MAHARASHTRA AGRICULTUAL UNIVERSITIES

AGRICUTURAL POLYTECHNIC
(LOWER AGRICULTURAL EDUCATION)

LABORATORY MANUL
First year (Agri. Diploma)

SUBJECT – General Science - I

(Chemistry)

Prepared By

Dr.S.S.Kolape
Principal, ATS, Puntamba.
Shri. B. M. Belhekar
Agril. Asstt. ATS, Puntamba.
 MAHARASHTRA AGRICULTUAL UNIVERSITIES
AGRICULTURE POLYTECHNIC
(LOWER AGRICULTURAL EDUCATION)
Practical
Course Title: General Science– I (Chemistry) First Year
Index
Practical No. Name of the experiment

1 Orientation of basic laboratory techniques

a) Cutting glass tube and glass rod, b) Bending a glass tube

c) Drawing out a glass jet, d) Study of burner

2 Preparation of lyophilic solution, Starch or Gum,

3 Study of emulsifying agents in stabilising the emulsion of oil

4 Determination of pH of acid, base, salt and fruit juices

5 Comparison of pH of strong acid and weak acid having same

concentration

6 pH change due to common ion effect related to weak acids and weak

bases

7 Preparation of standard solution of oxalic acid

8 Volumetric estimation of sodium hydroxide by standard solution

9 Qualitative analysis for detection of one cation and one anion in a

given salt (Inorganic compound).

10 Qualitative analysis for detection of Nitrogen, Sulphur, Chlorine,

Bromine and Iodine in organic compound.

 EXPERIMENT No. 1
ORIENTATION OF BASIC LABORATORY TECHNIQUES

A) Cutting glass tube and glass rod

Aim: To learn the technique of cutting glass tube and glass rod.

Requirements: Glass tube, glass rod, glass cutting file.

Procedure:
Hold the glass tube or the glass rod to be cut with your hand
firmly keeping the thumb close to cutting point and take the support
of the table. Create a scratch across the tubing or rod surface by
means of cutting file. Only make one single cut with a smooth
movement of the hand. Do not ‘saw’ the glass with the file it otherwise
would give multiple scratch.
Now hold firmly the tube/rod with your both hands keeping the
thumbs behind the scratch and on either side of the scratch mark
and break by jerk bending facing away from you. For safety place a
piece of towel to cover your hand. If the cut part bears sharp edges
rub it gently on some hard flat surface like stone or cement concrete
of simply heat edges.

B) Bending a glass tube

Aim: To learn the technique of bending glass tube.

Requirements: Glass tube and burner, wire gauze.

Procedure:
Take the glass tube to be bent, hold with your both hands apart
leaving portion of the tube to be bent. Heat this portion using high
blue flame of the burner. When this part softens apply gentle bending
pressure and stop heating when desired bend angle is reached. Place
on wire gauze for cooling.
C) Drawing out a glass jet
Aim: To learn the technique of drawing out a glass jet.
Requirements: Glass tube, glass cutting file, burner.

Procedure:
Take the desired glass tube, hold with your both apart leaving
portion of the tube to be jetted ie narrowed. Heat this portion using
high blue flame of the burner. When this part softens, take away from
the flame and stretch gently up to desired length. Cut the narrowed
part from the middle with the file and place on suitable place for
cooling.
D) Study of burner

Aim: Study of burner.

Observe your laboratory burner carefully. It has a heavy metallic

base with a nozzle for fuel gas to come out. The base bears a side tube
that is connected with rubber tube which supplies the fuel gas. The
base is connected with detachable hollow metallic tube, barrel, with a
hole at its base to permit air to enter in. This hole can be monitored
by a rotating collor to control the intake of air. When this hole is
closed yellow reducing flame is obtained which produces black shoot.
Therefore it is partly opened and adjusted to get oxidizing blue flame
free from black it is flame is used for heating purposes.
The burner needs periodic cleaning of the nozzle with a fine
metal wire. Also the rubber tube needs periodic inspection and must
be replaced by a new one if required.
 EXPERIMENT No. 2
PREPARATION OF LYOPHILIC SOLUTION, STARCH OR
GUM.

Theory:
There are two types of solution:
i) Lyophilic Solution: When there is a great affinity between
dispersed phase and dispersion medium. eg starch sol, gum sol.

ii) Lyophobic solution: When there is no or little affinity between

dispersed phase and dispersion medium. e.g. Al(OH)3 solution,
Fe(OH)3 solution, As2O3 solution.

Aim: To prepare lyophilic solution of starch (or gum).

Requirements: Starch or gum, distilled water, small beakers (100 ml

capacity), funnel’ glass rod, filter paper etc.

