Professional Documents
Culture Documents
NO
I PREPARATION OF INORGANIC COMPOUNDS
III ELECTROCHEMISTRY
3 To study the variation of cell potential in Zn/Zn2+//Cu2+/ Cu cell with change in concentration of
electrolytes at room temperature.
IV CHEMICAL KINETICS
4 To study the effect of concentration on the rate of reaction between sodium thiosulphate and
Hydrochloric acid
V SURFACE CHEMISTRY
5 Preparation of colloidal solution of starch , egg albuin , Ferric hydroxide and Aluminium
hydroxide.
VI VOLUMETRIC ANALYSIS
6 Determination of molarity and strength of KmnO4 solution using M/20 solution of ferrous
ammonium sulphate
7 Determination of molarity and strength of KmnO4 solution using M/40 solution of oxalic acid
Aim :
Mohr’s salt is prepared by dissolving an equimolar mixture of hydrated ferrous sulphate and ammonium
sulphate in water containing a little sulphuric acid and then subjecting the resulting solution to crystallization
when light green crystals of ferrous ammonium sulphate separate out.
Materials Required
Ferrous sulphate, Ammonium sulphate,m Dil. Sulphuric acid, Ethyl alcohol,Beakers, China
dish, Funnel, Glass rod, Tripod stand, Wire gauze, Wash bottle , Measuring jar
Procedure
1. First take 7g ferrous sulphate 3.5g ammonium sulphate in a clean 250ml beaker.
2. To this add about 2-3ml of dil.sulphuric acid to prevent the hydrolysis of ferrous sulphate.
3. In another beaker, boil about 20ml of water for 5 minutes.
4. Add the boiling hot water to the contents in the first beaker in small quantities at a time.
5. Stir the contents of the beaker with a glass rod until the salts have completely dissolved.
6. Filter the solution into a china dish.
7. Now heat the solution in the china dish until its crystallisation point is reached. Then transfer
the solution into a crystallising dish and keep it undisturbed.
8. On cooling, crystals of Mohr’s salt separate.
9. Decant the mother liquor and wash the crystals with a small quantity of alcohol and then dry
the crystals by placing them between filter paper pads.
10. Find the weight of the crystals.
Observations
Theory
Potash alum is prepared by dissolving an equimolar mixture of hydrated aluminium sulphate in minimum
amount of water containing a little of sulphuric acid anfd then subjecting the solution to crystallization , when
octahedral crystals of potash alum separate out.
Materials Required
Potassium sulphate, Aluminium sulphate, Dil. Sulphuric acid, Distilled water, Beakers, China
dish, Funnel,Glass rod, Tripod stand, Wire gauze, Burner, Wash bottle, Measuring jar
Procedure
Observations
Theory
Acetanilide is prepared by acetylating aniline with acetic anhydride in the presence of glacial acetic
acid
Materials Required
Procedure
1. Take 5ml of acetic anhydride in a clean dry 250ml RB flask and add 5 ml of glacial acetic
acid and shake the contents thoroughly.
2. To this mixture add 5ml of aniline and fit a water condenser.
3. Boil this mixture over a sand bath for 10min.
4. Pour the liquid from the RB flask into 200ml ice-cold water taken in a beaker. While adding
stir the contents of the beaker vigorously using a glass rod.
5. Filter the white precipitate formed and wash it with cold water.
6. Recrystallise from hot water containing a few drops of etanol . Weigh the crystals and record
the yield
7. Determinre the melting point of the compound.
Observation
The weight of acetanilide = 3g
Melting point = 1130c
Precautions
Theory
The nitration of aniline is difficult to carry out with nitrating mixture since –NH2 gets oxidized . So the amini
group is first protected by acetylation to form acetanilide which is then nitrated to give p- nitroacetanide as
amajor product. And o – nitro acetanide as a minor product. Recrystallisation from ethanol readily removes
the more soluble ortho compound .
Materials Required
Acetanilide- 5g ,Glacial acetic acid- 5ml,Conc.sulphuric acid -10ml, Fuming nitric acid -2ml
Procedure
1. Take 5g powdered acetanilide and 5ml of glacial acetic acid in a conical flask and stir the
mixture using a glass rod.
2. Take 2ml of fuming nitric acid in a clean test tube and cool it in a freezing mixture taken in a
beaker. Carefully add 2ml of conc.sulphuric acid drop by drop while constantly shaking and
cooling it.
3. Add 8ml of conc.sulphuric acid drop by drop into the conical flask containing acetanilide and
glacial acetic acid and cool it in a freezing mixture. Stir the contents and wait until the
temperature becomes less than 5oC.
4. To the cooled contents in the flask, add the nitrating mixture prepared in the 2nd step, drop
by drop while stirring constantly. While adding the nitrating mixture, the temperature of the
mixture in the flask should not rise above 25oC. Remove the conical flask from the freezing
mixture and allow it to stand for 30min at room temperature.
5. Pour the contents of the flask into a beaker containing crushed ice. Stir it well and filter the
precipitate obtained and wash it thoroughly with cold water.
6. Recrystallisation of p-Nitro acetanilide: Dissolve the precipitate obtained above in 20ml
methylated spirit. Warm it to get a clear solution. Filter the hot solution and cool the filtrate
in ice. P-Nitro acetanilide is obtained as colourless crystals. Wash the crystals with cold
water and then dry the crystals and measure the weight of the crystals.
Observation
The weight of p-nitroacetanilide = 3.5 g
Melting point : = 2140c
Precautions
ELECTRO CHEMISTRY
Aim : To study the variation of cell potential in Zn/Zn2+//Cu2+/ Cu cell with change in concentration of
electrolytes at room temperature.
Theory
Reduction potential of an electrode increases with increase in concentration of the electrolyte.
Mn+(aq)+ne– ———->M(s)
In the zinc-copper electrochemical cell zinc electrode acts as anode while copper electrode acts as cathode.
Procedure
Repeat the experiment by taking different concentrations of zinc sulphate and copper sulphate solutions.
Conclusion
EMF of the cell increases with decrease in cone, of the electrolyte around anode and increase in cone, of the
electrolyte around cathode.
( To be done on the left hand side )
1M 1M 1.1V
1M 0.5M 1.091V
1M 0.025M 1.052V
1M 0.0125M 1.043V
0.5M 1M 1.108V
0.025M 1M 1.147V
0.0125M 1M 1.156V
Expt No 4 Date:
CHEMICAL KINETICS
AIM :
To study the effect of concentration on the rate of reaction between sodium thiosulphate
and hydrochloricacid.
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 the increase in the concentration of the reactants. The effect of concentration of reactants on
rate of a reaction can be studied easily by the reaction between sodium thiosulphate and hydrochloric
acid.
Na2S203 + 2HCl ——–> S(s) + 2NaCl(aq) + SO2(g) + H2O(l)
The insoluble sulphur, formed during the reaction, gives a milky appearance and makes the solution
opaque. Therefore, rate of reaction can be studied by measuring the time taken to produce enough
sulphur to make some mark invisible on a paper kept under the conical flask in which the reaction is
carried out.
Apparatus
Pipette (10 ml), stop-watch, two burettes and five conical flasks (100 ml).
Materials
Procedure
1. Wash the conical flasks with water and label them as 1, 2, 3, 4 and 5 respectively.
2. With the help of a burette, add 10, 20, 30, 40 and 50 ml of 0.1 M Na2S2O3 solution to the
flasks 1, 2, 3, 4 and 5 respectively.
3. Now add 40, 30, 20 and 10 ml of distilled water to the flask 1, 2, 3 and 4 respectively so that
volume of solution in each flask is 50 ml.
4. Take 10 ml of 1M HCl in a test tube with the help of a burette.
5. Add 10 ml of hydrochloric acid taken in a test tube to the conical flask No. 1 containing 10 ml
of 0.1 M Na2S2O3 and 40 ml of distilled water and start the stop-watch.
When half of the hydrochloric acid solution has been added. Shake the contents of the conical
flask and place it on the tile with a cross mark as shown in Fig.
6. Go on observing from top to downwards in the flask and stop the stop-watch when the cross
mark just becomes invisible. Note down the time.
7. Repeat the experiment by adding 10 ml of 1M HCl to flasks 2, 3,4 and 5 and record the time
taken in each case for the cross to become just invisible.
Result
From the graph, it is clear that 1/t is directly proportional to the cone, of Na2S2O3 solution. But y is a
direct measure of rate of the reaction, therefore, rate of the reaction between Na2S2O3 and HCl is
directly proportional to the cone, of Na2S2O3 solution taken. Hence, rate of this reaction is directly
proportional to the concentration of Na2S2O3, which is one of the reactants.
Note. It may be noted that the reaction rate also increases when the amount of sodium thiosulphate is
kept constant but the concentration of hydrochloric acid is increased.
Precautions
1. The apparatus must be thoroughly clean. If the same conical flask is to be used again and
again, it should be thoroughly washed with cone. HNO3 and then with water.
2. Measure the volumes of sodium thiosulphate solution, hydrochloric acid and distilled water
very accurately.
3. Use the same tile with the same cross-mark for all observation,
4. Complete the experiment at one time only so that there is not much temperature variation.
5. Start the stop-watch immediately when half of the hydrochloric acid solution has been added
to sodium thiosulphate solution.
6. View the cross-mark through the reaction mixture from top to bottom from same height for all
observations.
