CHEMISTRY PRACTICAL WORK

INDEX
I. Basic Laboratory Techniques
1. BUNSEN BURNER
2. TEST TUBES
3. FLASKS, BEAKERS AND SEPARATING FUNNELS
4. MEASURING VOLUME OF LIQUIDS
II. Physical Chemistry Experiments
1. STUDY OF VARIATION OF CELL POTENTIAL WITH CHANGE IN CONCENTRATION
2. STUDY OF SHIFT IN EQUILIBRIUM WITH CHANGE IN CONCENTRATION OF REACTANTS
III. Volumetric Analysis
A. ALKALIMETRY
1. Expt. No.1: ESTIMATION OF NaOH
2. Expt. No.3: ESTIMATION OF KOH
B. ACIDIMETRY
1. Expt. No.2: ESTIMATION OF NITRIC ACID
2. Expt. No.6: ESTIMATION OF SULPHURIC ACID
C. REDOX TITRATIONS – PERMANGANOMETRY
1. Expt. No.4: ESTIMATION OF MOHR’S SALT
2. Expt. No.5: ESTIMATION OF OXALIC ACID
IV. Reactions of anions and cations
V. Salt Analysis
SALT NO. 1
SALT NO. 2
SALT NO. 3
SALT NO. 4
SALT NO. 5
SALT NO. 6
SALT NO. 7
SALT NO. 8
VI. Reactions of Organic Compounds
1. Reactions of Carboxylic acid
2. Reactions of Phenol
3. Reactions of amines
4. Reactions of Aldehydes
5. Reactions of Ketones
 BASIC LABORATORY TECHNIQUES
1. BUNSEN BURNER
(A) Parts of Bunsen Burner
a. The Base
Heavy metallic base is connected to a side tube called gas tube. Gas from the source enters
the burner through the gas tube and passes through a small hole called Nipple or Nozzle and
enters into the burner tube under increased pressure and can be burnt at the upper end of
the burner tube.
b. The Burner Tube
It is a long metallic tube having two holes diametrically opposite to each other near the
lower end which form the air vent. The tube can be screwed at the base. The gas coming
from the nozzle mixes with the air coming through the air vent and burns at its upper end.
c. The Air Regulator
It is a short metallic cylindrical sleeve with two holes diametrically opposite to each other.
When it is fitted to the burner tube, it surrounds the air vent of the burner tube. To control
the flow of air through the air vent, size of its hole is adjusted by rotating the sleeve.

Fig. 1.1 : Bunsen burner Fig. 1.2 : Parts of Bunsen burner

When the flow of air is correctly adjusted, the temperature of the flame becomes quite high.
This is called non-luminous flame. Various zones of flame are shown below in Fig. 1.3.
 Fig. 1.3 : Zones of flame of Bunsen burner
(B) Principal Parts of Bunsen Flame
i. The Inner Dark Cone, A E C
This is innermost dark cone, which is just above the burner tube. It consists of unburnt
gases. This zone is the coldest zone of the flame and no combustion takes place here.
ii. The Middle Blue Cone, A D C E A
This is middle part of the flame. This becomes luminous when the air vent is slightly closed.
Luminosity of this part is due to the presence of unburnt carbon particles produced by
decomposition of some gas. These particles get heated up to incandescence and glow but do
not burn. Since the combustion is not complete in this part, the temperature is not very
high.
iii. The Outer Non-luminous Mantle, A B C D A
This is purplish outer cone. It is the hottest part of the flame. It is in direct contact with the
atmosphere and combustion is quite complete in this zone.
(C) Striking Back of the Bunsen Burner
Striking back is the phenomenon in which flame travels down the burner tube and begins to
burn at the nozzle near the base. This happens when vents are fully open. The flow of much
air and less gas makes the flame become irregular and it strikes back. The tube becomes
very hot and it may produce burns on touching. This may melt attached rubber tube also. If
it happens, put off the burner and cool it under the tap and light it again by keeping the air
vent partially opened.
 2. TEST TUBES
Test tubes of different volumes are available but usually for this level of chemistry practical
work, test tubes of 125 mm (length) × 15 mm (diameter), 150 mm (length) × 15 mm
(diameter) and 150 mm (length) × 25 mm (diameter) are used. Test tubes are available with
or without rim around the mouth. Test tubes of smaller width are used for carrying out
reactions, which do not require heating or when heating is required for a short period. Only
one third of the test tube should be filled while carrying out a reaction. The test tube of
bigger diameter is called boiling tube. It is used when large volume of solution is required to
be heated. Test tube holder is used to hold a test tube while heating a mixture or solution in
it. Test tube stand should be used to keep test tubes containing solutions in the upright
position (Fig.1.4).

Fig. 1.4 : Stand carrying boiling tubes and test tubes of different sizes
 3. FLASKS, BEAKERS AND SEPARATING FUNNELS
Mostly round bottom and conical flasks (also called Erlenmeyer flask) are used in chemistry
laboratory. These are available in various capacities ranging from 5 mL-2000 mL. Choice of
the size and type depends upon the amount of solution to be handled and the type of
reaction to be carried out. Generally, for heating or refluxing a reaction mixture contained in
a round bottom flask, direct flame / sand bath / water bath, is used. Conical flasks are
employed for carrying out certain reactions at room temperature or lower temperatures.
These are specially used for carrying out volumetric titrations.

Beakers of various capacities ranging from 5 mL to 2000 mL are available and are employed
for the purpose of preparing solutions, for carrying out precipitation reactions and for
evaporation of solvents etc.

Separating funnels are used for separating immiscible liquids. Separating funnels of various
sizes and shapes are available (Fig. 1.5).

Fig. 1.5 : Separating funnels of various shapes

 4. MEASURING VOLUME OF LIQUIDS
Usually volumetric flasks, graduated cylinders, pipettes and burettes are used for measuring
volume of liquids. Volumetric flasks and cylinders are graduated to measure volume of a
liquid at a certain temperature. Pipettes and burettes are calibrated to deliver certain
specific volume of a liquid at a specified temperature. The capacity mark is usually etched on
the glass of the equipment. Aqueous solutions wet the glass surface, therefore these form
concave meniscuses when filled in these equipment. Central part of the meniscus is rather
flat (Fig. 1.5 a).

