National Public School

Koramangala, Bangalore

Grade-11
Chemistry Practical Work Book

Name:
Class and section:
Roll number:

Sl.No. Date Experiment name Semester No of

1
 periods

1.
Date: Cutting a glass tube Experiment No.1 1

2. Bending a glass tube Cutting a glass tube 1

Aim:
3. Determination of melting point of an organic compound 1
To cut a glass tube of required length.
4. Preparation of standard solution of oxalic acid 1
Procedure:
5. 1. Select a glass tube
Volumetric analysis 1
free of cracks. 1

6. 2. Place it on the bench, hold it to

Introduction firmly
anionand make a single deep scratch with triangular
analysis 1 file. Do not
3 apply too
much pressure.
7. 3. Place the thumbs on each side
Introduction to of the scratch
cation analysisat equal distance from it. Apply1 gentle pressure
4 and give a
quick bending motion towards you until it breaks smoothly.
8. 4. The ends of theIntroduction
tube can be to salt analysis
further smoothened by rotating the ends in a flame1 for 2-3 minutes.
5 Edges
will be smoothened. Allow it to cool while holding in your hand.
9. Salt analysis 1 1 6
Precautions:
10. Salt analysis 2 1 7
1. Make a single deep scratch at the desired length with one stroke of the file.
2. To avoid injury hold the glass tube with theSemester-2
help of a thick piece of cloth.
3. Do not heat the end for long time. It may seal the end or make it narrower.
1. Salt analysis 3 2 1

2.
Date: Preparation of standard Experiment
solution of sodium
No.2 carbonate 2 2

3. Volumetric analysis 2 Bending a glass tube 2 3

4.
Aim: Organic analysis 1 2 4
To bend a glass tube.
5. Organic analysis 2 2 5
Procedure:
6. Crystallization 2 6
1. Hold the glass tube between the thumb and fingers; introduce it lengthwise in the luminous flame of
7. burner. Keep theSalt
tube rotating4 till it softens.
analysis 2 7
2. Now apply gentle pressure so that it bends by its own weight. When the desired angle is formed, remove
8. the tubing from Salt
the flame.
analysis 5 2 8
3. Place the bend limb on the asbestos sheet. Press it gently so as to make it coplanar. Allow the tubing to
9. cool. Salt analysis 6 2 9

10. Revision 2 10
Precautions:
1. Do not try to bend very small glass tubes. Index
2. While heating, the tube should be rotated in order to ensure uniform heating.
3. Do not apply too much force. Tube may break.

2
Date: Experiment No. 3
Determination of melting point of an Organic compound

Aim:
To determine the melting point of naphthalene.

Apparatus and chemicals:

100 ml beaker, thermometer, iron stand, clamp, tripod stand, stirrer, capillary tube, spatula and
naphthalene.

Theory:
Melting point of a substance is the temperature at which solid and liquid forms of a substance are in
equilibrium with each other at constant atmospheric pressure.

Procedure:
1. Powder the crystalline substance. Take a capillary tube and seal its one end by heating. For filling the
substance make a heap of the powdered substance and push the open end of the capillary tube into the
heap. Some substance will enter into it. Now tap the sealed end of the capillary tube gently. Fill the
capillary tube up to 2-3 mm.
2. Attach the capillary tube to a thermometer which is immersed in a bath of liquid paraffin. The surface
tension of the bath liquid is sufficient to hold the capillary tube in position.
3. Heat the beaker slowly and go on stirring the liquid in the beaker so that the temperature remains
uniform throughout. For this, a glass loop stirrer is moved up and down. When the temperature is within
15º of the melting point of the pure substance, the flame is lowered. Now the temperature is allowed to
rise slowly.
4. The temperature is noted when the substance starts melting. The temperature is noted again when it is
completely melted. The average of the two readings gives the correct melting point of the substance.

Observations:
Temperature at which the unknown substance begins to melt =
Temperature at which the unknown substance completely melts =
Hence, melting point of the unknown substance = (t1 +t2)/2 =

Result:
Melting point of naphthalene =

Precautions:
1. Use dry and powdered sample.
2. Keep the lower end of the capillary tube and the thermometer at the same level.
3. Heating should be gradual and the water bath should be stirred regularly to maintain uniform
temperature.

Date: Experiment No. 4

3
 Preparation of standard solution of oxalic acid

Aim:
To prepare 0.1N standard solution of oxalic acid.

Apparatus and chemicals:

Oxalic acid crystals, 100ml standard flask, funnel, spatula, wash bottle and balance.

Theory:
Oxalic acid (H2C2O4.2H2O) is a primary standard. A primary standard is a substance which is stable and
available in the purest form and whose standard solution can be made directly by weighing a known quantity.
Its concentration does not change even on long standing.
A solution whose concentration is known is called a standard solution. Concentration of a solution is
generally expressed in terms of molarity or normality. A standard solution can be prepared by weighing an
amount of the solid and dissolving it in a known amount of water.
Normality (N) is defined as the number of gram equivalents of solute per litre of solution.

mass x 1000
N=
Eq. Wt. x volume
Hence the amount of mass required for making 0.1N, 100 ml standard solution of oxalic acid will be;
w = 0.1 x 63 x 100 = 0.63g
1000
Equivalent mass of an acid (or base) is obtained by dividing the molecular mass by the number of available
hydrogen ions (hydroxyl ions) per molecule.

Procedure:
Weigh 0.63g of oxalic acid crystals and transfer that into a 100ml standard flask using a funnel. Wash
the funnel with small amount of water into the standard flask. Dissolve the oxalic acid crystals using small
amount of water at a time till there is no speck of oxalic acid crystals left. Now add water till the lower
meniscus of the solution touches the 100ml mark. Put a stopper on the flask and shake the contents to get a
homogeneous solution of oxalic acid.

Result:
Amount of oxalic acid crystals dissolved in 100ml = 0.63g
Strength of solution = 0.1N

Date: Experiment No.5

Volumetric analysis – 1

4
Aim:
To prepare standard oxalic acid solution and to determine the percentage purity of sodium hydroxide.
The given Sodium hydroxide solution contains 4 g of sodium hydroxide per litre of the solution.

Apparatus and chemicals required:

Burette, pipette, conical flask, funnel, Sodium hydroxide solution, oxalic acid crystals and
phenolphthalein.

Chemical Equation:

2NaOH + H2C2O4 → Na2C2O4 + 2H2O

Procedure:
Weigh 0.63 g of oxalic acid crystals and transfer the crystals into a 100ml standard flask using a funnel.
Add small amounts of water and try to dissolve the oxalic acid crystals completely. Wash the funnel also with
small amount of water into the standard flask. If there is no speck of oxalic acid left behind, add water till the
lower meniscus touches the 100 ml mark. Put a stopper on the flask and shake the contents to get a
homogeneous solution of oxalic acid.
Wash the burette with water and rinse it with Sodium hydroxide solution. Fill it up with the same and
note the initial reading. Rinse a clean pipette with standard Oxalic acid solution and pipette out exactly 10ml of
the same into a clean conical flask. Add a drop of phenolphthalein indicator to the conical flask. Titrate the
oxalic acid solution against the Sodium hydroxide solution taken in the burette till a pale permanent pink colour
appears. Note the final reading. Repeat the titrations for concordant values.