( To be done on the left hand side)
Observations
4 40 10 50 0.08 10 60 0.0167
5 50 0 50 0.10 10 159
0.006
Plot a graph between 1/t (in seconds) and the concentration of sodium thiosulphate by taking 1/t along
ordinate (vertical axis) and cone, of Na2S2O3 along abscissa (horizontal axis). It should be a straight sloping
line.
Expt No : 5 Date :
SURFACE CHEMISTRY
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.
Apparatus
Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar, tripod stand, wire-
gauze and burner.
Materials Required
Soluble starch (500 mg) and distilled water.
Procedure
Precautions
‘
Aim: To prepare colloidal solution of egg albumin
Theory
Egg albumin which is obtained from eggs forms lyophilic sols with cold water. The sol is quite stable and is
not affected by the presence of traces of impurities.
Apparatus
Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar, tripod stand, wire-
gauze and burner.
Material required
Procedure
Precautions
The apparatus used for preparing the sol should be properly cleaned.
Distilled water should be used for preparing sols in water.
Egg albumin sol is prepared at room temperature because in hot solution the precipitation of egg albumin
takes place.
The yellow yolk should be separated completely from the egg albumin before using the later in the
experiment.
Addition of egg albumin should be done very slowly and while constantly stirring so as to disperse the
colloidal particles well in the solution.
Aim : To prepare ferric hydroxide sol
Theory
Ferric hydroxide forms a lyophilic sol. The substance such as metal hydroxides or sulphides are insoluble and
do not really give colloidal solutions on treatment with water are called hydrophobic colloids.
Ferric hydroxide is prepared by the hydrolysis of ferric chloride with boiling distilled water.
Hydrochloric acid which is produced during tries to destabilize the sol and hence must be removed from the sol by
dialysis .
Procedure
Take a 250 ml conical flask and clean it using the steaming out process.
To this cleaned conical flask, add 100 ml of distilled water using a measuring cylinder.
Bring the water to boil by placing the flask over a Bunsen burner.
Add ferric chloride solution dropwise to the boiling water using a dropper.
Continue heating until a deep red or brown solution of ferric hydroxide is obtained.
Note: Replace the water lost by evaporation during boiling at regular intervals.
Keep the contents of the conical flask undisturbed for some time at room temperature.
Label the solution as Ferric Hydroxide Sol.
Precautions
Since ferric hydroxide sol is affected by impurities, the apparatus required for the preparation of sol should
be thoroughly cleaned by the steaming out process.
Add ferric chloride solution dropwise.
Heating is continued till the desired sol is obtained.
Hydrochloric acid formed as a result of hydrolysis of ferric chloride is removed by dialysis process
otherwise it would destabilise the sol.
( To be done on left hand side )
Aim : To prepare aluminium hydroxide sol
Theory
Dialysis is done to remove hydrochloric acid because aluminium hydroxide solis affected by the
presence of ionic impurities.
Materials Required
Procedure
Take a 250 ml conical flask and clean it using the steaming out process.
To this cleaned conical flask, add 100 ml of distilled water using a measuring cylinder.
Bring the water to boil by placing the flask over a Bunsen burner.
Add aluminium chloride solution dropwise to the boiling water using a dropper.
Continue heating until a white coloured solution of aluminium hydroxide is obtained.
Note: Replace the water lost by evaporation during boiling at regular intervals.
Keep the contents of the conical flask undisturbed for some time at room temperature.
Label the solution as Aluminium Hydroxide Sol.
Precautions
The apparatus required for the preparation of the sol should be thoroughly cleaned through
the steaming out process.
Add aluminium chloride solution dropwise.
Heating is continued till the desired sol is obtained.
Hydrochloric acid formed as a result of hydrolysis of aluminium chloride is removed by
dialysis process otherwise it would destabilise the sol.
Expt No ____6_____ Date ___________
VOLUMETRIC ANALYSIS
AIM
To determine the molarity and strength of KMnO4 solution by titrating it against 1/20 M standard solution
of ferrous ammonium sulphate.
MOLECULAR EQUATION
INDICATOR
END POINT
PROCEDURE
(i) Weigh 1.96 g of ferrous ammonium sulphate and transfer it into a 100 mL measuring flask through a
funnel. Transfer the solid sticking to the funnel with the help of distilled water into the flask and add 3 mL of
Conc H2SO4 into the flask drop wise to get the clear solution. Shake the flask till the substance dissolves and
make the solution up to the mark.
(i) Rinse and fill the clean burette with potassium permanganate solution. Remove air bubbles if any, from
the burette tip by releasing some solution through it.
(ii) Rinse the pipette with M/20 Mohr’ s salt and pipette out 10 mL of 0.05 M ferrous ammonium sulphate
solution in a conical flask and add half test tube (≈ 5 mL) full of (2.0 M) H2SO4 to it.
(iii) Titrate the above solution with potassium permanganate solution till the colour of the solution changes to
permanent pink. Swirl the content of the flask during the titration.
(iv) Repeat the titration, until three concordant readings are obtained.
RESULT
1) Molarity of KMnO4 =
2) Strength of KMnO4 =
OBSERVATION AND CALCULATION( To be done on the left hand side )
2 10
3 10
Concordant value = Y mL =
From the overall balanced chemical equation ., it is clear that 2 moles of KMnO4 react with 10 moles of
Mohr’s salt.
MFAS X VFAS
Where
MKMnO4 x = 1/5
0.05 x 10
MKmnO4 = 1 x 0.05 x 10 =
5 x _______
= ______ X 158
__________ g/ L
Expt No ____7_______ Date : ______________
AIM
To determine the concentration/molarity of KMnO4 solution by titrating it against a 1/40 M standard solution
of oxalic acid.
CHEMICAL EQUATION
Molecular equation
2Kmno4+3H2SO4→K2SO4+2MnSO4+3H2O+5[O]
H2C2O4.2H2O+[O]→2CO2+3[H2O]×5
2KMnO4+3H2SO4+5H2C2O4.2H2O→K2SO4+2MnSO4+18H2O+10CO2
Ionic equation
MnO−4+8H++5e−→Mn2++4H2O]×2
C2O2−4→2CO2+2e−]×5
2MnO−4+16H++5C2O2−4→2Mn2++8H2O+10CO2
INDICATOR
END POINT
PROCEDURE
(i) Weigh 0.315 g of oxalic acid and transfer it into a 100 mL measuring flask through a funnel. Transfer
the solid sticking to the funnel with the help of distilled water into the flask. When the oxalic acid in the flask
is completely dissolved , add enough water and make the solution up to the mark.
(i) Rinse and fill a clean burette with potassium permanganate solution. Remove the air bubble, if any, (ii)
Take 10 mL of 0 .025 M oxalic acid solution in a conical flask and add half of the test tube full ( ≈ 5 mL) of
2.0 M H2SO4 to it to prevent the formation of any precipitate of manganese dioxide during the course of the
titration.
(iii) Heat the oxalic acid solution upto 50°– 60°C before titrating it with potassium permanganate solution
taken in the burette.
(iv) Note the initial reading of the volume of permanganate solution in the burette and add it in small
volumes to the hot oxalic acid solution while swirling the contents of the flask gently. The end point is
indicated by the appearance of permanent light pink colour
(v) Repeat the titration till three concordant readings are obtained.
RESULT
1) Molarity of KMnO4 =
2) Strength of KMnO4 =
OBSERVATION AND CALCULATION( To be done on the left hand side )
2 10
3 10
Concordant value = y = mL
From the overall balanced chemical equation ., it is clear that 2 moles of KMnO4 react with 5 moles of oxalic
acid .
Where
MKMnO4 X = 2/5
0.05 x 10
MKmnO4 = 2 x 0.025 x 10 =
5 x _______
= ______ X 158
__________ g/ L
QUALITATIVE ANALYSIS OF INORGANIC SALTS
Preliminary tests
Experiment Observation Inference
Color Colorless/White Fe2+, Fe3+,Mn2+,Co2+,Cu2+may
be absent
4) Smell
Take a pinch of the salt Ammoniacal smell NH4+, may be present
between the fingers and rub it
with a drop of water. Vinegar like smell CH3COO- may be present
Characteristic smell of
ammonia gas is obtained
which gives white fumes when Presence of NH4+
glass rod dipped in Dil HCl is
brought near the mouth of the
test tube.
ii)
Sublimate formed White sublimate Presence of NH4+
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
If no reaction in cold, add a Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present.
the test tube containing salt
and heat.
Brown ring Test A brown ring is formed at the Presence of NO3- is confirmed
Salt solution + equal volume junction of layers of acid and
of freshly prepares ferrous the solution
sulphate solution.Add a drop
of Conc H2SO4 slowly along
the sides of the test tube.
Sodium chromate
Leadchromate
Soluble complex
Confirmatory Test for CH3COO-
Ester test:
Salt + iml of Conc. H2SO4and Presence of CH3COO-
warm. Add C2H5OH . Add Pleasant fruity smell confirmed
contents in to a beaker full of
water
COOH
COOH COONa
Ester TeST
fruity smell
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
White
White ppt
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Pass H2S gas through the Black precipitate is formed Group II is present (Cu2+,
above solution Pb2+)
O.S + Solid Ammonium Reddish/ White gelatinous Group III is present (Al3+,
chloride + Ammonium precipitate is formed Fe3+)
hydroxide in excess till the
solution become basic.