Fig. 1.5 : (a) Water forming curved surface in the glass apparatus
(b) Noting the reading
Calibration of the apparatus coinciding with this flat portion of the meniscus gives a measure
of the volume of the liquid. Therefore, while making final adjustment of volume or noting
the reading, the curved surface of the liquid should appear touching the etched mark when
viewed by keeping the eye level aligned to the etched mark (Fig. 1.5 b). This helps in
avoiding the parallax errors (error caused by the change in position of the observer). Note
that if the liquid forms convex meniscus or is coloured and opaque e.g. KMnO4 solution then
reading coinciding with upward surface is noted. In flasks and pipettes capacity mark is
etched on the narrow part of the equipment to minimize the error in noting the level of
meniscus. Graduated cylinders are not used for very precise measurements, so they need
not be narrow. Burettes and pipettes are used to measure the volume of a liquid accurately.
Measuring Cylinder Burette Pipette
 PHYSICAL CHEMISTRY EXPERIMENTS
Experiment No.1
STUDY OF VARIATION OF CELL POTENTIAL WITH CHANGE IN CONCENTRATION
Aim:
To study the variation in cell potential of the cell Zn|Zn2+||Cu2+|Cu with change in
concentration of electrolytes (CuSO4 /ZnSO4 ) at room temperature.
Theory :
The cell under investigation in this experiment is represented as follows:
Zn(s)|Zn2+(aq., 1.0M) ||Cu2+(aq., x M)|Cu(s)
Here x M denotes varying concentrations of Cu2+(aq) ions. In other words, to study the
variation in cell potential with concentration, the concentration of Cu2+ (aq.) is varied while
that of Zn2+ (aq) is kept constant. The measured cell potential enables us to calculate the
electrode potential of Cu2+/Cu electrode for each concentration of copper (II) ions. This
variation is theoretically depicted according to Nernst equation. The variation in the
electrode potential of Cu2+/Cu electrode consequently brings variation in the cell potential
according to the relation: Ecell = E Cu2+/Cu − E Zn2+ /Zn . This equation clearly suggests that even if
E Zn /Zn is kept constant, the variation in E Cu /Cu would bring corresponding variation in Ecell
2+ 2+

(cell potential). Similarly, keeping the concentration of Cu2+ ions constant, one can study the
variations in the cell potential with the variation in concentration of Zn2+ ions.
Material Required :
• Zinc plate : One
• Copper plate : One
• Beaker (50 mL) : Six
• Voltmeter (Potentiometer) : One
• Salt bridge : One

Fig.1.1 Set up of Zn(s)|Zn2+(aq., 1.0M) ||Cu2+(aq., x M)|Cu(s) cell

Procedure:
(i) Set up the cell as given in Fig. 1.1, using 1.0 M ZnSO4 and 0.2 M CuSO4 solution.
(ii) Measure the potential difference of the cell and also keep record of the polarity of the
electrodes (this will enable us to give a sign to the cell potential ECell).
(iii) Remove the salt bridge as soon as the cell potential measurement is over.
(iv) Replace the beaker of 0.2 M CuSO4 with 0.1 M CuSO4 solution in the beaker. Place the
salt bridge in position and note the cell potential.
(v) Repeat this procedure for other solutions of copper sulphate in decreasing order of
concentrations of copper sulphate solution.
(vi) Calculate log [Cu2+(aq)] and then E Cu2+
/Cu for each variation in the concentration of
copper (II) in the solution.
(vii) Record electrode potential values of Cu2+(aq)/Cu(s) electrode for different
concentrations of Cu2+ ions as given in Table 4.1.
(viii) Plot a graph for the variation of cell potential with concentration taking ( E Cu 2+
/Cu ) on y-
axis and log [Cu2+(aq)] on x-axis.
Observation:

Result:
Write conclusion on the basis of data obtained.
Experiment No.2
STUDY OF SHIFT IN EQUILIBRIUM WITH CHANGE IN CONCENTRATION OF REACTANTS
Aim:
Study of shift in equilibrium in the reaction of ferric ions and thiocyanate ions by increasing
the concentration of any one of these ions.
Theory:
The equilibrium reaction between ferric chloride and potassium thiocyanate is conveniently
studied through the change in the intensity of colour of the solution. Fe 3+(aq) + SCN–(aq) →
[Fe(SCN)]2+(aq) (Blood red colour).
The equilibrium constant for the above reaction may be written as:
K = [[Fe(SCN)]2+ (aq)] [Fe (aq)] 3+ [SCN (aq)] –
Here K is constant at a constant temperature. Increasing the concentration of either Fe 3+ ion
or thiocyanate ion would result in a corresponding increase in the concentration of
[Fe(SCN)]2+ ions. In order to keep the value of K constant, there is a shift in equilibrium, in
the forward direction and consequently an increase in the intensity of the blood red colour
which is due to [Fe(SCN)]2+ . At equilibrium colour intensity remains constant.
Material Required:

