THE PSBB MILLENNIUM SCHOOL

DLF Garden City, Thazhambur,

Chennai-600130

CHEMISTRY LABORATORY MANUAL

CLASS 12

Name of the student:

Roll number:

1
2
INDEX

1. Preparation of standard solution

2. Estimation of KMnO4 using std Oxalic acid

3. Estimation of KMnO4 using std Mohr’s salt solution.

4. Ascending chromatography

5. Circular chromatography

6. Preparation of starch sol

7. Preparation of alum

8. Preparation of dibenzal acetone

9. Study in variation of cell potential with change in concentration.

10. Kinetic study of the effect of concentration on the rate of reaction

11. Kinetic study of the effect of change in temperature on the rate of the reaction

12. Role of emulsifying agents

13. Thermochemistry - Enthalpy of dissolution of CuSO4

13. Analysis of alcoholic group

14. Analysis of phenolic group

15. Analysis of carbonyl group-aldehyde

16. Analysis of carbonyl group-ketone

17. Analysis of carboxylic group

18. Analysis of amino group.

19. Analysis of carbohydrates

20. Analysis of fats and oils

21. Analysis of proteins

22. Salt analysis general procedure [Not to be written in the record]

23. Salt analysis – Individual Salts

3
Expt.no.1

Observations and Calculations:

1. Weight of watch glass with Oxalic acid,w1g =---------------g

2. Weight of empty watch glass w2g =---------------g
3. Weight of Oxalic acid w3= w1 – w2 =------ -= -------------g
4. Volume of standard flask, V = -------------ml
5. Gram Molecular Mass of Oxalic acid = 126
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑂𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 𝑥 1000
6. Molarity of Oxalic acid, Mo = 𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑥 𝑉𝑜𝑙 𝑜𝑓 𝑠𝑡𝑑 𝑓𝑙𝑎𝑠𝑘

= = ----------M

LHS-PG 1

4
Experiment no.1

Preparation of standard solution

1. Aim: - To prepare the standard solution of M/40 Oxalic acid.

2. Theory: - A solution whose concentration is known, is called a standard solution. The
Standard sodium carbonate solution, std oxalic acid solution etc. are some examples.
Concentration of a solution is defined as the amount of a solute present in a definite
volume of the solvent. It can be expressed in terms of normality, molarity, molality etc

Molarity: Molarity of a solution is defined as the number of gram moles of the solute
per litre of the solution. It is denoted by ‘M’

3. Procedure:-
• About 0.63g of oxalic acid is taken in a watch glass and weighed using chemical
balance. It is noted down as w1.
• The contents of the watch glass are transferred into standard flask using a funnel
and the contents are washed down the funnel using a little amount of water.
• The empty watch glass is weighed and the weight is noted down as w2.
• The oxalic acid is dissolved using water and the funnel is washed down
thoroughly with water into the standard flask.
• Remove the funnel and using a wash bottle pour in more water till the level of
water reaches just below the etched mark on the neck of the standard flask.
Using a dropper add the last few drops of water so that the lower end of the
meniscus coincides with the etched mark.
• Close the bottle with the stopper and shake it thoroughly so that the solution
concentration becomes uniform throughout.
• Knowing the weight of oxalic acid added, the molarity of the solution can be
calculated.
• Label the solution.
4. Precautions:-
i. The watch glass should be weighed soon after the transfer of the component.
ii. The lower meniscus should coincide with the etched mark on the standard flask.
iii. The standard flask should be closed properly so that no leakage happens which
may alter the molarity.
5. Result :- The molarity of the solution = ---------M.

5
Experiment no.2
1. Key notes:-
a) Ionic equation: 2MnO4- + 16H+ + 5C2O4 2- 2Mn+2 + 8H2O + 10CO2
b) Molecular equation
2KMnO4 + 8H2SO4 + 5 H2C2O4 .2H2O K2SO4 + 2MnSO4 + 10CO2 + 18H2O

c) Burette solution: KMnO4

d) Pipette solution: Std Oxalic acid
e) Indicator : KMnO4 (self-indicator)
f) Colour change : Colourless to permanent pale pink colour
g) Weight of oxalic acid required to prepare the given standard solution,
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑥 𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑡𝑑 𝑓𝑙𝑎𝑠𝑘
w = 1000
0.025 𝑥 126 𝑥 100
= 1000
= -----------g
2. Observations and Calculations
Weight of watch glass and oxalic acid =xg
Weight of empty watch glass =yg
Weight of Oxalic acid = (x-y) g

𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑂𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 𝑥 1000

Molarity of the Oxalic acid prepared, MO= 𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑥 𝑉𝑜𝑙 𝑜𝑓 𝑠𝑡𝑑 𝑓𝑙𝑎𝑠𝑘

(𝑥−𝑦) 𝑥 1000
= =
126 𝑥 100

=-------M

Burette readings: STD OXALIC ACID X KMnO4

Sl.no. Volume of Burette readings Volume of
Oxalic acid Initial Final KMnO4
(ml) (ml)

1. 20

2. 20

3. 20

Concordant value = --------ml

𝑀𝐾 𝑉𝐾 𝑀𝑂 𝑉𝑂
𝑛𝑘
= 𝑛𝑂
𝑀𝑂 𝑉𝑂 𝑛𝐾
MK = 𝑛𝑂 𝑉𝐾

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Expt no.2
Estimation of Potassium Permanganate Using Standard Oxalic Acid

AIM: To determine the strength of the given KMnO4 solution using std Oxalic acid
solution
Theory: In this titration, KMnO4 is the titrant and oxalic acid is the analyte. Here, potassium
permanganate is the oxidizing agent and oxalic acid is the reducing agent. The reaction between
potassium permanganate and oxalic acid is carried out in an acidic medium because the
permanganate ion in the acidic medium is a very strong oxidizing agent. Acidity is introduced
by adding dil. H2SO4.

Molecular equation

2KMnO4 + 8H2SO4 + 5 H2C2O4 .2H2O K2SO4 + 2MnSO4 + 10CO2 +18H2O

Ionic equation 2MnO4- + 16H+ + 5C2O4 2- 2Mn+2 + 8H2O + 10CO2

From the balanced chemical equation, it is clear that 2 moles of KMnO4 reacts with 5 moles
of oxalic acid.

According to the molarity equation,

Procedure

• Weigh the required amount of Oxalic acid crystals to prepare M/40 Oxalic acid
solution. Prepare 100ml of the solution in a standard flask. Rinse the pipette using this
solution and pipette out 20ml of the same Oxalic acid solution into a conical flask.
• Rinse the cleaned burette with the given KMnO4 solution and fill it with the same
solution. Note the initial reading.

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 𝑀𝑂 𝑥 20 𝑥 2
= 5 𝑥 𝑉𝐾

=--------M
Weight per litre of KMnO4 = 𝑀𝐾 𝑥 158
= ------ x 158 = g/L

8
 • Add one full test tube(20ml) of dil. sulphuric acid into the above conical flask having
Oxalic acid solution and heat the solution to about 60-700C (bearable warmth).
• Add KMnO4 solution from the burette in small volumes with constant shaking. Make
sure the potassium permanganate drops get decolourised before the next drop is added.
Continue adding till a permanent pale pink colour is imparted to the solution on addition
of a last single drop of KMnO4 solution. Note the final reading of the burette
• Repeat for concordant values.
Result
i) Molarity of KMnO4 ,Mk = ----M
ii) Weight per litre of KMnO4=----g/L

Precautions
• c
• Read the upper meniscus while taking burette reading with KMnO4 solution.
• If oxalic acid or some oxalate is to be titrated, add required amount of dil.H2SO4 and heat
the flask to 60°-70°C.
• Let no drop of solution be at the tip of the burette at the end point.
• Add about an equal volume of dil.H2SO4 to the solution to be titrated before adding
KMnO4.
• Do not rinse the titration flask with the solution.
• Give a rotatory motion to the titration flask throughout the titration.
• Place the titration flask containing solution on a white tile to see the colour change
correctly.

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 Expt no.3
Key notes:-
a) Ionic equation
MnO4- + 8H+ + 5Fe 2+ Mn+2 + 4H2O + 5Fe 3+
b) Molecular equation
2KMnO4 + 8H2SO4 + 10[FeSO4.(NH4)2SO4.6H2O] 2MnSO4 + K2SO4 +
68H2O +5 Fe2(SO4)3 + 10(NH4)2SO4
c) Burette solution: KMnO4
d) Pipette solution: Std FAS solution
e) Indicator : KMnO4 (self-indicator)
f) Colour change : Colourless to permanent pale pink colour
g) Weight of oxalic acid required to prepare the given standard solution,
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑥 𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑡𝑑 𝑓𝑙𝑎𝑠𝑘
w= 1000
0.05 𝑥 392 𝑥 100
= 1000

= -----------g
3. Observations and Calculations
Weight of watch glass and FAS =xg
Weight of empty watch glass =yg
Weight of FAS = (x-y) g =
=
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐹𝐴𝑆 𝑥 1000
Molarity of the FAS prepared, MFAS= 𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑥 𝑉𝑜𝑙 𝑜𝑓 𝑠𝑡𝑑 𝑓𝑙𝑎𝑠𝑘
( 𝑥−𝑦) 𝑥 1000
= =
392 𝑥 100
=-------M

Burette readings: STD FAS X KMnO4

Sl.no. Volume of FAS Burette readings Volume of
solution (ml) Initial Final KMnO4 (ml)

1. 20

2. 20

3. 20

Concordant value = --------ml

𝑀𝐾 𝑉𝐾 𝑀𝐹 𝑉𝐹 𝑀𝐹 𝑉𝐹 𝑛𝐾
= MK =
𝑛𝑘 𝑛𝐹 𝑛𝐹 𝑉𝐾

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Expt no.3

Estimation of KMnO4 using std Mohr’s salt solution.

Aim:- To determine the strength of the given KMnO4 solution using M/20 FAS solution.

Theory:- In this titration, potassium permanganate is the oxidizing agent and Mohr’s salt is the
reducing agent. Mohr’s salt is a double salt of ferrous sulphate and ammonium sulphate and its
composition is FeSO4 (NH4)2SO4.6H2O. It is a primary standard. Therefore, its standard
solution can be prepared directly. Ferrous ions of Mohr’s salt undergo hydrolysis in aqueous
solution. To prevent the hydrolysis, Conc. H2SO4 needs to be added to the Mohr’s salt crystals
during the preparation of its standard solution.

In this titration, the MnO4- ion is reduced to Mn2+ in the presence of acid and Fe2+ ions of
Mohr’s salt is oxidized to Fe3+. The chemical reaction that occurs in this titration can be
represented by the following chemical equations.

Molecular equation

2KMnO4 + 8H2SO4 + 10[FeSO4 (NH4)2SO4.6H2O] 2MnSO4 + K2SO4 + 68H2O +5 Fe2 (SO4)3 +

10(NH4)2SO4
Ionic equation: MnO4- + 8H+ + 5Fe 2+ Mn+2 + 4H2O + 5Fe 3+

From the overall balanced chemical equation, it is clear that 2 moles of potassium
permanganate react with 10 moles of Mohr’s salt.