Inference:
The Normality of NaOH solution =
Weight per litre of NaOH solution = g/L
% purity of NaOH solution = %

Precautions:
1. Before taking any liquid in the burette or pipette, it should be rinsed with their respective solution.
2. The conical flask (titration flask) should not be rinsed with any solution as it may change the volume and
concentration of the solution. It should be simply washed only with water.
3. Read the lower meniscus for colourless liquids and upper meniscus for coloured liquids.

Observations:
Burette solution - Sodium hydroxide solution
Pipette solution - Standard oxalic acid solution
Indicator - Phenolphthalein
End point - Colourless to pale permanent pink colour

5
Equation:
2NaOH + H2C2O4 → Na 2C2O4 + 2H2O
Titration between Standard oxalic acid and Sodium hydroxide
Sl.No. Burette readings Volume of NaOH Volume of oxalic
solution (ml) acid solution(ml)
Initial Final

Concordant value = ml

Calculations:
Preparation of the standard oxalic acid solution:
Mass= Normality x Eq. wt. x Volume
1000
m = 0.1x 126/2 x 100 = 0.63g
1000
Normality and weight per litre of NaOH
Volume of oxalic solution (V1) = 10 ml
Normality of oxalic acid solution (N1) = 0.1 N
Volume of Sodium hydroxide solution (V2) = ml
Normality of Sodium hydroxide solution (N2) = ?
As, V1N1=V2N2
N2 = V1N1 / V2 =
The Normality of Sodium hydroxide solution =

Weight per litre of Sodium hydroxide solution = Eq.Weight x Normality

= g/L

% purity of Sodium hydroxide solution = Weight of pure NaOH x100

Weight of impure NaOH

= Weight of pure NaOHx100 =

4
Date: Experiment No.6 (,7&8)

Salt Analysis
Aim:
To analyze the given salt systematically and report one anion and one cation present in the salt.
Preliminary tests:
No. EXPERIMENT OBSERVATION INFERENCE
1. Note the colour of the salt a) Blue a) May be Cu2+
6
 b) Green b) May be Cu2+ or Ni2+
c) Pale pink c) May be Mn2+
d) Deep pink d) May be Co2+
e) Yellow or brown e) May be Fe3+
f) White or colourless f) Absence of Cu2+,Ni2+,
Fe3+, Mn2+ and Co2+
2. Note the odour of the salt a) Ammonical smell a)Presence of NH4+
b) Vinegar smell b)Presence of CH3COO-
c) Rotten egg smell c)Presence of hydrated S2-
3. Solubility test:
a) To a pinch of the salt taken in i) Soluble in water i)Absence of heavy metal
a test tube add 2 cc of water. carbonates
ii) Insoluble in water ii) Presence of heavy metal
carbonates

b) To a pinch of the given salt i) Soluble in dil.HCl i) Absence of Pb2+

add 2 cc of dil.HCl and shake
well. ii) Insoluble in dil.HCl ii) Presence of Pb2+
4. Flame test:
Take a spatula of salt in a a) Apple-green flame a) Presence of Ba2+
watch glass. Add a drop or b) Crimson red flame b) Presence of Sr2+
two of con.HCl to it and make c) Brick red flame c) Presence of Ca2+
a paste. Introduce this paste d) Blue green flame d) Presence of Cu2+
into the non-luminous flame e) No characteristic colour e) Absence of Ba2+,Sr2+,
using a glass rod. Ca2+, Cu2+
Acid radical analysis:
5. Dilute acid test: a) Brisk effervescence is noted. a) Presence of CO32- is
To the salt taken in a test tube A colourless odourless gas confirmed.
add dil.HCl and warm. turning lime water milky is
evolved.
MCO3 + 2HCl → MCl2 + H2O + CO2↑
CO2 + Ca(OH)2 → CaCO3↓ + H2O
(Milky white)
b) A colourless gas with the b) Presence of S2-
smell of rotten egg is evolved. It
turns lead acetate paper black.
MS +2HCl → MCl2 + 2H2S (Rotten egg smell)
(CH3COO)2Pb + H2S → 2CH3COOH + PbS↓ (Black)
c) Colourless gas, smell like that c) Presence of SO32-
of burning sulphur, which turns
acidified potassium dichromate
paper green is evolved.
MSO3 + HCl → MCl2 + SO2 + H2O
d) No characteristic reaction d) Absence of CO32-, S2-,
SO32- (Group I acid radicals)
6. Con. Acid test: a) A colourless gas with an a) Presence of Cl-
To a small amount of the salt irritating smell which gives
7
 taken in a test tube add con. dense white fumes when a glass
H2SO4 and heat slightly. rod dipped in NH4OH solution is
introduced.
MCl + H2SO4 → MHSO4 + HCl
NH4OH + HCl → NH4Cl + H2O
(Dense white fumes)
b) Reddish-brown gas which b) Presence of Br -
turns moist starch-iodide paper
blue is evolved.
2MBr2 + 3H2SO4 → 2MHSO4 + 2H2O + SO2 + Br2
(Reddish-brown)
c) Violet vapours which turn c) Presence of I -
moist starch paper blue-black are
evolved.
2MI + 3H2SO4 → 2MHSO4 + 2H2O + SO2 + I2 (Violet)
d) Colourless gas with a smell of d) Presence of CH3COO-
vinegar which turns moist blue
litmus paper red is evolved.
(CH3COO)2M + H2SO4 → MSO4 + 2CH3COOH
(Vinegar smell)
e) Slight brown fumes turning e) Presence of NO3-
FeSO4 solution black are
evolved.
M NO3 + H2SO4 → MHSO4 + HNO3
6FeSO4 + 2HNO3 + 3H2SO4 → 3Fe2(SO4)3 + 2NO + 4H2O
FeSO4 + NO → FeSO4.NO (Black)
f) Colourless gas which turns f) Presence of C2O42-
lime water milky is evolved.

C2O4M + H2SO4 → H2 C2O4 + MSO4

C2O4H2 + H2SO4 → CO2 +CO + H2O
g) No characteristic reaction g) Absence of Cl-, Br -, I-,
NO3-, CH3COO- , C2O42-
(Group II acid radicals)

Note: Sodium carbonate extract:

1. When to prepare:
a) If the salt is insoluble or partly soluble in water.
b) If the salt is coloured.
c) If the salt contains Pb2+
d) If the salt gives characteristic coloured flame in the flame test.
2. Why to prepare:
To convert the salt to a soluble, colourless sodium salt of the given anion.
3. How to prepare:
To 1 part of the salt add 3 parts of Na2CO3 and 1 test tube of water. Boil well for two minutes.
Cool and filter. The filtrate is called the sodium carbonate extract (S.E).
8
Confirmatory tests for acid radicals:

7. Tests for PO43-:

a) Ammonium molybdate Canary yellow precipitate is Confirms presence of PO43-
test: formed.
To the salt add con. HNO3 2M3PO4 + 3(NH4)2MoO4 → 2(NH4)3PO4 + 3M2MoO4
and heat. Then add excess M2MoO4 + 2HNO3 → 2MNO3 + H2MoO4(Molybdic acid)
of ammonium molybdate H2MoO4 → H2O + MoO3
solution. (NH4)3PO4 + 12MoO3 +6H2O → (NH4)3PO4.12MoO3.6H2O
(Ammonium phosphor molybdate-
canary yellow precipitate)
b) To the water extract (W.E A white precipitate is formed. Confirms presence of PO43-
– salt dissolved in water)
or (S.E – acidified with M2HPO4 + MgCl2 + NH4OH → MgNH4PO4↓ + 2MCl+ H2O
dil.HCl), boil off CO2 and (white)
then add magnesia mixture
(Magnesia mixture
preparation - add NH4Cl to
Mg2+ solution, add NH4OH
till a strong smell of NH3 is
got)
Tests for SO42-:
8. To the W.E or (S.E A white precipitate insoluble in Confirms presence of SO42-
a) acidified with dil.HCl) add con.HCl is obtained.
BaCl2 solution.
MSO4 + BaCl2 → MCl2 + BaSO4 (white)

To the W.E or (S.E White precipitate soluble in Confirms presence of SO42-

b) acidified with dil. excess of (CH3COO)NH4 is
CH3COOH), add formed.
(CH3COO)2Pb MSO4 + (CH3COO)2Pb → (CH3COO)2M + PbSO4 (white)
PbSO4 + 2(CH3COO)NH4 → (NH4)2SO4 + (CH3COO)2Pb

9. Tests for S2-:

a) To the W.E or S.E Black precipitate is formed. Presence of S2- is confirmed.
acidified with acetic acid,
(CH3COO)2Pb + MS → (CH3COO)2M + PbS↓ (Black)
add (CH3COO)2Pb
solution.
b)
Sodium nitroprusside test: Purple colour is obtained. Presence of S2- is confirmed.
To a portion of the S.E or
(W.E to which some Na2S + Na2[Fe(CN)5NO] → Na4[Fe(CN)5NOS] (Violet)
NaOH has been added) add
2 drops of sodium
nitroprusside solution.
10 Tests for SO32- :
9
a) To the W.E (or S.E A white precipitate is obtained. Presence of SO32- is confirmed.
acidified with dil. Acetic
acid) add a few drops of MSO3 + BaCl2 → BaSO3 + 2NaCl
BaCl2 solution

b) To the W.E (or S.E) add A green colouration is Presence of SO32- is confirmed.
K2Cr2O7 solution and dil. obtained.
H2SO4 MSO3 + H2SO4 → MSO4 + H2O + SO2
K2Cr2O7 + 4H2SO4 → K2SO4 + Cr2(SO4)3 + 4H2O + 3[O]
SO2 + H2O + [O] → H2SO4
11. Tests for Cl- :
a) Chromyl chloride test: Red vapours are evolved. Presence of Cl- is confirmed.
To a pinch of the solid salt
taken in a test tube add
potassium dichromate
followed by con. H2SO4 Yellow solution is got.
and heat. Pass the red
vapours through NaOH
solution. To the yellow Yellow precipitate is obtained.
solution add sufficient
quantity of CH3COOH and
(CH3COO)2Pb.
4NaCl+K2Cr2O7+3H2SO4 → 2CrO2Cl2+2Na2SO4+K2SO4+3H2O
(Red vapours)
4NaOH + CrO2Cl2 → 2Na2CrO4 + 2NaCl + 2H2O
(Yellow)
Na2CrO4 + (CH3COO)2Pb → PbCrO4 + 2 CH3COONa
(Yellow ppt)

b) Silver nitrate test:

To the W.E or (S.E A curdy white precipitate fully Presence of Cl- is confirmed
acidified with HNO3), add soluble in excess of NH4OH is
a few drops of AgNO3 got.
solution. AgNO3 + MCl → MNO3 + AgCl (Curdy white)
AgCl + 2NH4OH → [Ag(NH3)2]Cl + 2H2O
c) To a pinch of the solid salt A greenish yellow gas is Presence of Cl- is confirmed.
taken in a test tube add a evolved.
few grains of MnO2 and 2MCl + MnO2 + 3H2SO4 → MnSO4 + 2MHSO4 + 2H2O + Cl2
add con. H2SO4.
12. Tests for Br- :
a) To a pinch of the substance Reddish brown vapours turning Presence of Br- is confirmed.
taken in a test tube add a moist starch paper yellow and
few grains of MnO2 and 2- moist starch iodide paper blue
5 cc of H2SO4 and warm. are evolved.

10
 2MBr + MnO2 + 2H2SO4 → MnSO4 + 2MHSO4 + 2H2O + Br2 (Red-
brown)
b)
To the W.E or S.E in a test An orange – brown organic Presence of Br- is confirmed
tube add fresh chlorine layer is formed.
water and then a few drops 2Br- + Cl2 → 2Cl- + Br2
of CCl4. Shake well. (Br2 being a covalently bonded non-polar liquid, dissolves in a non – polar
solvent like CCl4 easily to give the organic layer).
Preparation of chlorine water: To prepare chlorine water, take either KMnO4 or a few grains of MnO2
and add con.HCl. Close the mouth of the test tube for 5 seconds. The resulting liquid can be used as
chlorine water. (The chlorine water prepared from MnO2 is very strong. Therefore it must be used
sparingly).

c) To the W.E or (S.E A straw coloured precipitate is Presence of Br- is confirmed

acidified with dil. HNO3) formed which is partly soluble
add a few drops of AgNO3 in NH4OH solution.
solution.
2AgNO3 + MBr2 → M(NO3)2 + 2AgBr (Straw coloured)

13. Tests for I- :

a) To a pinch of the substance Violet vapours which turn Presence of I- is confirmed
taken in a test tube add a moist starch paper blue are
few grains of MnO2 and 2- obtained.
5 cc of H2SO4 and warm. 2MI + MnO2 + 3H2SO4 → MnSO4 + 2MHSO4 + 2H2O + I2
(Violet)

b) To the W.E or S.E in a test A pink organic layer is Presence of I- is confirmed

tube add fresh chlorine obtained.
water and then a few drops
of CCl4. Shake well. 2I- + Cl2 → 2Cl- + I2 (Violet)
To the W.E or (S.E A yellow precipitate Presence of I- is confirmed
c) acidified with dil. HNO3) completely insoluble in
add a few drops of AgNO3 NH4OH is got.
solution.
AgNO3 + MI → MNO3 + AgI (Yellow)
14. Tests for NO3- :
a) To a pinch of the salt taken The solution turns green and Presence of NO3- is confirmed.
in a test tube add con. there is profuse evolution of
H2SO4 and warm. Then brown fumes which turn
add 1-2 copper turnings. FeSO4 solution black.

MNO3 + H2SO4 → MHSO4 + HNO3

Cu + 4HNO3 → Cu(NO3)2 + 3H2O + 2NO2

11
 (green) (brown)
6FeSO4 + 3H2SO4 + 2HNO3 → 3Fe2(SO4)3 + 2NO + 4H2O
FeSO4 + NO → FeSO4.NO ( Brown-black)
b) Repeat the above test using Profuse evolution of brown Presence of NO3- is confirmed.
paper pellets instead of fumes which turn FeSO4
copper turnings. solution black is seen.