Procedure:
(i) Dissolve 0.100 g ferric chloride in 100 mL of water in a beaker and 0.100 g potassium
thiocyanate in 100 mL of water in another beaker.
(ii) Mix 20 mL of ferric chloride solution with 20 mL of potassium thiocyanate solution. Blood
red colour will be obtained. Fill this solution in a burette.
(iii) Take five boiling tubes of same size and mark them as a,b,c, d and e.
(iv) Add 2.5 mL of blood red solution to each of the boiling tubes from the burette.
(v) Add 17.5 mL of water to the boiling tube ‘a’ so that total volume of solution in the boiling
tube ‘a’ is 20 mL. Keep it for reference.
(vi) Now take three burettes and label them as A, B, and C.
(vii) Fill burette A with ferric chloride solution, burette B with potassium thiocynate solution
and burette C with water.
(viii) Add 1.0 mL, 2.0 mL, 3.0 mL and 4.0 mL of ferric chloride solution to boiling tubes b, c, d
and e respectively from burette A.
(ix) Now add 16.5 mL, 15.5 mL, 14.5 mL, and 13.5 mL of water to boiling tubes b, c, d and e
respectively from burette C so that total volume of solution in each boiling tube is 20 mL.
(x) Compare the colour intensity of the solution in each boiling tube with the colour intensity
of reference solution in boiling tube ‘a’.
(xi) Take another set of four clean boiling tubes. Add 2.5 mL of blood red solution to each of
the boiling tubes from the burette. Repeat the experiment by adding 1.0 mL, 2.0 mL, 3.0 mL
and 4.0 mL of potassium thiocyanate solution from burette B to the boiling tubes b′, c′, d′,
and e′ respectively followed by addition of 16.5 mL, 15.5 mL, 14.5 mL and 13.5 mL of water
respectively to these test tubes. Again compare the colour intensity of the solution of these
test tubes with reference equilibrium solution in boiling tube ‘a’.
(xii) Record your results in tabular form as in Tables 4.1 and 4.2.
(xiii) You may repeat the observations with different amounts of potassium thiocyanate and
ferric chloride solution and compare with the reference solution.
Observations:
Result:
 REACTIONS OF ANIONS AND CATIONS
A. REACTIONS OF ANIONS
1. Reactions of Carbonate Ion, CO32-
No. Experiment Observation Inference
1. Take 0.1 g of salt in a A colourless odourless CO2 gas is evolved, which
test tube, add dilute gas is evolved with brisk turns lime water milky and
hydrochloric acid. effervescence which then colourless as per the
turns lime water milky. following reactions:
On passing the gas for Na2CO3 + 2HCl → 2NaCl + H2O
some more time, +CO2
milkiness disappears. Ca(OH)2 + CO2 → CaCO3 + H2O
CaCO3 + CO2 + H2O →Ca
(HCO3 )2
2. Take 0.1 g of salt in a A white precipitate, White precipitate is due to
test tube, add a few mL which dissolves in dil. the formation of BaCO3,
of BaCl2 solution and HCl with the evolution of which reacts with dil. HCl
then dilute hydrochloric a colourless gas forming soluble BaCl2 and CO2
acid. gas.

2. Reactions of Sulphide Ion, S2-

No. Experiment Observation Inference
1. Take 0.1 g of salt in a A colourless gas is H2S gas is evolved, which has
test tube, add dilute evolved with smell of smell of rotten egg
hydrochloric acid. rotten egg. Na2S + 2HCl → 2NaCl + H2S
2. Take 0.1 g of salt in a A black precipitate is Black precipitate is due to the
test tube, add a few mL formed formation of PbS
of Pb(CH3COO)2 Na2S + Pb(CH3COO)2 →
solution. 2CH3COONa + PbS

3. Reactions of Acetate Ion, CH3COO–

No. Experiment Observation Inference
1. A little of the salt is Smells like It indicates the presence of acetate
rubbed with dil. sulphuric vinegar ions.
acid and smell noted. 2CH3COONa + H2SO4 → Na2 SO4 +
2CH3COOH
2. Take 0.1 g of salt in a Fruity odour It indicates the presence of acetate
china dish and add 1 mL ions and is due to the formation of
of ethanol. Then add ethyl acetate.
about 0.2 mL of conc. CH3COOH + C2H5OH → CH3COOC2H5 +
H2SO4 and heat. H2O
 3. Take 0.1 g of salt in a test Deep red colour Acetate gives deep red colour due
tube and neutral ferric to the formation of complex ion
chloride solution is which decomposes on heating to
added. give Iron (III) dihydroxyacetate as
brown red precipitate.
6CH3COO– + 3Fe3+ + 2H2O →
[Fe3 (OH)2 (CH3COO)6 ]+ + 2H+
[Fe3 (OH)2 (CH3COO)6 ]+ + 4H2O →
3[Fe (OH)2 (CH3COO)] + 3CH3COOH + H+

4. Reactions of Chloride Ion, Cl–

No. Experiment Observation Inference
1. Take 0.1 g of salt in a dry A colourless gas Colourless gas with pungent smell is
test tube and 3-4 drops with pungent HCl and white fumes is due to
of conc. H2SO4 added. smell, which gives NH4Cl as described below:
dense white fumes NaCl + H2SO4 → NaHSO4 + HCl
when a glass rod HCl + NH3 → NH4Cl
dipped in
ammonium
hydroxide is
brought near the
mouth of the test
tube.
2. Take 1 mL of test solution A curdy white It indicates the presence of Cl– ions
in a test tube, acidify it precipitate is and is due to the formation AgCl,
with dil. HNO3 add silver obtained which is which dissolves in NH4OH due to
nitrate solution. soluble in the formation of a complex,
ammonium [Ag(NH3)2 ]Cl.
hydroxide NaCl + AgNO3 → NaNO3 + AgCl
solution. AgCl + 2NH4OH → [Ag(NH3)2 ]Cl +
2H2O
3. Take 0.1 g of salt in a dry A light greenish It indicates the presence of Cl– ions.
test tube, 3-4 drops of yellow pungent Cl2 gas is evolved.
conc. H2SO4 added and a gas is evolved. MnO2 + 2NaCl + 2H2SO4 → Na2SO4
little MnO2 powder is + MnSO4 + 2H2O + Cl2
added.

5. Reactions of Bromide Ion, Br–

No. Experiment Observation Inference
1. Take 0.1 g of salt in a dry Reddish brown It indicates the presence of Br–
test tube and 3-4 drops fumes of bromine ions.
of conc. H2SO4 added.
 are evolved in 2NaBr + 2H2SO4 → Br2 + SO2 +
excess. Na2SO4 + 2H2O
2. Take 1 mL of test solution A pale-yellow It indicates the presence of Br– ions
in a test tube, acidify it precipitate is and is due to the formation AgBr,
with dil. HNO3 add silver obtained which which dissolves in NH4OH with
nitrate solution. dissolves in difficulty
NH4OH with NaBr + AgNO3 → NaNO3 + AgBr
difficulty

6. Reactions of Iodide Ion, I–

No. Experiment Observation Inference
1. Take 0.1 g of salt in a dry Deep violet It indicates the presence of I– ions.
test tube and 3-4 drops vapours with a 2NaI + 2H2SO4 → I2 + SO2 + Na2SO4
of conc. H2SO4 added. pungent smell are + 2H2O
evolved.
2. Take 1 mL of test solution A yellow It indicates the presence of I– ions
in a test tube, acidify it precipitate and is due to the formation AgI,
with dil. HNO3 add silver insoluble in which is insoluble in NH4OH.
nitrate solution. excess of NH4OH NaI + AgNO3 → NaNO3 + AgI