Procedure

• Prepare 100ml of M/20 FAS solution by dissolving the required amount of Mohr’s salt
in water. Add less than quarter test-tube of dil sulphuric acid through the funnel into
the standard flask during the preparation.
• Rinse and fill the burette with the given KMnO4 solution and note down the initial
reading.
• Rinse the pipette with the above solution and pipette out 20ml of the above solution
into conical flask followed by 20ml of dil sulphuric acid.
• Titrate the FAS solution with the KMnO4 solution in the burette till you get a permanent
pale pink colour. Note the final reading of the burette.
• Repeat the titration for concordant values.

Result
i) Molarity of KMnO4, Mk = ----M
ii) Weight per litre of KMnO4 =----g/L

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 𝑀𝐹 𝑥 20 𝑥 1
MK = =
5 𝑥 𝑉𝐾

=--------M
Weight per litre of KMnO4 = Mk x158 = ____ x 158
= ------g/L

Result
i) Molarity of KMnO4, Mk = ----M
ii) Weight per litre of KMnO4=----g/L

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Precautions:
• Rinse the pipette and burette first with distilled water then with the
corresponding solutions.
• Close the pipette with the index finger.
• Do not blow out the last drop of the solution from the jet end of the pipette.
• Do not allow any air bubbles to remain inside the burette.
• Read the upper meniscus while taking burette reading with KMnO4 solution.
• If oxalic acid or some oxalate is to be titrated, add required amount of
dil.H2SO4 and heat the flask to 60°-70°C.
• Let no drop of solution be at the tip of the burette at the end point.
• Add about an equal volume of dil.H2SO4 to the solution to be titrated before
adding KMnO4.
• Do not rinse the titration flask with the solution.
• Give a rotatory motion to the titration flask throughout the titration.
• Place the titration flask containing solution on a white tile to see the colour
change correctly.

13
Observations

Sl.no. Colour of the Distance travelled by the Distance RF value

spot component from the original line travelled by the
(cm) solvent from the
original line (cm)

Calculations: Rf(Pb2+) =

Rf(Cd2+) =

Inference

• Rf value of Pb2+ = ……………

• Rf value of Cd2+ = …………..

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Expt no. 4
Ascending Chromatography

Aim: Separation of the constituents of a mixture of inorganic compounds containing two

cations, Pb2+ and Cd2+, using a chromatographic technique.

Theory: Ascending paper chromatography is a type of partition chromatography which

depends on the continuous differential partitioning of components of a mixture between the
stationary phase and the mobile phase. Here the stationary phase is considered to be the water
molecules bound to the cellulose network of chromatographic paper mobile phase is the
solvent. The relative adsorption of each component of the mixture is expressed in terms of its
Retardation factor (Rf) (Retention factor). It is defined as the distance moved up or travelled
by the component from the original line to the distance travelled by the solvent from the
original line.

The two cations to be separated being colourless, a developer is needed. In the present case,
ammonium sulphide (NH4)2S can be used to locate the position of these ions on
chromatographic paper or plate.

Materials required: Pb(NO3)2, Cd(NO3)2, chromatography sheets, isopropyl alcohol, (NH4)2S

and water.

Procedure:

• On a Whatman No. 1 filter paper with the help of a pencil, mark a line at a distance of
3 cm from one of the ends of this paper.
• Put a spot of the mixture [ Lead nitrate & Cadmium nitrate] on the marked line with
the help of a fine capillary.
• Hang the filter paper in a jar containing a mixture of ethanol, 6.0 M HNO3, and distilled
water, in the ratio 8:1:1.
• Keep the jar as such till the mobile phase (solvent) rises to two-thirds of the length of
the paper.
• Remove the filter paper from the jar, mark the solvent front.
• Spray ammonium sulphide solution on the chromatography paper to obtain spots of
yellow and black colour. Mark the position of spots with a pencil and allow the paper
to dry. Measure the distance moved by the solvent front and the different spots of the
cations with respect to the reference line. This distance is the shortest distance between
the reference line and the centre of different spots.
• Record the observations in tabular form. Calculate the Rf value for each cation.
Inference:
(i) Rf value of Pb2+ ions is __________.
(ii) R f value of Cd2+ ions is __________.

15
Observations
Distance travelled by the Distance travelled by the
component from the centre solvent from the centre
SI Rf
Components
No. (cm) (cm) value

1 2

1. Red

2. Blue

Calculations: Rf(red) =

Rf(blue) =

Inference

• Rf value of red ink = ……………

• Rf value of blue ink = …………..

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Expt no.5 Circular Chromatography

Aim: Separation of components from a mixture of red and blue inks

Theory

Circular paper chromatography is a type of partition chromatography which depends on the

continuous differential partitioning of components of a mixture between the stationary phase
and the mobile phase. Here the stationary phase is considered to be the water molecules bound
to the cellulose network of chromatographic paper mobile phase is the solvent. The relative
adsorption of each component of the mixture is expressed in terms of its Retardation factor
(Rf) (Retention factor). It is defined as the distance moved up or travelled by the component
from the original line to the distance travelled by the solvent from the original line

Materials required: red and blue ink, chromatography sheets, isopropyl alcohol or acetone,
water

Procedure:

• Take a circular Whatman filter paper and mark its centre. Cut a thin strip along the
radius, about 2cm away from the centre and bend it to make it vertical.
• Using a fine capillary tube, put a drop of the mixture of red and blue inks at the centre
of the paper. Let it dry in air.
• Put another drop on the same spot and dry again, so that the spot is rich in the mixture.
• Pour equal amounts of isopropyl alcohol or acetone and distilled water into a dry
petridish and mix it well using a glass rod. This is used as the solvent.
• The filter paper is kept on the petridish in such a way that the tail was touching the
developing solvent. A funnel is kept inverted on the paper to provide uniform tension
in all directions
• Develop the chromatogram. The different components of the mixture here appear as
bands or rings.
• Dry the filter paper and put pencil marks at the centre of the red and blue ink spots.
• Measure the distance of the two spots from the original line and the distance of the
solvent from the centre of the paper.
• Calculate the Rf values of the red and blue inks using the formula.

Inference

• Rf value of red ink = ……………

• Rf value of blue ink = …………..

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Expt. No. 6 Preparation of Starch solution

Aim: To prepare starch solution

Theory

Colloids are the dissolved state of substances that either do not pass, or pass very slowly
through a parchment paper or animal membrane. A few examples of colloids are starch, glue
and gelatine.

Depending upon the nature of the interaction between the dispersed phase and dispersion
medium sols can be classified into two types.

1. Lyophilic sols
2. Lyophobic sols

A colloidal solution where there is a strong attraction between the dispersed phase and
dispersion medium, i.e., the dispersed phase has great affinity for the dispersion medium that
results in the extensive solvation of the colloidal particles. In such solids, the dispersed phase
does not easily precipitate and the sols are quite stable. These sols are reversible in nature.

Materials required

Soluble starch, distilled water, beaker, glass rod, Bunsen burner

Procedure

• Weigh a small quantity (500mg or 1 g) of soluble starch on an electronic balance.

• Transfer the weighed quantity of starch into a mortar and add few drops of distilled
water.
• Grind the starch using the pestle to make a thin paste and transfer the paste into a 50 ml
beaker.
• Take about 100 ml of distilled water in a 250 ml beaker and heat the beaker till the
water starts to boil.
• Pour the starch paste slowly into the boiling water while stirring using a glass rod.
• Continue boiling for about 10 minutes and then allow the beaker to cool.
• Filter the contents of the beaker, through a filter paper fixed in a funnel and collect the
filtrate.
• Label the filtrate as Starch Sol.
• Take a parchment bag and fold it in the shape of a bag.
• Tie it to the end of the stem of a funnel with a thread.
• Pour the given starch sol containing sodium chloride into the parchment bag through
the funnel till the bag is two-third full.
• Take a 400 ml beaker and fill it upto three-fourth with distilled water and place it over
an iron stand.

18
 • Dip the parchment bag into the distilled water and fix the funnel in position using a
clamp.
• Allow it to stand for about half an hour.
• Withdraw about 1 ml of water from the beaker using a dropper and transfer it into a
test tube.
• Add a few drops of iodine solution to the test tube.
• As no blue colour appears, it indicates the absence of starch in water. This means that
starch molecules do not diffuse through a parchment membrane.
• Now withdraw another 1 ml of water from the beaker and transfer it into another test
tube.
• Add a few drops of silver nitrtate solution to it.
• A white precipitate of silver chloride is produced immediately indicating the presence
of chloride ions and hence NaCl in water. It means that sodium ions and chloride ions
diffuse through the parchment membrane. As Na+ and Cl- diffuse out of the starch
sol, it gets free from the ions gradually.
• In order to check whether NaCl is completely removed change the water in the beaker
with fresh distilled water and again place the parchment bag containing sol in it.
• After about 10 minutes, test for the presence of Cl- ions.
• If no white precipitate is formed, Cl- ions are absent and dialysis is complete otherwise
dialysis should be continued.

Precautions

• Distilled water should be used for preparing sols in water.

• Starch should be converted into a fine paste before adding to boiling water.
• Starch paste should be added in a thin stream to boiling water.
• Constant stirring of the contents is necessary during the preparation of the sol.

19
Expt no.7 Preparation of Alum crystals

Aim: To prepare alum crystals.

Theory

Alums are double salts with the formula X2SO4.Y2 (SO4).24H2O where X and Y are mono and
trivalent metal ions respectively. In potash alum, they are made by mixing together a saturated
solution of potassium sulphate and aluminium sulphate followed by crystallization. This can
be represented as

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

The potash alum thus obtained is a transparent octahedral crystal

Procedure

2 grams of potassium sulphate were dissolved in minimum amount of water in a beaker to get
its saturated solution. Similarly a saturated solution of 5g of aluminium sulphate was prepared
in water in a separate beaker which contained a few drops of dilute sulphuric acid. Both
solutions were mixed and heated to crystallization point and left aside. Crystals formed were
isolated by decantation and then dried using filter paper.

Result

Thus octahedral transparent crystals of potash alum were obtained.

Precautions

• Excess water should not be used in dissolving potassium sulphate and aluminium
sulphate.
• Solution containing the double salt must be free of all impurities
• Solution when left aside for crystallization must be covered with a watch glass.
It should not be quickly cooled by keeping in cold water.
• Addition of dilute sulphuric acid must not be forgotten. It prevents the hydrolysis
of aluminium sulphate to ammonium hydroxide.