MNO3 + H2SO4 → MHSO4 + HNO3

C + 4HNO3 → CO2 + 2H2O + 4NO2
(Brown)
c) Brown ring test:
To the W.E or (S.E A brown ring is formed at the Presence of NO3- is confirmed
acidified with dil. HNO3) junction of the two liquids.
add freshly prepared
FeSO4 solution. Then add MNO3 + H2SO4 → MHSO4 + HNO3
con.H2SO4 along the sides 6FeSO4 + 3H2SO4 + 2HNO3 → 3Fe2(SO4)3 + 2NO + 4H2O
of the test tube, in drops. FeSO4 + NO → FeSO4.NO ( Brown)
(Nitroso ferrous sulphate)
Tests for CH3COO- :
15. To a small amount of the
a) substance taken in a test A pleasant fruity smell of ester Presence of CH3COO- is confirmed
tube add con.H2SO4 and is got.
warm. Then add C2H5OH CH3COOM + H2SO4 → MHSO4 + CH3COOH
and shake well. Pour the CH3COOH + C2H5OH → CH3COOC2H5 + H2O
contents of the test tube (Fruity smell)
into a beaker of water. Stir
the solution.
b) To the W.E or (S.E Red colour is formed. Presence of CH3COO- is confirmed
acidified with dil.HCl) add
neutral FeCl3 solution and CH3COOM + FeCl3 → (CH3COO)3Fe (red) + 3MCl
decant. Red colour disappears and a
red-brown precipitate is formed
after some time.
(CH3COO)3Fe + 2H2O → Fe(CH3COO)(OH)2 + 2CH3COOH
(Red-brown)
16. Tests for C2O42- :
a) To a small amount of W.E. A white precipitate is Presence of C2O42- is confirmed.
(SE) add small amount of obtained.
acetic acid and boil off MC2O4 + CaCl2 → CaC2O4 + MCl2
CO2. Now add CaCl2
solution. The pink colour of KMnO4 Presence of C2O42- is confirmed.
b) Take a pinch of the salt in solution is decolourized and
a test tube and add CO2 is evolved.
dil.sulphuric acid. Warm 2KMnO4 + 3H2SO4 + 5H2C2O4 → K2SO4 + 2MnSO4 + 10CO2 + 8H2O
and add 2 drops of dil.
KMnO4 solution.

12
Basic radical analysis:
Preparation of Original Salt Solutions: (OS)
To the solid salt, add ¼ test tube of water and shake well. If it is insoluble in cold water, heat the
salt and water mixture. If it is insoluble even in hot water, dissolve the salt in minimum quantity of dilute HCl.
Boil well. The resulting solution is called the Original Salt solution.
For lead salts, add dil HCl to the salt. Collect the white precipitate by decanting the supernatant liquid.
To the white precipitate add ½ a test tube of water and boil. The resultant solution is the Original Salt
solution.
Tests for zero group:

No. EXPERIMENT OBSERVATION INFERENCE

1. To the given salt taken in a A colourless gas with pungent Presence of NH4+ is
test tube, add NaOH and heat. smell, giving dense white fumes confirmed
with a rod dipped in conc. HCl is
obtained.

NH4+ + NaOH → H2O + Na+ + NH3 (Pungent odour)

NH3 + HCl → NH4Cl (dense white fumes)
2. To the OS add NaOH and a A red brown precipitate is Presence of NH4+ is
few drops of Nessler’s formed. confirmed
reagent.
NH3+2K2HgI4+ 3NaOH → NH2.HgO.HgI +3NaI +4KI +2H2O
(Red brown)

Inter group separation:

No. EXPERIMENT OBSERVATION INFERENCE

2+
I. To the OS add dil. HCl White precipitate Pb may be present.
Pb2+ + 2HCl → PbCl2 ↓ (White) + 2H+
No precipitate Absence of Group I radical
II. To the above add H2S solution Black precipitate Cu2+ may be present.
Cu2+ + H2S → CuS↓ (Black) + 2H+
Yellow precipitate As3+ may be present
2As3++ 3H2S → 6HCl + As2S3
No precipitate Absence of Group II
radicals.
III. To the OS add NH4Cl till it Brown precipitate Fe3+ may be present.
dissolves and add 2 drops of 3+ -
Fe + 2OH → Fe(OH)3 (Brown)
conc.HNO3 and boil. Cool and Gelatinous white precipitate. Al3+ may be present.
then add excess NH4OH solution 3+ -
Al + 2OH → Al(OH)3 (Gelatinous white)
till a pungent smell of NH3 is No characteristic precipitate. Absence of Group III
obtained. radicals.

IV. Add H2S to the above solution Black precipitate Co2+ or Ni2+ may be present.
Co + H2S → CoS↓ (black) + 2H+
2+

Ni2+ + H2S → NiS↓ (black) + 2H+

13
 White precipitate Zn2+ may be present.
Zn + H2S → ZnS↓ (white) + 2H+
2+

Buff precipitate Mn2+ may be present.

Mn + H2S → MnS↓ (buff) + 2H+
2+

No characteristic precipitate. Absence of Group IV

radicals.
V. Boil the above solution to expel White precipitate Ba2+, Sr2+ or Ca2+ may be
H2Sgas. Add NH4Cl till it present.
dissolves and add 2 drops of Ba2+ + CO32- → BaCO3↓
conc.HNO3 and boil. Cool and Sr2+ + CO32- → SrCO3↓
then add excess NH4OH solution Ca2+ + CO32- → CaCO3↓
till a pungent smell of NH3 is No characteristic precipitate. Absence of Group V
obtained. Finally add (NH4)2CO3. radicals.
VI. To the OS add NH4Cl, excess of White precipitate Mg2+ may be present.
NH4OH and Na2HPO4 Mg2+ + NH4OH + Na2HPO4 → MgNH4PO4↓ + H2O + 2Na+

No characteristic precipitate Absence of Group VI

radical.

Confirmatory Tests for basic radicals:

Group I:-
Tests for Pb2+
1. To the OS add K2CrO4 Yellow precipitate is obtained. Presence of Pb2+ is
solution. confirmed.
Pb + K2CrO4 → PbCrO4 ↓ (yellow) + 2K+
2+

2. To the OS add KI solution A yellow precipitate which is Presence of Pb2+ is

soluble when heated and confirmed.
reappears as golden spangles is
obtained.
Pb2+ + 2KI → PbI2↓ + K+
3. To the OS add H2SO4 solution A white precipitate soluble in Presence of Pb2+ is
(CH3COO)NH4 is obtained. confirmed.
Pb2+ + H2SO4 → PbSO4↓ + 2H+
PbSO4 + (CH3COO)NH4 → (NH4)SO4 + (CH3COO)2Pb

Group II:-
Tests for Cu2+
1. To the OS add NH4OH in A light blue precipitate Presence of Cu2+
drops to excess dissolving in excess to give a confirmed.
deep blue solution.
Cu2+ + 2OH- → Cu(OH)2 (pale blue)
Cu(OH)2+ 4NH4OH →[Cu(NH3)4](OH)2 (deep blue) + 4H2O

14
 2. To the OS add K4[Fe(CN)6] Chocolate brown precipitate is Presence of Cu2+
formed. confirmed.
Cu + K4[Fe(CN)6] → Cu2[Fe(CN)6] ↓ + 4K+
2+

