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CHEMISTRY PRACTICAL RECORD WRITING

FOR CLASS XII


@

Educate  Enrich  Enlighten

TOPIC
EXPERIMENTS 1 - 30

1
CHEMISTRY
CLASS XII
RECORD WRITING AND LAB SESSION INSTRUCTIONS

All the students are supposed to wear Lab Coat and Safty gloves if necesasry.

* Records must be written in a blue ball point or dot pen. Ink pens or gel inks are not

allowed.

* Wear Lab coats During Lab classes.

* Everybody should carry their observation manual with them in every lab class.

* Lab sessions will not be carried out for the students who are absent for a lab class with

out completing the session that they have missed.

* All Chemical Equations,Tabular column,Observations , calculations and Diagrams

should be done on left blank side of the record.

* The record books should be covered & name labelled prior to all.

* All the regular routine activities carried out during the lab cycles should be performed

daily on a regular basis in order to perform well in the final lab cycle.

2
CHEMISTRY
CLASS XII
PRACTICAL EXAM MODEL PAPER

CHEMISTRY PRACTICAL EXAMINATION : 043 MAX MARKS : 30


TIME : 3 HRS

1. Prepare........... Solution of FAS. Using this find the strength and Molarity of KMnO4 solution.
8 Marks
2. Analyse the given salt for the presence of a acid and basic radicals present in it.
a. Report the acid and basic radicals to the examiner.
b. Record the observation and result. 8 Marks

3. Analyse the given Biomolecule present in it.


Report with the systematic procedure. 6 Marks

4. Project Work 4 Mark

5. Record and Viva. 4 Mark

3
Paste os starch

Glass
rod
Beaker

Wire gauze

Tripod stand

Burner

Preparation of Starch Sol

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4
01

SURFACE CHEMISTRY
AIM: To prepare colloidal solution (sol) of starch.

THEORY

Starch forms a lyophilic sol when water is used as the dispersion


medium. The formation of sol is accelerated by heating. The starch sol
can be prepared by heating starch and water at about 100 C. It is quite
stable and is not affected by the presence of any electrolytic impurity.

APPARATUS

Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle


and mortar, tripod stand, wire-gauze and burner.

MATERIALS REQUIRED
Soluble starch (500 mg) and distilled water.

PROCEDURE

1.Take 500 mg of starch in a mortar and add few ml of distilled water.

2.Grind the starch to make a thin paste and transfer this paste to a 50 ml beaker.
3.Take about 100 ml of distilled water in a 250 ml beaker and heat the
beaker so that water starts boiling.
4.Pour the paste slowly with stirring into boiling water in the beaker (Fig. 2.1).
5.Continue boiling for about 10 minutes and then allow the beaker to cool.

6.Filter the contents of the beaker through a filter-paper, fixed in a


funnel. Label the filtrate ‘Starch Sol’.

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5
6
PRECAUTIONS
1. The apparatus used for preparing sol should be properly cleaned.
2. Distilled water should be used for preparing sols in water.
3. Starch should be converted into a fine paste before adding to
boiling water.
4. Starch paste should be added in a thin stream to boiling water.
5. Constant stirring of the contents is necessary during the
preparation of the sol.

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03
8
02

SURFACE CHEMISTRY

AIM: To prepare colloidal solution (or sol) of egg albumin.

THEORY
Egg albumin which is obtained from eggs forms lyophilic sol with
cold water. The sol is quite stable and is not affected by the presence of
traces of impurities.

APPARATUS

Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle

and mortar, tripod stand, wire-gauze and burner.

MATERIALS REQUIRED

An egg and distilled water.

PROCEDURE

1.Break the outer shell of the egg by striking it with a glass rod and
collect its colourless liquid along with yellow yolk. Decant the co-
lourless liquid into another beaker. This colourless liquid is known
as egg albumin.

2.Prepare 100 ml of 5% (w/v) solution of sodium chloride in a


250 ml beaker. To this solution add egg albumin in small portions

with constant stirring. This process should take 15-20 minutes.


3.Filter the contents of the beaker through a filter paper, fixed in a

funnel, and collect the filtrate.Label this filtrate as ‘egg-albumin


sol’.

9
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10
PRECAUTIONS
1.The apparatus used for preparing the sol should be absolutely clean.
2. Distilled water should be used for preparing the sol.

3. Egg albumin sol is prepared at room temperature because


hot solution the precipitation of egg albumin takes place.

4. The yellow yolk should be separated completely from the egg


albumin before using the latter in the experiment.
5. Addition of egg albumin should be done very slowly and with

constant stirring so as to disperse the colloidal particles well in


solution.

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03
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03

SURFACE CHEMISTRY

AIM: To prepare ferric hydroxide, [ Fe ( OH )3 ] sol.

THEORY
Ferric hydroxide forms a lyophobic sol.The substance such
as metal hydroxides or sulphides which are insoluble and do not
readily give colloidal solutions on treatment with water are called
lyophobic colloids.

Ferric hydroxide sol is prepared by the hydrolysis of ferric chlo-


ride with boiling distilled water. The reaction that takes place
can be represented as
Boil
FeCl 3 ( aq ) + 3H 2 O ( l ) 
→ Fe ( OH )3 ( s ) + 3HCl ( aq )

Ferric chloride Red sol

The hydrolysis reaction produces insoluble ferric hydroxide


particles which undergo agglomerisation to yield bigger particles
of colloidal dimensions. These particles adsorb Fe 3+ ions preferen-
tially from the solution to give positive charge to the sol particles.
Stability of the sol is due to the charge on the sol particles. Hydro-
chloric acid which is produced during hydrolysis destabilizes the
sol and hence it must be removed from the sol by dialysis process
otherwise sol will not be stable.

APPARATUS
Conical flask (250 ml), beaker (250 ml), a boiling-tube,
glass-rod, funnel, round-bottom flask, iron stand with a clamp,
wire-gauze, tripod-stand, burner and a burette or a dropper.

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14
MATERIALS REQUIRED
2% solution of ferric chloride (prepared by dissolving 2 g of pure
FeCl 3 in 100ml distilled water) and distilled water.

PROCEDURE

1. Take a 250 ml conical flask and clean it by steaming-out process


as shown in Fig.2.2.
2. To this cleaned flask, add 100 ml of distilled water and heat it to

boil by placing the flask on a wire-gauze.


3. Add ferric chloride solution dropwise (by the use of a burette or a

dropper) to the boiling water.


4. Continue heating until deep red to brown solution of ferric
hydroxide is obtained. Replace the water lost by evaporation
during boiling at regular intervals.

5. Keep the contents of conical flask undisturbed for sometime


at room temperature. Label the solution as “ferric hydroxide sol”.

PRECAUTIONS
1. Since ferric hydroxide sol is affected by impurities, the apparatus
required for the preparation of sol should be thoroughly cleaned
by steaming-out process.

2. Add ferric chloride solution dropwise.


3. Heating is continued till the desired sol is obtained.
4. Hydrochloric acid formed as a result of hydrolysis of ferric

chloride is removed by dialysis process otherwise it would desta-


bilise the sol.

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04

SURFACE CHEMISTRY

AIM: To prepare colloidal solution of arsenious sulphide, [ As 2 S 3 ].

THEORY
Arsenious sulphide, As 2 S 3 is a lyophobic colloid. It is obtained by
the hydrolysis of arsenious oxide ( As2 O 3 ) with boiling distilled water,
followed by passing H2 S gas through the solution obtained.
Boil
→ 2As ( OH )3
As 2 O 3 + 3H 2 O 

2As ( OH )3 + 3H 2 S → As 2 S 3 + 6H 2 O

(Light yellow sol)

In the colloidal solution of arsenious sulphide, each particle is


surrounded by HS − ions, produced by the dissociation of H2 S . This sul-
phide ion layer is further surrounded by the counter ion layer of H+
ions.

APPARATUS

Conical flasks (250 ml), beaker (250 ml), round-bottom flask


(500 ml), glass-rod, funnel, glass tubing, filter-paper, tripod stand,
wire-gauze, iron stand with clamp, burner, etc.

MATERIALS REQUIRED

Solid arsenious oxide, H2 S gas and distilled water.

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PROCEDURE
1. Clean a conical flask (250 ml) by the use of steaming-out process.
2. To this cleaned flask, add 0.2g of As2 O 3 solid and add 100 ml of
distilled water.
3. Boil the solution for about 10 minutes (Fig. 2.3).
4. Filter the above hot solution through flutted filter paper and
receive the filtrate in another beaker (Fig. 2.4.).
5. Pass a slow current of H2 S into As2 O 3 solution as shown in Fig. 2.5.
The solution develops a yellow colour due to formation of As 2 S 3 .
Continue passing H2 S till the intensity of colour does not change
further.

6. Expel excess of H2 S gas from the sol by boiling the sol till the
escaping gas does not turn lead acetate paper black.
7. Filter the solution through flutted-filter paper and collect the
bright yellow filtrate in a dry conical flask and cork it.
Label it as “Arsenious Sulphide Sol”.

PRECAUTIONS
1. Use cleaned apparatus since As 2 S 3 sol is affected by even traces of

impurities.
2. Handle arsenious oxide with care since it is highly poisonous.
Wash your hands immediately everytime after handling
this chemical. While doing this experiment do not eat or drink
anything.