Part 1 – cool under tap White crystalline precipitate Presence of Pb2+ confirmed
Part 1 + KI solution
Yellow precipitate is formed Pb2+ confirmed
which dissolves in boiling
water crystalizes on cooling
Part 2 + K2CrO4 solution
Yellow precipitate soluble in Pb2+ confirmed
NaOH
Lake test :
Lake test
1) NaOH TEST
BARIUM
Analysis of Group VI
Flame Test:
Absence of Ba2+, Pb2+, Zn2+
Take a small amount of salt on No characteristic colour to the orMn2+, Ca2+ ,Sr2+
a watch glass and make a flame
paste with con. HCl. Heat the
mixture strongly in the flame
Salt in a dry test tube + Conc. Reddish brown vapors with Group II acid radical Br- may
H2SO4 pungent smell be present
Note : chemical equations for the confirmatory tests should be written on un ruled page in
pencil for both acid and basic radicals.
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
RESULT
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3- is
piece of Cu or paper ball to evolved absent
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radical SO42- is confirmed
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
O.S + Solid Ammonium / White gelatinous precipitate Group III is present (Al3+,
chloride + Ammonium is formed Fe3+)
hydroxide in excess till the
solution become basic.
Lake test :
RESULT
Flame Test:
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3- is
piece of Cu or paper ball to evolved absent
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
O.S + SolidAmmonium
chloride + Ammonium Group III is absent
hydroxide in excess till the No precipitate
solution become basic.
Pass H2S gas through the / white precipitate is formed Group IV is present
above solution White (Zn2+)
RESULT
Flame Test:
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the white precipitate is formed Group IV is present
above solution White (Zn2+)
4) Smell
Take a pinch of the salt NH4+, CH3COO- S2- are
between the fingers and rub it No characteristic smell absent
with a drop of water.
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
No white precipitate is
O.S + 1 to 2 ml of Dil. HCl formed Group I is absent
Group IV is absent
Pass H2S gas through the No precipitate
above solution
Analysis of Group VI
RESULT
Flame Test:
Sublimate formed
No White sublimate Absence of NH4+
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
No white precipitate is
O.S + 1 to 2 ml of Dil. HCl formed Group I is absent
Group IV is absent
No precipitate
Pass H2S gas through the
above solution
White precipitate
O.S + Solid Ammonium Group VI (Mg2+) is present
Chloride + Ammonium
Hydroxide + Ammonium
Hydrogen Phosphate
Analysis of Group VI
RESULT
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the
above solution No black precipitate is
formed Group II is absent
RESULT
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
Confirmatory Test for Cl-
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Presence of CO3 2-
Dry heating test
Heat a pinch of the salt in a
dry test tube Colorless odorless gas turning Absence of NH4+
lime water milky
i) Gas evolved
Presence of Ba2+,Sr2+,Ca2+,
Mg2+,Al3+
No White sublimate
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
s liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
RESULT
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the
above solution No black precipitate is
formed Group II is absent
Abesence of NH4+
Sublimate No White sublimate
Residue Brown when hot , yellow Presence of Pb2+
when cold
No characteristic observation
If no reaction in cold, add a Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present.
the test tube containing salt
and heat.
Brown ring Test A brown ring is formed at the Presence of NO3- is confirmed
Salt solution + equal volume junction of layers of acid and
of freshly prepares ferrous the solution
sulphate solution.Add a drop
of Conc H2SO4 slowly along
the sides of the test tube.
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is Present
O.S + 1 to 2 ml of Dil. HCl white precipitate is formed
Part 1 – cool under tap White crystalline precipitate Presence of Pb2+ confirmed
RESULT
Aim : To Test the presence of Alcoholic Group in the given sample of organic compound
ESTER TEST H+
white fumes
Aim : To Test the presence of a for phenolic Group in the given sample of organic compound
violet complex
Tollens test
2gA(NH3)2 -
+ CH3CHO + 3 OH- CH3COO + 2Ag + 4NH3 + 2H2O
Fehling’s test
RED
Aim : To Test the presence of a for ketonic Group in the given sample of organic compound
2, 4 DNPH Test
Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test tube
effervescence carboxylic
Carbonate and add a pinch of sodium bicarbonate to it.
is observed. group.
Test
The given sample of organic compound has carboxylic acid group in it.
ESTER TEST H+
Solubility Test
Aim : To identify the functional group present in the given compound with relevant chemical
test
Physical Tests:
Chemical Tests:
Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test tube
effervescence carboxylic
Carbonate and add a pinch of sodium bicarbonate to it.
is observed. group.
Test
It is a clear, volatile liquid with a characteristic pleasant odor, and a burning taste. It is completely miscible
with water in all ratios and with organic solvents. Melting point: -117 °C and Boiling point: 78 °C
Chemical Tests:
Physical Tests:
Smell
Chemical Tests
Physical Tests:
Smell : Smell
Physical Tests:
Chemical Tests
Physical Tests:
Smell :
Chemical Tests
Physical Tests:
Smell :
Chemical Tests
Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test
effervescence is carboxylic
Carbonate tube and add a pinch of sodium bicarbonate to it.
observed. group.
Test
III ELECTROCHEMISTRY
3 To study the variation of cell potential in Zn/Zn2+//Cu2+/ Cu cell with change in concentration of
electrolytes at room temperature.
IV CHEMICAL KINETICS
4 To study the effect of concentration on the rate of reaction between sodium thiosulphate and
Hydrochloric acid
V SURFACE CHEMISTRY
5 Preparation of colloidal solution of starch , egg albuin , Ferric hydroxide and Aluminium
hydroxide.
VI VOLUMETRIC ANALYSIS
6 Determination of molarity and strength of KmnO4 solution using M/20 solution of ferrous
ammonium sulphate
7 Determination of molarity and strength of KmnO4 solution using M/40 solution of oxalic acid
Aim :
Mohr’s salt is prepared by dissolving an equimolar mixture of hydrated ferrous sulphate and ammonium
sulphate in water containing a little sulphuric acid and then subjecting the resulting solution to crystallization
when light green crystals of ferrous ammonium sulphate separate out.
Materials Required
Ferrous sulphate, Ammonium sulphate,m Dil. Sulphuric acid, Ethyl alcohol,Beakers, China
dish, Funnel, Glass rod, Tripod stand, Wire gauze, Wash bottle , Measuring jar
Procedure
11. First take 7g ferrous sulphate 3.5g ammonium sulphate in a clean 250ml beaker.
12. To this add about 2-3ml of dil.sulphuric acid to prevent the hydrolysis of ferrous sulphate.
13. In another beaker, boil about 20ml of water for 5 minutes.
14. Add the boiling hot water to the contents in the first beaker in small quantities at a time.
15. Stir the contents of the beaker with a glass rod until the salts have completely dissolved.
16. Filter the solution into a china dish.
17. Now heat the solution in the china dish until its crystallisation point is reached. Then transfer
the solution into a crystallising dish and keep it undisturbed.
18. On cooling, crystals of Mohr’s salt separate.
19. Decant the mother liquor and wash the crystals with a small quantity of alcohol and then dry
the crystals by placing them between filter paper pads.
20. Find the weight of the crystals.
Observations
Theory
Potash alum is prepared by dissolving an equimolar mixture of hydrated aluminium sulphate in minimum
amount of water containing a little of sulphuric acid anfd then subjecting the solution to crystallization , when
octahedral crystals of potash alum separate out.
Materials Required
Potassium sulphate, Aluminium sulphate, Dil. Sulphuric acid, Distilled water, Beakers, China
dish, Funnel,Glass rod, Tripod stand, Wire gauze, Burner, Wash bottle, Measuring jar
Procedure
Observations
Theory
Acetanilide is prepared by acetylating aniline with acetic anhydride in the presence of glacial acetic
acid
Materials Required
Procedure
8. Take 5ml of acetic anhydride in a clean dry 250ml RB flask and add 5 ml of glacial acetic
acid and shake the contents thoroughly.
9. To this mixture add 5ml of aniline and fit a water condenser.
10. Boil this mixture over a sand bath for 10min.
11. Pour the liquid from the RB flask into 200ml ice-cold water taken in a beaker. While adding
stir the contents of the beaker vigorously using a glass rod.
12. Filter the white precipitate formed and wash it with cold water.
13. Recrystallise from hot water containing a few drops of etanol . Weigh the crystals and record
the yield
14. Determinre the melting point of the compound.
Observation
The weight of acetanilide = 3g
Melting point = 1130c
Precautions
Theory
The nitration of aniline is difficult to carry out with nitrating mixture since –NH2 gets oxidized . So the amini
group is first protected by acetylation to form acetanilide which is then nitrated to give p- nitroacetanide as
amajor product. And o – nitro acetanide as a minor product. Recrystallisation from ethanol readily removes
the more soluble ortho compound .
Materials Required
Acetanilide- 5g ,Glacial acetic acid- 5ml,Conc.sulphuric acid -10ml, Fuming nitric acid -2ml
Procedure
7. Take 5g powdered acetanilide and 5ml of glacial acetic acid in a conical flask and stir the
mixture using a glass rod.
8. Take 2ml of fuming nitric acid in a clean test tube and cool it in a freezing mixture taken in a
beaker. Carefully add 2ml of conc.sulphuric acid drop by drop while constantly shaking and
cooling it.
9. Add 8ml of conc.sulphuric acid drop by drop into the conical flask containing acetanilide and
glacial acetic acid and cool it in a freezing mixture. Stir the contents and wait until the
temperature becomes less than 5oC.
