EXPERIMENT -1

Aim: To determine the melting point of organic compounds like Naphthalene .

Material required: Naphthalene, the aluminium block, stand with clamp, capillary tube,
tripod, thermometer, and kerosene burner
Experimental setup:
A. Procedure to determine melting point of Naphthalene:

1. Take a capillary tube and close its one end by heating the end in the flame for 2-3
minutes while continuously rotating it.
2. Take naphthalene on a tile and crush it into a fine powder.
3. As shown in the figure below, firmly hold the closed end of the capillary tube
between your finger and thumb.
4. Dip the open end of the capillary tube in the finely powdered naphthalene.
5. Gently tap the capillary tube on the table to fill the compound in the capillary tube
to about a length of 1–2 cm.

Figure (a)

6. With the help of a thread, attach the capillary tube to a thermometer as shown in the
figure below.

Figure (b)

7. Place the capillary tube in the groove of the aluminium block.

8. Double check that the capillary tube holding the naphthalene is in the middle of the
groove.
9. Place the Aluminium block on a tripod stand above the kerosene burner and start
heating the block with the burner.
10. Keep continuous watch of the temperature and note the temperature as soon as the
substance starts to melt.
11. Make note of the temperature (t1) as soon as the compound begins to melt.
12. Make note of the temperature (t2) as soon as the compound is melted completely.
13. The average of the two readings gives the correct melting point of the substance.
Observation:
Temperature t1 = 790 C
Temperature t2 = 81.50 C
Melting point of Naphthalene = t1+ t2/2= 79+81.5/2 = 80.25 0 C

Precautions:
 Make sure the sample of Naphthalene and Benzoic acid are dry and powdered.
 Keep the capillary tube and the thermometer at a similar level.
 Tightly pack the powder into the capillary tube without any air gaps
 EXPERIMENT -2
Aim: To determine the boiling point of organic compounds like Benzene.
Material required: Benzene, the aluminium block, fusion tube, stand with clamp, capillary
tube, tripod, thermometer, and kerosene burner
Experimental setup:
A. Procedure to determine boiling point of Benzene:

1. Take a capillary tube and close its one end by holding the end in the flame and
rotate it for 2-3 minutes.
2. Transfer a few mL of benzene to the fusion tube.
3. Dip the capillary tube into the liquid in the fusion tube keeping the sealed end up.
4. Insert the tube in one of the holes of aluminium block and insert the thermometer
in the other hole.
5. Make sure that the liquid is visible in the fusion tube after it is put in the hole.
6. Place the Aluminium block on the tripod.
7. Start heating the block with the help of a kerosene burner.
8. Note down the temperature soon as the regular streams of bubbles are seen out of
liquid in the fusion tube.
Observation:
Temperature t1 = 78.0 0 C

Temperature t2 = 81.00 C
Melting point of Naphthalene = t1+ t2/2= 78.0+81.0/2 = 79.5 0 C

Precautions:

 Ensure that the capillary tube is properly sealed.

 The seal point of the capillary tube should be well within the liquid.
 EXPERIMENT -3
Aim: To Purify an impure sample of copper sulphate (CuSO4. 5 H20)
Material required: 50 mL capacity Beaker, filtration unit, watch glass, kerosene burner
and CuSO4. 5 H20
Experimental setup:
A. Procedure of crystallization of copper sulphate:

1. Prepare a clear solution of copper sulphate.

2. Dissolve 0.8 g of CuSO4.5H20 in about 8 mL of water and add 1-2 drops of about 6
mL H2SO4 to it.
3. Heat the solution for a while and filter it using a filtration unit.
4. Transfer the solution from the filtration unit to another beaker and allow it to cool
to room temperature.
5. The crystals will appear.
6. Filter, wash these crystals and let them dry.
7. Weigh the crystals and report the yield.