Procedure: [Procedure for starch solution and Gum solution is

same]
1) Take about 60 ml of distilled water in a clean beaker and start
heating on wire
gauze.

2) In another clean small beaker take about 200 mg (0.2g) starch. Add
about 1 to
2 ml distilled water and make its paste with the help o glass rod.

3) To this paste of starch add the hot distilled water in small portions
at a time and stir well with each addition. After adding about 60 ml of
hot water, heat the content further to let it just boils. Then leave it for
cooling.

4) After cooling, filter through filter paper to remove insoluble starch,

if any. The filtrate so obtained is the solution of starch.
 EXPERIMENT No. 3
STUDY OF ROLE OF EMULSIFYING AGENTS IN
STABILISING THE EMULSION OF OIL.

Theory: Emulsions are lyophobic colloid in nature. Water and oil on

vigorous shaking form emulsion but is unstable. Hence on standing
get separated into two layers. It is called as demulsification.

However it can stabilize by the addition of stabilizing agent which

forms a very thin protecting layer between water and oil, and reduce
the interfacial surface tensions. Emulsifying agents differ in their
ability to stabilize the emulsions.

Aim: To study the role of emulsifying agents in stabilising the

emulsion of an oil.

Requirements: Synthetic detergent, Gum Arabic, Soap, Cotton seed

oil, measuring pipette or cylinders, stop watch.

Procedure:
Part-I: Preparation of solutions of ‘stabilising agents’.

1) Take 0.5 g of gum Arabic and dissolve in 50 ml of water, if required

heat to dissolve.

2) Similarly weight 0.5 g synthetic detergent and dissolve in 50 ml of

water.

3) Likewise weight 0.5g powdered soap and dissolve in 50ml of water,

if required heat to dissolve.

Part-II: Main Experiment:

1) Take three test tubes and label them as T-1, T-2 and T-3. Add 5ml
of oil with measuring pipette (or cylinder) in each of these tubes.

2) Add 5ml of distilled water to each of this containing oil. Two layers
are seen.

3) Shake well, any one out of T-1, T-2, T-3, after closing its opening
with thumb. You will notice that water and oil mix together but on
standing they get
separated in short time and two layers are again seen, indicating the
instability of emulsion.
4) Now add 5ml gum solution to T-1 and again shake well in the same
way. Water and oil again mix together to form the emulsion. Keep T-1
on test tube stand, start the stop watch immediately and record the
time for the separation of two layers. It is called demulsification time.
Record it.

5) Repeat the same procedure for T-2 by adding 5ml synthetic

detergent solution and record the demulsification time.

6) Similarly repeat the same procedure for T-3 by adding 5ml soap
solution to T-3 and record the demulsification time.

Conclusion: Greater the demulsification time the better is the

emulsifying power of the emulsifying agent.

Observation Table:

Test Tube Emulsifier used Demulsification Time,

sec.
T-1 Gum Arabic
T-2 Synthetic
detergent
T-3 Soap
 EXPERIMENT No. 4
DETERMINATION OF PH OF ACID, BASE, SALT AND
FRUIT JUICES

Theory: pH is defined as the negative logarithm to the base 10 of the

molar concentration of H+ ions in the solutions.

pH = -log10[H+]

Similarly pOH is defined as the negative logarithm to the base of

molar concentration of OH ions the solution.

pOH = -log10[OH-]

Note that pH + pOH = 14

Acidic, basic and neutral solutions: Measurement of pH indicates

the acidic, basic or neutral nature of the solution.

Acidic solution Neutral solution Basic solution

For acidic solution For pure water or For basic solution
[H+] > [OH]. neutral solution [H+] < [OH].
[H+] > 10-7 mol dm-3 pH = pOH = 7 [H+] < 10-7 mol dm-3
And pH < 7 and pH > 7

Aim: Determination of pH of solutions of i) Acids ii) Bases iii)

Salts and iv) Fruit juices – using pH paper or universal indicator.

Requirements: Universal indicator, pH paper, distilled water, test

tubes, test tube stand, glass rod etc.

Procedure;
Theoretical Aspects:
1) Wash all the apparatus and rinse with distilled water every time.

2) Some fruits are juicy like sweet lime, water melon, orange etc. Their
juice can be directly taken and tested.

3) But some fruits are not juicy like apple, papaya, chiku etc. For
such fruits, take their small pieces in a test tube, add few ml distilled
water, crush with glass rod, filter and use the filtrate for testing their
pH
4) Testing with pH paper: pH papers in the form of strips are
available. Make small pieces of a strip and place them on filter paper
away from each other. Dip the tip of glass rod in the solution to be
tested and touch with the pH paper to make it wet. The pH paper
imparts certain colour. Match the colour with colour chart provided
and note the corresponding pH.