7. Reactions of Nitrate Ion, NO3–

No. Experiment Observation Inference
1. Take 0.1 g of salt in a dry Evolution of It indicates the presence of nitrate
test tube, 3-4 drops of brown fumes ions. Brown fumes are due to
conc. H2SO4 added and liberation of NO2
heated. NaNO3 + H2SO4 → NaHSO4 + HNO3
4HNO3 → 4NO2 + O2 + 2H2O
2. Take 0.1 g of salt in a dry Evolution of It indicates the presence of nitrate
test tube, 3-4 drops of excess of brown ions. Brown fumes are due to
conc. H2SO4 added and fumes liberation of NO2
heated with few copper 2NaNO3 + 4H2SO4 + 3Cu → 3 CuSO4 +
turnings or chips. Na2SO4 + 4H2O + 2NO
2NO + O2 → 2NO2
3. Take 1 mL of an aqueous A dark brown ring It indicates the presence of NO3–
solution of the salt and is formed at the ions.
add 2 mL conc. H2 SO4 junction of the NaNO3 + H2SO4 → NaHSO4 + HNO3
slowly. Mix the solutions two solutions due 6FeSO4 + 3H2SO4 + 2HNO3 →
thoroughly and cool the to the formation 3Fe2(SO4)3 + 4H2O + 2NO
test tube under the tap. of nitroso ferrous FeSO4 + NO → [Fe(NO)]SO4
Now, add freshly sulphate
prepared ferrous
sulphate solution along
the sides of the test tube
dropwise so that it forms
a layer on the top.
8. Reactions of Sulphate Ion, SO4–
No. Experiment Observation Inference
1. Take 1 mL water extract White precipitate It indicates the presence of SO4–
of the salt in water, insoluble in conc. ions. White precipitate of barium
acidify with dilute HCl HCl or conc. HNO3 sulphate is insoluble in conc. HCl or
and add BaCl2 solution. is obtained. conc. HNO3.
2. Acidify the aqueous Appearance of It confirms the presence of SO4–
solution of the salt with white precipitate. ions.
acetic acid and add lead Na2SO4 + (CH3COO)2Pb → PbSO4 +
acetate solution. 2CH3COONa.

B. REACTIONS OF CATIONS
1. Reactions of Ammonium Ion, NH4+
No. Experiment Observation Inference
1. Take 0.1 g of salt in a test Smell of ammonia It indicates the presence of
tube and add 1-2 mL of and white fumes ammonium ions. Ammonia gas
NaOH solution to it and are observed evolved which reacts with HCl to
heat. when a glass rod give NH4Cl, which is visible as dense
dipped in white fume.
hydrochloric acid (NH4)2SO4 + 2NaOH → Na2SO4 + 2NH3
is brought near + 2H2O
the mouth of the NH3 + HCl → NH4Cl
test tube.
2. A little of the salt is Brown precipitate Brown colouration or a precipitate
mixed with NaOH or colouration is of basic mercury(II) amido-iodine is
solution and Nessler’s obtained. formed.
reagent is added. 2K2HgI4 + NH3 + 3KOH → HgO.Hg(NH2)I
+ 7KI + 2H2O

2. Reactions of Lead Ion, Pb2+

No. Experiment Observation Inference
1. Take a little of the salt White precipitate Presence of Pb2+ ions. Lead
solution and add dil. HCl. appears. chloride appears as white
precipitate.
Pb(NO3)2 + 2KI → PbCl2 + 2KNO3
2. Take a little of the salt A yellow A yellow precipitate of lead iodide
solution and add precipitate is is obtained which confirms the
potassium iodide obtained. presence of Pb2+ ions.
solution. Pb2+ + 2KI → PbI2 + 2K+
3. Take a little of the salt A yellow On addition of potassium chromate
solution and add precipitate is (K2CrO4 ) solution a yellow
obtained which is precipitate of lead chromate is
 potassium chromate soluble in NaOH obtained. This confirms the
solution. and insoluble in presence of Pb2+ ions.
ammonium Pb2+ + K2CrO4 → PbCrO4 + 2K+
acetate solution. The yellow precipitate (PbCrO4) is
soluble in hot NaOH solution.

3. Reactions of Copper ion, Cu2+

No. Experiment Observation Inference
1. Take a little of the Black precipitate, Presence of Cu2+ ions. Copper
salt(copper salt) solution insoluble in sulphide appears as black
and add dil. HCl and H2S yellow precipitate.
gas is passed through it. ammonium CuSO4 + H2S → CuS + H2SO4
sulphide is
formed.
2. Boil the precipitate A blue solution is Copper sulphide dissolves in nitric
formed in the above test obtained. acid due to the formation of
with dilute nitric acid and copper nitrate and it is converted
add a few drops of into CuSO4. It is soluble in excess of
alcohol and dil.H2SO4. ammonium hydroxide due to the
Then add excess of formation of tetraamminecopper
ammonium hydroxide (II) complex (deep blue solution).
solution. 3CuS + 8HNO3 → 3Cu(NO3)2 + 2NO + 3S +
4H2O
3. Acidify the above A chocolate The blue solution gives a chocolate
solution with acetic acid brown precipitate colouration due to the formation of
and add potassium is formed. copper ferrocyanide
ferrocyanide solution. i.e.Cu2[Fe(CN)6].

4. Reactions of Aluminium ion, Al3+

No. Experiment Observation Inference
1. Take a little of the salt A gelatinous It indicates the presence of
solution, add a small white precipitate aluminium ion (Al3+). Gelatinous
amount of solid is formed. white precipitate is due to the
ammonium chloride formation of hydroxide of
(NH4Cl) and an excess of aluminium.
ammonium hydroxide
(NH4OH) solution till it
smells of ammonia.
Shake the test tube.
 2. To the first part add A white a white gelatinous precipitate of
sodium hydroxide gelatinous aluminium hydroxide is formed
solution and warm. precipitate which is soluble in excess of
soluble in excess sodium hydroxide solution due to
of sodium the formation of sodium
hydroxide aluminate.
solution. AlCl3 + 3NaOH → Al(OH)3 + 3NaCl
Al(OH)3 + NaOH → NaAlO2 + 2H2O
3. Take 0.1 g of salt in a test Blue tinted ash is Blue ash is due to the formation of
tube, add 1-2 mL of formed. mixed oxides of cobalt and
coc.HNO3 and 3mL of aluminum
cobalt nitrate solution. CoO + Al2O3 → CoO. Al2O3 (Blue)
Heat it, a filter paper
strip impregnated with it
and burnt into ashes.