20
Expt no.8 Preparation of dibenzal acetone

Aim: To prepare dibenzal acetone using the given chemicals

Materials Required

• Benzaldehyde - 2.5ml,acetone - 1ml,10% NaOH solution - 5ml,Rectified spirit - 25ml

Conical flask, Beaker, Test tube, Funnel, Filter papers, Burner

Procedure

1. Take 2.5ml of benzaldehyde, 10ml of acetone and 25ml of rectified spirit in a conical
flask. Cork the flask and shake it to obtain a clear solution.
2. Take 5 ml of 10% NaOH solution in a test tube and add this to the conical flask drop
by drop by shaking the flask. Maintain the temperature of the reaction mixture between
20-25oC while adding the sodium hydroxide solution.
3. Cork the flask again and shake vigorously for about 10 minutes, releasing the pressure
from time to time.
4. Allow it to stand for about 20 minutes at room temperature and then cool in ice water
for a few minutes.
5. Filter the yellow-coloured solid and wash it with water.
6. Recrystallisation of Dibenzal acetone: Dissolve the above yellow-coloured crude solid
in the minimum amount of hot rectified spirit and then allow it to cool slowly. Pale
yellow crystals of dibenzal acetone separate. Filter the crystals and dry them by pressing
them between the folds of a filter paper, and then measure the weight of the crystals.

Observation

The weight of Dibenzal acetone = ___________ g.

Precautions

• Add NaOH drop wise to the reaction mixture while shaking of the flask continuously.
• Wash the precipitate with water to remove traces of NaOH sticking to it.
• Use minimum amount of rectified spirit to dissolve the crude sample for
crystallisation

21
Experiment No.9 (LHS)

Study of the variation of cell potential of Daniel cell with change in concentration of
electrolytes

Observations
Concentration of ZnSO4 solution Concentration of EMF of the Cell
Sl.No. (M) CuSO4 solution (M) (V)
1 1
1 0.5
1 0.25
0.5 1
0.25 1

22
Experiment no.9

Aim: To study the variation of cell potential with respect to the changes in the concentration
of electrolytes in a Daniel cell.

Materials required:

1M zinc sulphate solution, Copper sulphate solution, Zinc electrode, Copper

electrode, Beakers, Voltmeter, Salt bridge, connecting wires.

Theory: The anodic reaction is represented as:

The cathodic reaction is represented as:

The total cell reaction is: Zn(s) + Cu2+(aq) Zn2+ (aq) + Cu (s)

Preparation of salt bridge

• In a U-shaped tube heat 20gm of agar-agar gel and 5gm of KCl in a beaker.
• Suck the molten mixtures into U-shaped tube.
• Allow it to cool.
Procedure:

• Take two clean beakers.In one beaker take 1 M copper sulphate solution and in the
other take 1 M zinc sulphate solution.
• Take a copper strip and clean it using a sand paper.
• Dip the copper strip into the beaker containing the 1 M copper sulphate solution.
• Similarly, take a zinc strip and clean it using a sand paper.
• Then dip it into the beaker containing 1 M zinc sulphate solution.
• Take a salt bridge and connect the two solutions using the salt bridge.
• Take a voltmeter and connect the copper strip to the positive terminal and the zinc
strip to the negative terminal using connecting wires.
• Note the position of the pointer in the voltmeter and record the reading.
• Repeat the experiment by taking different concentrations of zinc sulphate and
copper sulphate solutions.

Result:-1. The Ecell decreases with increase in molar concentration of [Zn2+]. (Zinc sulphate solution).
2.The Ecell increases with increase in molar concentration of [Cu2+]. (CuSO4 solution)

Precautions: 1. Immediately after use, place the salt bridge in distilled water.
2.Very carefully dilute the solution to another concentration.
3.Always clean strips of copper and zinc with sandpaper and connect the wires before use.

23
 Expt .no 10

Kinetics study on the effect of concentration on rate of reaction.(LHS)

Observations

Time
Vol of
Total vol taken for
0.1M Vol of Conc of Vol of
Flask of cross to
Na2S2O3 water Na2S2O3 1M HCl 1/t (s-1)
No. solution become
solution (ml) solution (ml)
(ml) invisible
(ml)
t (s)
1 10 40 50 0.02
2 20 30 50 0.04
3 30 20 50 0.06
4 40 10 50 0.08
5 50 0 50 0.10

24
Expt .no 10

Kinetics study on the effect of concentration on rate of reaction.

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

Materials Required:

• Burettes
• Conical flasks
• Stop-watch
• 0.1M sodium thiosulphate (Na2S2O3) solution
• 1M HCl
• Distilled water.

Theory

The effect of concentration of the reactant on the rate of a reaction can be studied easily by
the reaction between sodium thiosulphate and hydrochloric acid.

• Theinsoluble sulphur formed remain in the mixture as a white or pale yellow precipitate
or a colloid that gives a milky appearance and makes the solution opaque. Therefore
the rate of the reaction can be studied by monitoring the opaqueness of the reaction.
This can be easily done by measuring the time taken (t) for forming a certain amount
of sulphur.
• We can plot a graph between 1/t (in second) and the concentration of sodium
thiosulphate by taking 1/t along ordinate axis and concentration of Na2S2O3 along
abscissa. The graph should be a straight slopping line.

25
Draw Graph

26
 • From the graph, it is clear that 1/t is directly proportional to the concentration of
Na2S2O3. But 1/t is a direct measure of the rate of the reaction. Therefore the rate of the
reaction between Na2S2O3 and HCl is directly proportional to the concentration of
Na2S2O3 solution.

Procedure

• Take five clean conical flasks and label them as A, B, C, D and E respectively.
• Add 10, 20, 30, 40 and 50 ml of 0.1M sodium thiosulphate solution to the flasks A, B,
C, D and E respectively.
• Then add 40, 30, 20 and 10ml of distilled water to the flask A, B, C and D respectively
so that volume of solution in each flask is 50ml.
• Add 10ml of 1M HCl to the conical flask A.
• When half of the HCl solution has been added to the conical flask, start the stop- watch
immediately.
• Shake the contents of the conical flask and place it on a white tile that has a cross mark
at the centre.
• Go on observing from the top of the flask and stop the stop-watch when the cross marks
just becomes invisible. Note down the time.
• Repeat the experiment by adding 10ml of 1M HCl to flasks B, C, D and E respectively
and record the time taken in each case for the cross to become just invisible.

Result:

From the graph it is proved that the rate of the reaction is directly proportional to the
concentration of the reactant.

27
Expt no.11

Kinetic study on the effect of change in temperature on rate of reaction.(LHS)

Observations:

Volume of 0.1M Na2S2O3 solution taken each time = 50 ml

Volume of 1M HCl added each time - 10 ml

Time taken
0
S.No. Temperature ( C) for the cross 1/t (s-1)
to become
invisible, t (s)

28
Expt no.11

Kinetic study on the effect of change in temperature on rate of reaction.

Aim:- To study the effect of change in temperature on the rate of reaction between
sodium thiosulphate and hydrochloric acid

Materials required:-

• Burettes
• Conical flasks
• Stop-watch
• 0.1M sodium thiosulphate (Na2S2O3) solution
• 1M HCl
• Distilled water

Theory:- For every 100C rise in temperature, the rate of the reaction becomes almost double.
As the temperature rises the fraction of molecules having kinetic energy greater than the
threshold energy also increases which increases the effective collisions per second.

Procedure:

• Take 50 ml of 0.1M Na2S2O3 solution in a 100 ml conical flask and note its
temperature with the help of a thermometer.
• Add 10 ml of 1M HCl to it and start the stopwatch immediately when half of the
hydrochloric acid solution has been added.
• Shake the contents of the flask gently and place it on the tile with a cross-mark.
• Observe the cross—mark from the top and note the time taken for the mark to
become just invisible.
• Empty the flask and clean it thoroughly with conc.HNO3 and then with water
• Take again 50 ml of 0.1M Na2S2O3 in conical flask and heat it so that the
temperature of the solution becomes (T+100 )C
• Remove the flask from the tripod stand and add 10 ml of 1M HCl to it and start
the stopwatch
• Shake the contents gently and place it on the tile having a cross-mark
• Note the time taken for the mark to become just impossible
• Repeat the experiment at ( T+20 )0C, ( T+30 )0C and ( T+40 )0C temperatures
and record the observations as given below

Graph

Plot a graph taking 1/t along the ordinate axis and temperature along the abscissa.

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

29
Exp. No.12 Role of emulsifying agents

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

tube emulsion detergent detergent
B
C
D
E

30
Experiment no.12.

Aim: To study the role of emulsifying agents to stabilize the emulsions of different oils.
Theory:
An emulsion is a colloid where both the dispersion medium and the dispersed phase are in
liquid form.
Here it has been differentiated based on their relative proportions.
The dispersed phase is in a smaller quantity and the dispersion medium is present in a larger
proportion.
If you mix oil and water, after shaking the mixture you will notice a slightly milky solution that
is soluble, is unstable and is known as an emulsion of oil in water. It will form two layers,
separating water and oil.
If you want to increase the stability of the emulsion of oil and water soap solution can be added.
Since it acts as an emulsifying agent. The interfacial surface tension between the two layers is
decreased by the carboxyl polar group.
Soap concentration is the optimum concentration required to complete the emulsification
process. To get an effective stabilization the amount should not be more or less than optimum
concentration.
Materials required: The materials required for the experiment are given below:Test tube,
Glass rod, Stopwatch, Soap or detergent, droppers, mustard oil, linseed oil, machine oil, and
castor oil.rocedure:
1. Take a test tube. Put 10mL of distilled water and dissolve 1g of detergent in it.
Vigorously shake the test tube and label the test tube as “A”.
2. Take 4 more test tubes and label them as B, C, D, E. Add 5mL distilled water in each
test tube. Put 10 drops of mustard oil in the test tube B, 10 drops of linseed oil in C, 10
drops of castor oil in D, and 10 drops of machine oil in test tube E.
3. Take the test tube B in your hand and shake it vigorously for 5 minutes and keep it aside
in a test tube Stand. Start your stopwatch to record the time required to separate the two
layers.
4. Follow the same process with other test tubes – C, D, and E.
5. Add two drops of soap solution or detergent which were prepared in test tube A into
each test tube. Shake each test tube for 5 minutes. And record the time taken to separate
the two layers.
6. Record the results

Precautions:
(a) Add an equal number of drops of a soap/detergent solution to all the test tubes.
(b) To minimise the error in recording the time required for the separation of layers in
different systems, shake all the test tubes for an identical time.
(c) Start the stopwatch immediately after shaking is stopped and stop it immediately when
the two layers separate.