Result: the quantity of pure sample of copper sulphate obtained is = 0.5 g

Precautions:
 Ensure that the crystals are washed well.
 Avoid overheating of the solution.
 The filtrate should be evaporated slowly by gentle heating of the solution.
 The solution should be cooled slowly and do not use any rapid cooling procedures.
 EXPERIMENT -4
Aim: To Purify an impure sample of Alum
Material required: 50 mL capacity Beaker, filtration unit, watch glass, kerosene burner
and Alum
Experimental setup:
A. Procedure of crystallization of Alum:

1. First, prepare a clear solution of alum by dissolving 1g of Alum sample in about 5

mL of water.
2. To this solution add 2 drops of H2SO4.
3. Heat the solution for a while and filter it using a filtration unit.
4. Transfer the solution from the filtration unit to another beaker and allow it to cool
down to room temperature.
5. Formation of the crystals is witnessed.
6. Filter and wash these crystals and allow them to dry.
7. Weigh the crystals and report the yield.

Result: the quantity of pure sample of Alum obtained is = 0.8 g

Precautions:
 Ensure that the crystals are washed well.
 Avoid overheating of the solution.
 The filtrate should be evaporated slowly by gentle heating of the solution.
 The solution should be cooled slowly and do not use any rapid cooling procedures
 EXPERIMENT-5
Aim: Determination of pH of Solutions like fruit juices of different acids, bases, and salts
using universal indicator.
Material required: Universal indicator, sample solutions, test tubes, white tile and
dropper
Procedure of determination of PH using universal indicator:

1. Take the given samples of fruit juices like lemon, orange, pineapple, and apple in a
separate test tube.
2. Make sure you have taken at least 2 mL of juices in each test tube.
3. Use a separate dropper to transfer each juice sample into a test tube.
4. Add two drops of universal indicator.
5. Mix the content thoroughly by shaking it gently.
6. Refer the pH chart to match the colour that appears in the test tube. (match the
colour produced with standard colour pH chart)
7. Record your observation

Observation:
Determination of pH Using Universal Indicator on different samples of fruit juice
Sample Colour with pH indicator pH inference
Apple juice red colour 3-4 Moderate acidic
Pineapple juice Orange red 2-3 Strong acidic
Orange juice Orange 4-5 Moderate acidic
Lemon juice Yellowish orange 2-3 Strong acidic

Procedure:

 Carefully match the colour of the solution that appears with the standard colour
pH chart.
 Add the equal quantity of indicator into the juice sample
 EXPERIMENT-6
Aim: To compare the pH of solutions of strong and weak acids of the same concentration –
hydrochloric acid (HCl) and acetic acid (CH3COOH).
Material required: 0.1M HCl, 0.01M HCl, 0.001M HCl, 0.0001 M HCl, and 0.00001M HCl
test tubes, glass rod, and universal indicator.
Procedure of determination of PH using universal indicator:

1. Take 2-3 drops of solutions of the given concentration on pH paper with the help of
glass rod.
2. Observe the change in colour of the pH paper
3. Match the shade of the pH paper with standard pH indicator chart.
4. Note the approximate pH of the sample

Observation:
Determination of pH Using Universal Indicator on different samples of fruit juice
Sample Colour with pH Approximate pH= - log[H+]
indicator pH
0.1M HCl Red 1-2 1
0.01M HCl Orange red 2-3 2
0.001M HCl Orange 3-4 3
0.0001M HCl Orange 4-5 4
Procedure:

 Ensure to handle the test tube carefully.

 Do not add more indicator.
 Keep the pH paper clean.
 Compare the colour of the solution in the test tube and pH paper colour exactly
with the standard pH indicator chart.
 EXPERIMENT – 7
Aim: To determine the molarity of the given solution of sodium hydroxide (NaOH) by
titrating it against standard solution of (0.05M) oxalic acid.
Apparatus Required: Burette, pipette, conical flask, burette stand, white porcelain tile, etc.
Chemical Required: Standard solution of (0.05 M) oxalic acid, NaOH solution,
phenolphthalein indicator.
Theory: This is an alkalimetry type of titration. The titration is in between weak acid
(H2C2O4.2H2O) and strong base (NaOH)

(COOH)2 + 2NaOH → (COONa) 2 + 2H2O

Indicator: phenolphthalein
End point: colourless to light pink
Observations: -
1. Preparation of standard solution: -
Weight of empty water glass (W1) = 21.7200 g
Weight of watch glass + Mohr’s salt (W2) = 23.2950 g
Weight of oxalic acid = W2 – W1 = (23.2950 – 21.7200) g = 1.575 g
Volume of oxalic acid = 250 ml
Volume of oxalic acid taken for each titration (V2) = 20 ml
2. Titration of standard solution with NaOH Solution:
Observation Table:

S.N. Volume of oxalic Burette reading Volume of

acid used (V1 ml) NaOH used Concordant
Initial Final Volume (V2)

1. 20 ml 0.0 16.8 16.8 ml

2. 20 ml 0.0 16.6 16.6 ml 16.6 ml

3. 20 ml 0.0 16.6 16.6 ml

Calculations:
1. determination of molarity of NaOH solution: M1= molarity of NaOH soln =?
2 moles of NaOH requires 1 moles of oxalic acid V1= volume of NaOH soln= 14.6 ml
M2 = molarity of oxalic acid = M/50
M1V1 = 2 M2V2 V2= volume of oxalic acid = 20 ml
M1V1 = 2 M2V2
M1 x 16.6 = 2 x M/20 x20
M1= 0.120 M.
2. determination of strength of NaOH solution
Strength = Molarity x Molar Mass
= 0.120 x 40 = 4.8 g/liter.
Result: 1. Molarity of the given solution = 0.120 M.
2. Strength of the given solution = 4.80 g/liter.

Precaution:
 Wash the burette with water before and after titration is over.
 Wash the watch glass carefully so that there is no crystal left on the watch glass.
 The last few drops should be added using a pipette to avoid any extra addition of
distilled water above the mark on the neck.
 EXPERIMENT – 8
Aim: To determine the molarity of the given hydrochloric acid (HCl) solution by using a
standard solution of (0.05M) sodium carbonate (Na2CO3).
Apparatus Required: Burette, comical flask, pipette, burette stand, test tube, white tile,
watch glass, volumetric flask (250ml) beaker, funnel glass rod, weight box, wash bottle.
Chemical Required: Standard solution of (0.05 M) Na2CO3, HCl solution, methyl orange
indicator.
Theory: This is an acidimetry titration. The titration is between strong acid (HCl) and weak
base (Na2CO3).
Molecular equation:

Na2CO3(s) + 2 HClaq → 2 NaClaq + CO2(g) + H2O(l)

Indicator: Methyl orange
End point: yellow to pink
Observations: -
1. Solution in a burette: Hydrochloric acid solution
2. Solution by a pipette: sodium carbonate solution
Observation Table:

S.N. Volume of sodium Burette reading Volume of

Carbonate used (V1 HCl used Concordant
Initial Final Volume (V2)
ml)

1. 10 ml 0.0 9.9 9.9 ml

2. 10 ml 0.0 9.7 9.7 ml 9.7 ml

3. 10 ml 0.0 9.7 9.7 ml

Calculations:
1. determination of molarity of HCl solution:
1 mole of Na2CO3 requires 2 moles of HCl M1= molarity of HCl soln =?
V1= volume of HCl soln = 9.7 ml
2 M1V1 = M2V2 M2 = molarity of Na2CO3 soln = M/20
V2= volume of Na2CO3 soln = 10 ml
M1V1 = 1/2 M2V2
M1 x 9.7 = 1/2 x 0.05 x10
M2 = 0.025 M
2. determination of strength of KMNO4 solution
Strength = Molarity x Molar Mass
= 0.025 x 36.5 = 0.9125 g/liter.
Result: 1. Molarity of the given solution = 0.025 M.
 2. Strength of the given solution = 0.9125 g/liter.
Precaution:

 While weighing does not spill the substance on balance pan.