5. Reactions of Zinc ion, Zn2+

No. Experiment Observation Inference
1. Take a little of the salt A white It indicates the presence of zinc ion
solution, add a small precipitate is (Zn2+). White precipitate is due to
amount of solid formed. the formation of ZnS.
ammonium chloride
(NH4Cl) and an excess of
ammonium hydroxide
(NH4OH) solution. Then
H2S gas is passed through
it.
2. To a little of the salt A white White precipitate is zinc hydroxide,
solution, sodium precipitate of zinc which dissolves in excess of NaOH
hydroxide solution is hydroxide, which solution on heating due to the
added. is soluble in formation of sodium
excess of NaOH zincate(Na2ZnO2).
solution on ZnCl2 + 2NaOH → Zn(OH)2 + 2NaCl
heating. Zn(OH)2 + 2NaOH → Na2ZnO2 +
2H2O
3. Take 0.1 g of salt in a test Green tinted ash Green ash is due to the formation
tube, add 1-2 mL of is formed. of mixed oxides of cobalt and zinc
coc.HNO3 and 3mL of CoO + ZnO → CoO. ZnO (Green)
cobalt nitrate solution.
Heat it, a filter paper
strip impregnated with it
and burnt into ashes.

6. Reactions of Manganese ion, Mn2+

No. Experiment Observation Inference
 1. Take a little of the salt A Flesh coloured It indicates the presence of
solution, add a small precipitate is manganese ion (Mn2+). Flesh
amount of solid formed. coloured precipitate is due to the
ammonium chloride formation of MnS.
(NH4Cl) and an excess of
ammonium hydroxide
(NH4OH) solution. Then
H2S gas is passed through
it.
2. To a little of the salt A white White precipitate of manganese
solution, sodium precipitate hydroxide is formed which turns
hydroxide solution is formed which brown due to atmospheric
added. turns brown on oxidation into hydrated manganese
keeping. dioxide.
Mn(OH)2 (white)+ [O] →
MnO(OH)2(brown)

7. Reactions of Barium ion, Ba2+

No. Experiment Observation Inference
1. Take a little of the barium A white coloured White precipitate is due to the
salt solution, add a small precipitate is formation of barium carbonate.
amount of solid NH4Cl formed.
and an excess of NH4OH
solution followed by solid
ammonium carbonate
(NH4)2CO3 .
2. To a little of the salt A yellow Potassium chromate (K2CrO4 )
solution, add acetic acid precipitate solution gives a yellow precipitate
and potassium chromate appears. of barium chromate.
solution. BaCl2 + 2CH3COOH → (CH3COO)2Ba +
2HCl
(CH3COO)2Ba + K2CrO4 → BaCrO4 +
2CH3COOK
3. Perform the flame test A grassy green Ba2+ ions impart green colour to
with a mixture of the salt flame is obtained. nonluminous flame.
and conc. HCl.

8. Reactions of Strontium ion, Sr2+

No. Experiment Observation Inference
1. Take a little of the A white coloured White precipitate is due to the
strontium salt solution, precipitate is formation of strontium carbonate.
add a small amount of formed.
solid NH4Cl and an excess
of NH4OH solution
followed by solid
 ammonium carbonate
(NH4)2CO3 .
2. To a little of the salt A white White precipitate of strontium
solution, add acetic acid precipitate is sulphate with ammonium sulphate,
and ammonium sulphate formed. (NH4)2SO4
solution. Heat and SrCO3 + 2CH3COOH → (CH3COO)2Sr + H2O
scratch the sides of the + CO2
(CH3COO)2Sr + (NH4)2SO4 → SrSO4 +
test tube with a glass rod 2CH3COONH4
and cool.
3. Perform the flame test A crimson-red Sr2+ ions impart crimson-red colour
with a mixture of the salt flame. to nonluminous flame.
and conc. HCl.

9. Reactions of Calcium ion, Ca2+

No. Experiment Observation Inference
1. Take a little of the A white coloured White precipitate is due to the
calcium salt solution, add precipitate is formation of calcium carbonate.
a small amount of solid formed.
NH4Cl and an excess of
NH4OH solution followed
by solid ammonium
carbonate (NH4)2CO3 .
2. To a little of the salt A white A white precipitate of calcium
solution, add ammonium precipitate is oxalate is obtained.
oxalate solution and formed. (CH3COO)2Ca + (NH4)2C2O4 → (COO)2Ca +
shake well. 2CH3COONH4
3. Perform the flame test A brick red flame. Ca2+ ions impart brick-red colour to
with a mixture of the salt nonluminous flame.
and conc. HCl.

10. Reactions of Magnesium ion, Mg2+

No. Experiment Observation Inference
1. Take a little of the salt A white White crystalline precipitate of
solution, add a small crystalline magnesium ammonium phosphate
amount of solid NH4Cl precipitate is is formed.
and excess of NH4OH formed. Mg2+ + Na2HPO4 → Mg(NH4)PO4 + NH4OH
solution followed by + 2Na+ + H2O.
disodium
hydrogenphosphate
solution. The inner walls
of the test tube are
scratched with a glass
rod.
 2. To a little of the salt A white A white precipitate of calcium
solution, add ammonium precipitate is oxalate is obtained.
oxalate solution and formed. (CH3COO)2Ca + (NH4)2C2O4 → (COO)2Ca +
shake well. 2CH3COONH4
3. Take 0.1 g of salt in a test Pink tinted ash is Mixed oxides of Co and Mg is pink
tube, add 1-2 mL of produced. in colour.
coc.HNO3 and 3mL of
cobalt nitrate solution.
Heat it, a filter paper
strip is impregnated with
it and burnt into ashes.