10. To the cooled contents in the flask, add the nitrating mixture prepared in the 2nd step, drop
by drop while stirring constantly. While adding the nitrating mixture, the temperature of the
mixture in the flask should not rise above 25oC. Remove the conical flask from the freezing
mixture and allow it to stand for 30min at room temperature.
11. Pour the contents of the flask into a beaker containing crushed ice. Stir it well and filter the
precipitate obtained and wash it thoroughly with cold water.
12. Recrystallisation of p-Nitro acetanilide: Dissolve the precipitate obtained above in 20ml
methylated spirit. Warm it to get a clear solution. Filter the hot solution and cool the filtrate
in ice. P-Nitro acetanilide is obtained as colourless crystals. Wash the crystals with cold
water and then dry the crystals and measure the weight of the crystals.
Observation
The weight of p-nitroacetanilide = 3.5 g
Melting point : = 2140c
Precautions
ELECTRO CHEMISTRY
Aim : To study the variation of cell potential in Zn/Zn2+//Cu2+/ Cu cell with change in concentration of
electrolytes at room temperature.
Theory
Reduction potential of an electrode increases with increase in concentration of the electrolyte.
Mn+(aq)+ne– ———->M(s)
In the zinc-copper electrochemical cell zinc electrode acts as anode while copper electrode acts as cathode.
Procedure
Repeat the experiment by taking different concentrations of zinc sulphate and copper sulphate solutions.
Conclusion
EMF of the cell increases with decrease in cone, of the electrolyte around anode and increase in cone, of the
electrolyte around cathode.
( To be done on the left hand side )
1M 1M 1.1V
1M 0.5M 1.091V
1M 0.025M 1.052V
1M 0.0125M 1.043V
0.5M 1M 1.108V
0.025M 1M 1.147V
0.0125M 1M 1.156V
Expt No 4 Date:
CHEMICAL KINETICS
AIM :
To study the effect of concentration on the rate of reaction between sodium thiosulphate
and hydrochloricacid.
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 the increase in the concentration of the reactants. The effect of concentration of reactants on
rate of a reaction can be studied easily by the reaction between sodium thiosulphate and hydrochloric
acid.
Na2S203 + 2HCl ——–> S(s) + 2NaCl(aq) + SO2(g) + H2O(l)
The insoluble sulphur, formed during the reaction, gives a milky appearance and makes the solution
opaque. Therefore, rate of reaction can be studied by measuring the time taken to produce enough
sulphur to make some mark invisible on a paper kept under the conical flask in which the reaction is
carried out.
Apparatus
Pipette (10 ml), stop-watch, two burettes and five conical flasks (100 ml).
Materials
Procedure
8. Wash the conical flasks with water and label them as 1, 2, 3, 4 and 5 respectively.
9. With the help of a burette, add 10, 20, 30, 40 and 50 ml of 0.1 M Na2S2O3 solution to the
flasks 1, 2, 3, 4 and 5 respectively.
10. Now add 40, 30, 20 and 10 ml of distilled water to the flask 1, 2, 3 and 4 respectively so that
volume of solution in each flask is 50 ml.
11. Take 10 ml of 1M HCl in a test tube with the help of a burette.
12. Add 10 ml of hydrochloric acid taken in a test tube to the conical flask No. 1 containing 10 ml
of 0.1 M Na2S2O3 and 40 ml of distilled water and start the stop-watch.
When half of the hydrochloric acid solution has been added. Shake the contents of the conical
flask and place it on the tile with a cross mark as shown in Fig.
13. Go on observing from top to downwards in the flask and stop the stop-watch when the cross
mark just becomes invisible. Note down the time.
14. Repeat the experiment by adding 10 ml of 1M HCl to flasks 2, 3,4 and 5 and record the time
taken in each case for the cross to become just invisible.
Result
From the graph, it is clear that 1/t is directly proportional to the cone, of Na2S2O3 solution. But y is a
direct measure of rate of the reaction, therefore, rate of the reaction between Na2S2O3 and HCl is
directly proportional to the cone, of Na2S2O3 solution taken. Hence, rate of this reaction is directly
proportional to the concentration of Na2S2O3, which is one of the reactants.
Note. It may be noted that the reaction rate also increases when the amount of sodium thiosulphate is
kept constant but the concentration of hydrochloric acid is increased.
Precautions
7. The apparatus must be thoroughly clean. If the same conical flask is to be used again and
again, it should be thoroughly washed with cone. HNO3 and then with water.
8. Measure the volumes of sodium thiosulphate solution, hydrochloric acid and distilled water
very accurately.
9. Use the same tile with the same cross-mark for all observation,
10. Complete the experiment at one time only so that there is not much temperature variation.
11. Start the stop-watch immediately when half of the hydrochloric acid solution has been added
to sodium thiosulphate solution.
12. View the cross-mark through the reaction mixture from top to bottom from same height for all
observations.
( To be done on the left hand side)
Observations
4 40 10 50 0.08 10 60 0.0167
5 50 0 50 0.10 10 159
0.006
Plot a graph between 1/t (in seconds) and the concentration of sodium thiosulphate by taking 1/t along
ordinate (vertical axis) and cone, of Na2S2O3 along abscissa (horizontal axis). It should be a straight sloping
line.
Expt No : 5 Date :
SURFACE CHEMISTRY
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.
Apparatus
Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar, tripod stand, wire-
gauze and burner.
Materials Required
Soluble starch (500 mg) and distilled water.
Procedure
Precautions
‘
Aim: To prepare colloidal solution of egg albumin
Theory
Egg albumin which is obtained from eggs forms lyophilic sols with cold water. The sol is quite stable and is
not affected by the presence of traces of impurities.
Apparatus
Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar, tripod stand, wire-
gauze and burner.
Material required
Procedure
Precautions
The apparatus used for preparing the sol should be properly cleaned.
Distilled water should be used for preparing sols in water.
Egg albumin sol is prepared at room temperature because in hot solution the precipitation of egg albumin
takes place.
The yellow yolk should be separated completely from the egg albumin before using the later in the
experiment.
Addition of egg albumin should be done very slowly and while constantly stirring so as to disperse the
colloidal particles well in the solution.
Aim : To prepare ferric hydroxide sol
Theory
Ferric hydroxide forms a lyophilic sol. The substance such as metal hydroxides or sulphides are insoluble and
do not really give colloidal solutions on treatment with water are called hydrophobic colloids.
Ferric hydroxide is prepared by the hydrolysis of ferric chloride with boiling distilled water.
Hydrochloric acid which is produced during tries to destabilize the sol and hence must be removed from the sol by
dialysis .
Procedure
Take a 250 ml conical flask and clean it using the steaming out process.
To this cleaned conical flask, add 100 ml of distilled water using a measuring cylinder.
Bring the water to boil by placing the flask over a Bunsen burner.
Add ferric chloride solution dropwise to the boiling water using a dropper.
Continue heating until a deep red or brown solution of ferric hydroxide is obtained.
Note: Replace the water lost by evaporation during boiling at regular intervals.
Keep the contents of the conical flask undisturbed for some time at room temperature.
Label the solution as Ferric Hydroxide Sol.
Precautions
Since ferric hydroxide sol is affected by impurities, the apparatus required for the preparation of sol should
be thoroughly cleaned by the steaming out process.
Add ferric chloride solution dropwise.
Heating is continued till the desired sol is obtained.
Hydrochloric acid formed as a result of hydrolysis of ferric chloride is removed by dialysis process
otherwise it would destabilise the sol.
( To be done on left hand side )
Aim : To prepare aluminium hydroxide sol
Theory
Dialysis is done to remove hydrochloric acid because aluminium hydroxide solis affected by the
presence of ionic impurities.
Materials Required
Procedure
Take a 250 ml conical flask and clean it using the steaming out process.
To this cleaned conical flask, add 100 ml of distilled water using a measuring cylinder.
Bring the water to boil by placing the flask over a Bunsen burner.
Add aluminium chloride solution dropwise to the boiling water using a dropper.
Continue heating until a white coloured solution of aluminium hydroxide is obtained.
Note: Replace the water lost by evaporation during boiling at regular intervals.
Keep the contents of the conical flask undisturbed for some time at room temperature.
Label the solution as Aluminium Hydroxide Sol.
Precautions
The apparatus required for the preparation of the sol should be thoroughly cleaned through
the steaming out process.
Add aluminium chloride solution dropwise.
Heating is continued till the desired sol is obtained.
Hydrochloric acid formed as a result of hydrolysis of aluminium chloride is removed by
dialysis process otherwise it would destabilise the sol.
Expt No ____6_____ Date ___________
VOLUMETRIC ANALYSIS
AIM
To determine the molarity and strength of KMnO4 solution by titrating it against 1/20 M standard solution
of ferrous ammonium sulphate.
MOLECULAR EQUATION
INDICATOR
END POINT
PROCEDURE
(i) Weigh 1.96 g of ferrous ammonium sulphate and transfer it into a 100 mL measuring flask through a
funnel. Transfer the solid sticking to the funnel with the help of distilled water into the flask and add 3 mL of
Conc H2SO4 into the flask drop wise to get the clear solution. Shake the flask till the substance dissolves and
make the solution up to the mark.
(i) Rinse and fill the clean burette with potassium permanganate solution. Remove air bubbles if any, from
the burette tip by releasing some solution through it.
(ii) Rinse the pipette with M/20 Mohr’ s salt and pipette out 10 mL of 0.05 M ferrous ammonium sulphate
solution in a conical flask and add half test tube (≈ 5 mL) full of (2.0 M) H2SO4 to it.