31
Observations and calculations [LHS]:

A. Determination of Calorimeter constant

Temperature readings:
Tc (0C) Th (0C) Tm (0C)

4.184 𝑥
W= = JK-1

B. Determination of Enthalpy of dissolution

C. Temperature readings:
T1(0C) T2 (0C)

Total mass of the solution = Mass of Solvent + Mass of Solute = (100 + W1 ) g =

Change in temperature = (T2 - T1 ) °C

Enthalpy change of the calorimeter (beaker) = W (T2 - T1 )

Enthalpy change of solution for (T2 – T1)0C = [(100 + W1 ) (T2 - T1 )] 4.184 J

Total enthalpy change of the Calorimeter = [W (t'2 - t'1 ) + (100 + W1 ) (t'2 – t'1 )] × 4.184 J
(beaker) and solution

Heat liberated on dissolution of 1 g copper sulphate =

[W (t′2 − t′1 ) + (100 + W1 ) (t′2 – t′1 )] × 4.184
W1
=

Since 1 mol of copper sulphate weighs 249.5 g. Therefore,

∆sol H of CuSO4 .5H2O = 249.5 × Heat liberated on dissolution of 1 g copper sulphate

32
Expt. No. 13
Thermochemistry calculations – Enthalpy of dissolution of CuSO4
Aim: To determine the enthalpy of dissolution of copper sulphate/ potassium nitrate.
Theory: Measurement of heat changes is carried out in vessels called calorimeters. During the
measurement of heat changes, the calorimeter, thermometer, and stirrer also absorb some heat;
this amount of heat should also be known. It is called the calorimeter constant. The method of
mixtures is used to determine the calorimeter constant. To determine the calorimeter constant,
a known volume of hot water at a specified temperature is added to the known volume of water
contained in the calorimeter at room temperature. Since energy is conserved, the heat taken by
the calorimeter and cold water should be equal to the heat given by hot water. Thus, we can
write the following equation :
∆H1 + ∆H2 = –∆H3

Enthalpy change Enthalpy Enthalpy

of calorimeter, change of change of
stirrer and cold water hot water
thermometer

Let Tc , Th and Tm be temperatures of cold water, hot water, and mixture respectively.
The calorimeter constant W can be found using the formula

In thermochemical measurements, generally, aqueous solutions have water as the reaction

medium, and the temperature changes result due to the chemical reactions taking place in the
solution. According to the law of conservation of energy, the sum of enthalpy changes taking
place in the calorimeter (loss and gain of energy) must be zero. Thus, we can write the following
equation

Enthalpy of a solution is the amount of heat liberated or absorbed when one mole of a solute
(solid/liquid) is dissolved in such a large quantity of solvent (usually water) that further dilution
does not make any heat changes.
Material Required: Beakers, Thermometer (110°C), Glass rod, Cotton wool, Small wooden
block Small piece of cardboard Stirrer, and Copper sulphate/ potassium nitrate.
Procedure:
A. Determination of Calorimeter constant of calorimeter (Beaker)
• Take 100 mL of water in a calorimeter and insert a thermometer and stirrer in
it.

33
 • Record the temperature of water. Let this temperature be tc °C.
• In another one marked ‘B’ take 100 mL of hot water (50-60°C). (vi) Note the
exact temperature of hot water. Let this temperature be th °C.
• Lift the cardboard and pour the hot water contained in calorimeter B into
calorimeter A. Stir the mixed water and note the temperature. Let this
temperature be tm °C.
• Calculate the calorimeter constant of the beaker by using the expression given
below. (Remember the three temperatures are in the order th > tm >tc ).

B. Determination of Enthalpy of Dissolution

• Take 100 mL of distilled water in the beaker of which the calorimeter constant
has been determined.
• Record the temperature of water already taken in the calorimeter. Let this be t'1
°C.
• Add weighed amount, say W1 g of well-powdered copper sulphate in water and
stir the solution with a stirrer till the entire amount of copper sulphate dissolves.
• Note down the temperature attained by the solution after the addition of copper
sulphate. Let this be t'2 °C.
• Calculate the enthalpy of dissolution of copper sulphate using the observed
details.
Result
Enthalpy change in the dissolution of copper sulphate/potassium nitrate is _______
Jmol–1.
Precautions–
(a) To record the temperature of water, use a thermometer with 0.1°C graduation.
(b) In the determination of calorimeter constant record the temperature of hot water
just before mixing.
(c) (f) Avoid using very large amounts of copper sulphate/potassium nitrate.
(d) Stir the solution well to dissolve the solid and record the temperature. Avoid too
much stirring, it may produce heat due to friction.
(e) Weigh copper sulphate carefully as it is hygroscopic in nature.

34
 Experiment 14

Analysis of functional groups- Test for Alcoholic groups

State of the organic compound: Liquid

Colour and odour of the compound: Colourless and odourless

Tests for Alcoholic Group

Experiment Procedure Observation Inference

Brisk
effervescence is
Sodium metal Take about 1 ml of the given liquid in a dry test tube,
due to the
Test add about 1gram of anhydrous calcium sulphate and Brisk
evolution of
shake well to remove water. Filter the liquid into effervescence is
hydrogen gas
another clean dry test tube and add a small piece of produced.
indicating the
sodium metal.
presence of
alcoholic group.

Take about 1 ml of the give liquid in a clean dry test

tube, add about 1 ml glacial acetic acid and 2-3
A fruity smell is Presence of
Ester Test drops of conc. sulphuric acid. Warm the mixture on
produced. alcoholic group.
a water bath for about 10 minutes. Pour it into about
20 ml of cold water taken in a beaker and smell.

Ceric Take about 1 ml of the given liquid in a clean dry Pink or red
Presence of
ammonium test tube and add few drops of ceric ammonium colour is
alcoholic group.
nitrate Test nitrate reagent and shake it well. developed.

Result: The given organic compound has alcohol as its functional group

35
 Expt no.15
TESTS FOR PHENOLIC GROUP

State of the organic compound: Liquid

Colour and odour of the compound: Colourless/ pink with phenolic smell

Experiment Procedure Observation Inference

Presence of
Place a drop of the given liquid (or a crystal Blue litmus
Litmus Test phenolic
if solid) on a moist blue litmus paper. turns to red.
group.
Take about 1 ml of neutral ferric chloride Presence of
Ferric chloride Violet colour is
solution in a clean test tube and add 2-3 drops phenolic
Test seen.
of the given liquid (or the crystal is solid). group.
Take a small quantity of sodium nitrite in a
clean dry test tube and add about 1 ml of the
A deep blue or
given liquid (or crystal if solid). Heat the test
green
tube very gently for half a minute and allow
colouration is
it to cool. Then add about 1 ml of conc.
seen. Presence of
Liebermann’s sulphuric acid and shake the test tube to mix
the contents. phenolic
Test
group.
Colour turns to
Add distilled water carefully to the test tube.
red.
Deep blue or
Add excess of sodium hydroxide solution to
green colour
the test tube.
appears.
Result: The given organic compound has phenol as its functional group

36
 Expt no.16 TESTS FOR CARBONYL GROUP

State of the organic compound: Liquid

Colour and odour of the compound: Colourless with a pleasant smell

Take a small quantity of the given compound in

2,4- a clean dry test tube, and add rectified spirit Yellow or
Presence of
Dintrophenyl until the compound just dissolves. Now add a orange
carbonyl
hydrazine few drops of 2, 4-dinitrophenyl hydrazine precipitate is
group.
Test solution. Cork the test tube, shake the mixture, formed.
and allow it to stand for 5 minutes.

Take about 2 ml of saturated solution of sodium White

Sodium Presence of
bisulphite in a clean test tube and add a small crystalline
bisulphite carbonyl
quantity of the given compound. Cork the test precipitate is
Test group.
tube, shake and leave it for 15-20 minutes. formed.

Differentiating Tests for Aldehydes

Experiment Procedure Observation Inference

Presence of
Dissolve a small quantity of the given
Pink colour is aldehydic
Schiff’s Test compound in a clean test tube and add about 1
seen. group is
ml of Schiff’s reagent and shake it well.
confirmed.

Take about 1 ml of silver nitrate solution in a

clean test tube and add 2-3 ml of dilute NaOH
solution. A brown precipitate of silver oxide Presence of
Tollen’s Test Shining silver
forms. Now add dilute ammonia solution aldehydic
(Silver mirror mirror is
dropwise until the brown precipitate of silver group is
test) formed.
oxide just dissolves. To this add 3-4 drops of confirmed.
the given liquid (or 0.1 g if solid) and warm the
test tube on a water bath for about 5 minutes.

Take 1 ml each of Fehling’s solution A and B Presence of

Red
Fehling’s in a test tube. Add 4-5 drops of the given aldehydic
precipitate is
Test organic liquid (or 0.2g if solid) and warm the group is
formed.
test in a water bath for 4-5 minutes. confirmed.

Result: The given organic compound has aldehyde as its functional group

37
Expt.no.17
Tests for ketonic group
State of the organic compound: Liquid

Colour and odour of the compound: Colourless with pleasant smell

Take a small quantity of the given compound in

2,4- a clean dry test tube, add rectified spirit until the Yellow or
Presence of
Dintrophenyl compound just dissolves. Now add few drops of orange
carbonyl
hydrazine 2, 4-dinitrophenyl hydrazine solution. Cork the precipitate is
group.
Test test tube, shake the mixture and allow it to stand formed.
for 5 minutes.

Take about 2 ml of saturated solution of sodium White

Sodium Presence of
bisulphite in a clean test tube and add a small crystalline
bisulphite carbonyl
quantity of the given compound. Cork the test precipitate is
Test group.
tube, shake and leave it for 15-20 minutes. formed.

Take about 1 ml of silver nitrate solution in a clean

test tube and add 2-3 ml of dilute NaOH solution. A
Tollen’s brown precipitate of silver oxide forms. Now add No Shining
Presence of
Test dilute ammonia solution dropwise until the brown silver
Ketonic group
(Silver precipitate of silver oxide just dissolves. To this add mirror is
is confirmed.
mirror test) 3-4 drops of the given liquid (or 0.1 g if solid) and formed.
warm the test tube on a water bath for about 5
minutes.

Dissolve a small quantity of sodium nitroprusside

Presence of
Sodium in about 1 ml of distilled water in a clean test tube
Red ketonic
nitroprusside and then add a small quantity of the given
colouration. group is
Test compound. Shake the test tube well and add sodium
confirmed.
hydroxide solution drop wise.

Result: The given organic compound has ketone as its functional group

38
 Expt no. 18 Tests for Carboxylic Group
State of the organic compound: Solid / Liquid

Colour and odour of the compound: Colourless and odourless

Experiment Procedure Observation Inference

Presence of
Litmus Place a drop of the given liquid (or a crystal if solid) on Blue litmus turns
carboxylic
Test a moist blue litmus paper. to red.
group.

Sodium
Brisk Presence of
Hydrogen Take 1 ml of the given organic compound in a test tube
effervescence is carboxylic
Carbonate and add a pinch of sodium bicarbonate to it.
observed. group.
Test

Take a small quantity of the given organic compound in

a clean test tube, add 1 ml of ethyl alcohol and 1-2 drops Presence of
Ester Test of conc. sulphuric acid into it. Heat the reaction mixture Fruity smell. carboxylic
on a water bath for about 5 minutes. Pour the mixture group.
into a beaker containing water.