 Rotate the knob of balance gently.
 Keep the weights in weights box at proper places after weighing
 Wash the watch glass carefully so that even a single crystal is not left on the
watch glass.
 Bring the watch glass close to funnel while transferring weighed substance and
transfer it gently. Wash it repeatedly with distilled water.
 Wash the burette with water after titration is over.
 Last few drops should be added using pipette to avoid extra addition of
distilled water above the mark on the neck of the measuring cylinder.
 Experiment No.9
Aim: - To analyse the given sample of salt for detection of one acidic and one basic radical

Detection of acidic radical(anion)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt + Dil. H2SO4 No gas evolves Dil. H2SO4group is
absent
2. Salt + Con. H2SO4 Colourless gas with Chloride (Cl-) may
pungent smell be present
evolves
3. Confirmatory test for chloride:
(a) Salt + Dil. HNO3 + AgNO3 White ppt soluble in Chloride (Cl-) is
solution ammonia solution confirmed

(b) Chromyl chloride test:- Red b colour vapors

 Salt + K2Cr2O7 + Conc. H2SO4 + evolves
warm Solution turns
 Pass the vapours through yellow Chloride (Cl-) is
NaOH solution Yellow precipitate is confirmed
 Add lead acetate and dil. formed
Acetic acid to yellow solution

Detection of basic radical(cation)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt + NaOH solution + heat Colourless gas with Zero group is
ammonical smell present NH4+ may
evolves be present
2. Confirmatory test of NH4+ :-
(a) put glass rod dipped in conc. HCl Dense white fumes
acid on the mouth of test tube generate around NH4+ Confirm
glass rod
(b) Salt + conc. NaOH + Nessler Brown solution NH4+ Confirm
reagent + Warm

Result: in given sample of salt on acidic radical chloride (Cl -) and one basic radical
ammonium (NH4+) is present.
 Experiment No.10
Aim: - To analyse the given sample of salt for detection of one acidic and one basic radical

Detection of acidic radical(anion)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt + Dil. H2SO4 and warm solution Colourless gas with Acetate (CH3COO- )
vinegar like smell may be present
evolves
2. Confirmatory test for Acetate:
(a) Oxalic acid test: take 1 g of salt in Smell of vinegar Acetate (CH3COO- )
test tube and add small amount of obtained is confirmed
oxalic acid + one -two drops of
distilled water

(b) Ferric Chloride test: take 1 g of Deep red color Acetate (CH3COO- )
salt in test tube and add 1-2 ml appears is confirmed
distilled water , shake well and add
1-2 ml of neutral ferric chloride
solution to it

Detection of basic radical(cation)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt + NaOH solution + heat No gas evolve Zero group is
absent
2. Prepare original solution of salt by Cleat solution is Water soluble salt is
dissolving in 20 ml of water formed present
3. Small amount of OS + Dil. HCl White precipitate is Group -I is present
solution formed Pb2+ may be present
4. Confirmatory test of Pb2+: dissolve
the precipitate in hot water and
divide it into three parts
(a) part -1 + KI solution Yellow precipitate Pb2+ is confirmed
(b) part-2 + potassium chromate Yellow precipitate is
obtained which is Pb2+ is confirmed
(c) part-3 + few drops of alcohol + soluble in NaOH
dil. H2SO4 White precipitate is
obtained which is Pb2+ is confirmed
soluble in
ammonium acetate

Result: in given sample of salt on acidic radical acetate (CH3COO-) and one basic radical
lead (Pb2+) is present.
 Experiment No.11
Aim: - To analyse the given sample of salt for detection of one acidic and one basic radical

Detection of acidic radical(anion)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt solution + dil H2SO4 Colourless, Group A anion
colourless gas with (CO32- may be
brisk effervescence present)
which turn lime
water milky
2. Confirmative test :
(a) BaCl2 Test : Salt solution + BaCl2 White ppt of BaCO3 CO32-Confirmed

(b) MgSO4 Test : Salt solution + White ppt of MgCO3 CO32- Confirmed
MgSO4

Detection of basic radical(cation)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt + NaOH solution + heat Colourless gas with Zero group is
ammonical smell present NH4+ may
evolves be present
2. Confirmatory test of NH4+ :-
(a) put glass rod dipped in conc. HCl Dense white fumes
acid on the mouth of test tube generate around NH4+ Confirm
glass rod
(b) Salt + conc. NaOH + Nessler Brown solution NH4+ Confirm
reagent + Warm

Result: in given sample of salt on acidic radical carbonate (CO32-) and one basic radical
ammonium (NH4+) is present.
 Experiment No.12
Aim: - To analyse the given sample of salt for detection of one acidic and one basic radical