(chocolate brown)
Tests forAs3+
Dissolve the yellow
precipitate obtained (inter
group separation) in
con.HNO3 and divide it into
two parts.
1. To a part of the solution add A yellow precipitate is formed. Presence of As3+ is
ammonium molybdate confirmed.
solution and heat. As2S3 + 10HNO3 → 2H3AsO4 + 10NO2 + 3S +2H2O
H3AsO4 + 12(NH4)2MoO4 + 21HNO3 →
(NH4)3AsO4.12MoO3 + 21NH4NO3 + 12H2O
(yellow ppt of ammonium arseno molybdate)
2. Make the second part of the Awhite precipitate is formed. Presence of As3+ is
solution alkaline with NH4OH confirmed.
and add magnesia mixture. H3AsO4 + MgSO4 + 3NH4OH → Mg(NH4)2AsO4 +
(NH4)2SO4 + 3H2O (white)

Group III:
Tests for Al3+
1. To the OS add NaOH in drops A gelatinous white precipitate is Presence of Al3+ confirmed.
to excess obtained.
Al3++ 3 NaOH → Al(OH)3 ↓ (gelatinous white)+ 3Na+
A blue lake is formed. Presence of Al3+ confirmed.
Al3++ OH- → Al(OH)3 ↓
2. Blue Lake test : Al(OH)3 ↓ + blue dye → Blue lake
To the OS add a drop of blue (Blue lake is the blue litmus absorbed in a jelly like Al(OH)3
litmus solution and then add to form a blue floating precipitate in a clear solution).
ammonium hydroxide
solution in drops till the
solution turns alkaline.
Tests for Fe3+
1. To the OS add a drop of Prussian blue colour is formed. Presence of Fe3+ confirmed.
K4[Fe(CN)6] 4Fe3++3 K4[Fe(CN)6] → Fe4[Fe(CN)6]3 + 12K+
(Prussian blue)

Blood red colour is formed. Presence of Fe3+ confirmed.

2. To the OS add a few drops of 4Fe3++3 KCNS → Fe(CNS) 3 (blood red) + 3K+
dil HCl followed by a drop of
KCNS solution
Group IV:-

15
 Tests for Zn2+
1. To the OS add NaOH in drops A white precipitate soluble in Presence of Zn2+
to excess. excess is obtained. confirmed.
Zn + 2 NaOH → Zn(OH)2↓ (white) + 2Na+
2+

Zn(OH)2+ 2 NaOH → Na2ZnO2 (soluble) + 2H2O

2. To the OS add a drop of A greenish white precipitate is Presence of Zn2+
K4[Fe(CN)6] obtained. confirmed.
4Zn +3 K4[Fe(CN)6] → Zn2[Fe(CN)6] + 4K+
2+

Tests for Mn2+

1. To the OS add NaOH in drops A white precipitate which turns Presence of Mn2+
to excess. brown and finally black on long confirmed.
standing, is formed.
Mn2++ 2 NaOH → Mn(OH)2↓ (white) + 2Na+
Mn(OH)2+ 2 NaOH → Na2MnO2(soluble) + 2H2O
2. To a small quantity of the Pinkish purple colour is Presence of Mn2+
above precipitate add 3 ml of obtained. confirmed.
conc. HNO3 and a small
amount of PbO2. Boil the Mn(OH)2 + 2 HNO3 → Mn(NO3)2 + 2H2O
solution. Cool. Pour into half a Mn(NO3)2+5 PbO2+6 HNO3 → 2HMnO4+5Pb(NO3)2+2 H2O
test tube of water.

Tests for Ni2+

1. To the OS add 2 drops of Apple-green precipitate if Presence of Ni2+
NaOH solution. formed. confirmed.
Ni2++ 2 NaOH → Ni(OH)2↓ (apple-green) + 2Na+

2. To the OS add Cherry red precipitate is formed. Presence of Ni2+

dimethylglyoxime dissolved in confirmed.
NH4OH

Tests for Co2+

1. To the OS add NH4Cl, NH4OH Red brown precipitate is Presence of Co2+
and two drops of K3[Fe(CN)6] formed. confirmed.
solution

2. To the OS add I ml of KCNS The organic layer is stained Presence of Co2+

solution and 2 ml of acetone. blue. confirmed.
Shake well. Co2+ + 4CNS- → [Co(CNS)4]2-
16
Group V:- [Dissolve the ppt in acetic acid. Divide solution into 3 parts]

Test for Ba2+

1. To the OS add K2CrO4 Yellow precipitate is obtained. Presence of Ba2+ is
solution. confirmed.

Ba2+ + K2CrO4 → BaCrO4 ↓ (yellow) + 2K+

Test for Sr2+
2. To the OS add (NH4)2SO4 White precipitate is formed. Presence of Sr2+ is
solution. confirmed.
Sr + (NH4)2SO4 → SrSO4↓ (white)+ 2NH4+
2+

Test for Ca2+

3. To the OS add (NH4)2C2O4 White precipitate is formed.Presence of Ca2+ is
solution. confirmed.
Ca + (NH4)2C2O4 → CaC2O4↓ (white)+ 2NH4+
2+

Group VI:-

Test for Mg2+

1. To the OS add NH4Cl, White precipitate is obtained. Presence of Mg2+ is
NH4OH and confirmed.
Na2HPO4solution.
Mg2+ + NH4OH + Na2HPO4 → MgNH4PO4↓ + H2O + 2Na+

2. To the above precipitate add a Pink ash is obtained. Presence of Mg2+ is confirmed
drop of Co(NO3)2 solution.
Dip a filter paper into it and
burn it. Note the colour of the
ash.

Result:
The given salt contains
Cation –
Anion –
The given salt is

17
 ----------

Date: Experiment No-9

SALT ANALYSIS – (1)
Aim: To analyse the given salt systematically and report one anion and one cation present in the salt.

Preliminary tests:

No. EXPERIMENT OBSERVATION INFERENCE

1. Note the colour of the salt White Absence of Cu2+,Ni2+, Fe3+,

Mn2+ and Co2+

2. Note the odour of the salt No characteristic Absence of NH4+ , CH3COO-,

odour S2-

3. Solubility test:
To a pinch of the salt taken in a test tube add 2
a) cc of water. i) Insoluble in water i) Presence of heavy
To a pinch of the given salt add 2 cc of dil.HCl metal carbonates
and shake well.
b) i) Absence of Pb2+
i) Soluble in dil.HCl

4. Flame test:
Take a spatula of salt in a watch glass. Add a
drop or two of con.HCl to it and make a paste. No characteristic Absence of Ba2+,Sr2+,
Introduce this paste into the non-luminous colour observed Ca2+, Cu2+
flame using a glass rod.

Acid radical analysis:

18
5. Dilute acid test: d) No characteristic d) Absence of CO32-, S2-,
To the salt taken in a test tube add dil.HCl and reaction
warm. SO32- (Group I acid radicals)

6. Con. Acid test:

To a small amount of the salt taken in a test
g) No characteristic g) Absence of Cl-, Br -, I-,
tube add con. H2SO4 and heat slightly.
reaction NO3-, CH3COO- , C2O42-
(Group II acid radicals)

Sodium carbonate extract:

To 1 part of the salt add 3 parts of Na2CO3 and 1 test tube of water. Boil well for two minutes. Cool and filter.
The filtrate is called the sodium carbonate extract (S.E).