(iii) Titrate the above solution with potassium permanganate solution till the colour of the solution changes to
permanent pink. Swirl the content of the flask during the titration.
(iv) Repeat the titration, until three concordant readings are obtained.
RESULT
3) Molarity of KMnO4 =
4) Strength of KMnO4 =
OBSERVATION AND CALCULATION( To be done on the left hand side )
2 10
3 10
Concordant value = Y mL =
From the overall balanced chemical equation ., it is clear that 2 moles of KMnO4 react with 10 moles of
Mohr’s salt.
MFAS X VFAS
Where
MKMnO4 x = 1/5
0.05 x 10
MKmnO4 = 1 x 0.05 x 10 =
5 x _______
= ______ X 158
__________ g/ L
Expt No ____7_______ Date : ______________
AIM
To determine the concentration/molarity of KMnO4 solution by titrating it against a 1/40 M standard solution
of oxalic acid.
CHEMICAL EQUATION
Molecular equation
2Kmno4+3H2SO4→K2SO4+2MnSO4+3H2O+5[O]
H2C2O4.2H2O+[O]→2CO2+3[H2O]×5
2KMnO4+3H2SO4+5H2C2O4.2H2O→K2SO4+2MnSO4+18H2O+10CO2
Ionic equation
MnO−4+8H++5e−→Mn2++4H2O]×2
C2O2−4→2CO2+2e−]×5
2MnO−4+16H++5C2O2−4→2Mn2++8H2O+10CO2
INDICATOR
END POINT
PROCEDURE
(i) Weigh 0.315 g of oxalic acid and transfer it into a 100 mL measuring flask through a funnel. Transfer
the solid sticking to the funnel with the help of distilled water into the flask. When the oxalic acid in the flask
is completely dissolved , add enough water and make the solution up to the mark.
(i) Rinse and fill a clean burette with potassium permanganate solution. Remove the air bubble, if any, (ii)
Take 10 mL of 0 .025 M oxalic acid solution in a conical flask and add half of the test tube full ( ≈ 5 mL) of
2.0 M H2SO4 to it to prevent the formation of any precipitate of manganese dioxide during the course of the
titration.
(iii) Heat the oxalic acid solution upto 50°– 60°C before titrating it with potassium permanganate solution
taken in the burette.
(iv) Note the initial reading of the volume of permanganate solution in the burette and add it in small
volumes to the hot oxalic acid solution while swirling the contents of the flask gently. The end point is
indicated by the appearance of permanent light pink colour
(v) Repeat the titration till three concordant readings are obtained.
RESULT
3) Molarity of KMnO4 =
4) Strength of KMnO4 =
OBSERVATION AND CALCULATION( To be done on the left hand side )
2 10
3 10
Concordant value = y = mL
From the overall balanced chemical equation ., it is clear that 2 moles of KMnO4 react with 5 moles of oxalic
acid .
Where
MKMnO4 X = 2/5
0.05 x 10
MKmnO4 = 2 x 0.025 x 10 =
5 x _______
= ______ X 158
__________ g/ L
QUALITATIVE ANALYSIS OF INORGANIC SALTS
Preliminary tests
Experiment Observation Inference
Color Colorless/White Fe2+, Fe3+,Mn2+,Co2+,Cu2+may
be absent
4) Smell
Take a pinch of the salt Ammoniacal smell NH4+, may be present
between the fingers and rub it
with a drop of water. Vinegar like smell CH3COO- may be present
Characteristic smell of
ammonia gas is obtained
which gives white fumes when Presence of NH4+
glass rod dipped in Dil HCl is
brought near the mouth of the
test tube.
xiii)
Sublimate formed White sublimate Presence of NH4+
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
If no reaction in cold, add a Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present.
the test tube containing salt
and heat.
Brown ring Test A brown ring is formed at the Presence of NO3- is confirmed
Salt solution + equal volume junction of layers of acid and
of freshly prepares ferrous the solution
sulphate solution.Add a drop
of Conc H2SO4 slowly along
the sides of the test tube.
Sodium chromate
Leadchromate
Soluble complex
Confirmatory Test for CH3COO-
Ester test:
Salt + iml of Conc. H2SO4and Presence of CH3COO-
warm. Add C2H5OH . Add Pleasant fruity smell confirmed
contents in to a beaker full of
water
COOH
COOH COONa
Ester TeST
fruity smell
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
White
White ppt
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Pass H2S gas through the Black precipitate is formed Group II is present (Cu2+,
above solution Pb2+)
O.S + Solid Ammonium Reddish/ White gelatinous Group III is present (Al3+,
chloride + Ammonium precipitate is formed Fe3+)
hydroxide in excess till the
solution become basic.
Part 1 – cool under tap White crystalline precipitate Presence of Pb2+ confirmed
Part 1 + KI solution
Yellow precipitate is formed Pb2+ confirmed
which dissolves in boiling
water crystalizes on cooling
Part 2 + K2CrO4 solution
Yellow precipitate soluble in Pb2+ confirmed
NaOH
Lake test :
Lake test
3) NaOH TEST
BARIUM
Analysis of Group VI
Flame Test:
Absence of Ba2+, Pb2+, Zn2+
Take a small amount of salt on No characteristic colour to the orMn2+, Ca2+ ,Sr2+
a watch glass and make a flame
paste with con. HCl. Heat the
mixture strongly in the flame
Salt in a dry test tube + Conc. Reddish brown vapors with Group II acid radical Br- may
H2SO4 pungent smell be present
Note : chemical equations for the confirmatory tests should be written on un ruled page in
pencil for both acid and basic radicals.
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
RESULT
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3- is
piece of Cu or paper ball to evolved absent
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radical SO42- is confirmed
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
O.S + Solid Ammonium / White gelatinous precipitate Group III is present (Al3+,
chloride + Ammonium is formed Fe3+)
hydroxide in excess till the
solution become basic.
Lake test :
RESULT
Flame Test:
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3- is
piece of Cu or paper ball to evolved absent
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
O.S + SolidAmmonium
chloride + Ammonium Group III is absent
hydroxide in excess till the No precipitate
solution become basic.
Pass H2S gas through the / white precipitate is formed Group IV is present
above solution White (Zn2+)
RESULT
Flame Test:
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the white precipitate is formed Group IV is present
above solution White (Zn2+)
4) Smell
Take a pinch of the salt NH4+, CH3COO- S2- are
between the fingers and rub it No characteristic smell absent
with a drop of water.
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
No white precipitate is
O.S + 1 to 2 ml of Dil. HCl formed Group I is absent
Group IV is absent
Pass H2S gas through the No precipitate
above solution
Analysis of Group VI
RESULT
Flame Test:
Sublimate formed
No White sublimate Absence of NH4+
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
No white precipitate is
O.S + 1 to 2 ml of Dil. HCl formed Group I is absent
Group IV is absent
No precipitate
Pass H2S gas through the
above solution
White precipitate
O.S + Solid Ammonium Group VI (Mg2+) is present
Chloride + Ammonium
Hydroxide + Ammonium
Hydrogen Phosphate
Analysis of Group VI
RESULT
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the
above solution No black precipitate is
formed Group II is absent
RESULT
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
Confirmatory Test for Cl-
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Presence of CO3 2-
Dry heating test
Heat a pinch of the salt in a
dry test tube Colorless odorless gas turning Absence of NH4+
lime water milky
v) Gas evolved
Presence of Ba2+,Sr2+,Ca2+,
Mg2+,Al3+
No White sublimate
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
s liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
RESULT
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the
above solution No black precipitate is
formed Group II is absent
Abesence of NH4+
Sublimate No White sublimate
Residue Brown when hot , yellow Presence of Pb2+
when cold
No characteristic observation
If no reaction in cold, add a Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present.
the test tube containing salt
and heat.
Brown ring Test A brown ring is formed at the Presence of NO3- is confirmed
Salt solution + equal volume junction of layers of acid and
of freshly prepares ferrous the solution
sulphate solution.Add a drop
of Conc H2SO4 slowly along
the sides of the test tube.
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is Present
O.S + 1 to 2 ml of Dil. HCl white precipitate is formed
Part 1 – cool under tap White crystalline precipitate Presence of Pb2+ confirmed
RESULT
Aim : To Test the presence of Alcoholic Group in the given sample of organic compound
ESTER TEST H+
white fumes
Aim : To Test the presence of a for phenolic Group in the given sample of organic compound
violet complex
Tollens test
2gA(NH3)2 -
+ CH3CHO + 3 OH- CH3COO + 2Ag + 4NH3 + 2H2O
Fehling’s test
RED
Aim : To Test the presence of a for ketonic Group in the given sample of organic compound
2, 4 DNPH Test
Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test tube
effervescence carboxylic
Carbonate and add a pinch of sodium bicarbonate to it.
is observed. group.
Test
The given sample of organic compound has carboxylic acid group in it.
Aim : To Test the presence of a for Amino Group in the given sample of organic compound
Solubility Test
Aim : To identify the functional group present in the given compound with relevant chemical
test
Physical Tests:
Chemical Tests:
Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test tube
effervescence carboxylic
Carbonate and add a pinch of sodium bicarbonate to it.
is observed. group.