Detection of acidic radical(anion)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt solution + dil. H2SO4 solution No gas is evolved Group A radical
absent
2. Salt + Conc. H2SO4 + Heat Brown Colourled Group B radical
gas (NO2) is evolved (NO3- may be
present)
3 Confirmatory test of NO3 -: Deep blue colored NO3- confirmed
(a) Diphenyl amine test: salt + Conc. solution
H2SO4 + diphenyl amine
(b) Ring Test: Salt + Freshly prepared Brown ring is NO3- confirmed
FeSO4 + Conc. H2SO4 along the side formed at the
of the test tube junction of two
liquids

Detection of basic radical(cation)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt + NaOH solution + heat No gas evolve Zero group is
absent
2. Prepare original solution of salt by Cleat solution is Water soluble salt is
dissolving in 20 ml of water formed present
3. Small amount of OS + Dil. HCl White precipitate is Group -I is present
solution formed Pb2+ may be present
4. Confirmatory test of Pb2+: dissolve
the precipitate in hot water and
divide it into three parts
(a) part -1 + KI solution Yellow precipitate Pb2+ is confirmed
(b) part-2 + potassium chromate Yellow precipitate is
obtained which is Pb2+ is confirmed
(c) part-3 + few drops of alcohol + soluble in NaOH
dil. H2SO4 White precipitate is
obtained which is Pb2+ is confirmed
soluble in
ammonium acetate

Result: in given sample of salt on acidic radical nitrare (NO3-) and one basic radical Lead
(Pb2+) is present.
 Experiment No.13
Aim: - To analyse the given sample of salt for detection of one acidic and one basic radical

Detection of acidic radical(anion)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt solution + dil H2SO4 solution No gas is evolved Group A radical
absent
2. Salt solution + Conc. H2SO4 solution No Gas is evolved Group B radicals
absent
3 Salt soluiton + BaCl2 solution White precipitate is SO42- may be
formed present
4 Confirmatory test of SO42-:
(a) dissolve the ppt in Dil. HCl or Dil. Ppt remains SO42- is confirmed
HNO3 solution insoluble
(b) Salt Solution + lead acetate White ppt. formed SO42- is confirmed
solution
(c) Add ammonium acetate Solution Ppt becomes SO42- is confirmed
(CH3COONH4 ) to above ppt soluble

Detection of basic radical(cation)

S.N. EXPERIMENT OBSERVATION INFERENCE
1 Salt + NaOH solution + heat No gas evolve Zero group is
absent
2. Prepare original solution of salt by Cleat solution is Water soluble salt is
dissolving in 20 ml of water formed present
3. Small amount of OS + Dil. HCl No ppt is formed 1st Group is absent
solution
4. Pass the H2S gas to above solution Black ppt is formed 2nd Group is present
(Cu2+) may be
present
5 Confirmatory test of Cu2+: Dissolve Solution turns
above ppt in HNO3 and Divide the bluish green
above solution in 2 parts.
(a) part 1 + NH4OH solution Deep Blue color Cu2+ is confirmed
solution obtained

(b) part 2 + K4[Fe (CN)6] solution Brown color ppt is Cu2+ is confirmed
formed

Result: in given sample of salt on acidic radical Sulphate (SO42-) and one basic radical
Copper (Cu2+) is present.
 EXPERIMENT – 14
Aim: to understand the process of shift in equilibrium between ferric ion and thiocyanate
ions by either increasing/ decreasing the concentration of the ions.
Material required: Ferric chloride (0.1 M), potassium thiocyanate (0.1 M) and potassium
chloride (0.1 M), 2 Beakers of 100 mL capacity, 250 mL Beaker, 6 Boiling tubes, 4 Burettes,
2 Glass droppers, 1 Test tube stand, 1 Glass rod