19
OBSERVATIONS

Flask 0.1 M KI 2.5 M Water Starch 0.5 M sodi- 3% hydrogen Time for ap-
solution H 2 SO 4 solution um thiosul- peroxide solu- parence of
(ml) (ml) (ml) phate solu- tion (ml) blue colour
(ml) tion (ml)
A
B
C
D

Time required for the blue colour to first appear in:


Flask A- Sec
Flask B- Sec
Flask C- Sec
Flask D- Sec

03
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05

CHEMICAL KINETICS
AIM: To study the reaction rate of reaction of iodide ions with
hydrogen peroxide at different concentrations of iodide ions.

THEORY
Hydrogen peroxide oxidizes iodide ions to iodine in acidic
medium
H 2 O 2 + 2I − + 2H + → 2H 2 O + I 2

The reaction is monitored by adding a known volume of


sodium thiosulphate solution and starch solution to the
reaction mixture. Iodine liberated at once reacts with sodium
thiosulphate solution and is reduced to iodide ions.
Fast
I 2 + 2S 2 O 3 2 − 
→ S 4 O 6 2 − + 2I −

When thiosulphate ions are completely consumed, the


liberated iodine reacts with starch solution and gives blue colour
I 2 + Starch → Blue complex

The time elapsed before the appearance of blue colour, gives


an idea about the rate of the reaction.

APPARATUS AND CHEMICALS


4 Conical flasks (250 ml), measuring cylinder, burette,
pipette (5 ml), stop-watch, 0.1 M KI solution, 2.5 M H2 SO 4 , starch
solution, ‘3%’ H2 O 2 solution, 0.05 M sodium thiosulphate solution.

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PROCEDURE
1. Take four 250 ml conical flasks and label them as A, B, C
and D.
2. Add 10 ml, 20 ml, 40 ml and 60 ml of 0.1 M KI solution to

the flasks A, B, C and D respectively.


3. Add 10 ml of 2.5 M H2 SO 4 to each flask.

4. Add water to make the volume of solution 100 ml in each


flask.
5. Add 5 ml starch solution to each flask.

6. Add 10 ml of 0.05 M sodium thiosulphate solution to each

flask with the help of a burette.


7. Add 5 ml of 3% hydrogen peroxide solution to flask A with

the help of a pipette and start the stop watch immediately.


Stir the mixture and watch for the blue colour to appear.
Note the time when the blue colour just appears.
8. Repeat the step 7 with the solutions in flasks B, C and D.

9. Record the observations in tabular form.

Time required for the blue colour to first appear in:


Flask A- Sec
Flask B- Sec
Flask C- Sec
Flask D- Sec

CONCLUSION
The rate of the reaction increases with increase in
concentration of iodide ions.

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PRECAUTIONS
1. Always use a freshly prepared solution of sodium

thiosulphate.
2. Concentration of KI solution should be higher than the
concentration of sodium thiosulphate solution.
3. Use freshly prepared starch solution.

4. Do not suck hydrogen peroxide solution with mouth but


use a pipette.

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06

THERMOCHEMISTRY

AIM:Determine the enthalpy of neutralisation of hydrochloric acid


with sodium hydroxide solution.

THEORY
Heat is evolved during neutralisation of an acid with an
alkali. Known volumes of the standard solutions of an acid and
alkali are mixed and the change in temperature is observed and

from this, the enthalpy of neutralisation is calculated. Enthalpy


of neutralisation is the heat evolved when one gram equivalent
of the acid is completely neutralised by a base in dilute solution.

REQUIREMENTS
(a) Apparatus. a wide-mouthed polythene bottle (to serve as
calorimeter), a rubber cork having two holes, thermometer
(1/10th degree), stirrer fitted with a cork on the handle, and a
100 ml measuring cylinder.
(b)Chemicals. 1.0 M hydrochloric acid and 1.0 M sodium
hydroxide solution.

PROCEDURE
A. Determination of Calorimeter Constant
1. Put 100 ml of distilled water in polythene bottle with a
thermometer and stirrer.
2. Note the temperature ( t 1C ).

3. Heat some water in a beaker to a temperature 20 − 30 C higher than


that of room temperature.

27
OBSERVATIONS
Initial temperature of the acid and base = t 1C 34OC

Final temperature after neutralisation = t 2C 39.3OC



Change in temperature, = ( t 2 − t 1 ) C 5.3OC
Mass of the mixture solution after neutralisation = 200 g*

Calorimeter constant of calorimeter = W J / C 54.34j/ OC

CALCULATIONS

Heat produced during neutralisation of 100 ml of 1.0 M HCl

= ( 200 + W ) × ( t 2 − t 1 ) × 4.184 Joules

∴ Heat produced during neutralisation of 1000 ml of 1 M HCl

1000
= ( 200 + W ) × ( t 2 − t 1 ) × 4.184 × Joules
100

( 200 + W ) × ( t 2 − t 1 ) × 4.184
(200 + 54.34)x5.3x4.184
= kJ =
100 100
Since heat is produced during neutralisation, the enthalpy of
neutralisation is negative.

( 200 + W ) × ( t 2 − t 1 ) × 4.184 =56.4kj/mole


Enthalpy Of neutralisation = − kJ
100

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28
4. Put 100 ml of this warm water in another beaker.
5. Note the temperature of this water. Let it be t 2C .
6. Add warm water from the beaker into the polythene bottle with
out any loss of time.
7. Stir the contents.
8. Read the temperature attained after mixing. Let it be t 3C .
B. Determination of Enthalpy of Neutralisation
1. Clean and dry the polythene bottle.
2. Place 100 ml of 1.0 M hydrochloric acid solution in it.
3. Record the temperature of the acid solution.
4. Similarly, note the initial temperature of the sodium hydroxide
solution taken in a separate vessel.
5. Both the solutions should have the same temperature, otherwise
wait for some time so that they attain the same temperature.
6. Transfer 100 ml of sodium hydroxide solution into the acid
solution quickly.
7. Immediately fit the cork having the thermometer and the
stirrer in the mouth of the polythene bottle (Fig. 4.1) and stir well.
8. Note the temperature after small intervals till it becomes
constant.
9. Record the highest temperature (to 0.1 ) reached.

RESULT
The enthalpy of neutralisation of HCl with NaOH is -56.4kJ/mole.

Percentage error =.......

29
OBSERVATIONS

Conc. of EMF of the cell


Concentration of CuSO 4 solution
ZnSO 4 solution

03
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07

ELECTROCHEMISTRY
AIM:To study the variation of cell potential in Zn | Zn 2 + || Cu 2 + | Cu cell
with change in concentration of electrolytes ( CuSO 4 and ZnSO 4 )
at room temperature.

THEORY
Reduction potential of an electrode increases with increase in
concentration of the electrolyte.
M n + ( aq ) + ne − → M ( s )

In the zinc-copper electrochemical cell zinc electrode acts as



anode while copper electrode acts as cathode.
=E cell E cathode − Eanode
E cell increases if E cathode increases and Eanode decreases. Thus, using

higher conc. of Cu 2 + and lower conc. of Zn 2 + ions increase the E cell of Zn |



Zn 2 + || ( t 2 − t|1 )WCJ./ C

The relation between conc. of the electrolyte and the standard


electrode potential is given in the form of Nernst equation :


HCl

APPARATUS AND CHEMICALS


One beaker, a porous pot, connecting wires, milli voltmeter, sand
paper, zinc strip,copper strip, 1M ZnSO 4 solution and 1M CuSO 4

solution.

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PROCEDURE
1. Take copper sulphate solution in a clean beaker.
2. Clean the copper strip with the help of sand paper and dip it
into copper sulphate solution.
3. Take zinc sulphate solution in a porous pot.
4. Clean the zinc strip with the help of sand paper and dip it
into zinc sulphate solution.
5. Keep the porous pot in the beaker.
6. Connect the copper strip with the positive terminal and zinc strip
with the negative terminal of a voltmeter as shown in Fig. 5.3.
7. Note the position of the pointer in the voltmeter and record the
reading in your note-book.
Repeat the experiment by taking different concentrations of zinc
sulphate and copper sulphate solutions.

CONCLUSION
EMF of the cell increases with decrease in conc. of the electrolyte
around anode and increase in conc. of the electrolyte around cath-
ode.

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03
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08

PREPERATION OF IN ORGANIC COMPOUNDS


AIM: To prepare a pure sample of ferrous ammonium sulphate
(Mohr’s salt) [ FeSO 4 . ( NH 4 )2 SO 4 .6H2 O ].

THEORY
Mohr’s salt is prepared by dissolving an equimolar mixture of
hydrated ferrous sulphate and ammonium sulphate in water
containing a little of sulphuric acid, and then subjecting the
resulting solution to crystallisation when light green crystals of
ferrous ammonium sulphate. FeSO 4 . ( NH 4 )2 SO 4 .6H2 O separate out.
FeSO 4 .7H 2 O + ( NH 4 )2 SO 4 → FeSO 4 . ( NH 4 )2 SO 4 .6H2 O + H2 O

Ferrous sulphate Ammonium sulphate Mohr’s salt


278 132 392

REQUIREMENTS

Two beaker (250 ml), china-dish, funnel, funnel stand, glass


rod, wash-bottle, tripod stand and wire-gauze.
Ferrous sulphate crystals, ammonium sulphate crystals, dilute
sulphuric acid and ethyl alcohol.