Result: The given organic compound has carboxylic acid as its functional group

39
 Expt no.19 Tests for Amino Group

State of the organic compound: Liquid

Colour and odour of the compound: Brown with fishy smell

Experiment Procedure Observation Inference

Take a small quantity of the given compound in a clean Compound is

Solubility Compound may
test tube and add 2-3 ml of dil. HCl and shake the test soluble in dil.
Test be amine.
tube well. HCl.

Place a drop of the given liquid (or a pinch of solid) on Red litmus Compound may
Litmus Test
a moist red litmus paper. turns to blue. be amine.

Take three test tubes A, B and C. In test tube A,

dissolve a small quantity of the compound in 2 ml of
HCl. In test tube B, prepare an aqueous solution of Presence of
Formation of a
Azo-Dye sodium nitrite. In test tube C, dissolve a small quantity aromatic
red or orange
Test of β-naphthol in dilute sodium hydroxide. Place all the primary amine
dye.
three test tubes in an ice bath. Now add sodium nitrite is confirmed.
solution into test tube A and the resulting solution is
added to test tube C.

Result: The given organic compound has aromatic amine as its functional group

40
Expt no. 20
FOOD STUFF ANALYSIS
Analysis of Carbohydrates

Observation

SI Inference
Experiment Observation
No.

Solubility test
a)Soluble May be
1. Take a small amount of the carbohydrate
given sample in a test tube and
add 3 ml of distilled water into b)Insoluble
it and shake the test tube well. May be starch

Molisch’s test
A red violet
Take about 2 ml of aqueous (purple) ring is
2. solution of the sample in a test formed at the Presence of
tube and add few drops of junction of two carbohydrate
Molisch’s reagent into it. Pour
layers.
1 ml conc. H2SO4 slowly along
the side of the test tube.

Fehling’s test
A reddish
Take 2 ml of aqueous solution precipitate is
presence of a
3. of the sample in a test tube and formed.
reducing sugar
add 1-2 ml each of Fehling’s
No reddish
solution A and Fehling’s Absence of
solution B into it. Keep the test precipitate
reducing sugar
tube in a boiling water bath.

Benedict’s test

Take 1-2 ml of aqueous Reddish

solution of the sample in a test A reddish precipitate
4. tube and add 1-2 ml of precipitate is indicates the
Benedict’s reagent. Keep the formed presence of a
test tube in a boiling water reducing sugar.
bath.

41
 Tollen’s test

Take 2-3 ml of aqueous

5.
solution of the sample in a test A shinning silver
A shinning silver
tube and add 2-3 ml of Tollen’s mirror indicates
mirror is formed
reagent. Keep the test tube in a the presence of a
boiling water bath for 10 reducing sugar.
minutes.

Iodine test

Take a small amount of Appearance of

Appearance of blue
6. aqueous solution of the sample blue colouration
in a test tube and add 1-2 drops colouration indicates the
of iodine solution into it. presence of starch

42
Expt no.21 Analysis of Oils & Fats.

SI.
No Experiment Observation Inference
.

Oil or fat is
Sample is immiscible.
present.

Water
Oil or fat is
Sample is miscible.
absent.

Sample forms a lower layer which Oil or fat is

1. dissolves on heating. present.
Alcohol
Sample does not dissolve even on Oil or fat is
Solubility heating. absent.

Oil or fat is
Sample is miscible.
present.
Chloroform
Oil or fat is
Sample is immiscible.
absent.

Transluscent Spot test

Transluscent spot appears on the presence of oil or

2. Place a little of the substance on a
filter paper and press it on the folds filter paper fat
of the filter paper and unfold the
filter paper.

43
Expt no:22 Analysis of Proteins

SI No. Experiment Observation Inference

Biuret test

Take a small quantity of the

dispersion of the sample in a
1. test tube and add 2 ml of Bluish violet colour is
10%NaOH solution into it. formed.
Now add 4-5 drops of 1%
Presence of protein
CuSO4 solution and warm the
mixture for about 5 minutes.

Xanthoproteic test

Take about 2 ml of the sample

2. in a test tube and add few A yellow precipitate is
Presence of protein
drops of conc. HNO3 into it formed.
and heat the test tube.

Millon’s test

Take 1-2 ml of the sample in a White precipitate which

3. test tube and add 2 drops of changes to brick red on
Millon’s reagent. boiling Presence of protein.

44
45
46
 GENERAL PROCEDURE FOR SALT ANALYSIS
Sl
No. Experiment Observation Inference

Absence of Ni,Cu ,Mn,Co

Colourless and ferric salts
Brown presence of ferric salts
1 Colour and appearance bright pink presence of cobalt salts
presence of manganese
pale pink salts
Green presence of nickel salts
Blue presence of copper salts
2 Solubility
Solubility of the salt tested in
presence of water soluble
a) water Soluble salts
b)dil.HCl a)effervescence with the
evolved gas turning lime
water milky May be Carbonate
b)vinegar smell with
effervescence presence of acetate
c)gas with rotten egg
smell turning lead
acetate paper black Presence of sulphide
d)Pale yellow gas turning
ferrous sulphate solution
black was evolved Presence of nitrite
e) pungent smelling gas
which turns acidified
dichromate paper green
was evolved Presence of sulphite
f) white ppt may be group I cation
3 Flame test

No characteristic colour Absence of group 5

imparted by the flame cations and Copper salts

A small amount of the paste of the salt in conc.HCl

was introduced into the non-luminous flame by a) bluish green colour presence of Copper cation
means of a match stick
b) brick red colour presence of Calcium salt
c)scarlet red colour presence of Strontium salt
d) Apple green or grassy
presence of Barium salt
green colour
4 Action of heat

47
 A small amount of the salt is heated in a dry test
tube a)Violet vapours Presence of iodide
b) Reddish brown gas Presence of bromide or
was evolved nitrate
c) colourless , pungent
gas presence of chloride
d) colourless gas with
rotten egg smell Presence of sulphide
e) strong vinegar smell presence of acetate
f)colourless gas with a
pungent smell turning presence of ammonium
red litmus blue salt
g)colour of salt changed
from blue to white Presence of Copper salt
h)colour of salt changed
from green to brown
and finally black presence of Nickel salt
h)colour of salt changed
to yellow when hot and
turns white when cold presence of zinc salt
g)colourless odourless
gas turning lime water
milky presence of carbonate
e) No characteristic Absence of any hydrated
change salts

Preparation of sodium carbonate extract

About 2g of the salt is mixed with twice its amount of sodium carbonate and mixed with about 20 ml of water . It
is boiledto half the volume ,cooled and filtered . The filterate is called sodium carbonate extract.
Preparation of original solution
A little of the salt is dissolved in water/dil.HCl to prepare the original salt solution

TEST FOR ACID RADICALS

Sl
no EXPERIMENT OBSERVATION INFERENCE
1 TEST WITH Dil SULPHURIC ACID
a) Brisk effervescence May be
with evolution of a a) carbonate
colourless ,odourless
Take a little of the salt in a dry test tube and add 2- gas. b) sulphite
3 ml dil sulphuric acid into it. b)colourless gas with
smell of burning sulphur.
c) colourless gas with
smell of rotten eggs c) sulphide
2 TEST WITH Conc.SULPHURIC ACID
Take a little of the salt in a dry test tube and add 2- a) Pungent smelling gas
3 ml conc. sulphuric acid into it. May be chloride
which gives dense white

48
 fumes when a glass rod
dipped in ammonium
hydroxide is shown to
the evolving gas.
b) reddish brown gas May be bromide
c) violet colour gas May be iodide
d) brown colour gas May be nitrate
e) colourless gas with May be acetate
smell of vinegar
3 Test for SULPHATE
White ppt insoluble in
Take 2-3 ml of SCE and add a few drops of dil.HCl conc HCl
Presence of sulphate
followed by 2-3 ml of BaCl2 solution.

4 Test for Phosphate- Ammonium Molybdate Test

Take 2-3 ml of SCE or about 1 g of the salt in a test Canary yellow ppt or
tube and add a few drops of conc.nitric acid and phosphate is confirmed
colouration
heat it. To this add a few drops of ammonium
molybdate reagent and heat it again followed by
cooling.
CONFIRMATORY TESTS
CARBONATES

Presence of carbonate
Take 2-3 g of the salt and add dil sulphuric acid Lime water turns milky
confirmed
into it. Pass the evolving gas through lime water
SULPHITE
Take 2-3 g of the salt and add potassium
Green colouration is Presence of sulphite
dichromate solution into it and 2-3 drops of
obtained confirmed
dil.sulphuric acid.
SULPHIDE
Take a few drops of salt solution add few drops of Presence of sulphide
acetic acid followed by 1ml of lead acetate Black ppt
confirmed
solution
HALIDES ( CHLORIDE , BROMIDE, IODIDE)
a) curdy white ppt
soluble in ammonium May be chloride
hydroxide solution
Take the salt or SCE in a test tube and add dil nitric b) light yellow ppt
1 acid . Boil off CO2 gas . Cool it and add a few drops partially soluble in May be bromide
of silver nitrate solution ammonium hydroxide

c) yellow ppt insoluble in May be iodide

ammonium hydroxide

49
2 Chromyl chloride test for chloride

reddish brown vapours

are evolved which when
A little of the salt along with 2g potassium passed through NaOH Presence of chloride
dichromate and 3-4ml conc. Sulphuric acid is solution and treated confirmed
heated carefully in a dry hard glass test tube . with acetic acid and lead
acetate will give a yellow
ppt.
NITRATE

Dark brown fumes are

1 Take salt in atest tube and add conc. Sulphuric acid Presence of nitrate
formed
and Cu turnings into it and heat .
2 BROWN RING TEST

Take salt solution or SCE in atest tube and add Presence of nitrate
freshly prepared ferrous sulphate solution and Brown ring is formed at confirmed
incline the test tube at 450 and add conc sulphuric the junction of two
acid along the sides of the test tube. liquids
ACETATE
Take SCE or salt solution in a test tube and add Red colouration is
Acetate is confirmed
neutral ferric chloride solution formed
SULPHATE

Take salt solution or SCE in a test tube and add Presence of sulphate
White ppt
acetic acid and lead acetate to it . confirmed

RESULT :- The given salt contain ----------------- as acid radical

TEST FOR BASIC RADICALS

Test for group zero – ammonium
Pungent ammonia
smelling gas is evolved
which forms dense
Take a pinch of the salt in a test tube and add white fumes when a
May be ammonium
sodium hydroxide solution and heat it gently glass rod dipped in
conc.HCl is brought near
the mouth of the test
tube
CONFIRMATORY
Presence of ammonium
Take a little of the salt in a test tube and add NaOH Chocolate -brown ppt
confirmed .
solution and Nessler's reagent

Test for group one - lead cation

Take salt solution in a test tube and add dil.HCl .
White ppt May be Lead

CONFIRMATORY

50
 Filter the above ppt and add 2-3 ml of water and White ppt dissolves May be Lead
boil. Divide this colourless solution into 2 parts
Presence of lead
a) Yellow ppt
To one part add few drops of KI solution confirmed

