3. Beaker

Procedure

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Preparation of Reagents

1. Bromine Water: Take 5ml of bromine, add 100 ml of distilled water and shake
well. Decant off the clear liquid.

(c) Libermann’s Test:

1. Place the crystals of sodium nitrite in a clean dry test tube.


2. Add 1ml of phenol to the sodium nitrite solution.
3. Heat the mixture gently and allow it to cool.
4. Add 1ml of concentrated sulfuric acid to it and shake the contents.
5. Observe the change in the colour of the solution.
6. Dilute the solution with water so that the given compound turns red if a phenolic
group is present.
7. Now add sodium hydroxide solution, the blue colour solution or green colour
solution appears.

(d) Bromine Water Test:

1. Dissolve the given organic compound in glacial acetic acid.


2. Add bromine water solution to this dropwise.
3. If the colour of bromine disappears then it indicates the presence of phenol.

Observations

Libermann’s test Deep blue colour solution shows the presence of phenol.

Bromine water Formation of white precipitate shows the presence of


test phenol.

Results
The given organic compound is Phenol.

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Precautions

1. The ferric chloride solution used should be freshly prepared and should be
neutral and very dilute.
2. Phenol should be handled with care because it is toxic and corrosive nature.
3. Bromine should not be inhaled because it causes irritation.
4. Concentrated acids should be handled with care.

Viva Questions

1. Name the intermediate compound formed in the phthalein dye test?

Ans:- The intermediate compound formed in the phthalein dye test is


phenolphthalein.

2. What type of reaction takes place when phenol is treated with bromine
solution?

Ans:- Aromatic electrophilic substitution reaction takes place when bromine is treated
with phenol.

3. In the preparation of ferric chloride solution the brown precipitate formed


is?

Ans:- The brown precipitate formed during the preparation of ferric chloride solution
is ferric hydroxide.

4. Name the reagent used in Phthalein dye test.

Ans:- In Phthalein dye test phthalic anhydride is used as a reagent. A pink colour dye
is formed on adding excess sodium hydroxide and the colour disappears.

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Experiment no. 10 (b) (ii)

Aim
To identify the presence of aldehydes or ketones functional group in the given
organic compound.

Theory
1. 2,4-dinitrophenylhydrazine test

The difference between ketone and aldehyde is the carbonyl group present in
aldehydes can be easily oxidised to carboxylic acids, whereas the carbonyl group in
ketones is not oxidised easily. This difference in reactivity is the basis for the
distinction between aldehydes and ketones. They are generally distinguished by the
following tests.

1. Fehling’s test
2. Tollen’s test

(a) 2,4-Dinitrophenyl Hydrazine Test:

Aldehydes and ketones react with 2,4-dinitrophenylhydrazine to give an orange-


yellow precipitate.

The chemical reaction is given below.

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Distinguishing Tests between Aldehydes and Ketones:

(d) Fehling’s Test:

Fehling’s solution is a complex compound of Cu2+. When the aldehyde compound is


treated with Fehling’s solution Cu2+ is reduced to Cu+ and the aldehyde is reduced to
acids. During the reaction, a red precipitate is formed.

Aromatic aldehydes do not respond to Fehling’s test. An aqueous solution of the


compound may be used instead of an alcoholic solution. Formic acid also gives this
test.

Note: The appearance of red precipitate confirms the presence of an aldehydic


group.

(e) Tollen’s Test: (Silver Mirror Test)

This test is also called the silver mirror test. Tollens reagent consists of silver
ammonia complex in ammonia solution. Aldehydes react with Tollens reagent giving
a grey-black precipitate or a silver mirror. Always a freshly prepared Tollen’s reagent
should be used. Aldehydes are oxidised to the corresponding acids, and silver in
Tollens reagent is reduced from +1 oxidation state to its elemental form. Generally,
ketones do not respond to this test.