Precautions:
1. Take a 250 ml beaker thoroughly washed and clean.
2. Put 10 ml of 0.1 M FeCl3 solution in it by using a measuring cylinder.
3. Add 10 ml of 0.1 M KSCN solution with the help of measuring cylinder.
4. A deep red colour is obtained due to complex formation [Fe (SCN)] 2+ (aq).
5. Dilute the above deep red solution by adding 50 ml of distilled water.
6. Take four test tubes and label them as A, B, C and D. Add 10 ml of the deep red solution
to each of the four test-tubes.
7. Arrange the test tubes in a test tube stand [Fig. 7.1].
8. Add 5 ml of distilled water to test tube A; 5 ml of 0.1M FeCl 3 solution to test tube B ; 5
ml of 0.1 M KSCN solution to test tube C and 5 ml of 0.1 M KC1 solution to test tube D.
9. Shake all the tubes well.
10. Now compare the intensity of the colours in test tubes, B, C and D with the red colour
in test tube A taken as reference tube.
11. The intensity of the red colour corresponds to concentration of complex [Fe
(SCN)]2+ and if the concentration of this ion increases, the colour intensity will also
increase
Observation:
Test tube Substance added Change in colour Effect on the Shift of
at equilibrium concentration equilibrium
of [Fe(SCN)]2+
A 5 ml of water Reference colour - -
B 5 ml of 0.1 M Colour deepens Increases Towards right
FeCl3 solution
C 5 ml of 0.1 M KSCN Colour deepens Increases Towards right
solution
D 5 ml of 0.1 M KC1 Colour becomes Decreases Toward left
solution lighter
Conclusion: Increase in concentration of either of the reactants (Fe3+ ions or SCN– ions) shifts
the equilibrium in the forward direction (towards right), on the other hand decrease in
concentration of any of the reactants shifts the equilibrium in the backward direction
(towards left).
 EXPERIMENT-15
Aim: To detect the halogens, nitrogen and sulphur in an organic compound.

Theory:
It is a general test for the detection of halogens, nitrogen and sulphur in an organic
compound. These elements are covalently bonded to the organic compounds. In order to
detect them, these must be converted into their ionic forms. This is done by fusing the
organic compound with sodium metal. The ionic compounds formed during the fusion are
extracted in aqueous solution and can be detected by simple chemical tests. The extract is
called sodium fusion extract or Lassaigne's extract.

Test for nitrogen:

The carbon and nitrogen present in the organic compound on fusion with sodium
metal gives sodium cyanide (NaCN) soluble in water. This is converted in to sodium
ferrocyanide by the addition of sufficient quantity of ferrous sulphate. Ferric ions generated
during the process react with ferrocyanide to form Prussian blue precipitate of ferric
ferrocyanide.

Na + C + N → NaCN

6NaCN + FeSO4 → Na4[Fe(CN)6] + Na2SO4

Sodium ferrocyanide

Na4[Fe(CN)6] + Fe3+ → Fe4[Fe(CN)6]3

Ferric ferrocyanide
Test for Halogen:

Halogens present in an organic compound forms sodium halide on fusion with sodium
metal. Sodium halide extracted with water can be easily identified by adding silver nitrate
solution after acidifying with dil. HNO3.

If chlorine is present, a white curdy precipitate soluble in ammonium hydroxide solution is

formed.

Na + Cl → NaCl

NaCl + AgNO3 → AgCl + NaNO3

If bromine is present, an yellowish white precipitate sparingly soluble in ammonium

hydroxide solution is formed.

Na + Br → NaBr

NaBr + AgNO3 → AgBr + NaNO3

If iodine is present, an yellow precipitate insoluble in ammonium hydroxide solution is

formed.
 Na + I → NaI

NaI + AgNO3 → AgI + NaNO3

Test for Sulphur:

If sulphur is present in the organic compound, sodium fusion will convert it into sodium
sulphide. Sulphide ions are readily identified using sodium nitroprusside.

Na + S → Na2S

Na2S + Na2[Fe(CN)5NO] → Na4[Fe(CN)5NOS]

Sodium nitroprusside violet colour
Test for both Nitrogen and Sulphur:

If both nitrogen and sulphur are present in an organic compound, sodium fusion will convert
it into sodium thiocyanate which then react with Fe3+ to form blood colour complex
[Fe(SCN)]2+

Na + C + N + S → NaSCN

Fe3+ + 2Na → [Fe(SCN)]2+

Note: If the Lassaigne's extract containing excess of sodium metal, sodium cyanide and
sulphides are formed instead of sodium thiocyanate.

NaSCN + 2Na → NaCN + Na2S

Here in this type of cases, both sulphur and nitrogen are to be identified in separate tests.