Test
It is a clear, volatile liquid with a characteristic pleasant odor, and a burning taste. It is completely miscible
with water in all ratios and with organic solvents. Melting point: -117 °C and Boiling point: 78 °C
Chemical Tests:
Physical Tests:
Smell
Chemical Tests
Physical Tests:
Smell : Smell
Chemical Tests
Experiment Procedure Observation Inference
Take a small quantity of the given compound in a
Violet colour
m- clean test tube and add about 0.1g of finely Presence of
is formed
Dinitrobenzene powdered m-dinitrobenzene. Now add about 1 ml ketonic group
which slowly
Test of dilute sodium hydroxide solution and shake it is confirmed.
fades away.
well.
Dissolve a small quantity of sodium nitroprusside
Sodium in about 1 ml of distilled water in a clean test tube Presence of
Red
nitroprusside and then add a small quantity of the given ketonic group
colouration.
Test compound. Shake the test tube well and add is confirmed.
sodium hydroxide solution dropwise.
Physical Tests:
Chemical Tests
Physical Tests:
Smell :
Chemical Tests
Physical Tests:
Smell :
Chemical Tests
BIOMOLECULAR ANALYSIS
This test is based on the fact that oils and fats are soluble in
organic solvents 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 three test-
tubes and observe the solubility
1)Water i) Sample is
Solubility
Test immiscible
3) Sample is
3)Chloroform miscible
Expt No 21 Date :
Aim : To detect the presence of carbohydrates ,fats and proteins in different samples of food
stuffs
Result:
Result:
III ELECTROCHEMISTRY
3 To study the variation of cell potential in Zn/Zn2+//Cu2+/ Cu cell with change in concentration of
electrolytes at room temperature.
IV CHEMICAL KINETICS
4 To study the effect of concentration on the rate of reaction between sodium thiosulphate and
Hydrochloric acid
V SURFACE CHEMISTRY
5 Preparation of colloidal solution of starch , egg albuin , Ferric hydroxide and Aluminium
hydroxide.
VI VOLUMETRIC ANALYSIS
6 Determination of molarity and strength of KmnO4 solution using M/20 solution of ferrous
ammonium sulphate
7 Determination of molarity and strength of KmnO4 solution using M/40 solution of oxalic acid
Aim :
Mohr’s salt is prepared by dissolving an equimolar mixture of hydrated ferrous sulphate and ammonium
sulphate in water containing a little sulphuric acid and then subjecting the resulting solution to crystallization
when light green crystals of ferrous ammonium sulphate separate out.
Materials Required
Ferrous sulphate, Ammonium sulphate,m Dil. Sulphuric acid, Ethyl alcohol,Beakers, China
dish, Funnel, Glass rod, Tripod stand, Wire gauze, Wash bottle , Measuring jar
Procedure
21. First take 7g ferrous sulphate 3.5g ammonium sulphate in a clean 250ml beaker.
22. To this add about 2-3ml of dil.sulphuric acid to prevent the hydrolysis of ferrous sulphate.
23. In another beaker, boil about 20ml of water for 5 minutes.
24. Add the boiling hot water to the contents in the first beaker in small quantities at a time.
25. Stir the contents of the beaker with a glass rod until the salts have completely dissolved.
26. Filter the solution into a china dish.
27. Now heat the solution in the china dish until its crystallisation point is reached. Then transfer
the solution into a crystallising dish and keep it undisturbed.
28. On cooling, crystals of Mohr’s salt separate.
29. Decant the mother liquor and wash the crystals with a small quantity of alcohol and then dry
the crystals by placing them between filter paper pads.
30. Find the weight of the crystals.
Observations
Theory
Potash alum is prepared by dissolving an equimolar mixture of hydrated aluminium sulphate in minimum
amount of water containing a little of sulphuric acid anfd then subjecting the solution to crystallization , when
octahedral crystals of potash alum separate out.
Materials Required
Potassium sulphate, Aluminium sulphate, Dil. Sulphuric acid, Distilled water, Beakers, China
dish, Funnel,Glass rod, Tripod stand, Wire gauze, Burner, Wash bottle, Measuring jar
Procedure
Observations
Theory
Acetanilide is prepared by acetylating aniline with acetic anhydride in the presence of glacial acetic
acid
Materials Required
Procedure
15. Take 5ml of acetic anhydride in a clean dry 250ml RB flask and add 5 ml of glacial acetic
acid and shake the contents thoroughly.
16. To this mixture add 5ml of aniline and fit a water condenser.
17. Boil this mixture over a sand bath for 10min.
18. Pour the liquid from the RB flask into 200ml ice-cold water taken in a beaker. While adding
stir the contents of the beaker vigorously using a glass rod.
19. Filter the white precipitate formed and wash it with cold water.
20. Recrystallise from hot water containing a few drops of etanol . Weigh the crystals and record
the yield
21. Determinre the melting point of the compound.
Observation
The weight of acetanilide = 3g
Melting point = 1130c
Precautions
Theory
The nitration of aniline is difficult to carry out with nitrating mixture since –NH2 gets oxidized . So the amini
group is first protected by acetylation to form acetanilide which is then nitrated to give p- nitroacetanide as
amajor product. And o – nitro acetanide as a minor product. Recrystallisation from ethanol readily removes
the more soluble ortho compound .
Materials Required
Acetanilide- 5g ,Glacial acetic acid- 5ml,Conc.sulphuric acid -10ml, Fuming nitric acid -2ml
Procedure
13. Take 5g powdered acetanilide and 5ml of glacial acetic acid in a conical flask and stir the
mixture using a glass rod.
14. Take 2ml of fuming nitric acid in a clean test tube and cool it in a freezing mixture taken in a
beaker. Carefully add 2ml of conc.sulphuric acid drop by drop while constantly shaking and
cooling it.
15. Add 8ml of conc.sulphuric acid drop by drop into the conical flask containing acetanilide and
glacial acetic acid and cool it in a freezing mixture. Stir the contents and wait until the
temperature becomes less than 5oC.
16. To the cooled contents in the flask, add the nitrating mixture prepared in the 2nd step, drop
by drop while stirring constantly. While adding the nitrating mixture, the temperature of the
mixture in the flask should not rise above 25oC. Remove the conical flask from the freezing
mixture and allow it to stand for 30min at room temperature.
17. Pour the contents of the flask into a beaker containing crushed ice. Stir it well and filter the
precipitate obtained and wash it thoroughly with cold water.
18. Recrystallisation of p-Nitro acetanilide: Dissolve the precipitate obtained above in 20ml
methylated spirit. Warm it to get a clear solution. Filter the hot solution and cool the filtrate
in ice. P-Nitro acetanilide is obtained as colourless crystals. Wash the crystals with cold
water and then dry the crystals and measure the weight of the crystals.
Observation
The weight of p-nitroacetanilide = 3.5 g
Melting point : = 2140c
Precautions
ELECTRO CHEMISTRY
Aim : To study the variation of cell potential in Zn/Zn2+//Cu2+/ Cu cell with change in concentration of
electrolytes at room temperature.
Theory
Reduction potential of an electrode increases with increase in concentration of the electrolyte.
Mn+(aq)+ne– ———->M(s)
In the zinc-copper electrochemical cell zinc electrode acts as anode while copper electrode acts as cathode.
Procedure
Repeat the experiment by taking different concentrations of zinc sulphate and copper sulphate solutions.
Conclusion
EMF of the cell increases with decrease in cone, of the electrolyte around anode and increase in cone, of the
electrolyte around cathode.
( To be done on the left hand side )
1M 1M 1.1V
1M 0.5M 1.091V
1M 0.025M 1.052V
1M 0.0125M 1.043V
0.5M 1M 1.108V
0.025M 1M 1.147V
0.0125M 1M 1.156V
Expt No 4 Date:
CHEMICAL KINETICS
AIM :
To study the effect of concentration on the rate of reaction between sodium thiosulphate
and hydrochloricacid.
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 the increase in the concentration of the reactants. The effect of concentration of reactants on
rate of a reaction can be studied easily by the reaction between sodium thiosulphate and hydrochloric
acid.
Na2S203 + 2HCl ——–> S(s) + 2NaCl(aq) + SO2(g) + H2O(l)
The insoluble sulphur, formed during the reaction, gives a milky appearance and makes the solution
opaque. Therefore, rate of reaction can be studied by measuring the time taken to produce enough
sulphur to make some mark invisible on a paper kept under the conical flask in which the reaction is
carried out.
Apparatus
Pipette (10 ml), stop-watch, two burettes and five conical flasks (100 ml).
Materials
Procedure
15. Wash the conical flasks with water and label them as 1, 2, 3, 4 and 5 respectively.
16. With the help of a burette, add 10, 20, 30, 40 and 50 ml of 0.1 M Na2S2O3 solution to the
flasks 1, 2, 3, 4 and 5 respectively.
17. Now add 40, 30, 20 and 10 ml of distilled water to the flask 1, 2, 3 and 4 respectively so that
volume of solution in each flask is 50 ml.
18. Take 10 ml of 1M HCl in a test tube with the help of a burette.
19. Add 10 ml of hydrochloric acid taken in a test tube to the conical flask No. 1 containing 10 ml
of 0.1 M Na2S2O3 and 40 ml of distilled water and start the stop-watch.
When half of the hydrochloric acid solution has been added. Shake the contents of the conical
flask and place it on the tile with a cross mark as shown in Fig.
20. Go on observing from top to downwards in the flask and stop the stop-watch when the cross
mark just becomes invisible. Note down the time.
21. Repeat the experiment by adding 10 ml of 1M HCl to flasks 2, 3,4 and 5 and record the time
taken in each case for the cross to become just invisible.