SALT ANALYSIS (8)

REACTIONS OF ORGANIC COMPOUNDS
(Carboxylic acid, Phenol, Aniline, Aldehydes and Ketones)
1. Reactions of Carboxylic acid group, -COOH
No. Experiment Observation Inference
1. Litmus Test: The carboxylic Carboxylic acid gives H3O+ ions
The substance is treated acid turns blue which turns blue litmus, red
with a moist blue litmus litmus, red. R-COOH + H2O → R-COO– + H3O+
paper.
2. Sodium Bicarbonate Test: Carbon dioxide is CO2 is evolved due to the reaction,
The substance is treated evolved with RCOOH + NaHCO3 → RCOONa +
with sodium bicarbonate a brisk H2O + CO2↑ (brisk effervescence)
solution. effervescence.
(Phenol does not give
this test).
3. Esterification Test: A pleasant smell This reaction is known as
The substance is mixed is observed. esterification.
with alcohol in the H2SO4
RCOOH + R-OH → RCOO-R (Ester) +
presence of a few drops H2O
of conc. sulphuric acid Ester has a pleasant fruity smell.
and boiled in a water
bath for some minutes.

2. Reactions of Phenol, C6H5OH

No. Experiment Observation Inference
1. Litmus Test: Blue litmus turns Phenol gives H3O+ ions which turns
The substance is treated red. blue litmus, red
with a moist blue litmus C6H5OH + H2O → C6H5-O– + H3O+
paper.
 2. Sodium Bicarbonate Test: No brisk Phenol does not react with sodium
The substance is treated effervescence. bicarbonate, since it is weakly
with sodium bicarbonate acidic
solution.
3. Ferric Chloride Test: Violet Complex formation occurs as
Aqueous solution of the colouration. shown below:
substance is treated with 6C6H5OH + FeCl3 → [Fe(C6H5O)6]3– (violet
freshly prepared neutral complex)+ 3HCl + 3H+
ferric chloride solution.

3. Reactions of Aniline, C6H5NH2

No. Experiment Observation Inference
1. Litmus Test: Red litmus turns Amines give OH– ions and hence
The substance is treated blue. show basic property.
with a moist blue litmus C6H5-NH2 + H2O → C6H5-NH3+ + OH–
paper.
2. Solubility Test: Soluble Amines are basic in nature, so they
The substance is treated dissolve in mineral acids.
with dil. HCl. C6H5NH2 + HCl → C6H5NH3+Cl–
3. Carbylamine Test: An unpleasant It confirms the presence of primary
The substance is treated odour noticed. amine.
with chloroform and KOH R-NH2 + 3KOH + CHCl3 →
solution. RNC(isocyanide) + 3KCl + 3H2O

4. Reactions of Aldehyde, R-CHO

No. Experiment Observation Inference
1. 2,4-Dinitrophenyl Orange-yellow Aldehydes and ketones react with 2,4-
Hydrazine Test: precipitate is dinitrophenylhydrazine to give an
A little of the substance formed orange-yellow precipitate.
is treated
with 2,4-
dinitrophenylhydrazine
or Borsch’s reagent.
2. Schiff’s Reagent Test: The pink colour The colouration is due to the
The substance is added is restored. formation of complex compound.
to a few mL of Schiff’s Aldehydes abstract sulphurous acid
reagent, in a test tube. from Schiff’s reagent and restore the
pink colour.
3. Fehling’s Test: A red precipitate When the aldehyde compound is
Fehling’s solution is a is formed. treated with Fehling’s solution Cu2+ is
complex compound of reduced to Cu+ and the aldehyde is
Cu2+, prepared by mixing reduced to acids. The red precipitate
alkaline CuSO4 and is due to the formation of Cu2O.
sodium potassium
 tartrate solutions. The
given compound is
heated with Fehling’s
solution in a water bath.

4 Tollen’s Test(Silver Black silver Tollen’s reagent consists of silver

Mirror Test): mirror is ammonia complex in ammonia
A little of the substance formed. solution. Aldehydes react with Tollen’s
is warmed with Tollen’s reagent giving a grey-black precipitate
reagent in a water bath or a silver mirror. Ag in Tollens reagent
for a few minutes. is reduced from +1 oxidation state to
its elemental form.
RCHO + 2[Ag(NH3)2]OH → R-
COONH4 + 3NH3 + H2O + 2Ag↓(silver
mirror)

5. Reactions of Ketone, R2CO

No. Experiment Observation Inference
1. 2,4-Dinitrophenyl Orange-yellow Aldehydes and ketones react with 2,4-
Hydrazine Test: precipitate is dinitrophenylhydrazine to give an
A little of the substance formed. orange-yellow precipitate.
is treated
with 2,4-
dinitrophenylhydrazine
or Borsch’s reagent.
2. Schiff’s Reagent Test: The pink colour Ketones, in general, do not respond to
The substance is added is not restored. this reaction.
to a few mL of Schiff’s
reagent, in a test tube.
3. Fehling’s Test: No red Ketones are difficult to get oxidised by
Fehling’s solution is a precipitate is Cu2+ions in these conditions
complex compound of formed.
Cu2+, prepared by mixing
alkaline CuSO4 and
sodium potassium
tartrate solutions. The
given compound is
heated with Fehling’s
solution in a water bath.

4. Tollen’s Test(Silver No silver mirror Generally, ketones do not respond to

Mirror Test): is formed. this test.
A little of the substance
is warmed with Tollen’s
reagent in a water bath
for a few minutes.
 VOLUMETRIC ANALYSIS

A. ACIDIMETRY AND ALKALIMETRY

Expt. No.1
Estimation of Sodium hydroxide
Aim:
Estimate the mass of sodium hydroxide in the whole of the given solution using standard HCl
solution containing 3.75 g HCl per litre of the solution.
Principle:
NaOH + HCl → NaCl + H2O
Procedure:
The given NaOH solution is made up to 100mL in a clean standard flask. Standard HCl
solution is filled in the burette. 20 mL of the made-up NaOH solution is pipetted out into a
clean conical flask and one or two drops of phenolphthalein indicator is added into it, which
give pink colour to the solution. Then it is titrated against standard HCl solution from the
burette. At the end point the pink coloured solution changes to colourless solution. The
titration is repeated to get concordant values. Readings are recorded and calculations are
made.
Observations:
NaOH X Standard HCl (Phenolphthalein)