Presence of lead
b) To the second part add few drops potassium Yellow ppt
confirmed
chromate solution
Test for group two - Copper & arsenic cations
Black ppt Presence of copper
Pass hydrogen sulphide through the solution taken
for group I analysis if group I is absent Yellow ppt Presence of Arsenic
CONFIRMATORY- copper
Collect the black ppt and dissolve in 50% nitric acid and divide into 3 parts
a) To one part add few drops of ammonium blue solution is abtained Presence of copper
hydroxide solution

Presence of copper
b) To the second part add few drops of acetic acid Chocolate -brown ppt
confirmed
and potassium ferrocyanide solution
CONFIRMATORY-Arsenic

Filter the above ppt and dissolve it in conc.nitric Presence of Arsenic

Yellow ppt
acid . Add solid crystals of ammonium molybdate confirmed
and boil it.
Test for group three - Ferric and aluminium
ions

a)Reddish-brown ppt Presence of ferric ion

If grp II is absent , boil off hydrogen sulphide from

the solution and add 1ml of conc. Nitric acid and b) Gelatinous white ppt Presence of aluminium ion
boil it again .To the clear filtrate add ammonium
chloride and then ammonium hydroxide till the
solution distinctly smells of ammonia.
CONFIRMATORY

Collect the ppt obtained in grp III in a test tube and dissolve it in dil HCl and divide it into two parts

FERRIC ION
To the second part add potassium ferrocyanide Prussian blue Presence of ferric ion
a)
solution colouration is formed confirmed
ALUMINIUM ION

51
 To the first part add excess of ammonium Gelatinous white ppt is Presence of aluminium ion
a)
hydroxide solution obtained
b)

Blue ppt floats in Presence of aluminium ion

LAKE TEST -To the second part add dil HCl
colorless solution confirmed
followed by 3-4 drops of blue litmus solution and
then add ammonium hydroxide solution till the
blue colour develops
If there is no ppt in grp III ,add excess ammonium chloride and excess ammonium hydroxide to the salt solution
and divide it into 3 parts for the detection of grp IV grp V and grp VI
Test for group IV - Cobalt , Nickel, Zinc and Manganese ions
To the first part pass hydrogen sulphide gas presence of nickel or
black ppt
cobalt ions
presence of manganese
buff coloured ppt ion
dirty white ppt presence of zinc ions
CONFIRMATORY Nickel and cobalt ions
Yellow residue Presence of nickel
1 Filter the black ppt and dissolve it in aqua regia .
Heat the solution to dryness Blue residue Presence of cobalt

Presence of nickel
2 Dissolve the residue in distilled water and add a Bright rose red ppt
confirmed
few drops of ammonium hydroxide and dimethyl
glyoxime ( DMG )
Take blue residue in a test tube and dissolve it in pink colour solution is
3 Presence of cobalt
distilled water . formed
Take the salt solution and warm it . Add NaOH A blue colouration is
4 cobalt is confirmed
solution . obtained
CONFIRMATORY - Manganese ion

Dissolve the buff coloured ppt in minimum quantity of dil HCl and boil off hydrogen sulphide gas from it .
white ppt formed turns
presence of manganese
1 Add NaOH solution to this brown black with
ion
bromine water
CONFIRMATORY -Zinc ion
Dissolve the dirty white ppt in minimum quantity of dil HCl and boil off hydrogen sulphide gas . Diide the
soluion into two parts
Presence of zinc
White ppt
1 To the first part add aqueous solution of NaOH . confirmed

To the second part add few drops of potassium bluish white ppt is Presence of zinc
2
ferrocyanide solution formed confirmed

52
 Test for group V - Calcium , strontium and barium ions

To the second part of the third group solution,add

ammonium hydroxide solution and ammonium White ppt Presence of group V ions
carbonate solution in excess.

Collect white ppt from group V and dissolve it in acetic acid and heat it.Divide the solution into three parts .
CONFIRMATORY - Barium ion
Yellow ppt Presence of Barium
To the first part , add potassium chromate solution
Presence of Barium
Flame test Apple - green flame confirmed
CONFIRMATORY - Strontium ion
To the third part, add ammonium sulphate white ppt Presence of strontium
solution confirmed
Flame test Crimson red flame Presence of strontium
confirmed
CONFIRMATORY - Calcium ion
To the second part of the solution add ammonium Presence of calcium
white ppt
oxalate confirmed
Presence of calcium
Flame test Brick red ppt confirmed
Test for group VI - Magnesium ion
white ppt
To the third part, add diammonium hydrogen Maybe magnesium
phosphate solution
Shiny pink colour
To this white ppt add NaOH followed by Titan Magnesium cation present
yellow

Confirmatory Test

A little of the salt solution is boiled with

Concentrated nitric acid & Cobalt nitrate Presence of magnesium
A pink ash is obtained
solution A filter paper dipped in it is burnt to cation confirmed
ash by burning .

RESULT
CATION
ANION
CHEMICAL FORMULA
CHEMICAL NAME

53
I Analysis of Ammonium sulphate

Preliminary tests

Sl No. Experiment Observation Inference

Absence of
Ni2+,Cu2+
1 Colour and appearance Colourless
,Mn2+,Co2+ and
ferric salts

Solubility
2 Solubility of the salt tested in:
presence of
water soluble
a) water Soluble salts
b)dil.HCl No characteristic Absence of
observation carbonate,lead
etc.

Flame test
A small amount of the paste of the Absence of
No characteristic colour
salt in conc.HCl was introduced goup V and II
imparted by the flame
into the non-luminous flame using cations
a match stick

3
4 Action of heat

colourless gas with a

pungent Maybe
A small amount of the salt is
ammoniacal smell ammonium
heated in a dry test tube
turning red litmus salt
blue

Preparation of sodium carbonate extract

About 2g of the salt is mixed with twice its amount of sodium carbonate and mixed with about 20
ml of water. It is boiled to half the volume, cooled and filtered. The filtrate is called sodium
carbonate extract.
Preparation of orginal solution
A little of the salt is dissolved in water / dil HCl to prepare the original salt solution
Analysis of anions
Sl no EXPERIMENT OBSERVATION INFERENCE
CARBONATE

54
 No characteristic Absence of
1
Take 1 mL of the sodium observation carbonate
carbonate extract in a atest tube
and add 4-5 ml of dil sulphuric acid
into it.
ACETATE

Take a little quantity of sodium

carbonate extract in a test tube No characteristic Absence of
2.
and add 2 ml of conc. sulphuric observation acetate
acid
CHLORIDE

Take little quantity of sodium

carbonate extract and add 1-2 ml
of concentrated sulphuric acid. No characteristic Absence of
3
Bring glass rod dipped in observation chloride
ammonium hydroxide near to the
mouth of the test tube.

NITRATE

Take a little quantity of sodium

carbonate extract in a test tube No characteristic Absence of
4
and add 2-3 ml of conc. sulphuric observation nitrate
acid and add Cu turnings to it.

Test for SULPHATE

55
 Take 2-3 ml of sodium carbonate
extract and add 1-2 ml of dil.HCl May be
5 White ppt is formed
followed by 1-2 ml of BaCl2 sulphate
solution.

CONFIRMATORY TEST FOR

SULPHATE

a) Collect the percipitate and

Precipitate does not dissolve Sulphate is
dissolve it in concentrated
in conc. Hydrochloric acid confirmed
hydrochloric acid

b) Take 2-3 ml of sodium

carbonate extract or aqueous
white precipitate of lead Sulphate is
solution of salt and add few drops
sulphate is obtained confirmed
of acetic acid and lead acetate
solution

TEST FOR
BASIC
RADICALS
Test for group zero – ammonium

Pungent ammonia smelling

Take a pinch of the salt in a test
gas is evolved which forms May be
1 tube and add sodium hydroxide
dense white fumes when a ammonium
solution and heat it gently glass rod dipped in conc. HCl
is brought near the mouth of
the test tube
CONFIRMATORY

Presence of
Chocolate -brown ppt ammonium
Take a little of the salt in a test confirmed
tube and add NaOH solution and
Nessler's reagent.
RESULT :-
Cation: Ammonium NH4+
Anion: Sulphate SO42-
Chemical Formula:(NH4)2SO4
Chemical Name:Ammonium
Sulphate

56
II Analysis of Aluminium Chloride (AlCl3)

Preliminary Test :-

S.No Experiment Observation Inference

1. Colour: Colourless Absence of Cu2,+, Ni2+, Co2+,

Mn2+ and ferric salts.

2. Solubility:
i) in H2O Soluble Presence of H2O soluble salts
Absence of carbonate and
ii) in HCl Soluble group I cation
3. Flame Test:
A small amount of the salt No change Absence of Ca2+, Ba2+, Sr2+,
made into a paste with conc. and Cu2+
HCl was introduced into the
non-luminous flame by
means of a match stick
4. Action of Heat:
A small amount of the salt is Colourless, pungent gas is May be Chloride
heated in a dry test tube evolved

Preparation of Sodium Carbonate Extract

About 2g of the salt is mixed with twice its amount of sodium carbonate and mixed with about 20 ml
of water. It is boiled to half the volume, cooled and filtered. The filtrate is called sodium carbonate
extract.

Preparation of Original Solution

A little of the salt is dissolved in water / dil HCl to prepare the original salt solution

1. Analysis of Anions :-

S.No Experiment Observation Inference

1. Test for Carbonate:

Take a little of the salt in a No Change Absence of Carbonate
dry test tube and add 2-3 ml
of dil. Sulphuric Acid
2. Test for Acetate:
No gas with smell of vinegar Absence of Acetate

57
 Take a little of the sodium
carbonate extract in a test
tube and add 2-3 ml conc.
Sulphuric Acid into it.
3. Test for Chloride:
Take a little of the sodium Pungent Gas evolved which May be Chloride
carbonate extract in a test forms dense white fumes
tube and add 2-3 ml conc. when a glass rod dipped in
Sulphuric Acid into it. ammonia solution is shown.

Confirmatory Test:
Take the SCE in a test tube Curdy white ppt. soluble in
and add dil. nitric acid. Boil Ammonium Hydroxide Presence of chloride anion
off CO2 gas. Cool it and add a solution confirmed
few drops of silver nitrate
solution
NITRATE
Take a little quantity of
sodium carbonate extract in
4 a test tube and add 2-3 ml of No characteristic observation Absence of nitrate
conc. sulphuric acid and add
Cu turnings to it.

Test for SULPHATE

Take 2-3 ml of sodium
carbonate extract and add 1-
5 No characteristic observation Absence of Sulphate
2 ml of dil.HCl followed by 1-
2 ml of BaCl2 solution.

2. Analysis of Cation :-

S.No Experiment Observation Inference

1. Test for Group 0:

Ammonium Cation:
Take a pinch of the salt in a No characteristic change Absence of Ammonium
test tube and add sodium
hydroxide solution and heat
it gently.