Result
From the graph, it is clear that 1/t is directly proportional to the cone, of Na2S2O3 solution. But y is a
direct measure of rate of the reaction, therefore, rate of the reaction between Na2S2O3 and HCl is
directly proportional to the cone, of Na2S2O3 solution taken. Hence, rate of this reaction is directly
proportional to the concentration of Na2S2O3, which is one of the reactants.
Note. It may be noted that the reaction rate also increases when the amount of sodium thiosulphate is
kept constant but the concentration of hydrochloric acid is increased.
Precautions
13. The apparatus must be thoroughly clean. If the same conical flask is to be used again and
again, it should be thoroughly washed with cone. HNO3 and then with water.
14. Measure the volumes of sodium thiosulphate solution, hydrochloric acid and distilled water
very accurately.
15. Use the same tile with the same cross-mark for all observation,
16. Complete the experiment at one time only so that there is not much temperature variation.
17. Start the stop-watch immediately when half of the hydrochloric acid solution has been added
to sodium thiosulphate solution.
18. View the cross-mark through the reaction mixture from top to bottom from same height for all
observations.
( To be done on the left hand side)
Observations
4 40 10 50 0.08 10 60 0.0167
5 50 0 50 0.10 10 159
0.006
Plot a graph between 1/t (in seconds) and the concentration of sodium thiosulphate by taking 1/t along
ordinate (vertical axis) and cone, of Na2S2O3 along abscissa (horizontal axis). It should be a straight sloping
line.
Expt No : 5 Date :
SURFACE CHEMISTRY
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.
Apparatus
Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar, tripod stand, wire-
gauze and burner.
Materials Required
Soluble starch (500 mg) and distilled water.
Procedure
13. Take 500 mg of starch in a mortar and add few ml of distilled water.
14. Grind the starch to make a thin paste and transfer this paste to a 50 ml beaker.
15. Take about 100 ml of distilled water in a 250 ml beaker and heat the beaker so that water starts
boiling.
16. Pour the paste slowly with stirring into boiling water in the beaker (Fig. 2.1).
17. Continue boiling for about 10 minutes and there allow the beaker to cool.
18. Filter the contents of the beaker through a filter-paper, fixed in a funnel.
Label the filtrate ‘Starch Sol’.
Precautions
11. The apparatus used for preparing sol should be properly cleaned.
12. Distilled water should be used for preparing sols in water.
13. Starch should be converted into a fine paste before adding to boiling water.
14. Starch paste should be added in a thin stream to boiling water.
15. Constant stirring of the contents is necessary during the preparation of the sol.
( To be done on the left hand side )
‘
Aim: To prepare colloidal solution of egg albumin
Theory
Egg albumin which is obtained from eggs forms lyophilic sols with cold water. The sol is quite stable and is
not affected by the presence of traces of impurities.
Apparatus
Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar, tripod stand, wire-
gauze and burner.
Material required
Procedure
Precautions
The apparatus used for preparing the sol should be properly cleaned.
Distilled water should be used for preparing sols in water.
Egg albumin sol is prepared at room temperature because in hot solution the precipitation of egg albumin
takes place.
The yellow yolk should be separated completely from the egg albumin before using the later in the
experiment.
Addition of egg albumin should be done very slowly and while constantly stirring so as to disperse the
colloidal particles well in the solution.
Aim : To prepare ferric hydroxide sol
Theory
Ferric hydroxide forms a lyophilic sol. The substance such as metal hydroxides or sulphides are insoluble and
do not really give colloidal solutions on treatment with water are called hydrophobic colloids.
Ferric hydroxide is prepared by the hydrolysis of ferric chloride with boiling distilled water.
Hydrochloric acid which is produced during tries to destabilize the sol and hence must be removed from the sol by
dialysis .
Procedure
Take a 250 ml conical flask and clean it using the steaming out process.
To this cleaned conical flask, add 100 ml of distilled water using a measuring cylinder.
Bring the water to boil by placing the flask over a Bunsen burner.
Add ferric chloride solution dropwise to the boiling water using a dropper.
Continue heating until a deep red or brown solution of ferric hydroxide is obtained.
Note: Replace the water lost by evaporation during boiling at regular intervals.
Keep the contents of the conical flask undisturbed for some time at room temperature.
Label the solution as Ferric Hydroxide Sol.
Precautions
Since ferric hydroxide sol is affected by impurities, the apparatus required for the preparation of sol should
be thoroughly cleaned by the steaming out process.
Add ferric chloride solution dropwise.
Heating is continued till the desired sol is obtained.
Hydrochloric acid formed as a result of hydrolysis of ferric chloride is removed by dialysis process
otherwise it would destabilise the sol.
( To be done on left hand side )
Aim : To prepare aluminium hydroxide sol
Theory
Dialysis is done to remove hydrochloric acid because aluminium hydroxide solis affected by the
presence of ionic impurities.
Materials Required
Procedure
Take a 250 ml conical flask and clean it using the steaming out process.
To this cleaned conical flask, add 100 ml of distilled water using a measuring cylinder.
Bring the water to boil by placing the flask over a Bunsen burner.
Add aluminium chloride solution dropwise to the boiling water using a dropper.
Continue heating until a white coloured solution of aluminium hydroxide is obtained.
Note: Replace the water lost by evaporation during boiling at regular intervals.
Keep the contents of the conical flask undisturbed for some time at room temperature.
Label the solution as Aluminium Hydroxide Sol.
Precautions
The apparatus required for the preparation of the sol should be thoroughly cleaned through
the steaming out process.
Add aluminium chloride solution dropwise.
Heating is continued till the desired sol is obtained.
Hydrochloric acid formed as a result of hydrolysis of aluminium chloride is removed by
dialysis process otherwise it would destabilise the sol.
Expt No ____6_____ Date ___________
VOLUMETRIC ANALYSIS
AIM
To determine the molarity and strength of KMnO4 solution by titrating it against 1/20 M standard solution
of ferrous ammonium sulphate.
MOLECULAR EQUATION
INDICATOR
END POINT
PROCEDURE
(i) Weigh 1.96 g of ferrous ammonium sulphate and transfer it into a 100 mL measuring flask through a
funnel. Transfer the solid sticking to the funnel with the help of distilled water into the flask and add 3 mL of
Conc H2SO4 into the flask drop wise to get the clear solution. Shake the flask till the substance dissolves and
make the solution up to the mark.
(i) Rinse and fill the clean burette with potassium permanganate solution. Remove air bubbles if any, from
the burette tip by releasing some solution through it.
(ii) Rinse the pipette with M/20 Mohr’ s salt and pipette out 10 mL of 0.05 M ferrous ammonium sulphate
solution in a conical flask and add half test tube (≈ 5 mL) full of (2.0 M) H2SO4 to it.
(iii) Titrate the above solution with potassium permanganate solution till the colour of the solution changes to
permanent pink. Swirl the content of the flask during the titration.
(iv) Repeat the titration, until three concordant readings are obtained.
RESULT
5) Molarity of KMnO4 =
6) Strength of KMnO4 =
OBSERVATION AND CALCULATION( To be done on the left hand side )
2 10
3 10
Concordant value = Y mL =
From the overall balanced chemical equation ., it is clear that 2 moles of KMnO4 react with 10 moles of
Mohr’s salt.
MFAS X VFAS
Where
MKMnO4 x = 1/5
0.05 x 10
MKmnO4 = 1 x 0.05 x 10 =
5 x _______
= ______ X 158
__________ g/ L
Expt No ____7_______ Date : ______________
AIM
To determine the concentration/molarity of KMnO4 solution by titrating it against a 1/40 M standard solution
of oxalic acid.
CHEMICAL EQUATION
Molecular equation
2Kmno4+3H2SO4→K2SO4+2MnSO4+3H2O+5[O]
H2C2O4.2H2O+[O]→2CO2+3[H2O]×5
2KMnO4+3H2SO4+5H2C2O4.2H2O→K2SO4+2MnSO4+18H2O+10CO2
Ionic equation
MnO−4+8H++5e−→Mn2++4H2O]×2
C2O2−4→2CO2+2e−]×5
2MnO−4+16H++5C2O2−4→2Mn2++8H2O+10CO2
INDICATOR
END POINT
PROCEDURE
(i) Weigh 0.315 g of oxalic acid and transfer it into a 100 mL measuring flask through a funnel. Transfer
the solid sticking to the funnel with the help of distilled water into the flask. When the oxalic acid in the flask
is completely dissolved , add enough water and make the solution up to the mark.
(i) Rinse and fill a clean burette with potassium permanganate solution. Remove the air bubble, if any, (ii)
Take 10 mL of 0 .025 M oxalic acid solution in a conical flask and add half of the test tube full ( ≈ 5 mL) of
2.0 M H2SO4 to it to prevent the formation of any precipitate of manganese dioxide during the course of the
titration.
(iii) Heat the oxalic acid solution upto 50°– 60°C before titrating it with potassium permanganate solution
taken in the burette.
(iv) Note the initial reading of the volume of permanganate solution in the burette and add it in small
volumes to the hot oxalic acid solution while swirling the contents of the flask gently. The end point is
indicated by the appearance of permanent light pink colour
(v) Repeat the titration till three concordant readings are obtained.
RESULT
5) Molarity of KMnO4 =
6) Strength of KMnO4 =
OBSERVATION AND CALCULATION( To be done on the left hand side )
2 10
3 10
Concordant value = y = mL
From the overall balanced chemical equation ., it is clear that 2 moles of KMnO4 react with 5 moles of oxalic
acid .