Sl. Volume of Burette Volume of

No. NaOH in mL Reading HCl in mL
Initial Final

Volume of HCl solution = ……… mL

Calculations:
(i) To find the Normality of HCl solution:
Mass per litre of HCl = ……… g L-1
Gram equivalent mass of HCl = 36.5 g equivalent-1
Mass per litre of HCl
Normality of HCl, N1 = Gram equivalent mass = …….. = ……… N

(ii) Estimation of NaOH:

Volume of HCl (V1) = ………….. mL
Normality of HCl (N1) = ……… N
Volume of NaOH solution pipetted out, V2 = 20 mL
Volume of HCl X Normality of HCl
Normality of NaOH (N2) = Volume of NaOH
N1V1
= V2

=…………
=………….. N
Gram equivalent mass of NaOH = 40 g equivalent-1
Mass per litre of NaOH solution = Normality of NaOH solution x Gram equivalent
mass = …………
= ………………. g L-1
Mass per litre X 100
Mass of NaOH in the whole of the given solution = 1000

= ……………..g
= ……….. g
Result:
Mass of NaOH in the whole of the given solution = ………………..g
Expt. No.2
Estimation of Nitric Acid
Aim:
Estimate the mass of nitric acid in the whole of the given solution using standard sodium
carbonate solution containing 5.35 g Na2CO3 per litre of the solution.
Principle:
Na2CO3 + 2HNO3 → 2NaNO3 + H2O + CO2
Procedure:
The given HNO3 solution is made up to 100mL in a clean standard flask and filled in the
burette. 20 mL of the standard Na2CO3 solution is pipetted out into a clean conical flask and
two drops of methyl orange indicator is added into it, which give yellow colour to the
solution. Then it is titrated against HNO3 solution from the burette. At the end point the
yellow coloured solution changes to orange -red colourled solution. The titration is repeated
to get concordant values. Readings are recorded and calculations are made.
Observations:
Standard Na2CO3 X HNO3 solution(Methyl Orange)

Sl. Volume of Burette Volume of

No. Na2CO3 in Reading HNO3 in mL
mL Initial Final

Volume of HNO3 solution = ……… mL

Calculations:
(i) To find the Normality of Na2CO3 solution:
Mass per litre of Na2CO3 = ……… g L-1
Gram equivalent mass of Na2CO3 = 53.0 g equivalent-1
Mass per litre of Na2CO3
Normality of Na2CO3, N1 = = …….. = ……… N
Gram equivalent mass

(ii) Estimation of HNO3:

Volume of Na2CO3 (V1) = 20 mL
Normality of Na2CO3 (N1) = ……… N
Volume of HNO3 solution, V2 = ………. mL
Volume of Na2CO3X Normality of Na2CO3l
Normality of HNO3 (N2) = Volume of HNO3
N1V1
= V2

=…………
=………….. N
Gram equivalent mass of HNO3 = 63 g equivalent-1
Mass per litre of HNO3 solution = Normality of HNO3 solution x Gram equivalent mass
= …………
= ………………. g L-1
Mass per litre X 100
Mass of HNO3 in the whole of the given solution = 1000

= ……………..
= ……….. g
Result: Mass of HNO3 in the whole of the given solution = ………………..g
Expt. No.3
Estimation of Potassium hydroxide
Aim:
Estimate the mass of potassium hydroxide in the whole of the given solution using standard
H2SO4 solution containing 4.95 g H2SO4 per litre of the solution.
Principle:
2KOH + H2SO4 → K2SO4 + 2H2O
Procedure:
The given KOH solution is made up to 100mL in a clean standard flask. Standard H2SO4
solution is filled in the burette. 20 mL of the made-up KOH solution is pipetted out into a
clean conical flask and one or two drops of phenolphthalein indicator is added into it, which
give pink colour to the solution. Then it is titrated against standard H2SO4 solution from the
burette. At the end point the pink coloured solution changes to colourless solution. The
titration is repeated to get concordant values. Readings are recorded and calculations are
made.
Observations:
KOH X Standard H2SO4 (Phenolphthalein)

Sl. Volume of Burette Volume of

No. KOH in mL Reading H2SO4 in mL
Initial Final

Volume of H2SO4 solution = …….. mL

Calculations:
(i) To find the Normality of H2SO4 solution:
Mass per litre of HCl = ……… g L-1
Gram equivalent mass of H2SO4 = 49.0 g equivalent-1
Mass per litre of H2SO4
Normality of H2SO4, N1 = = …….. = ……… N
Gram equivalent mass

(ii) Estimation of KOH:

Volume of H2SO4 (V1) = ………….. mL
Normality of H2SO4 (N1) = ……… N
Volume of KOH solution pipetted out, V2 = 20 mL
Volume of H2SO4 X Normality of H2SO4
Normality of KOH (N2) = Volume of KOH
N1V1
= V2

=………… =………….. N
Gram equivalent mass of KOH = 56.0 g equivalent-1
Mass per litre of KOH solution = Normality of KOH solution x Gram equivalent mass
= …………
= ………………. g L-1
Mass per litre X 100
Mass of KOH in the whole of the given solution = 1000

= ……………..
= ……….. g
Result:
Mass of KOH in the whole of the given solution = ………………..g
Expt. No.4
Estimation of Sulphuric Acid
Aim:
Estimate the mass of sulphuric acid in the whole of the given solution using standard
potassium carbonate solution containing 6.85 g K2CO3 per litre of the solution.
Principle:
K2CO3 + H2SO4 → K2SO4 + H2O + CO2
Procedure:
The given H2SO4 solution is made up to 100mL in a clean standard flask and filled in the
burette. 20 mL of the standard K2CO3 solution is pipetted out into a clean conical flask and
two drops of methyl orange indicator is added into it, which give yellow colour to the
solution. Then it is titrated against H2SO4 solution from the burette. At the end point the
yellow coloured solution changes to orange -red coloured solution. The titration is repeated
to get concordant values. Readings are recorded and calculations are made.
Observations:
Standard K2CO3 X H2SO4 solution(Methyl Orange)