Confirmatory tests for acid radicals:

7. Tests for PO43-:

a) Ammonium molybdate test: Canary yellow precipitate is Confirms presence of PO43-

formed.
To the salt add con. HNO3 and
heat. Then add excess of
ammonium molybdate 2M3PO4 + 3(NH4)2MoO4 → 2(NH4)3PO4 + 3M2MoO4
solution. M2MoO4 + 2HNO3 → 2MNO3 + H2MoO4(Molybdic acid)

H2MoO4 → H2O + MoO3

(NH4)3PO4 + 12MoO3 +6H2O → (NH4)3PO4.12MoO3.6H2O

(Ammonium phosphor molybdate-

canary yellow precipitate)

b) To the water extract (W.E –

salt dissolved in water) or (S.E A white precipitate is formed. Confirms presence of PO43-
– acidified with dil.HCl), boil
off CO2 and then add magnesia

19
 mixture M2HPO4 + MgCl2 + NH4OH → MgNH4PO4↓ + 2MCl+ H2O

(Magnesia mixture preparation (white)

- add NH4Cl to Mg2+ solution,
add NH4OH till a strong smell
of NH3 is got)

Basic radical analysis:

Preparation of Original Salt Solutions: (OS)

To the solid salt, add ¼ test tube of water and shake well, since it is insoluble in cold water, heat
the salt and water mixture. Sine it is insoluble even in hot water, dissolve the salt in minimum quantity of
dilute HCl. Boil well. The resulting solution is called the Original Salt solution.

Tests for zero group:

No. EXPERIMENT OBSERVATION INFERENCE

1. To the given salt taken in a test No characteristic reaction Absence of NH4+ ion.
tube, add NaOH and heat.

Inter group separation:

No. EXPERIMENT OBSERVATION INFERENCE

I. To the OS add dil. HCl No characteristic precipitate. Absence of Group I radical

Pb2+
II. To the above add H2S No characteristic precipitate. Absence of Group II radicals.
Cu2+ , As3+
III. To the OS add NH4Cl and then No characteristic precipitate. Absence of Group III
NH4OH radicals. Fe3+, Al3+

IV. Add H2S to the above solution White precipitate Zn2+ may be present.
Zn2+ + H2S → ZnS↓ (white) +
2H+
Confirmatory Tests for basic radicals:

Group IV:-
Tests for Zn2+

1. To the OS add NaOH in drops to A white precipitate soluble in Presence of Zn2+ confirmed.
excess. excess is obtained.

20
 Zn2++ 2 NaOH → Zn(OH)2↓ (white) + 2Na+

Zn(OH)2+ 2 NaOH → Na2ZnO2 (soluble) + 2H2O

2. To the OS add a drop of A greenish white precipitate is Presence of Zn2+ confirmed.

K4[Fe(CN)6] obtained.

4Zn2++3 K4[Fe(CN)6] → Zn2[Fe(CN)6] + 4K+

Result:
The given salt contains
Cation – Zn2+
Anion – PO43-
The given salt is Zn3 (PO4)2, Zinc phosphate.

Date: Experiment No.10

Salt Analysis-2
Aim:
To analyze the given salt systematically and report one anion and one cation present in the salt.
Preliminary tests:
No. EXPERIMENT OBSERVATION INFERENCE
1. Note the colour of the salt No characteristic colour Absence of Cu2+, Ni2+, Fe3+,
observed. Mn2+ and Co2+
2. Note the odour of the salt No characteristic odour Absence of NH4+
observed. CH3COO-
S2- ions
3. Solubility test:
a) To a pinch of the salt taken in Insoluble in water ii) Presence of heavy metal
a test tube add 2 cc of water. carbonates

b) To a pinch of the given salt ii) Insoluble in dil.HCl ii) Presence of Pb2+
add 2 cc of dil.HCl and shake
well.
4. Flame test:
Take a spatula of salt in a No characteristic flame colour Absence of Ba2+,Sr2+, Ca2+,
watch glass. Add a drop or observed. Cu2+
two of con.HCl to it and make
a paste. Introduce this paste
into the non-luminous flame
using a glass rod.
Acid radical analysis:
5. Dilute acid test: d) No characteristic reaction d) Absence of CO32-, S2-,
To the salt taken in a test tube SO32- (Group I acid radicals)
add dil.HCl and warm.

21
6. Con. Acid test: a) A colourless gas with an a) Presence of Cl-
To a small amount of the salt irritating smell which gives
taken in a test tube add con. dense white fumes when a glass
H2SO4 and heat slightly. rod dipped in NH4OH solution is
introduced.
MCl + H2SO4 → MHSO4 + HCl
NH4OH + HCl → NH4Cl + H2O
(Dense white fumes)

Sodium carbonate extract:

To 1 part of the salt add 3 parts of Na2CO3 and 1 test tube of water. Boil well for two minutes. Cool and
filter. The filtrate is called the sodium carbonate extract (S.E).

Confirmatory tests for acid radicals:

Tests for Cl- :

a) Chromyl chloride test: Red vapours are evolved. Presence of Cl- is confirmed.
To a pinch of the solid salt
taken in a test tube add
potassium dichromate
followed by con. H2SO4 Yellow solution is got.
and heat. Pass the red
vapours through NaOH
solution. To the yellow Yellow precipitate is obtained.
solution add sufficient
quantity of CH3COOH and
(CH3COO)2Pb.
4NaCl+K2Cr2O7+3H2SO4 → 2CrO2Cl2+2Na2SO4+K2SO4+3H2O
(Red vapours)
4NaOH + CrO2Cl2 → 2Na2CrO4 + 2NaCl + 2H2O
(Yellow)
Na2CrO4 + (CH3COO)2Pb → PbCrO4 + 2 CH3COONa
(Yellow ppt)

b) Silver nitrate test:

To the W.E or (S.E A curdy white precipitate fully Presence of Cl- is confirmed
acidified with HNO3), add soluble in excess of NH4OH is
a few drops of AgNO3 got.
solution. AgNO3 + MCl → MNO3 + AgCl (Curdy white)
AgCl + 2NH4OH → [Ag(NH3)2]Cl + 2H2O
c) To a pinch of the solid salt A greenish yellow gas is Presence of Cl- is confirmed.
taken in a test tube add a evolved.
few grains of MnO2 and 2MCl + MnO2 + 3H2SO4 → MnSO4 + 2MHSO4 + 2H2O + Cl2
add con. H2SO4.
Basic radical analysis:
Preparation of Original Salt Solutions: (OS)
22
 To the solid salt, add ¼ test tube of water and shake well. If it is insoluble in cold water, heat the
salt and water mixture. If it is insoluble even in hot water, dissolve the salt in minimum quantity of dilute HCl.
Boil well.
Collect the white precipitate by decanting the supernatant liquid. To the white precipitate add ½ a test
tube of water and boil. The resultant solution is the Original Salt solution.
Tests for zero group:

No. EXPERIMENT OBSERVATION INFERENCE

1. To the given salt taken in a No characteristic reaction Absence of NH4+
test tube, add NaOH and heat. observed.

Inter group separation:

No. EXPERIMENT OBSERVATION INFERENCE

2+
I. To the OS add dil. HCl White precipitate Pb may be present.
Pb + 2HCl → PbCl2 ↓ (White) + 2H+
2+

No precipitate Absence of Group I radical

Confirmatory Tests for basic radicals:

Group I:-
Tests for Pb2+
1. To the OS add K2CrO4 Yellow precipitate is obtained. Presence of Pb2+ is
solution. confirmed.
Pb2+ + K2CrO4 → PbCrO4 ↓ (yellow) + 2K+
2. To the OS add KI solution A yellow precipitate which is Presence of Pb2+ is
soluble when heated and confirmed.
reappears as golden spangles is
obtained.
Pb2+ + 2KI → PbI2↓ + K+
3. To the OS add H2SO4 solution A white precipitate soluble in Presence of Pb2+ is
(CH3COO)NH4 is obtained. confirmed.
2+ +
Pb + H2SO4 → PbSO4↓ + 2H
PbSO4 + (CH3COO)NH4 → (NH4)SO4 + (CH3COO)2Pb

Result:
The given salt contains
Cation – Pb2+
-
Anion – Cl
The given salt is Lead chloridePbCl2

********************
23
Date: Experiment No.11

Salt Analysis-3
Aim:
To analyze the given salt systematically and report one anion and one cation present in the salt.
Preliminary tests:

No. EXPERIMENT OBSERVATION INFERENCE

1. Note the colour of the salt White or colourless Absence of Cu2+,Ni2+, Fe3+,
Mn2+ and Co2+
2. Note the odour of the salt Ammonical smell Presence of NH4+

3. Solubility test:
a) To a pinch of the salt taken in i) Soluble in water i)Absence of heavy metal
a test tube add 2 cc of water. carbonates

b) To a pinch of the given salt i) Soluble in dil.HCl i) Absence of Pb2+

add 2 cc of dil.HCl and shake
well.
4. Flame test:
Take a spatula of salt in a No characteristic flame colour Absence of Ba2+,Sr2+, Ca2+,
watch glass. Add a drop or Cu2+
two of con.HCl to it and make
a paste. Introduce this paste
into the non-luminous flame
using a glass rod.
Acid radical analysis:
5. Dilute acid test: a) Brisk effervescence is noted. a) Presence of CO32- is
To the salt taken in a test tube A colourless odourless gas confirmed.
add dil.HCl and warm. turning lime water milky is
evolved.
MCO3 + 2HCl → MCl2 + H2O + CO2↑
CO2 + Ca(OH)2 → CaCO3↓ + H2O
(Milky white)

Basic radical analysis:

24
Preparation of Original Salt Solutions: (OS)
To the solid salt, add ¼ test tube of water and shake well. If it is insoluble in cold water, heat the
salt and water mixture. If it is insoluble even in hot water, dissolve the salt in minimum quantity of dilute HCl.
Boil well. The resulting solution is called the Original Salt solution.

Tests for zero group:

No. EXPERIMENT OBSERVATION INFERENCE

1. To the given salt taken in a A colourless gas with pungent Presence of NH4+ is
test tube, add NaOH and heat. smell, giving dense white fumes confirmed
with a rod dipped in conc. HCl is
obtained.

NH4+ + NaOH → H2O + Na+ + NH3 (Pungent odour)

NH3 + HCl → NH4Cl (dense white fumes)
2. To the OS add NaOH and a A red brown precipitate is Presence of NH4+ is
few drops of Nessler’s formed. confirmed
reagent.
NH3+2K2HgI4+ 3NaOH → NH2.HgO.HgI +3NaI +4KI +2H2O
(Red brown)

Result:
The given salt contains
Cation – NH4+
Anion – CO32-
The given salt is Ammonium carbonate.

********************

25
 Experiment No. 12
Preparation of standard solution of sodium carbonate

Aim:
To prepare 0.1N standard solution of sodium carbonate.

Apparatus and chemicals:

Anhydrous sodium carbonate crystals, 100ml standard flask, funnel, spatula, wash bottle and balance.

Theory:
Sodium carbonate is a primary standard. A primary standard is a substance which is stable and available
in the purest form and whose standard solution can be made directly by weighing a known quantity. Its
concentration does not change even on long standing.
A solution whose concentration is known is called a standard solution. Concentration of a solution is
generally expressed in terms of molarity or normality. A standard solution can be prepared by weighing an
amount of the solid and dissolving it in a known amount of water.
Normality(N) is defined as the number of gram equivalents of solute per litre of solution.

mass x 1000
N=
Eq.Wt. x volume
Hence the amount of mass required for making 0.1N, 100 ml standard solution of sodium carbonate will be;
m = 0.1 x 53 x 100 = 0.53g
1000
Equivalent mass of an acid (or base) is obtained by dividing the molecular mass by the number of available
hydrogen ions (hydroxyl ions) per molecule.

Procedure:
Weigh 0.53g of sodium carbonate crystals and transfer that into a 100ml standard flask using a funnel.
Wash the funnel with small amount of water into the standard flask. Dissolve the sodium carbonate crystals
using small amount of water at a time till there is no speck of sodium carbonate crystals left. Now add water till
the lower meniscus of the solution touches the 100ml mark. Put a stopper on the flask and shake the contents to
get a homogeneous solution of sodium carbonate.
Result:
Amount of sodium carbonate crystals dissolved in 100ml = 0.53g
Strength of solution = 0.1N

26
Date: Experiment No. 13
Volumetric analysis 2
Aim:
To prepare 100ml of approximately 0.1N Hydrochloric acid solution (by diluting the
concentrated HCl-12N) and to determine its exact strength by titrating against standard 0.1N Sodium
carbonate solution.

Apparatus and chemicals required:

Burette, pipette, conical flask, funnel, standard flask, solid Sodium carbonate, Concentrated HCl
and methyl orange.

Chemical Equation:
Na2CO3 + 2HCl → 2NaCl +CO2 + H2O
Procedure:
Weigh 0.53 g of sodium carbonate crystals and transfer that into a standard flask using a funnel.
Wash the funnel with small amount of water into the standard flask. Dissolve the sodium carbonate
crystals using small amount of water at a time till there is no speck of crystals left. Now add water till
the lower meniscus of the solution touches the 100ml mark. Put a stopper on the flask and shake the
contents to get a homogeneous solution of sodium carbonate.
Take nearly 70ml of water in a 100ml standard flask. Measure 0.83ml of concentrated HCl (12N)
and add to the flask with continuous shaking. When all the acid has been added and dissolved, add
enough water to fill the flask up to the mark. Shake well and label the flask.
Wash the burette with water and rinse it with Hydrochloric acid solution. Fill it up with the same
and note the initial reading. Rinse a clean pipette with standard Sodium carbonate solution and pipette
out exactly 10ml of the same into a clean conical flask. Add a drop of methyl orange indicator to the
conical flask. Titrate the standard Sodium carbonate solution against the Hydrochloric acid solution
taken in the burette till the straw yellow colour changes to orange (with a pinkish tinge). Note the final
reading. Repeat the titrations for concordant values.