PROCEDURE

1. Take a 250 ml beaker and wash it with water. Transfer 7.0 g


ferrous sulphate and 3.5g ammonium sulphate crystals to it.

Add about 2-3 ml of dilute sulphuric acid to prevent the


hydrolysis of ferrous sulphate.

2. In another beaker boil about 20 ml of water for about 5 minutes


to expel dissolved air.

35
OBSERVATIONS

Weight of crystals obtained = 6.8 g

Expected yield =8g

Colour of the crystals = Light Green.

Shape of the crystals = Monoclinic Shape

Note: The crystals of Mohr’s salt are monoclinic in shape.

03
36
3. Add the boiling hot water to the contents in the first beaker in small
instalments at a time. Stir with a glass rod until the salts have
completely dissolved.
4. Filter the solution to remove undissolved impurities and

transfer the filtrate to a china-dish.


5. Heat the solution in the china-dish for some time to concentrate
it to the crystallisation point.
6. Place the china-dish containing saturated solution over a beaker

full of cold water. On cooling crystals of Mohr’s salts separate out.


7. Decant off the mother liquor quickly. Wash the crystals in the
china-dish with a small quantity of alcohol to remove any
sulphuric acid sticking to the crystals.
8. Dry the crystals by placing them between filter paper pads.

Result : Colour of the crystals = Light Green.


Shape of the crystals = Monoclinic Shape

PRECAUTIONS

1. Cool the solution slowly to get good crystals.


2. Do not disturb the solution while it is being cooled.
3. Do not heat the solution for a long time as it may oxidize
ferrous ions to ferric ions.

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03
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09

PREPERATION OF ORGANIC COMPOUNDS

AIM:To prepare acetanilide from aniline.

THEORYl
Acetanilide is prepared by acetylating aniline with acetic anhy-
dride in the presence of glacial acetic acid. The chemical equation
can be written as:

O O O
  
NH 2 + CH 3 − C − O − C − CH 3 → NH − C − CH 3 + CH 3 COOH
Acetic anhydride
Aniline Acetanilide

APPARATUS
Round bottom flask (100 ml), water condenser, wire-gauze, glass
rod, tripod stand, burner, iron-stand, clamp, measuring cylinder, etc.

CHEMICALS REQUIRED
Aniline = 5 ml
Acetic anhydride = 5 ml
Glacial acetic acid = 5 ml

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PROCEDURE

1. Take 5 ml of acetic anhydride in a clean dry 100 ml conical flask


and add 5 ml of glacial acetic acid and shake the contents
thoroughly.

2. To this mixture taken in the flask, add 5 ml of aniline and fit a


water condenser.
3. Place the flask on a wire-gauze placed on a tripod stand as

shown in Fig. 8.1.


4. Boil the mixture for 10-15 minutes.
5. Allow the mixture to cool. Detach the condenser and pour the
liquid into about 150 ml ice-cold water contained in a beaker.
During addition, stir vigorously the contents of the beaker with
the help of glass rod.

6. Filter the white precipitates which separate out and wash with
cold water.
7. Recrystallise from hot water containing a few drops of ethyl
alcohol. Weigh the crystals and record the yield.
8. Determine the melting point of the compound.

RESULT
Weight of acetanilide obtained = 9 g
Melting point of acetanilide = 113  C

Note : Acetanilide has white flaky crystals. Its melting point in


113 C .

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PRECAUTIONS

1. Freshly distilled aniline should be used in order to get good

results or small amount of zinc can be added in the reaction


mixture. Zinc reduces the coloured impurities in the aniline
and also prevents its oxidation during the reaction.
2. Prolonged heating and use of excess of acetic anhydride should
be avoided.
3. Reactions mixture should first be cooled and then poured in ice-

cold water otherwise hydrolysis of acetanilide may take place.

43
Observations

Weight of watch glass = _______________ g


Weight of watch glass + Mohr’s salt = _______________ g
Weight of Mohr’s salt = 1.96g.
Volume of Mohr’s salt solution prepared = 100ml.
Molarity of Mohr’s salt solution = 0.05 M
Volume of Mohr’s salt solution taken for each titration = 10 ml

VOLUME OF KMnO4 SOLUTION VOLUME OF


VOLUME OF FAS (ml)
SL.NO KMnO4 SOLUTION
SOLUTION (ml)
INITIAL FINAL (ml)

1 --- --- --- -ml


2 --- --- --- -ml
3 --- --- --- -ml
4 --- --- --- -ml
5 --- --- --- -ml

Concordant volume = x ml (Say)

03
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10

VOLUMETRIC ANALYSIS

AIM: Prepare 0.05 M solution of ferrous ammonium sulphate (Mohr’s


salt). Using the solution find out the molarity and strength of the

given KMnO4 solution.

Chemical Equations Molecular equations

2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]


2FeSO4(NH4)2SO4.6H2O + H2SO4 + [O] → Fe2(SO4)3 + 2(NH4)2SO4+ 13H2O] x 5
2 KMnO4 + 8H2SO4 + 10FeSO4(NH4)2.SO4.6H2O → K2SO4+ 2MnSO4 +

5Fe2(SO4)3 + 10(NH4)2SO4+ 68H2O

Ionic Equations
MnO −4 + 8H + + 5e − → Mn 2+ + 4H 2O

Fe 2+ → Fe3+ + e − ] × 5

MnO −4 + 8H + + 5Fe 2+ → 5Fe3+ + Mn 2+ + 4H 2O

Indicator

KMnO4 is a self-indicator.

End Point

Colourless to permanent pink colour (KMnO4 in burette)

45
Calculations

(a) Molarity of the KMnO4 solution.


From the overall balanced chemical equation, it is clear that 2 moles
of KMnO4 react with 2 / 10 moles of Mohr’s salt.

M KMnO4 × VKMnO4 2
∴ =
M Mohr 's salt × VMohr 's salt 10

Where

M KMnO4 = Molarity of KMnO4 solution


VKMnO4 = Volume of KMnO4 solution
MMohr’s salt = Molarity of Mohr’s salt solution
VMohr’s salt = Volume of Mohr’s salt solution

MKMnO4 xX 2
=
0.05x10 10
2 1 2 =..........M
M KMnO4 = × =
10 x 10x

(b) Strength of the KMnO4 solution


Strength (in g/L) = Molarity x Molar mass
2
= × 158g / l
10x
Instructions for the Preparation of Solutions
Provide the following

1. Crystals of Mohr’s salt

2.M/100 KMnO4 solution (1.58 g/litre)


3. 4N or 2M H2SO4

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46
PROCEDURE :
1. Prepare 100ml of 0.05 M Mohr’s salt solution by dissolving 1.96g

of Mohr’s salt in water.Rinse the pipette with the 0.05M Mohr’s salt
solution and pipette out 10.0 ml of it in a washed titration flask.

2. Rinse and fill the burette with the given KMnO4 solution.

3. Add one test tube (~ 10ml) full of dilute sulphuric acid (~ 2 M) to


the solution in titration flask.

4. Note the initial reading of the burette.

5. Now add KMnO4 solution from the burette till a permanent light
pink colour is imparted to the solution in the titration flask on

addition of last single drop of KMnO4 solution.

6. Note the final reading of the burette

7. Repeat the above steps 4-5 times to get a set of three Concordant

readings.

RESULT :

Molarity of KMnO4 = _________________ M

Strength of the KMnO4 = _________________ g/L

47
Observations

Weight of Watch glass = ______________ g


Weight of (watch glass + oxalic acid) = ______________ g
Weight of oxalic acid = 0.315 g
Volume of solution prepared = 100 ml
Molarity of oxalic acid solution = M/40
Volume of oxalic acid solution taken for each titration = 10.0 ml

VOLUME OK KMnO4 SOLUTION


VOLUME OF
(ml) VOLUME OF KMnO4
SL.NO OXALIC ACID
SOLUTION (ml)
SOLUTION (ml) INITIAL FINAL

1 --- --- --- -ml

2 --- --- --- -ml

3 --- --- --- -ml

4 --- --- --- -ml

5 --- --- --- -ml

Concordant volume = x ml (say)

03
48
11

VOLUMETRIC ANALYSIS

M
AIM: Prepare solution of oxalic acid. With its help, determine the
40
molarity and strength of the given solution of potassium permanganate
(KMnO4).

2KMnO 4 + 3H 2SO 4 → K 2SO 4 + 2MnSO 4 + 342 O + 5[0]

Chemical Equations

2KNnO4 + 3H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5[O]

COOH
60 + 700C
.2H2O + [O] 2CO2 + 3HO] x 5

COOH
COOH

2KMnO4 + 2H2SO4 + 5 .2H2O + [O] k2SO4 + 2MnSO4 + 18H2O + 10CO2

COOH
Ionic equations
MnO-4 + 8H+ + 5e- Mn2+ + 4H2O] x 2

C2O42-­ + 2CO2 + 2e- ] x 5

2MnO- + 16H+ + 5C2O42- 2MN2+ + 8H2O + 10CO2

Indicator

KMnO4 is a self-indicator

End Point

Colourless to permanent pale pink colour (KMnO4 in burette)

49
Calculations
(a) Calculation of molarity of the KMnO4 solution
From the overall balanced chemical equation it is clear that 2 moles

of KMnO4 react with 5 moles of oxalic acid.