2. Test for Group I:

Lead Cation:
Take salt solution in a test No characteristic change Absence of Lead
tube and add dil. HCl.

58
3. Test for Group II:
Copper and Arsenic: No characteristic change Absence of Copper and
Pass Hydrogen Sulphide Arsenic Radicals
through the solution taken
for group I analysis if group I
is absent
4. Test for Group III:
Aluminium and Ferric ions:
If grp II is absent, boil off Gelatinous White ppt. May be Aluminium
Hydrogen Sulphide from the
solution and add 1ml of conc.
Nitric acid and boil it again.
To the clear filtrate add
Ammonium Chloride and
then Ammonium Hydroxide
till the solution distinctly
smells of Ammonia.
Confirmatory Test:
Dissolve ppt. in dil. HCl
followed by 3-4 drops of blue Blue ppt floats in colourless Presence of Aluminium
litmus solution and then add solution cation Confirmed
ammonium hydroxide
solution till the blue color
develops
3. Result :-
i) Anion: Chloride Cl-
ii) Cation: Aluminium Al3+
iii) Name of the Compound: Aluminium Chloride
iv) Formula of the compound: AlCl3

59
III Analysis of Lead Acetate

1. Preliminary experiment

Experiment Observation Inference

• Colour and Colourless Absence of Cu2+, Ca2+, Ni2+,
appearance: Co2+, Mn2+ and ferric salts.

• Solubility:
In H2O Soluble. Presence of water-soluble
salts.
In dil. HCl White precipitate is observed. May be Lead.
• Flame test:

A little amount of the No characteristic flame Absence of Ba2+, Ca2+, Sr2+ and
salt is treated with observed. Cu2+.
conc. HCl to make a
paste and a small
amount is brought into
a non-luminous flame
using a matchstick.

• Action of heat:

A little amount of the A strong smell of vinegar is May be Acetate.

salt is taken in a dry felt.
test tube and gently
heated over a flame.

2. Preparation of sodium carbonate extract:

Take a little salt in a dry test tube and add to it twice the amount of Sodium Carbonate
(Na2CO3). After adding 20ml of water to it boil it to half its volume. Cool and filter the
solution. This extract is called the sodium carbonate extract of the salt.

3. Preparation of original solution:

Take some salt in a dry test tube and add 3-4ml water to it. Shake the test tube well. This is
called the original solution of the salt.

60
 4.Analysis of anion:

Experiment Observation Inference

Test for Carbonate:

Take 3-4 ml of the sodium No characteristic observation. Absence of carbonate.

carbonate extract in a dry test
tube and treat it with 4 ml dil.
H2SO4.
Test for Acetate:

Take 3-4 ml of the sodium A colourless gas with a May be Acetate.

carbonate extract in a dry test characteristic smell of vinegar is
tube and treat it with 2-3 ml dil. evolved.
H2SO4.

Confirmatory Test:

A little amount of the sodium

carbonate extract is taken in a
dry test tube and a little neutral A red colour is obtained. Acetate is confirmed.
Ferric Chloride(FeCl3) solution is
added to it.
Test for Chloride:
Take a little of the sodium No characteristic change Absence of chloride anion
carbonate extract in a test tube
and add 2-3 ml conc. Sulphuric
Acid into it.

Test for Nitrate

Take a little quantity of sodium No characteristic change Absence of nitrate
carbonate extract in a test tube
and add 2-3 ml of conc. sulphuric
acid and add Cu turnings to it.
Test for Sulphate
Take 2-3 ml of sodium carbonate
extract and add 1-2 ml of dil.HCl No characteristic change Absence of Sulphate
followed by 1-2 ml of BaCl2
solution.

61
 4. Analysis of cation

Experiment Observation Inference

Test for Ammonium:

A little amount of the salt is

taken in a test tube and a little No characteristic observation. Absence of Ammonium.
sodium hydroxide solution is
added to it.
Test for Lead:

Take a little of the original White precipitate is obtained. May be lead.

solution, add dil. HCl and
shake the test tube well.

Filter the precipitate and

collect it in a test tube. Add 2-
3 ml of water to it and boil.

Now divide this solution into 2 White precipitate dissolves. May be lead.
parts.

To the first part add 4-5 ml of Yellow precipitate is formed. Lead is confirmed.
potassium iodide (KI) solution.

To the second part add a few

drops of potassium chromate Yellow precipitate is formed. Lead is confirmed.
(K2CrO4) solution.

5. Result:

Anion : The given anion is acetate.CH3COO-

Cation : The given cation is lead. Pb2+

Name of the compound : The given compound is lead acetate.

Formula of the compound : Pb(CH3COO)2

62
IV Analysis of Strontium carbonate

1.Preliminary experiment

Experiment Observation Inference

Colour and Appearance White Absence of Cu2+, Ba2+, Ni2+, Co2+,

Mn2+ and ferric salts.

Solubility in water Insoluble Absence of water soluble salts

Solubility in HCl effervescence with the evolved Maybe carbonate

gas turning lime water milky

Flame test

A paste of conc. HCl and salt is scarlet red May be Sr2+

introduced to non-luminous
flame.

Action of heat

Heat small amount of dry salt in colourless gas evolved turning Presence of carbonate
dry test tube lime water milky

2.Preparation of sodium carbonate extract

The salt is mixed with twice its amount of sodium carbonate and mixed with about 20ml of water.
This is then boiled to half its volume ,cooled and filtered. The filtrate is called sodium carbonate
extract.

3.Preparation of original solution

Salt is dissolved in water/ dil HCl to prepare the original solution.

4.Analysis of anion.

Experiment Observation Inference

CARBONATE

Add dil H2SO4 to a little amount Brisk effervescence is formed Maybe carbonate
of the sodium carbonate with the evolution of a
extract. colourless gas

Pass gas through the limewater Limewater turns milky Carbonate confirmed

63
 Test for Acetate:

Take a little of the sodium No gas with smell of vinegar Absence of Acetate
carbonate extract in a test tube
and add 2-3 ml conc. Sulphuric
Acid into it.

Test for Chloride:

Take a little of the sodium No pungent gas evolved Absence of Chloride

carbonate extract in a test tube
and add 2-3 ml conc. Sulphuric
Acid into it.

Test for nitrate

Take a little quantity of sodium

carbonate extract in a test tube No characteristic observation Absence of nitrate
and add 2-3 ml of conc.
sulphuric acid and add Cu
turnings to it.

Test for sulphate

Take 2-3 ml of sodium

carbonate extract and add 1-2 No characteristic observation Absence of Sulphate
ml of dil.HCl followed by 1-2 ml
of BaCl2 solution.

5. Analysis of cation

Experiment Observation Inference

GROUP 0

Add sodium hydroxide to salt No characteristic change Absence of group 0 cation

and heat

GROUP 1

Dil HCl is added to the salt No characteristic change Absence of lead cation
solution

GROUP 2

Pass H2S through the above No characteristic change Absence of copper or arsenic
solution cation

GROUP 3

64
 Boil off H2S from above solution No characteristic change Absence of ferric and
and add conc nitric acid and aluminium cation
boil. Add ammonium chloride
and ammonium hydroxide till it
smells of ammonia

If group three is absent, add excess of ammonium chloride and ammonium hydroxide to the salt
solution and divide it into three parts for the detection of group four, group five and group six.

GROUP 4

To the first part of group 3 No characteristic change Absence of group 4 cation

solution pass H2S gas.

GROUP 5

To the second part of group 3 white precipitate formed Presence of group 5 cation
solution add ammonium
hydroxide and ammonium
carbonate in excess

Dissolve the ppt in acetic acid and heat it .Divide the solution into 3 parts

To the 1st part add potassium No yellow precipitate Absence of barium

chromate solution

To the 2nd part add ammonium white precipitate formed strontium confirmed
sulphate

To the 3rd part add ammonium No white precipitate formed Absence of Calcium ion
oxalate

Flame test

A paste of conc. HCl and salt is scarlet red Presence of Sr2+ confirmed
introduced to non-luminous
flame.

6.Result

Anion : Carbonate CO32-

Cation : Strontium Sr2+

Name of the compound: Strontium Carbonate

Formula of the compound: SrCO3

65
V Analysis of zinc sulphate:

1.Preliminary experiment

Experiment Observation Inference

Colour and appearance: Colourless Absence of Ni2+, Cu2+, Mn2+,

Co2+, and ferric salts.

Solubility: Soluble Presence of water soluble

a)water salts.

b)dil.HCl Soluble Absence of carbonate, acetate,

and group1 cation.

Flame test: No characteristic colour Absence of Ca2+,Ba2+,Sr2+,Cu2+.

A small amount of paste of the imparted by the flame.
salt in conc.HCl was
introduced into a non-
luminous by means of a match
stick.
Action of heat: Colour of salt changes to Presence of zinc.
A small amount of salt is yellow when hot and turn to
heated in a dry test tube. white when cold.

2. Preparation of sodium carbonate extract:

About 2g of the salt is mixed with twice its amount of sodium carbonate and mixed with about 20 ml
of water . It is boiled to half the volume ,cooled and filtered . The filtrate is called sodium carbonate
extract.

3. Preparation of original solution:

A little of the salt / dil HCl is dissolved in water to prepare the original salt solution.

4. Analysis of anion.

Experiment Observation Inference

Carbonate: No characteristic observation Absence of carbonate
Take a little of the sodium
carbonate extract in a dry test
tube and add 2-3 ml dil
sulphuric acid into it.

Acetate: No characteristic observation Absence of acetate

66
 Take a little of the sodium
carbonate extract in a dry test
tube and add 2-3 ml conc.
sulphuric acid into it.

Chloride and nitrate: No characteristic observation Absence of chloride and

Take a little of the sodium nitrate
carbonate extract in a dry test
tube and add 2-3 ml conc.
sulphuric acid into it.

Sulphate:
Take 2-3 ml of SCE or salt White precipitate insoluble in Presence of sulphate
solution and add a few drops conc.HCl
of dil.HCl followed by 2-3 ml of
BaCl2 solution.

Confirmatory test:
Take salt solution or SCE in a White precipitate Presence of sulphate
test tube and add acetic acid confirmed
and lead acetate to it .

5. Analysis of cation

Experiment Observation Inference

Test for group zero –
ammonium:
Take a pinch of the salt in a
test tube and add sodium No characteristic observation Absence of ammonium
hydroxide solution and heat it
gently
Test for group one - lead
cation:
No characteristic observation Absence of lead
Take salt solution in a test tube
and add dil.HCl .

Test for group two - Copper & No characteristic observation Absence of group 2 cations
arsenic cations:
Pass hydrogen sulphide
through the solution taken for
group I analysis if group I is
absent

67
 Test for group three - Ferric No characteristic observation Absence of group 3 cations
and aluminium ions:
If grp II is absent , boil off
hydrogen sulphide from the
solution and add 1ml of conc.
Nitric acid and boil it again .To
the clear filtrate add
ammonium chloride and then
ammonium hydroxide till the
solution distinctly smells of
ammonia.