RCHO + 2[Ag(NH3)2]OH → R-COONH4 + 3NH3 + H2O + 2Ag↓(silver mirror)

Apart from aldehydes some other compounds also respond to Tollen’s test, but the
presence of aldehydes is confirmed when the given substance shows a positive test
for Tollen’s test, but if the given compound passes 2,4-dinitrophenylhydrazine test.

Note: The appearance of a shiny silver mirror confirms the presence of aldehydes.

Materials Required

1. Schiff’s reagent

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2. Silver nitrate solution


3. Fehling’s solutions A
4. Fehling’s solutions B
5. Dilute ammonium hydroxide solution
6. 2,4-Dinitrophenylhydrazine reagent
7. Chromic acid
8. Sulphuric acid
9. Sodium bisulphite
10. Test tubes
11. Test tube holder
12. Beaker

Diagram

Procedure for test of aldehydes and ketones

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(a) 2,4-Dinitrophenyl Hydrazine Test:

1. Dissolve the given organic compound in ethanol.


2. To this solution, add an alcoholic solution of 2,4-dinitrophenyl hydrazine.
3. Shake the mixture well.
4. If there is a formation of yellow to orange precipitate then the given compound is
an aldehyde or ketone.
5. An orange precipitate is obtained from carbonyl compounds in which the C=O
groups are conjugated with C=C.

(d) Fehling’s Test:

1. Fehling’s solution is prepared by mixing equal amounts of Fehling’s A and


Fehling’s B solution.
2. Take the given organic compound in a clean test tube.
3. Add Fehling’s solution to it and heat the solution gently.
4. If a brick-red precipitate appears, then the presence of aldehyde is confirmed.

(e) Tollen’s Test: (Silver Mirror Test)

1. Take 1ml of silver nitrate solution in a clean test tube.


2. Add dilute sodium hydroxide solution to it, and a brown precipitate forms.
3. Add dilute ammonia solution dropwise till the brown precipitate of silver oxide
dissolves.
4. To this freshly prepared Tollen’s reagent, add the given organic compound to be
tested.
5. Place the test tube in a warm water bath for about 5 to 10 minutes.
6. If there is the appearance of a silver mirror on the sides of the test tube confirms
the presence of an aldehyde.

Observations
2,4-Dinitrophenyl The formation of orange-yellow crystals indicates
Hydrazine Test the presence of the carbonyl group

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Fehling’s Test The appearance of red precipitate confirms the


presence of an aldehydic group.

Tollen’s Test (Silver The appearance of a shiny silver mirror confirms the
Mirror Test) presence of aldehydes.

Results
The given organic compound has aldehyde/ketone functional group.

Precautions:

1. The reagents should be freshly prepared to perform the test.


2. Not to heat the reaction mixture directly on the flame.
3. After performing the Tollen’s test, wash the test tube with nitric acid to destroy
the silver mirror, because it’s an explosive substance

Viva Questions

1. Name any one test to distinguish aldehyde from ketone.

Ans:- Tollens ‘ test is a qualitative laboratory test used to distinguish between an


aldehyde and a ketone, also known as a silver-mirror test. It takes advantage of the
fact that aldehydes are oxidized readily, while ketones are not.

2. What is Tollen’s reagent?

Ans:- Tollens reagent is ammoniacal silver nitrate with the chemical formula
[Ag(NH3)2]NO3.

3.What is the use of Schiff’s reagent?

Ans:- Schiff’s reagent is used to distinguish aldehydes and ketones.

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4.What is Fehling’s solution?

Ans:- The solution of Fehling is prepared by combining two separate solutions,


known as Fehling’s A and Fehling’s B. Fehling’s A is aqueous solution of deep blue
copper(II) sulphate. Fehling’s B is a colourless solution of Potassium sodium tartrate
(also known as Rochelle salt) made from strong alkali, commonly made from sodium
hydroxide.

5.What is Rochelle’s salt?

Ans:- Sodium potassium tartrate is called Rochelle’s salt.

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