M KMnO4 × VKMnO4 2
∴ =
M oxalic acid × Voxalic acid 5

Where

M KMnO4 = Molarity of KMnO4 solution

VKMnO4 = Volume of KMnO4 solution

Moxalic acid
= Molarity of oxalic acid solution

Voxalic acid = Volume of oxalic acid solution

MKMnO4 xX 2
=
1/ 40x10 5

1 =........M
M KMnO4 =
5x

(b) Calculation of strength of the KMnO4 solution


Strength (in g/l) = Molarity x Molar mass
1
= × 158 g/L
5x

Instructions for the Preparation of Solutions


Provide the following
1. Oxalic acid crystals
2. KMnO4 solution (1.58 g/litre)
3. 2M H2SO4

03
50
PROCEDURE
1. Weigh 0.315g of oxalic acid crystals and dissolve then in water
M
to prepare 100 ml of oxalic acid solution using a 100 ml
40
M
measuring flask. Rinse the pipette with the oxalic acid solution
40
and pipette out 10 ml of it in a washed titration flask.

2. Rise and fill the burette with the given KMnO4 solution

3. Add one test tube (~ 10 ml) full of dilute sulphuric acid (~ 2 M)

to the solute in titration flask.


4. Note the initial reading of the burette
5. Heat the flask 60-70°C and add KMnO4 solution from the burette

till a permanent light pink colour is imparted to the solution

in the titration flask on addition of a last single drop of KMnO4


solution.

6. Note the final reading of the burette

7. Repeat the above steps 4-5 times to get three Concordant readings.

RESULT :
Molarity of KMnO4 = _________________ M

Strength of the KMnO4 = _________________ g/L

51
Exp No : 12

QUALITATIVE ANALYSIS OF INORGANIC SALT (1)


EXPERIMENT OBSERVATION INFERENCE

Colour Colourless / white Fe+2, Fe+3, Mn+2, Fe+2, Cu+2,


Co+2,
May be absent

Physical state Crystalline solid NH4+,Cl-,Br-,NO3- may be absent

Solubility Soluble NH4+,Cl-,Br-, may be present.


Dry Heating test
Take dry test tube put the salt
and heat

(i) Gas evolved Reddish Brown gas evolved Presence of Br-.


(ii) Sublimate formed White sublimate on test-tube Presence of NH +
4
walls

EXPERIMENT OBSERVATION INFERENCE

Flame test

Make a paste with No characteristic colour Ca+2,Ba+2,Pb+2,Sr+2, may be


salt + Conc. Hcl and heat with observation absent
blue flame and observe the
colour change

Acid Radicals Test


EXPERIMENT OBSERVATION INFERENCE

Salt + Dil Hcl No Brisk Effervesce CO 3−2 absent

Salt + Conc. H2SO4 Reddish brown vapours Br- ,maybe present


With pungent smell

03
52
Confirmatory test for Br -.
EXPERIMENT OBSERVATION INFERENCE

Silver Nitrate test :

Salt + dilHNO3.Boil for some Pale yellow ppt is formed Presence of Br- is Confirmed.
time and add silver nitrate which is sparingly soluble in
NH4OH.

kBr + AgNo3 → kNO3 + AgBr ↓ ↓


Ppale Yelloow ppt
w ppt
Identification of Basic Radical
The O.S is prepared in H2O
EXPERIMENT OBSERVATION INFERENCE

Salt + NaOH boil Pungent smelling ammonia gas Group O is present NH +


4
evolved

Analysis of Group O
EXPERIMENT OBSERVATION INFERENCE

Salt + Dil NaOH Pungent smelling NH4 gas NH +


4 is present
Boil evolved which gives dense-
white fumes with glass rod
dipped Conc Hcl

NESSLER’S TEST
SALT+NaOH+ Nesslers Reddish brown PPt is formed NH +
4 is confirmed
Reagent

2K2[HgI4]+NH3+3KOH 
→ H2N.HgO.HgI4 ↓ +7KI+2H2O
Brown ppt
Result
Acid Radicals : Br-.
Basic Radicals : NH +
4
Salt : NH4Br.

04
53
Exp No : 13

QUALITATIVE ANALYSIS OF INORGANIC SALT(2)


Preliminary Test
EXPERIMENT OBSERVATION INFERENCE

Colour Colourless / white Fe+2, Fe+3, Mn+2, Fe+2, Cu+2,


Co+2,
May be absent

Physical state Crystalline solid NH +


4 ,Cl ,Br ,NO may be
- - 3

absent

Solubility Soluble NH +
4 . Cl ,Br , may be present.
- -

Dry Heating test :


Take dry test tube put the salt

and heat
(i) Gas evolved Reddish brown gas which turns Presence of NO 3−
ferrous sulphate solution black
(ii) Sublimate Formed Brown when hot,yellow when Presence of Pb2+
cold

EXPERIMENT OBSERVATION INFERENCE

Flame test

Salt + Conc Hcl No characteristic colour Ca+2,Ba+2,Sr+2, may be


Paste and heat with blue observation absent

flame it.

Acid Radicals Test


EXPERIMENT OBSERVATION INFERENCE

Salt + Dil Hcl No Brisk Effervesce CO 3−2 absent

Salt + Conc H2SO4 No characteristic observation Cl-,Br- ,may be absent


If no reaction add a piece of Reddish brown vapours are NO 3− may be present
Cupper and heat evolved

54
Confirmatory test for NO-3.
EXPERIMENT OBSERVATION INFERENCE

Brown ring test : A brown ring is formed at the NO 3− is present.


salt + equal volume of fresh- junction of two Layers.
ly prepared FeSO4 Solution
+ add drop by drop Conc
H2SO4, along the side of testubes

KNO3+H2SO4 → KHSO4+HNO3
6FeSO4+3H2So4+ HNO3 → 3Fe2(SO4)3+4H2O+2NO
FeSO4+NO+5H2O → [Fe(NO)(H2O)5]SO4.
Brown Ring
Basic Radicals
The O.S is prepared in H2O
EXPERIMENT OBSERVATION INFERENCE

Salt + NaOH Boil No Characteristic observation Group o is absent

O.S+ 1 or 2 ml of Dil Hcl No White ppt is formed Group 1 is absent (Pb+2)

O.S+2 ml of Dil Hcl +H2S gas Black ppt Group 2 is present,may be Pb+2
Confirmation For Pb+2.
EXPERIMENT OBSERVATION INFERENCE

Dissolve black ppt in Hot

Ammonium acetate solution

and divide it into 2 parts

Part 1: KI test Yellow PPt is boiling H2O


crystallization on cooling Pb+2confirmed

Part 2: K2CrO4 test Yellow ppt soluble in NaOH Pb+2 confirmed


Pb(NO3)2+2KI → 2KNO3+PbI2 ↓
(yellow ppt)
Pb(NO3)2+K2CrO4 → 2KNO3+PbCrO4 ↓
(yellow ppt)
Result −
Acid Radicals - NO3
Basic Radicals - Pb+2
Salt – Pb(NO3)2.

55
Exp No : 14

QUALITATIVE ANALYSIS OF INORGANIC SALT(3)

EXPERIMENT OBSERVATION INFERENCE

Colour white Fe+2, Fe+3, Cu+2,


May be absent
Physical state Amorphous CO3-2 may be present
In soluble in water CO3-2 may be present
Solubility

Dry Heating test


Take dry test tube put the salt
and heat

(i) Gas evolved colourless and odourless gas CO3-2 may be present
(ii)Residue White residue, glows on Ca+2, Mg+2,Ba+2,Sr+2 may be
heating present

Flame test
EXPERIMENT OBSERVATION INFERENCE

Salt + Conc Hcl Apple Green Ba+2, may be present


Paste and burn it

Acid Radicals Test


EXPERIMENT OBSERVATION INFERENCE

Salt + Dil Hcl Brisk Effervesce CO32- is Present

Confirmatory test for CO3-2.

EXPERIMENT OBSERVATION INFERENCE

Salt + dil Hcl pass the gas Lime water turns milky CO32- is confirmed
through Lime water
Salt + MgSO4 Solution White ppt CO 3−2 is is confirmed.

56
Lime water test :
CaCO3+2Hcl → CaCl2+CO2+H2O
Ca(OH)2+CO2 → CaCO3 ↓ H2O
(Milkiness)

Basic Radicals
Prepare of O.S Salt+H2O → insoluble → not O.S
O.S Salt+Hcl → soluble → O.S
EXPERIMENT OBSERVATION INFERENCE

Salt + NaOH Boil No Characteristic Group o is absent


O.S+ 1 on 2 ml of Dil Hcl No Characteristic Group I is absent

Pass H2S to the above No Characteristic Group II is absent


O.S+NH4Cl + NH4 OH No Characteristic Group III is absent
Pass H2S to the above No Characteristic Group IV is absent

OS + NH4Cl+NH4OH+(NH4)2
CO3 Sol White ppt Group V is Present

Conformation of Group V
EXPERIMENT OBSERVATION INFERENCE
Dissolve the ppt in the Hot Dil.