Inference:
The Normality of Hydrochloric acid solution =
Weight per litre of Hydrochloric acid = g/L

Precautions:
1. Before taking any liquid in the burette or pipette, it should be rinsed with their respective solution.
2. The conical flask (titration flask) should not be rinsed with any solution as it may change the
volume and concentration of the solution. It should be simply washed only with water.
3. Read the lower meniscus for colourless liquids and upper meniscus for coloured liquids.

27
Observations:
Burette solution - Hydrochloric acid solution
Pipette solution - Standard sodium carbonate solution
Indicator - Methyl orange
End point - Pale yellow to red

Equation:
2Na2CO3 + 2HCl → 2NaCl + H2O + CO2

Titration between Standard Sodium carbonate and Hydrochloric acid solution:

Sl.No. Burette readings Volume of HCl Volume of Na2CO3

solution (ml) solution(ml)
Initial Final

Concordant value = ml

Calculations:
Preparation of the approximately 0.1N solution of HCl:
N1V1 =N2V2 (Dilution formula)
12 x V1 = 0.1 x 100
V1 = 0.83ml
Preparation of the standard solution of Na2CO3:
Mass= Normality x Eq. wt. x Volume
1000
m = 0.1x 106/2 x 100 = 0.53g
1000
Normality and weight per litre of HCl:
Volume of Sodium carbonate solution (V1) = 10 ml
Normality of Sodium carbonate solution (N1) = 0.1 N
Volume of Hydrochloric acid solution (V2) =
Normality of Hydrochloric acid solution (N2) = ?
As, V1N1=V2N2
N2 = V1N1 / V2
The Normality of Hydrochloric acid solution =
Weight per litre of Hydrochloric acid = Eq.Weight x Normality
= g/L

Date: Experiment No. 14,15

Organic analysis (1 & 2)
28
Aim:
To detect the presence of Nitrogen, Sulphur and Chlorine in the given compound.

Apparatus:
Fusion tubes, china dish, beaker, funnel, tongs and test tubes.

Chemicals:
Sodium metal, ferrous sulphate solution, ferric chloride solution, sodium hydroxide, dilute
sulphuric acid, sodium nitroprusside, acetic acid and lead acetate.

Preparation of Sodium fusion extract or Lassaigne’s extract:

Take a small piece of freshly cut sodium in a fusion tube. Heat the tube on the flame of low
intensity till the sodium melts to a shiny globule. Remove the ignition tube from the flame and add an
equal amount of organic compound to it. Heat the tube again, first on very low flame and then on high
flame till the lower part of the fusion tube becomes red hot. Continue heating for 2 minutes and then
quickly place its red hot end under water (10-15 ml) taken in a china dish. The glass tube will break and
any sodium metal left unreacted will react with water. If the tube does not break, it may be crushed with
a clean heavy glass rod. Reaction of sodium with water is very vigourous and is sometimes explosive.
Do not bring your face close to the china dish until the reaction stops. Repeat the process at least 3 times
by taking a fresh piece of sodium. Boil the reaction mixture to reduce the volume to about 5 ml. Cool the
contents and filter them through a clean filter paper fixed in a funnel. Collect the filtrate in a test tube.
This filtrate is called the Lassaigne’s extract or the Sodium fusion extract used for the detection of
various elements present in it.
Detection of nitrogen

Sl.No. Experiment Observation Inference

1 Take 1 ml of the extract in a clean A blue or greenish The presence of

test tube. Add a pinch of ferrous blue solution is Nitrogen in the
sulphate and heat the mixture for obtained. organic compound
about 1 minute. Acidify the dil. is confirmed.
Sulphuric acid and then add ferric
chloride solution.

Na + C + N NaCN
2NaCN + FeSO4 Na2SO4 + Fe(CN)2
Fe(CN)2 + 4NaCN Na4[Fe(CN)6]
3Na4[Fe(CN)6] + 4Fe3+ Fe4[Fe(CN)6]3 + 12 Na+

Detection of nitrogen and sulphur:

Sl.No. Experiment Observation Inference

29
 1. Take 1 ml of the extract and add a A blood red Confirms the presence
few drops of neutral Ferric colour is obtained of nitrogen and
chloride solution to it. sulphur

Na + C + N + S NaCNS
FeCl3 + 3NaCNS Fe(CNS)3 + 3NaCl
Blood red

Detection of sulphur:

Sl.No. Experiment Observation Inference

1. Sodium nitroprusside test:
Take 1 ml of the extract in a test Violet colouration Confirms the presence
tube and add a few drops of is obtained. of sulphur in organic
Sodium nitroprusside solution to compound.
it.
2. Lead acetate test:
Take 1 ml of the Lassaigne’s A black ppt. is Confirms the presence
extract and add acetic acid and obtained. of sulphur.
lead acetate

2Na + S Na2S
Na2S + Na2[Fe(CN)5NO] Na4[Fe(CN)5NOS]

Na2S + (CH3COO)2Pb2 CH3COONa + PbS(Black)

Detection of chlorine:

Sl.No. Experiment Observation Inference

1. Silver nitrate test:
To about 2ml of the extract add White precipitate Confirms the presence of
1ml of con.nitic acid and boil for is obtained. chlorine in organic
some time. Cool the contents and compound.
add to it silver nitrate solution.

Na + Cl NaCl
NaCl + AgNO3 Ag Cl + NaNO3

Inference:
The given organic compound contains ---------------------

Date: Experiment No.16

Crystallisation

Aim:
To prepare crystals of pure copper sulphate from a given impure sample of the blue vitriol.

30
Apparatus and chemicals required:
Impure sample of copper sulphate, dil.sulphuric acid, 400ml beaker, a china dish, a funnel, petri dish,
and glass rod.

Procedure:
1. Preparation of solution: take about 25-30 ml of water and add to it small quantities of the powdered
impure copper sulphate, with constant stirring, till you get a saturated solution. Now add 2-3ml of
dil.sulphuric acid to make the solution clear. This prevents the hydrolysis of the copper sulphate.
2. Filtration of the solution: Filter the solution and collect the filtrate in a china dish. The insoluble
impurities are left as residue on the filter paper.
3. Concentration of the filtrate to crystallization: Heat the china dish on a sand bath till the solution is
reduced to about one third of its original volume. As the solution gets heated up, it is stirred well with a
glass rod to avoid crust formation on the sides of the dish. Don’t allow the solution in the dish to boil.
Remove a drop of the solution with the end of a glass rod and cool it by blowing. The appearance of a
crust or tiny crystals on the glass rod shows that the crystallization point has reached. Now stop heating
and transfer the hot saturated solution in a petri dish.
4. Cooling the hot saturated solution: Place the petri dish on a beaker containing water filled to the brim
and allow it to cool slowly for some time. Deep blue crystals of copper sulphate will appear. After
about half an hour, the crystallization is complete.
5. Separation of crystals and drying: Decant of the mother liquid carefully. Wash the crystals with little
ethyl alcohol containing small amount of cold water. Keep the crystals on a filter paper which soaks the
solution. Transfer the crystals on another filter paper and dry them by pressing gently between the folds
of the filter paper.

Precautions:
1. The filtrate should be evaporated slowly by gently heating during concentration.
2. The filtrate is to be evaporated only up to the crystallization point. It should never be heated to dryness.
3. The solution should be cooled slowly without disturbing it.

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