Where
MKMnO4 X = 2/5
0.05 x 10
MKmnO4 = 2 x 0.025 x 10 =
5 x _______
= ______ X 158
__________ g/ L
QUALITATIVE ANALYSIS OF INORGANIC SALTS
Preliminary tests
Experiment Observation Inference
Color Colorless/White Fe2+, Fe3+,Mn2+,Co2+,Cu2+may
be absent
4) Smell
Take a pinch of the salt Ammoniacal smell NH4+, may be present
between the fingers and rub it
with a drop of water. Vinegar like smell CH3COO- may be present
Characteristic smell of
ammonia gas is obtained
which gives white fumes when Presence of NH4+
glass rod dipped in Dil HCl is
brought near the mouth of the
test tube.
xxiv)
Sublimate formed White sublimate Presence of NH4+
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
If no reaction in cold, add a Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present.
the test tube containing salt
and heat.
Brown ring Test A brown ring is formed at the Presence of NO3- is confirmed
Salt solution + equal volume junction of layers of acid and
of freshly prepares ferrous the solution
sulphate solution.Add a drop
of Conc H2SO4 slowly along
the sides of the test tube.
Sodium chromate
Leadchromate
Soluble complex
Confirmatory Test for CH3COO-
Ester test:
Salt + iml of Conc. H2SO4and Presence of CH3COO-
warm. Add C2H5OH . Add Pleasant fruity smell confirmed
contents in to a beaker full of
water
COOH
COOH COONa
Ester TeST
fruity smell
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
White
White ppt
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Pass H2S gas through the Black precipitate is formed Group II is present (Cu2+,
above solution Pb2+)
O.S + Solid Ammonium Reddish/ White gelatinous Group III is present (Al3+,
chloride + Ammonium precipitate is formed Fe3+)
hydroxide in excess till the
solution become basic.
Part 1 – cool under tap White crystalline precipitate Presence of Pb2+ confirmed
Part 1 + KI solution
Yellow precipitate is formed Pb2+ confirmed
which dissolves in boiling
water crystalizes on cooling
Part 2 + K2CrO4 solution
Yellow precipitate soluble in Pb2+ confirmed
NaOH
Lake test :
Lake test
5) NaOH TEST
BARIUM
Analysis of Group VI
Flame Test:
Absence of Ba2+, Pb2+, Zn2+
Take a small amount of salt on No characteristic colour to the orMn2+, Ca2+ ,Sr2+
a watch glass and make a flame
paste with con. HCl. Heat the
mixture strongly in the flame
Salt in a dry test tube + Conc. Reddish brown vapors with Group II acid radical Br- may
H2SO4 pungent smell be present
Note : chemical equations for the confirmatory tests should be written on un ruled page in
pencil for both acid and basic radicals.
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
RESULT
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3- is
piece of Cu or paper ball to evolved absent
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radical SO42- is confirmed
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
O.S + Solid Ammonium / White gelatinous precipitate Group III is present (Al3+,
chloride + Ammonium is formed Fe3+)
hydroxide in excess till the
solution become basic.
Lake test :
RESULT
Flame Test:
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3- is
piece of Cu or paper ball to evolved absent
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
O.S + SolidAmmonium
chloride + Ammonium Group III is absent
hydroxide in excess till the No precipitate
solution become basic.
Pass H2S gas through the / white precipitate is formed Group IV is present
above solution White (Zn2+)
RESULT
Flame Test:
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the white precipitate is formed Group IV is present
above solution White (Zn2+)
4) Smell
Take a pinch of the salt NH4+, CH3COO- S2- are
between the fingers and rub it No characteristic smell absent
with a drop of water.
If no reaction in cold, add a No Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present
the test tube containing salt
and heat.
1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed
Salt solution + Lead acetate + White precipitate is obtained Presence of Group III acid
Aetic acid radica SO42- is confirmed
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
No white precipitate is
O.S + 1 to 2 ml of Dil. HCl formed Group I is absent
Group IV is absent
Pass H2S gas through the No precipitate
above solution
Analysis of Group VI
RESULT
Flame Test:
Sublimate formed
No White sublimate Absence of NH4+
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
No white precipitate is
O.S + 1 to 2 ml of Dil. HCl formed Group I is absent
Group IV is absent
No precipitate
Pass H2S gas through the
above solution
White precipitate
O.S + Solid Ammonium Group VI (Mg2+) is present
Chloride + Ammonium
Hydroxide + Ammonium
Hydrogen Phosphate
Analysis of Group VI
RESULT
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the
above solution No black precipitate is
formed Group II is absent
RESULT
Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl- may
H2SO4 gas which gives a dense white be present
fumes with glass rod dipped in
ammonium hydroxide is
exposed to the mouth of the
test tube
Confirmatory Test for Cl-
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Presence of CO3 2-
Dry heating test
Heat a pinch of the salt in a
dry test tube Colorless odorless gas turning Absence of NH4+
lime water milky
ix) Gas evolved
Presence of Ba2+,Sr2+,Ca2+,
Mg2+,Al3+
No White sublimate
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
s liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
RESULT
Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless odorless is present (CO32-)
gas
Confirmatory Test
1) Salt + Dil HCl , pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is absent
O.S + 1 to 2 ml of Dil. HCl No white precipitate is
formed
Pass H2S gas through the
above solution No black precipitate is
formed Group II is absent
Abesence of NH4+
Sublimate No White sublimate
Residue Brown when hot , yellow Presence of Pb2+
when cold
No characteristic observation
If no reaction in cold, add a Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present.
the test tube containing salt
and heat.
Brown ring Test A brown ring is formed at the Presence of NO3- is confirmed
Salt solution + equal volume junction of layers of acid and
of freshly prepares ferrous the solution
sulphate solution.Add a drop
of Conc H2SO4 slowly along
the sides of the test tube.
Detection of Basic radical:
Preparation of original solution(O S)
About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling tube in
the following order.
Group I is Present
O.S + 1 to 2 ml of Dil. HCl white precipitate is formed
Part 1 – cool under tap White crystalline precipitate Presence of Pb2+ confirmed
RESULT
Aim : To Test the presence of Alcoholic Group in the given sample of organic compound
ESTER TEST H+
white fumes
Aim : To Test the presence of a for phenolic Group in the given sample of organic compound
violet complex
Tollens test
2gA(NH3)2 -
+ CH3CHO + 3 OH- CH3COO + 2Ag + 4NH3 + 2H2O
Fehling’s test
RED
Aim : To Test the presence of a for ketonic Group in the given sample of organic compound
2, 4 DNPH Test
Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test tube
effervescence carboxylic
Carbonate and add a pinch of sodium bicarbonate to it.
is observed. group.
Test
The given sample of organic compound has carboxylic acid group in it.
Aim : To Test the presence of a for Amino Group in the given sample of organic compound
Solubility Test
Aim : To identify the functional group present in the given compound with relevant chemical
test
Physical Tests:
Chemical Tests:
Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test tube
effervescence carboxylic
Carbonate and add a pinch of sodium bicarbonate to it.
is observed. group.
Test
It is a clear, volatile liquid with a characteristic pleasant odor, and a burning taste. It is completely miscible
with water in all ratios and with organic solvents. Melting point: -117 °C and Boiling point: 78 °C
Chemical Tests:
Physical Tests:
Smell
Chemical Tests
Physical Tests:
Smell : Smell
Chemical Tests
Experiment Procedure Observation Inference
Take a small quantity of the given compound in a
Violet colour
m- clean test tube and add about 0.1g of finely Presence of
is formed
Dinitrobenzene powdered m-dinitrobenzene. Now add about 1 ml ketonic group
which slowly
Test of dilute sodium hydroxide solution and shake it is confirmed.
fades away.
well.
Dissolve a small quantity of sodium nitroprusside
Sodium in about 1 ml of distilled water in a clean test tube Presence of
Red
nitroprusside and then add a small quantity of the given ketonic group
colouration.
Test compound. Shake the test tube well and add is confirmed.
sodium hydroxide solution dropwise.
Physical Tests:
Chemical Tests
Physical Tests:
Smell :
Chemical Tests
Physical Tests:
Smell :
Chemical Tests
BIOMOLECULAR ANALYSIS
This test is based on the fact that oils and fats are soluble in
organic solvents 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 three test-
tubes and observe the solubility
1)Water i) Sample is
Solubility
Test immiscible
3) Sample is
3)Chloroform miscible
Expt No 21 Date :
Aim : To detect the presence of carbohydrates ,fats and proteins in different samples of food
stuffs
Result:
Result:
Result :
Ninhydrin Test.. Take about 2 ml of egg albumin dispersion in a test-tube Intense blue presence
and add 3-4 drops of Ninhydrin solution colouration of protein
This test is based on the fact that oils and fats are soluble in
organic solvents 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 three test-
tubes and observe the solubility
1)Water i) Sample is
Solubility
Test immiscible
3) Sample is
3)Chloroform miscible
Expt No 21 Date :
Aim : To detect the presence of carbohydrates ,fats and proteins in different samples of food
stuffs
Food sample Sample A Sample B Sample C Sample D
Taste Sweet Sweet Sweet Sweet
Solubility Soluble Soluble Soluble In soluble
Molisch’s Test Purple ring Purple ring Purple ring Purple ring
Fehling Test Red ppt Red ppt No Red ppt No Red ppt
Tollens test Shining silver Shining silver No silver mirror No silver mirror
mirror mirror
Iodine Test No blue No blue No blue blue colouration
colouration colouration colouration
Result:
Result :