Acatic acid divide into 3 parts


Part 1 + K2Cr2O4 Yellow ppt Ba+2 is confirm

Part 2 + Ammonium Sulphate No White ppt Sr2+ is Absent


Part 3 + Ammonium oxololate No White ppt Ca2+ absent
BaCO3+2CH3COOH → (CH3COO)2Ba+CO2 ↓ +H2O
(CH3OO)2Ba+K2CrO4 → 2(CH3COO)K+BaCrO4 ↓
Yellow ppt
Flame test
Take a small amount of salt on Ba+2 is Confirmed
watch glass and make a part
with Hcl that the mixture Apple green
Result :
Acid Radicals : CO3−2
Basic Radicals : Ba2+.
Salt : BaCO3.

57
Exp No : 15

QUALITATIVE ANALYSIS OF INORGANIC SALT(4)

EXPERIMENT OBSERVATION INFERENCE

Colour white Fe+2, Fe+3, Cu+2,CO+2,


May be absent

Physical state Crystalline Solid NH + −


4 ,Cl ,Br NO 3 may be
- -

absent
Solubility Soluble
NH + −
4 ,Cl ,Br NO may be
+ -

present

Smell No Characteristic smell NH +


4 ,CH3,COO may be
-

Take a pinch of the salt be- absent


tween the finger and rub it
with a drop of water

Flame test
EXPERIMENT OBSERVATION INFERENCE

Take a small amount of salt Crimson red colour Presence of Sr+2.


in a watch glass and make a
paste with Conc Hcl.Heat the
Mixture strongly in the flame

Dry Heating test


EXPERIMENT OBSERVATION INFERENCE

Heat a pinch of the salt Pungent Heating smell


(i) Gas evolved Greenish yellow gass which Presence of Cl-.
turns starch iodide paper blue
(ii) Residue White residue glows Heating Presence of Ba+2,Sr+2,Ca+2.Mg+2

58
Detection of Acid Radical
Analysis of group I acid Radicals
EXPERIMENT OBSERVATION INFERENCE
Salt + Dil Hcl No Brisk Effervesce CO32- is absent

Analysis of group II acid Radicals


EXPERIMENT OBSERVATION INFERENCE

Salt in dry test tube + Conc A colourless pungent smelling Cl − may be present
H2SO4 gas which forms with glass rod
dipped in NH4OH is dipped to
the mouth of the test tube

Confirmatory test for Cl-.


EXPERIMENT OBSERVATION INFERENCE
Chromyl Chloride Test

Salt + K2Cr2O7(s)+CONC Orange red vapour


H2SO4 warm
Pass vapour through NaOH Solution turns yellow

solution taken in the test tube


To the above yellow sol add Yellow ppt is obtained Cl − is confirmed

Acetic Acid and Lead acitate


Solution

Silver nitrate test

Salt + dil HNO3 heat and cool White ppt is formed Presence of Cl- is confirmed
acid AgNO3 solution
→ Agcl ↓ +NaNO3
NaCl+AgNO3 
(White ppt)

Agcl+2NH4OH 
→ [Ag(NH4)2]Cl+2H2O
Soluble complex

59
Detection of Basic Radicals
O.S is Prepared in H2O
EXPERIMENT OBSERVATION INFERENCE

Salt+NaOH boil No characteristic smell Group o is absent


O.S + dil Hcl No Characteristic observation Group I is absent
Pass H2S No Characteristic observation Group II is absent

O.S + NH4Cl + NH4OH is


excess No Characteristic observation Group III is absent
Pass H2S gas
No Characteristic observation Group IV is absent

O.S + NH4Cl + NH4OH+


(NH4)2CO3 solution White ppt is present Group V is present

EXPERIMENT OBSERVATION INFERENCE

Flame test
Take a small amount of salt on Crimson red colour Sr+2 confirmed.
watch glass and make a paste
with Conc Hcl heat the mixture
strength in the flame
Dissolve the ppt in the Hot Dil.
Acatic acid divide into 3 parts
Part 1+K2CrO4 No yellow ppt Ba2+ absent

Part 2+(NH4)2 SO4 White ppt Sr2+ Confirmed


Part 3 +Ammonium Oxolate No White ppt Ca2+ absent

SrCO 3+2CH 3COOH → (CH 3COO) 2S r +CO 2 ↑ +H 2O


(CH3COO)2Sr+(NH4)2SO4 → 2CH3COONH4+SrSO4 ↓
(White ppt)
Result :

Acid Radicals : Cl-.


Basic radicals – Sr+2.
The given salt is Srcl2.

60
16

QUALITATIVE ANALYSIS OF INORGANIC SALT(5)


Preliminary tests
EXPERIMENT OBSERVATION INFERENCE
Fe+2, Fe+3, May be absent
Colour Colourless / white

Physical state Crystalline Solid NH +


4 ,Cl , may be absent
-

Solubility Soluble
NH +
4 ,Cl ,Br may be present
- -

Smell
Take a pinch of the salt No Characteristic smell NH +
4 ,CH3COO S may be
- -2

between the finger and rub it absent


with a drop of water

Flame test
EXPERIMENT OBSERVATION INFERENCE

Take a small amount of salt on No Characteristic colour Ca+2,Sr+2,Ba+2,pb+2,may be


watch glass and make a paste absent.

with Conc Hcl.Heat the Mix-


ture strongly in the flame

Dry Heating test

EXPERIMENT OBSERVATION INFERENCE

Heat a pinch of the salt


(i) Gas Evolved Colourlesss gas with smells like SO42-, may be present.
burning sulpher
(ii) residue White recidue glows on heating Ca+2,Sr+2,Ba+2,Mg+2 me be
present

Detection of Acid Radical


Analysis of group I acid Radical
EXPERIMENT OBSERVATION INFERENCE
Salt + Dil Hcl No Brisk Effervesce
CO 3−2 is absent

61
Analysis of group II acid Radicals

EXPERIMENT OBSERVATION INFERENCE


Salt + Conc H2SO4 No Characterstic Observation Absence of Cl-,Br-
Add Copper and Heat No Reddish Brown Vapours NO3- is absent

Analysis of group III acid Radicals


Confirmatory test
EXPERIMENT OBSERVATION INFERENCE

Salt solution + Lead Acetate White ppt SO4-2 is confirmed.

Na2SO4+Pb(CH3COO)2 → PbSO4 ↓ +2CH3COONa


White ppt
Detection of Basic Radical
O.S is prepared in H2O
EXPERIMENT OBSERVATION INFERENCE

Salt + NaOH boil No Characteristic smell Group 0 absent

O.S + Dil.Hcl No Characteristic Observation Group I absent

Pass H2S to Above No Characteristic Observation Group II absent

O.S+NH4Cl(6)+NH4OH is
excess No Characteristic Observation Group III absent

Pass H2S No Characteristic Observation GroupI V absent


O.S +NH4Cl (5)+NH4OH+

(NH4)2CO3 No Characteristic Observation Group V absent


O.S+NH4Cl(s)+NH4OH+
(NH4)2HPO4 White ppt Group VI present
Analysis of group VI
EXPERIMENT OBSERVATION INFERENCE

O.S+NH4Cl(s)+NH4OH+ (2HPO4)H4 White ppt Mg+2 is confirmed


MgCl2+NH4OH+(NH ) HPO →Mg(NH )PO ↓ +2NH Cl+H O
4 2 4 4 4 4 2
(White ppt)
Result :
Acid Radicals : SO4-2.
Basic radicals : Mg+2.
The given salt is : MgSO4.

62
17

QUALITATIVE ANALYSIS OF INORGANIC SALT(6)


Preliminary tests
EXPERIMENT OBSERVATION INFERENCE
Colour Colourless / white Fe+2, Fe+3, Cu+2, May be absent
Physical state Amorphous solid
CO 32 − , may be present
Solubility Not Soluble in water
CO 32 − , may be present

Smell
Take a pinch of the salt be-
tween the finger and rub it
No Characteristic smell CH3COO- ,NH +
4,
S-2 may be
with a drop of water absent
Flame test
EXPERIMENT OBSERVATION INFERENCE

Take a small amount of salt on No Coloured Flame


Ba+2,Ca+2,Sr+2,Mg+2,may be
watch glass and make a paste absent.
with Conc Hcl.Heat the Mix-
ture strongly in the flame
Dry Heating test
EXPERIMENT OBSERVATION INFERENCE

(i) gas evolved Colourlessd and Oderless Gas CO3-2, may be Present.
(ii) Residue Yellow when Hot /White when cold Zn+ may be Present.

Detection of Acid Radical


Analysis of group I acid Radical
EXPERIMENT OBSERVATION INFERENCE
Salt + Dil Hcl Brisk Effervesce
CO 3−2 is present
Confirmatory test for CO 3−2
EXPERIMENT OBSERVATION INFERENCE
Salt+Dil.Hcl Liberated Gas Lime Water turns Milkey
Pass throw Lime water CO 3−2 is confirmed
Lime water test :
CaCO3+2Hcl → CaCl2+CO2+H2O
Ca(OH)2+CO2 → CaCO3 ↓ H2O
(Milkiness)
63
Detection of Basic Radical
Preperation of OS
Salt + water → In Soluble Not O.S

Salt + Dil Hcl → Soluble O.S


O.S is prepared in Hcl
EXPERIMENT OBSERVATION INFERENCE
Salt + NaOH boil
No Characteristic smell Group 0 absent
O.S + Hcl
No Characteristic Observation Group I absent
Pass H2S to Above No Characteristic Observation Group II absent

O.S+NH4Cl(s)+NH4OH is
excess No Characteristic Observation Group III absent
Pass H2S goes to above White ppt Group IV present

Analysis of group V
Conformation of Zn+2.
EXPERIMENT OBSERVATION INFERENCE

Dissolve the white ppt in Hcl


boil off H2S and divide it into
2 parts

Part1 + Dil NaOH droppers White ppt Zn+2 is confirmed


and excess White ppt Dissolves

Part 2+potassiumferrocyanide White or Blue white ppt Zn+2 is confirmed

1) ZnS+2Hcl → ZnCl +H S ↑
2 2
ZnCl2+2NaOH → Zn(OH)2 ↓ +2NaCl
(white ppt)
Zn(OH)2+2NaOH → Na2ZnO2+2H2O
Soluble
2) 2ZnCl2+K4[Fe(CN)6] → Zn2[Fe(CN)6] ↓ +4KCl
White or Bluish white ppt
Result :
Basic radicals : Zn+2.
Acid Radicals: CO-23.
The given salt is ZnCO3.