Sl. Volume of Burette Volume of

No. K2CO3 in mL Reading H2SO4 in mL
Initial Final

Volume of H2SO4 solution = ……… mL

Calculations:
(i) To find the Normality of K2CO3 solution:
Mass per litre of K2CO3 = ……… g L-1
Gram equivalent mass of K2CO3 = 69.0 g equivalent-1
Mass per litre of K2CO3
Normality of K2CO3, N1 = = …….. = ……… N
Gram equivalent mass

(ii) Estimation of H2SO4:

Volume of K2CO3 (V1) = 20 mL
Normality of K2CO3 (N1) = ……… N
Volume of H2SO4solution, V2 = ………. mL
Volume ofK2CO3X Normality of K2CO3l
Normality of H2SO4 (N2) = Volume of H2SO4
N1V1
= V2

=…………
=………….. N
Gram equivalent mass of H2SO4 = 49 g equivalent-1
Mass per litre of H2SO4= Normality of H2SO4solution x Gram equivalent mass
= ………… = ………………. g L-1
Mass per litre X 100
Mass of H2SO4 in the whole of the given solution = 1000

= ……………..
= ……….. g
Result:
Mass of H2SO4 in the whole of the given solution = ………………..g
 B. REDOX TITRATIONS
Expt. No.5
Estimation of Ferrous ammonium sulphate (Mohr’s salt, FeSO4 (NH4)2 SO4 . 6H2O)
Aim:
Estimate the mass of Ferrous ammonium sulphate, FeSO4 (NH4)2 SO4 . 6H2O in the whole of
the given solution using standard KMnO4 solution containing 3.16 g KMnO4 per litre of the
solution.
Principle:
2KMnO4 + 8H2SO4 + 10FeSO4.(NH4)2SO4 . 6H2O → K2SO4 + 2MnSO4 + 5Fe2(SO4)3 + 10(NH4)2SO4 +
68H2O
OR

MnO4– + 5Fe2+ + 8H+ → Mn2+ + 5Fe3+ + 4H2O

Procedure:
The given Mohr’s salt solution is made up to 100mL in a clean standard flask. Standard
KMnO4 solution is filled in the burette. 20 mL of the made-up Mohr’s salt solution is pipetted
out into a clean conical flask and 10 mL 0.1 M sulphuric acid solution is added into it. Then it
is titrated against standard KMnO4 solution from the burette. At the end point the colourless
solution changes to permanent pink coloured solution. The titration is repeated to get
concordant values. Readings are recorded and calculations are made.
Observations:
Mohr’s salt solution X Standard KMnO4

Sl. Volume of Burette Volume of

No. Mohr’s salt Reading KMnO4 in
in mL Initial Final mL

Volume of KMnO4 solution = …….. mL

Calculations:
(i) To find the Normality of KMnO4 solution:
Mass per litre of KMnO4 = ……… g L-1
Gram equivalent mass of KMnO4 = 36.5 g equivalent-1
Mass per litre of KMnO4
Normality of KMnO4, N1 = Gram equivalent mass = …….. = ……… N

(ii) Estimation of Mohr’s salt:

Volume of KMnO4 (V1) = ………….. mL
Normality of KMnO4 (N1) = ……… N
Volume of Mohr’s salt solution pipetted out, V2 = 20 mL
Volume of KMnO4X Normality of KMnO4
Normality of Mohr’s salt (N2) = Volume of Mohr’s salt solution
N1V1
= V2

=…………
=………….. N
Gram equivalent mass of Mohr’s salt = 392 g equivalent-1
Mass per litre of Mohr’s salt solution = Normality of Mohr’s salt solution x Gram
equivalent mass = …………
= ………………. g L-1
Mass per litre X 100
Mass of Mohr’s salt in the whole of the given solution = 1000

= ……………..
= ……….. g
Result:
Mass of Mohr’s salt in the whole of the given solution = ………………..g
Expt. No.6
Estimation of Oxalic acid
Aim:
Estimate the mass of oxalic acid(H2C2O4. 2H2O) in the whole of the given solution using
standard KMnO4 solution containing 3.16 g KMnO4 per litre of the solution.
Principle:
2KMnO4 + 3H2SO4 +5 H2C2O4.2H2O→ K2SO4 + 2MnSO4 + 10 CO2 + 18H2O
OR

2MnO4– + 5C2O42- + 16H+ → 2Mn2+ + 10 CO2 + 8H2O

Procedure:
The given oxalic acid solution is made up to 100mL in a clean standard flask. Standard
KMnO4 solution is filled in the burette. 20 mL of the made-up oxalic acid solution is pipetted
out into a clean conical flask and 10 mL 0.1 M sulphuric acid solution is added into it. It is
heated to 60oC. Then it is titrated against standard KMnO4 solution from the burette. At the
end point the colourless solution changes to permanent pink coloured solution. The titration
is repeated to get concordant values. Readings are recorded and calculations are made.
Observations:
Oxalic acid X Standard KMnO4

Sl. Volume of Burette Volume of

No. oxalic acid Reading KMnO4 in
in mL Initial Final mL

Volume of KMnO4 solution = …….. mL

Calculations:
(i) To find the Normality of KMnO4 solution:
Mass per litre of KMnO4 = ……… g L-1
Gram equivalent mass of KMnO4 = 36.5 g equivalent-1
Mass per litre of KMnO4
Normality of KMnO4, N1 = Gram equivalent mass = …….. = ……… N

(ii) Estimation of oxalic acid:

Volume of KMnO4 (V1) = ………….. mL
Normality of KMnO4 (N1) = ……… N
Volume of oxalic acid solution pipetted out, V2 = 20 mL
Volume of KMnO4X Normality of KMnO4
Normality of oxalic acid solution(N2) = Volume of oxalic acid solution
N1V1
= V2

=…………
=………….. N
Gram equivalent mass of oxalic acid(H2C2O4. 2H2O) = 63 g equivalent-1
Mass per litre of oxalic acid = Normality of oxalic acid solution x Gram equivalent
mass = …………
= ………………. g L-1
Mass per litre X 100
Mass of oxalic acid(H2C2O4. 2H2O) in the whole of the given solution = 1000

= ……………..
= ……….. g
Result:
Mass of oxalic acid(H2C2O4. 2H2O) in the whole of the given solution = ………………..g