If there is no ppt in grp III, add excess of NH4Cl and NH4OH into the original solution and divide it
into 3 parts for the detection of grp IV grp V and grp VI cations.

Test for group IV dirty white ppt Presence of zinc cation

To the first part pass hydrogen
sulphide gas
Confirmatory test-Zinc ion:
Dissolve the dirty white ppt in minimum quantity of dil HCl and boil off hydrogen sulphide gas .
Divide the soluion into two parts
To the first part add aqueous White ppt Presence of zinc confirmed
solution of NaOH .
To the second part add few bluish white ppt is formed Presence of zinc confirmed
drops of potassium
ferrocyanide solution
6.Result

Anion :. sulphate SO42-

Cation :. Zinc Zn2+

Name of the compound:. Zinc sulphate

Formula of the compound:. ZnSO4

68
VI Analysis of Copper Nitrate

1.Preliminary experiment

Experiment Observation Inference

Colour Blue Presence of Copper salts

Solubility: In Water Soluble Presence of water soluble

salts

Solubility: In HCl Soluble Absence of Pb2+,CO32-

Flame Test
A paste of conc HCl and salt is Bluish green colour imparted May be group 2 cation
introduced to the non- to the flame
luminous flame.

Action of Heat
Heat small amount of dry salt Colour of salt changed from Maybe copper
in dry test tube blue to white

2. Preparation of sodium carbonate extract:

About 2g of the salt is mixed with twice its amount of sodium carbonate and mixed with about 20 ml
of water. It is boiled to half the volume, cooled and filtered. The filtrate is called sodium carbonate
extract.

3. Preparation of original solution

A little of the salt is dissolved in water to prepare the original salt solution

4. Analysis of anion.

Experiment Observation Inference

Carbonate No change Absence of Carbonate

Take a little of the sodium
carbonate extract in a dry test
tube and add 2-3 ml dil
sulphuric acid into it.

Acetate No change Absence of Acetate

Take a little of the sodium
carbonate extract in a dry test
tube and add 2-3 ml conc.
sulphuric acid into it.

69
 Nitrate
Take a little of the sodium Light brown fumes of Nitrate May be Nitrate
carbonate extract in a dry test are formed
tube and add 2-3 ml conc.
sulphuric acid into it.

Add Copper Turnings and heat Brown fumes intensified. Nitrate confirmed
it.

Brown Ring Test

Take salt solution or SCE in a Brown ring is formed at the Nitrate confirmed
test tube and add freshly junction of two liquids
prepared ferrous sulphate
solution and incline the test
tube at 450 and add conc
sulphuric acid along the sides
of the test tube.

Sulphate
Take 2-3 ml of SCE or salt No characteristic change Absence of Sulphate
solution and add a few drops
of dil.HCl followed by 2-3 ml
of BaCl2 solution.

5. Analysis of cation

Experiment Observation Inference

Group 0: Ammonium
Take a pinch of the salt in a No change Absence of Ammonium
test tube and add sodium
hydroxide solution and heat it
gently
Group 1: Lead
Take salt solution in a test No change Absence of Lead
tube and add dil.HCl .
Group 2: Copper

Pass hydrogen sulphide Black ppt Presence of copper

through the solution taken for
group I analysis if group I is
absent

Confirmatory Test

Collect the black ppt and

dissolve in 50% nitric acid and
divide into 3 parts

70
 To one part add few drops of Blue solution is obtained Presence of copper confirmed
ammonium hydroxide solution

To the second part add few

drops of acetic acid and Chocolate -brown ppt Presence of copper confirmed
potassium ferrocyanide
solution.

6.Result

Anion : Nitrate NO3-

Cation : Copper Cu2+

Name of the compound: Copper Nitrate

Formula of the compound: Cu(NO3)2

71
VII Analysis of Magnesium Carbonate

1.Preliminary experiment

Experiment Observation Inference

Colour and Appearance White Absence of Ni2+, Cu2+, Mn2+,

Co2+ and Fe3+ salts

Solubility in water Insoluble Absence of water soluble salts

Solubility in HCl effervescence with the evolved Maybe carbonate

gas turning lime water milky

Flame test No characteristic colour Absence of Sr2+, Ba2+, Ca2+

imparted to the flame.
A paste of conc HCl and salt is
introduced to the non-
luminous flame.

Action of heat colourless gas evolved turning Presence of carbonate

lime water milky
Heat small amount of dry salt in
dry test tube

2.Preparation of sodium carbonate extract

The salt is mixed with twice its amount of sodium carbonate and mixed with about 20ml of water.
This is then boiled to half its volume and cooled. the filtrate is called sodium carbonate extract.

3.Preparation of original solution

Salt is dissolved in water to prepare the original solution.

4.Analysis of anion.

Experiment Observation Inference

Test for Carbonate Brisk effervescence is formed Maybe carbonate

with the evolution of a
Add dil H2SO4 to the given salt.
colourless gas

Pass gas through the limewater Limewater turns milky Carbonate confirmed

Test for Acetate:

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 Take a little of the sodium No gas with smell of vinegar Absence of Acetate
carbonate extract in a test tube
and add 2-3 ml conc. Sulphuric
acid into it.

Test for Chloride:

Take a little of the sodium No pungent gas evolved Absence of Chloride

carbonate extract in a test tube
and add 2-3 ml conc. Sulphuric
Acid into it.

Test for nitrate

Take a little quantity of sodium

carbonate extract in a test tube No characteristic observation Absence of nitrate
and add 2-3 ml of conc.
sulphuric acid and add Cu
turnings to it.

Test for sulphate

Take 2-3 ml of sodium

carbonate extract and add 1-2 No characteristic observation Absence of Sulphate
ml of dil.HCl followed by 1-2 ml
of BaCl2 solution.

5. Analysis of cation

Experiment Observation Inference

GROUP 0

Add sodium hydroxide to salt No characteristic change Absence of group 0 cation

and heat

GROUP 1

Dil HCl is added to the salt No characteristic change Absence of group 1 cation
solution

GROUP 2

Pass H2S through the above No characteristic change Absence of group 2 cation
solution

GROUP 3

Boil off H2S from above solution No characteristic change Absence of group 3 cation
and add conc nitric acid and
boil. Add excess ammonium

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 chloride and ammonium
hydroxide till it smells of
ammonia

If group 3 is absent add excess ammonium chloride and excess ammonium hydroxide to the original
solution and divide it into three parts.

GROUP 4

To the first part of group 3 No characteristic change Absence of group 4 cation

solution pass H2S gas.

GROUP 5

To the second part of group 3 No characteristic change Absence of group 5 cation

solution add ammonium
hydroxide and ammonium
carbonate in excess

GROUP 6

To the 3rd part add white precipitate Maybe Magnesium cation

diammonium hydrogen
orthophosphate

To the above ppt add NaOH Shiny pink colour Presence of Magnesium cation
followed by Titan yellow

The salt solution is boiled with pink ash Magnesium cation confirmed
conc HNO3 and cobalt nitrate
solution. Filter paper dipped in
it is burnt to ash.

6.Result

Anion : Carbonate CO32-

Cation : Magnesium Mg 2+

Name of the compound: Magnesium Carbonate

Formula of the compound: MgCO3

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VII Analysis of Manganese chloride

1.Preliminary experiment

Experiment Observation Inference

1)Colour and appearance Pale pink Maybe manganese

2)Solubility

solubility of salt tested in: Soluble presence of water soluble salts

a)water

b)dil. HCl Soluble Absence of carbonate ion and

group 1 cation

3)Flame test No characteristic colour Absence of Cu2+,Ca2+,Sr2+,Ba2+

imparted by the flame

4)Action of heat

A small amount of the salt is Colourless,pungent gas Maybe chloride

heated in a test tube

2.Preparation of sodium carbonate extract

About 2g of the salt is mixed with twice its amount of sodium carbonate and mixed with 20 ml
of water. It is boiled to half the volume, cooled and filtered.The filtrate is called sodium carbonate
extract.

3.Preparation of original solution

A little of the salt is dissolved in water to prepare original salt solution

4.Analysis of anion.

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Experiment Observation Inference

Test for carbonate:

Take a little of the sodium

carbonate extract in a dry test
No characteristic observation Absence of carbonate
tube and add 2-3 ml of dil.
sulphuric acid into it.

Test for acetate:

Take a little of the sodium

carbonate extract in a dry test
No characteristic observation Absence of acetate
tube and add 2-3 ml of conc.
sulphuric acid to it

Test for chloride:

Take the sodium carbonate Pungent smelling gas which

extract in a test tube and add 2- gives white dense fumes when a
Maybe chloride
3 ml of conc. sulphuric acid glass rod dipped in ammonium
hydroxide is shown to the
evolving gas

Confirmatory test:

Confirmatory test- Silver nitrate

test

Take a little of the sodium

Curdy white ppt soluble in May be chloride
carbonate extract and add
ammonium hydroxide solution
dil.nitric acid. Boil off carbon
dioxide gas .Cool it and add a
few drops of silver nitrate
solution

Confirmatory test

A little of the salt along with 2g Reddish-brown vapours are

potassium dichromate and 3- evolved. When the above gas is
Presence of chloride confirmed
4ml con. sulphuric acid is heated passed through NaOH solution
carefully in a dry hard glass test and treated with acetic acid and
tube lead acetate it gives a yellow
ppt .

5. Analysis of cation

Experiment Observation Inference

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Test for group zero-ammonium:

Take a pinch of the salt in a test

tube and add sodium hydroxide
No characteristic observation Not ammonium
solution and Nessler’s reagent

Test for group one-Lead:

Take salt solution in a test tube

and add dil.HCl
No characteristic observation Not lead

Test for group two-Copper and arsenic:

Pass hydrogen sulphide

through the solution from group
one analysis if group one is
absent. No characteristic observation Not copper or arsenic

Experiment Observation Inference

Test for group three-Ferric and Aluminium

If group two is absent, boil of

hydrogen sulphide from the
solution and add 1 ml of conc.
nitric acid and boil it again. To
clear the filtrate ammonium
chloride and then ammonium No characteristic observation Not ferric or aluminium
hydroxide till the solution
distinctly smells of ammonia.

If group three is absent, add excess of ammonium chloride and ammonium hydroxide to the salt
solution and divide it into three parts for the detection of group four, group five and group six.

Test for group four-Cobalt, Nickel, Zinc and Manganese

To the first part pass hydrogen Buff coloured precipitate Maybe manganese
sulphide gas

Confirmatory test:

Dissolve the buff coloured precipitate in minimum quantity of dil.HCl and boil off hydrogen sulphide

Add sodium hydroxide to this white precipitate formed turns Presence of manganese is
brown-black with bromine confirmed
water.

77
6.Result

Anion : Chloride Cl-

Cation : Manganese Mn2+

Name of the compound: Manganese chloride

Formula of the compound: MnCl₂

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