64
18

QUALITATIVE ANALYSIS OF INORGANIC SALT(7)


Preliminary tests
EXPERIMENT OBSERVATION INFERENCE

Colour Colourless / white Fe+2, Fe+3, May be absent


Physical state Crystalline Solid NH4+,Cl-,Br-,may be present

Solubility Soluble NH4+,Cl-,Br-,may be present


Smell
Take a pinch of the salt be- No Characteristic smell CH3COO- ,NH +
4,
S-2 may be
tween the finger and rub it absent
with a drop of water

Flame test
EXPERIMENT OBSERVATION INFERENCE

Take a small amount of salt a Brick red colour Ca+2 present.


watch glass and make a paste
with Conc Hcl.Heat the Mix-
ture strongly in the flame

Dry Heating test


EXPERIMENT OBSERVATION INFERENCE
(i) gas evolved Pungent smell Cl , may be present.
-

(ii) Residue White residue, Glows on Ba2+,Sr2+,Ca2+,Mg2+may be


heating present.

Detection of Acid Radical


Analysis of group I acid Radical

EXPERIMENT OBSERVATION INFERENCE


Salt + Dil Hcl No Brisk Effervesce
CO 3−2 is absent

Analysis of group II acid Radical


EXPERIMENT OBSERVATION INFERENCE
Salt + Conc H2SO4 Pungent smelling gas and
produce dent white fumes Cl − is present
formed when a rod dipped
in NaOH is brought near the
mouth of the test tube.

65
Confirmatory test for Cl −
EXPERIMENT OBSERVATION INFERENCE
Chromyl Chloride Test Red vapours
Salt+K2Cr2O7 + conH2SO4
warm

Pass the vapours through Solution turns yellow Cl- is confirmed


solution

To the above yellow solution


add acetic and lead acitate Yellow ppt is obtained

AgNO3 test
Salt + dil HNO3 boil and cool
add AgNO3 solution White ppt is formed Presence of Cl- is confirmed

Nacl+AgNO3 → Agcl ↓ +NaNO3


White ppt

Agcl+2NH4OH → [Ag(NH3)2]Cl+2H2O
Soluble Complex

Detection of Basic Radical


O.S is prepared in H2O
EXPERIMENT OBSERVATION INFERENCE

Salt + NaOH boil No Characteristic smell Group 0 absent


O.S + dil Hcl No Characteristic observations Group I absent
Pass H2S No Characteristic observations Group II absent

O.S+NH4Cl(s)+NH4OH is
excess No Characteristic observations Group III absent

Pass H2S gas to above White ppt Group IV present


O.S+NH4Cl(s)+NH4OH White ppt is present Group V is present
+(NH4)2CO3Solution

66
Analysis of group V
EXPERIMENT OBSERVATION INFERENCE

Dissolve the white ppt in Hcl


boil off H2S and divide it into
3 Parts
Part1 +K2CrO4 No ppt Ba+2 is absent
Part2 + Ammonium Sulphate No ppt Sr+2 is absent

Part 3+ ammonium Oxalate White ppt Ca2+ is confirmed


solution + NH4OH and Stretch
the sides of the test tube
CaCO3+2CH3COOH → (CH3COO)2Ca+CO2 ↑ +H2O

(CH3COO)2Ca+(NH4)2C2O4 → 2CH3COONH4+CaC2O4 ↓
White ppt

Flame test
EXPERIMENT OBSERVATION INFERENCE

Take a small amount of salt Brick red colour Ca+2 is confirmed


in watch glass and make a
paste with Conc Hcl heat the
mixture strongly

Result :
Acid Radicals: Cl-
Basic radicals : Ca+2
The given salt is CaCl2.

67
Exp No : 19

QUALITATIVE ANALYSIS OF INORGANIC SALT(8)


Preliminary tests
EXPERIMENT OBSERVATION INFERENCE
Colour Colourless / white Fe+2, Fe+3, May be absent
Physical state Crystalline Solids NH4+,Cl-,Br- may be absent
Solubility Soluble NH4+1 , Cl-,Br- may be present

Smell Vinegar like smell CH3COO- may be Present


Take a pinch of the salt
between the finger and rub it
with a drop of water

Dry Heating test


EXPERIMENT OBSERVATION INFERENCE

(i) gas evolved characteristic Vinegar like smell- CH3COO- may be Present.
(ii) Residue Brown when hot and Yellow Pb2+ may be Present.

when Cold

Detection of Acid Radical


Analysis of group I acid Radical
EXPERIMENT OBSERVATION INFERENCE
Salt + Dil Hcl No Effervesce
CO 3−2 is absent

Analysis of group II acid Radical


EXPERIMENT OBSERVATION INFERENCE
Salt + Conc H2SO4 Vinegar like smell
CH3COO − is present

68
Confirmatory test for CH3COO-
EXPERIMENT OBSERVATION INFERENCE
Test 1:Oxalic Acid Test

Salt + Solid Oxalic Acid Mix Smell like that of Vinegar CH3COO- is confirmed
and make a paste with a few
drops of water Rub the paste
and smell
Test 2: Ester test

Salt+Conc H2SO4 and heat Pleasant Fruity smell of Ester CH3COO- is confirmed

and cool.Add ethyl alchohal


shake and pour the contents in
a beaker full of water, stir

1. Oxacilic Acid Test

2. Ester Test
2CH3COONa+H2SO4 → Na SO + 2CH COOH
2 4 3

CH3COOH+C2H5OH → CH3COOC2H5+H2O
Ethyl Acetate
(Fruity Smell)

69
Detection of Basic Radical
O.S is prepared in H2O
EXPERIMENT OBSERVATION INFERENCE
Salt + NaOH boil No Characteristic smell Group 0 absent

O.S + dil HCl White ppt Group I Present

Analysis of group I
EXPERIMENT OBSERVATION INFERENCE

Boil white ppt with 5 - 10


ml of water on divide into 3
parts

Part1 + Cool with tap water White Crystalline ppt

Part2 + KI Yellow ppt Pb+2 isconfirmed


Part 3 + K2CrO4 Yellow ppt Pb+2 isconfirmed

PbCl2+2KI → PbI2 ↓ +2KCl


(yellow ppt)

Pbcl2+K2CrO4 → PbCrO4 ↓ +2KCl


Yellow ppt

Result :
Acid Radicals: CH3COO--
Basic radicals : Pb+2
The given salt is Pb(CH3COO)2.

70
20

QUALITATIVE ANALYSIS OF INORGANIC SALT(9)


Preliminary tests
EXPERIMENT OBSERVATION INFERENCE
Colour Pale Pink Colour Mn+2,May be present

Physical state Crystalline Solids CO3-2,is absent


Solubility Soluble in water NH4+,Cl-,Br-,may be present

Smell
Take a pinch of the salt be- No Characterstic smell NH4+,CH3COO-,S-2 may be
tween the finger and rub it
with a drop of water absent
Flame test
EXPERIMENT OBSERVATION INFERENCE

Take a small amount of salt


solution a watch glass and
make a paste with Conc Hcl. No characteristic colour Ca+2,Ba+2, Sr+2-may be absent
Heat the Mixture strongly in
the flame observation

Dry Heating test


Heat the salt
EXPERIMENT OBSERVATION INFERENCE

(i) gas evolved Colourless Gas with smells like SO4-2, may be present
Burning Sulpher
(ii) Residue Coloured salt becomes brown Mn may be present
2+

or black on Heating

Detection of Acid Radical


Analysis of group I acid Radical
EXPERIMENT OBSERVATION INFERENCE
Salt + Dil Hcl No Effervesce
CO 3−2 is absent

71
Analysis of group II acid Radical
EXPERIMENT OBSERVATION INFERENCE
Salt + Conc H2SO4 No Characterstic Observation Absence of Cl-,Br-
Add Copper and Heat No Reddish Brown Vapours NO3- is absent

Analysis of Group III Acid

Confirmatory test
EXPERIMENT OBSERVATION INFERENCE

Salt solution + Pb(CH3COO)2 White ppt SO4-2 is confirmed.

Na2SO4+Pb(CH3COO)2 → PbSO4 ↓ +2CH3COONa


White ppt

Detection of Basic Radical


O.S is prepared in H2O

EXPERIMENT OBSERVATION INFERENCE


Salt + NaOH boil
No Characteristic smell Group 0 absent
O.S + dil Hcl
No Characteristic Observation Group I absent
O.S + pass H2S
No Characteristic Observation Group II absent

O.S + NH4Cl(s)+NH4OH is
excess
No Characteristic Observation Group III absent
Pass H2S
Buff ppt,(Flesh) Coloured ppt Group IV present

Analysis of group IV.


