Chemistry
Chemistry
Chemistry
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Ⓒ Manish Verma
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CERTIFICATE
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ACKNOWLEDGEMENT
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Index
1. To Determine Cut and bend glass rods/tubes.
3. To prepare a sol of
a) Starch
b) Ferric hydroxide
c) Aluminium hydroxide
4. To prepare crystals of
5. Preparations of
a) Iodoform
b) Acetanilide
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.
10. (a) To Identify the Functional Groups present in the given organic compounds
and perform:
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Experiment - 1
Objective
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
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
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
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
Precautions
The solution should be cooled slowly and do not use any rapid cooling
procedures.
Viva Questions
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.
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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.
Soda-lime glass
11. Mention the various steps which are involved in the cutting of a glass tube.
Scratching
Breaking
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
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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.
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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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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: 100° C.
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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.
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: 10 mL.
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Experiment – 4
Aim
To prepare crystals of
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.
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.
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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
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Precautions
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.
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Observations
Yield 12g
Conclusion
Crystals of Ferrous ammonium sulphate (Mohr salt), FeSO 4.(NH4)2SO4.6H2O =
12.5g
Viva Questions
1. What are double salts? Give two examples.
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.
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.
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.
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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.
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Diagram
Procedure
Preparation of iodoform
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Crystallization of iodoform
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
Conclusion
Pale Yellow coloured 5g crystals of iodoform is prepared.
Precautions
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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.
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.
———————————————————————————————
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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.
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 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
Observation
Experimental value
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Calculations
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
Ans: The names of anode and cathode of a Daniel cell is, Anode – Zinc electrode,
Cathode – Copper electrode
Ans: Electrons flow through an external wire from the anode into the cathode. The
Daniel cell is a common galvanic cell.
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.
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
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.
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Observations
Calculations
Mass of oxalic acid dissolved in 100ml of standard solution = 4.9 g
10
𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦(𝑁) of standard oxalic acid = 𝑆𝑡𝑟𝑒𝑛𝑔𝑡ℎ/𝐸𝑞. 𝑤𝑡 = 4.9 × =𝑁
63.04
𝑁 ×𝑉 =𝑁×𝑉
Therefore,
𝑉
𝑁 =𝑁×
𝑉
𝑁 ×𝑉 =𝑁 ×𝑉
𝑉
𝑁 =𝑁 ×
𝑉
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Precautions
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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
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.
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
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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
Colour Inference
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.
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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.
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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.
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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
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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
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.
1. Solubility Product
2. Common Ion Effect
1. Solubility Product
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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
No characteristic Absence of
observation. above-
mentioned
anions.
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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
Results:
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
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.
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.
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.
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.
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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Aim
To Identify the Functional Groups, present in the given organic compounds and
perform:
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.
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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.
(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.
Materials Required:
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Diagram
Procedure:
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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:
Results
1. Baeyer’s test:
2. Bromine test:
Precautions:
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Viva Questions
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?
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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
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.
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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.
Observations
Libermann’s test Deep blue colour solution shows the presence of 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
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.
Ans:- The brown precipitate formed during the preparation of ferric chloride solution
is ferric hydroxide.
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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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
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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.
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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Diagram
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Observations
2,4-Dinitrophenyl The formation of orange-yellow crystals indicates
Hydrazine Test the presence of the carbonyl group
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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:
Viva Questions
Ans:- Tollens reagent is ammoniacal silver nitrate with the chemical formula
[Ag(NH3)2]NO3.
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