EXPERIMENT OBSERVATION INFERENCE

Dissolve the buff colour ppt in


dil.Hcl boil off H2S.
1. Sodium Hydroxide test

To the above solution add White ppt Formed Mn+2 is confirmed


NaOH Solution Shake.
Add Bromine Water to the It turns Black or Brown ppt Mn+2 is confirmed
White ppt.

72
EXPERIMENT OBSERVATION INFERENCE

2. Lead Peroxide test


Pink colour solution is formed Mn+2 is confirmed
To the black ppt obtained
in the above test add Conc
HNO3 and Lead peroxide boil
and cool and allow to settle

1.NaOH and Br2 water test


MnS+2Hcl → MnCl +H S ↑
2 2

MnCl2+2NaOH → Mn(OH)2 ↓ +2NaCl


(Whiteppt)

Br2+H2O → 2HBr+[O]

Mn(OH)2+[O] → MnO(OH)2 ↓
Brown ppt

2. PbO2 Test
MnS+2HNO3 → Mn(NO ) +H S
3 2 2

2Mn(NO3)2+5PbO2+6HNO3 → 2HMnO4+5Pb(NOP3)2+2H2O
Pink Solution

Result :
Acid Radicals: SO4-2
Basic radicals : Mn+2
The given salt is MnSO4

73
Exp No : 21

QUALITATIVE ANALYSIS OF IN ORGANIC SALT -10

Experiment Observations Inference

Colour White Fe2+, Co2+,Cu2+,Mn2+,absent

Physical state Crystalline NH4+,Cl-,Br4-,No3-,Al3+,Br3+ absent

Solubility Soluble NH4+,Cl-,Br4-,No3-,Present

Smell , wet a pinch of salt and rubb No Smell NH4+,CH3COO-,S2- absent


Flame test :

Heat paste of Salt + .Conc Hcl in Flame No Colour Ca2+,Sr2+,Ba2+,Zn2+,Mn2+,Pb2+,Absent

Dry heating test :

Heat salt in a dry test tube No gas CO32-,Cl-,Br-,CH3OO-,NH4+,NO-3,absent

Residue : White , glows on heating Ca2+,Sn2+,Ba2+,Mg2+,Al3+,Present

Detection of Acid Radical


Group I II III

Group reagent Dil.Hcl Conc.H2SO4 No reagent

CO2-3present / Cl-, Br-,NO3-,Present /

Radical present absent absent SO42- present

Identification of Acid Radical Group I


salt + dil . Hcl; No Reaction CO32- absent

Identification of Group II Acid Radical


Salt + Conc. H2SO4 + Copper

Piece No Reaction Cl-,Br-,NO3-,CH3COO-, absent

Identification of Group III Acid Radical


Salt + BaCl2 White ppt SO2-4 present

Confirmation of Acid Radicals


Salt +lead acetate + Acetic acid White ppt SO2-4, Confirmed

74
Na2So4+Bacl2→BaSo4+2Nacl
White ppt

Al(OH)3 + 3Hcl → Alcl3+3H2O


AlCl3+3NH4OH → 3NH4cl + Al(OH)3+ ↓
(Blue colour adsorbs
On this ppt)
Detection of Basic Radicals
Preparation of OS
Add a spatula of salt to solvent
Water Soluble O.S

Identification of Basic Radicals


Salt + NaOH,boil No Smell Group 0 absent

Salt + dil.Hcl No ppt Group I absent

Pass H2S gas pass through


Solution No ppt Group II absent

O.S +NH4Cl + NH4OH Excess White ppt Group III (Al3+) present

Conformation of Basic Radical

Lake test:

Dissolve ppt in dil.Hcl, add 2 Blue ppt Floating in Colourless Al3+ confirmed
drops of blue litmus, NaOH drop solution

wise

Result :
Anion : SO42-

Cation : Al3+
The given salt is Al2(SO4)3.

75
Experiment Samples

A B C D

Taste Sweet Sweet Sweet Sweet

Solubility Soluble Soluble Soluble In Soluble

Purple ring Purple ring Purple ring Purple ring


Molisch’s test
(Carbohydrate) (Carbohydrate) (Carbohydrate) (Carbohydrate)

Red ppt (Reducing Red ppt (Reducing no Red ppt (non no Red ppt (non
Fehling’s test
sugar) sugar) Reducing sugar) Reducing sugar)

Red ppt (Reducing Red ppt (Reducing no Red ppt (non no Red ppt (non
Benedict’s test
sugar) sugar) Reducing sugar) Reducing sugar)

No Blue Colouration No Blue Colouration No Blue Colouration Blue-black Coloura-


Iodine test
(Starch absent) (Starch absent) (Starch absent) tion (Starch present)

76
22

BIOMOLECULAR ANALYSIS
Qualitative Test For Carbohydrate:
Experiment Observation Inference

Taste Sweet / sweetless Sugar / non sugar

Solubility in water Solubility / insoluble Sugar / non sugar


Moliseh’s test – 1 mole of Sam-
ple + 2 – 3 drops of molisesh’s Purple ring at junction of 2
Carbohydrate present
layers
reagent add Conc.H2SO4 on sides
of test tube.
Fehling’s test :

1ml of sample + 1ml of Fehling’s Red ppt Reducing sugar

solution A and B ,heat

Benedict test :
1,l sample +
Red ppt Reducing sugar
1ml of reagent keep in water
bath

iodine test : 1 ml of sample 1


Blue – black colouration Stretch Present
drop of iodine solution

Result : The Given Food Stuff Contains :


Sample A - Contains reducing Sugar
Sample B – Contains Reducing sugar
Sample C – Contains non - Reducing sugar
Sample D – Contains Starch

77
Experiment Samples

E F

Biuret test Blue colour (portion present) Blue colour (Portion present)

Blue colournation (Protien Blue Colournation


Ninhydrin test
present) (Protien present)

Xanthoprotic test White ppt (Protien present) White ppt (Portion present)

78
23

QUALITATIVE TEST FOR PROTEIN


Test Observation Inference
Biuret test 1ml of sugar sample 1ml of Burette
Blue Colour Protein Present
reagent

Purple , blue Colouration intersi-


Protein present
Nihydrin test – 1ml of sample + ml regent ty , increases with heat

Xanthroprotien test 1ml of sample . 1ml of Conc


Wheat white ppt / yello ppt Protein present
HNO3 ,heat

Result :
The given food stuffs contain
Sample E : contains Proteins
Sample F : contains Proteins

79
Experiment Samples
G H

Solubility with water Insoluble (fat present) Insoluble (fat present)

Sample forms lower layers , dis-


Alcohol Fat present
solves on heating

CCl4 Miscible (fat present) Fat present

Transient spot test Fat present Fat present

Pungent smell
Acrolein test Pungent smell (fat present)
(fat present)

80
24

Qualitative Test for fats


Test Observation Inference

Solubility :

1ml / a pinch of sample + water Immiscible Fat present

1ml / a pinch of sample + alco- Sample forms lower layer that Fat present
hol dissolves on heating miscible

1ml / a pinch of sample + CCl4 Miscible Fat present

Translucent spot test : A pinch

of the sample is placed b/w the Translucent spot Fat present

Folds of Filter paper

Acrolien test : sample + KHSO4


Pungent smell Fat present
,heat

Result :
The given food stuffs contain
Sample G : contains Fat
Sample H : contains Fat

81
82
25

FUNCTIONAL GROUP ANALYSIS -1


Experiment Observation Inference

Physical State Liquid


Smell Pleasant smell ketonic group may be present

Solubility :
Aldehyde, Alchohol, Carboxylic,
Compound + water soluble ketonic groups may be present
Experiment Observation Inference

Test For Saturation : Colour does not disappear Compound is Saturated


(a) Dissolve the compound in

CCl4 ,add Br2 with continuous

shaking

b) Dissolve compound in water Pink Colour not discharged Compound is Saturated


or acetone and add alkaline
KMnO4

Tests for Functional Groups

Test for Carboxylic Group


NaHCO3 test : No Brisk Effervescence Carboxylic Group not present

Take 1ml of organic compound

and add a pinch of NaHCO3

Test for Alcohol Group


Ceric Ammonium nitrate test : No Red Colour Appears Alcholic Group absent

Add a few drops of Ceric

ammonium nitrate to 1 ml of

organic compounds in a dry test

tube

83
Chemical Equations:
-
CH3 COCH3 + OH-  → CH3COCH2 + H2O
-
CH3 COCH2- + [Fe(CN)5 NO]2-  → Fe(CN)5 NO.CH3 COCH2]3-
Nitroprusside ion Red Colouration

84
Test for Phenol Group

Neutral Fecl3 test : No Violet coloration Phenolic Group absent

Add 2 to 3 ml of compound to

Fecl3 in a test tube

Test for Carbonyl Group


2,4 - DNP test: Yellowish – orange Carbonyl group

Add a drop of 2,4 - DNP to the Precipitate Is present

compound

Test for -CHO Group


Schiff’s reagent test :

Add a drop of Schiff’s reagent to No -CHO group (Aldehyde)

compound in a dry test tube Appearance of magenta colour absent

Test for -CO Group


m -dinitrobenzene test :

Add about 0.1gm m - dinitro-

benzene , to the organic -CO group prescent.


compound then dilute .NaOH Violet color is obtained

Confirmatory test for -CO group


Sodium NitroPrusside test :

A small amount of organic com-

pound to sodium NitroPrusside

in Distilled water. Shake and add Red Colour is Obtained -CO group is Confirmed

NaOH dropwise (Ketone)

Result: :
The organic compound contains Ketonic group

85
Exp No : 26

FUNCTIONAL GROUP ANALYSIS -2


Experiment Observation Inference

Physical State Liquid

Smell Pungent smell Aldehydic group may be present

Solubility :
Aldehyde, Alchohol, Carboxylic,
Compound + water soluble ketonic groups may be present
Experiment Observation Inference

Test For Saturation : (a) Bro- Colour does not disappearing Compound is Saturated
mine water test : Add Bromine

water drop wise to compound

dissolved in CCl4.

(b) Alkaline KMnO4 test : Add

a drop of KMnO4 to Compound

dissolved in water .

b) Dissolve compound in water Pink colour not discharged Compound is Saturated

on acetone and add KMnO4

Test for the functional group


Test for the Carboxylic group
NaHCO3 test : No Briskeffervesence -COOH absent

Add a pinch of NaHO3 to com-

pound in a test tube

Test for Alcohol Group


Cerci Ammonium nitrate test : No Red Coloration -OH absent

Add a few drops of Cerric am-

monium nitrate to of organic


compounds in a dry test tube

86
Test for Phenolic Group
Neutral Fecl3 test : No Violet coloration Phenolic Group absent

Add 2 to 3 ml of compound to

Fecl3 in a test tube

Test for Carbonyl Group

2,4 DNP add a drop of 2,4 DNP orange - red Carbonyl group

to the compared Precipitate Is present

Test for – CHO Group


Schiff’s reagent test : Magenta colouration observed -CHO group (Aldehyde)
Add a drop of shift reagent to Is present

compound in a dry test tube

Confirmatory test for -CHO group


shining silver mirror formed -CHO group is confirmed
Tollen’s test:
organic compound + tollens

reagent heat in water bath and

then cool

Chemical Equations:
2 Ag ( NH 3 ) 2+ + RCHO + 3OH − → RCOO − + 2 Ag ↓ +4 NH 3 + 2 H 2O

Silver Mirror

Result :
The given organic compound contain Aldehydic group

87
Exp No : 27

FUNCTIONAL GROUP ANALYSIS -3


EXPERIMENT OBSERVATION INFERENCE

Physical state Solid


Smell Phenolic smell Phenol might be present
Solubility
Aldehyde, Alchohol, Carboxylic,
Compound + water Insoluble ketonic groups may be absent

Compound + Conc. Hcl Soluble Amine, phenolic group may be present


Experiment Observation Inference

Test For Saturation : Colour not Discharged Compound is Saturated

(a) Bromine water test : Add

Bromine Drop wise to compound

dissolved in CCl4.
(b) Alkaline KMnO4 test:
Compound is Saturated
Dissolve compound in water or Pink colour not discharged
acetone and add alkaline KMnO4

Test for the functional group


Test for the Carboxylic group
NaHCO3 test : No Briskeffervesence -COOH absent

Add a pinch of NaHCO 3 to

compound in a test tube

Test for Alcohol Group

Ceric Ammonium nitrate test : No Red Colour Appears -OH group absent
Add a few drops of ceric

ammonium nitrate to 1 ml of

organic compounds in a dry test

tube

88
Test for Phenolic Group

Neutral Fecl3 test : add a drop of Violet Colouration Phenolic Group present
component TO NEUTRAL Fecl3 in

a test tube.

Confirmatory test for Phenolic Group

Lieberamnns’s Test: Add Phenol Deep blue colour obtained Presence of phenolic group
to a Test tube with 2 – 3 crystals confirmed
of sodium nitrite heat , cool add
1 ml of Conc.H2So4 Shake well
and excess of NaOH
Chemical Equations:
FeCI3 + 6C6H5OH 
→[Fe(OC6H5 )]+ 3HCl
Ferric Phenol VioletComplex
Chloride

Chemical Equations:

Result :

The given organic compound contain Phenolic group.

89
Exp No : 28

FUNCTIONAL GROUP ANALYSIS - 4


Experiment Observation Inference
Physical State Liquid

Smell fruity smell Alcholic group may be present


Aldehyde, Alchohol, Carboxylic,
Solubility
ketonic groups may be present
Compound + Water Soluble

EXPERIMENT OBSERVATION INFERENCE

Test for saturation:

(a) Bromine water test: Add Colour not discharged Compound is saturated

bromine to compound dissolved

in CCl4.

(b) Alkaline KMnO4 test:


b) Dissolve compound in water
Pink colour not discharged Compound is saturated
or acetone and add alkaline
KMnO4

TESTS FOR FUNCTIONAL GROUPS


Test for Carboxylic Group

NaHCO3 test: Add a pinch of − COOH absent


No Brisk effervescence
NaHCO3 to compound in a test
tube

Test for Alcoholic Group

Ceric Ammonium Nitrate test: Red colour appears − OH group present

Add a drop of ceric Ammonium

Nitrate to compound in a dry test

tube

90
Confirmatory Test for Alcoholic Group

(ii) Ester test: Add glacial Fruity smell obtained Presence of − OH confirmed

acetic      acid and Conc. H2SO4


to     compound, warm in a
water     bath for 5 min, pour
into     water

Chemical Equation:

Result :
The given organic compound contain Alcoholic group

91
Exp No : 29

FUNCTIONAL GROUP ANALYSIS – 5


Experiment Observation Inference

Physical State Liquid


Fishy smell May be Amine
smell
Solubility :
Insoluble Aldehyde, Alchohol, Carboxylic,
Compound + water
ketonic groups may be absent
Compound + Conc.Hcl Soluble Amine group may be present

Experiment Observation Inference

Test For Saturation :

(a) Bromine water test : : Add Br NO Colour discharged compound is saturated


to Compound dissolved in CCl4.

b) Alkaline KMnO4 test:


Dissolve compound in water or NO Colour discharged
compound is saturated
acetone and add alkaline KMnO4

TTest for Carboxylic Group

NaHCO3 test: − COOH absent


No brisk effervescence
Add a pinch of NaHCO3 to com-

pound in a test tube

Test for Alcoholic Group

Ceric Ammonium Nitrate test: No Red colour appears − OH absent

Add a drop of ceric Ammonium

Nitrate to compound in a dry test

tube

92
Test For Carbonyl Group
no yellow ppt Carbonyl Group absent
2,4 - DNP test : add a few drops
to the organic compound

Test For –CHO Group

Shiff’s reagent add to organic com- no pink colour -CHO absent


pound in a dry test tube

Test for -CO GROUP


Sodium NitroPrusside test :
A small amount of organic compound to

sodium NitroPrusside in Distilled water. no red Colour is Obtained -CO group is absent

(Ketone)
Shake and add NaOH dropwise

Test For -NH2 group


Amino group Present
Carbylamine test:

Take 0.2gm of solid KOH in clean dry test


tube + 2ml of ethanol.Warm the test tube
untill the pallets dissolved to this add few
drops of chloroform small amount of the
given compound and warm gently. unpleasent odour

Confirmatory test: -
Azo dy test: Take 3 test tube ABC i test Red or Orange Dye -NH2 Group conformed
tube A, dissolve about 0.2 gm of compound
in a 2ml of dilute hcl.In test tube B prepare
an aqueous solution of soldium nitrite.In
test tube C dissolve 0.2gm of β naptol in Dil
sodium hydroxide.
Place all three test tube in Ice bath. Now add
sodium nitritate sol to test tube A. and the
result in the sol add to the Testtube C.

Chemical Equation :


Result :
The given organic compound contain Amino group

93
Exp No : 30

FUNCTIONAL GROUP ANALYSIS – 6


Experiment Observation Inference

Physical State Liquid

smell Vinegar like smell -COOH may be present

Solubility :

Compound + water soluble Aldehyde, Alchohol, Carboxylic,


ketonic groups may be present

Experiment Observation Inference

Test For Saturation : (a) Bromine Colour not Discharge Compounds is saturated

water test : Add Br- to Com-

pound dissolved in CCl4.

b) Alkaline KMnO4 test:


Dissolve compound in water or
acetone and add alkaline KMnO4

Test for Functional Group


Test for –COOH Brisk Effeerensence -COOH present
NaHCO3 test: Add NaHCO3 to

Compound.

Confirmatory test:
Easter Test : Add Ethyl Alcohol Fruity Smell -COOH Confirmed

and Conc .H2So4 to Compound

heat , put in beaker with water

94
Test for Alcoholic Group

Ceric Ammonium Nitrate tets: Not red colour -OH group absent

Add ceric ammonium nitrate to


compound in a dry test tube

Test for Phenolic Group

Neutral Fecl3 test : add a drop of No Violet Colouration Phenolic Group absent
component TO NEUTRAL Fecl3 in

a test tube.

Chemical Equations :
O
Conc
=

RCOOH + C2H5 OH  → R-C-O-C2H5+H2O


H 2SO 4
Ester
Result :
The given organic compound contains Carboxylic group

95
96

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