5) Testing with Universal indicater: Take about 2 ml of solution to

be tested in a test tube. Add on drop of universal indicator, shake and
match the colour developed with the colour chart provided and note
the corresponding pH.

Practical Aspects:
A) Learning with known solutions:

1. Acid solutions:
i) Take given 0.01N HC1 solution and find its pH as described above
either by universal indicator or pH paper. We know that its pH is 2.

ii) Now take 1 ml of 0.01 N HCl on a 100 ml cylinder and dilute to

100 ml with distilled water. It becomes 10-4 N HCl. Find its pH. We
know that its pH is 4

2. Base solutions
i) Take given 0.01 N NaOH solutions and find its pH. We know that its
pH is 12

ii) Now take 1 ml of 0.01 N NaOH in a 100 ml cylinder and dilute to

100 ml with distilled water. It becomes 10-4 N NaOH. Find its pH. We
know that its pH is 10.

3. Salt solutions:
i) Take few crystals of NaCl salt in a test tube, dissolve in few ml of
distilled water and test the pH. We know that its pH is 7.

ii) Take a few crystals of ammonium chloride, NH4Cl salt, dissolve in

few ml of distilled water and test the pH. We know, on the basis of
nature of salt, its pH is less than 7 ie acidic in nature.

iii) Take a few crystals of sodium acetate, CH3COONa salt, dissolve in

few ml of distilled water and test the pH. We know, on the basis of
nature of salt, its pH is more than 7 ie basic in nature.

B) Use of skill learnt:

4) Testing of fruit juices: Test different fruit juices and report their
pH. If juices are dark coloured, add 2 drops of universal indicator
instead of one drop, to subside the interference. Test at least four
seasonal fruits available like sweet lime, orange, water melon, melon,
apple, chiku, mango, grapes, papaya, banna, custard apple, pine
apple etc.

Observation Table:

No. Material pH Nature

1 0.01 N HCl 2 Acidic
2 0.0001 N HCl 4 Acidic
3 0.01 N NaOH 12 Basic
4 0.0001 N NaOH 10 Basic
5 NaCl 7 Neutral
6 NH4Cl
7 CH3COONa
8 Fruit (name)
9 Fruit (name)
10 Fruit (name)
11 Fruit (name)
 EXPERIMENT No. 5
COMPARISON OF PH OF STRONG ACID AND WEAK ACID
HAVING SAME CONCENTRATION.

Theory:
The degree of ionization of strong acid is more than that of weak
acid. Therefore even if their concentrations are same their pH would
not be same. Strong acid will have more [H+] ions ie less pH as
compared to weak acid having same concentration.

Aim: To compare the pH of solutions of strong acid with that of

weak acid having the same concentration.

Requirements: 0.01 N HCl, 0.01 N CH3COOH, 0.0001 N HCl, 0.0001

N CH3COOH, universal indicator, test tube, test tube stand, glass rod,
100 ml measuring cylinder.

Procedure:
1) Rinse test tube, glass rod and measuring cylinder with the distilled
water every time.

2) Take 2 ml of 0.01 N HCl in one test tube and 2 ml of 0.01 N

CH3COOH in another test tube.

3) Add 2 drops of universal indicator in each of these solutions and

shake. The solutions impart certain colour.

4) Match the colour of these solutions with that given on colour chart
and record the pH.

5) Similarly take 2 ml 0.0001 N HCl solution in one test tube and 2 ml

0.0001 N CH3COOH in another test tube. Add 2 drops of universal
indicator in each of these solutions, shake and record the pH after
matching with the colour chart.

6) Now take 1 ml 0.0001 N HCl with measuring pipette in a

measuring cylinder (10 ml capacity) and dilute to 10 ml with distilled
water. This gives 10-5 N HCl solution.

7) Take 2 ml of this 10-5 N HCl solution in a test tube and discard the
remaining 8 ml of it. Add 2 drops of universal indicator, shake, and
record the pH after matching with the colour chart.
8) In the same way 1 ml 0.0001 ml N CH3COOH with measuring
pipette in a measuring cylinder (10 ml capacity) and dilute to 10 ml
with distilled water. This gives 10-5 N CH3COOH solution.

9) Take 2 ml of this 10-5 N CH3COOH solution in a test tube and

discard the remaining 8 ml of it. Add 2 drops of universal indicator,
shake, and record the pH after matching with the colour chart.

Observation Table:

No. Acids pH
1 Strong acid 0.01 N HCl
Weak acid 0.01 N CH3COOH
2 Strong acid 0.0001 N HCl
Weak acid 0.0001 N CH3COOH
3 Strong acid 10-5 N HCl
Weak acid 10-5 N CH3COOH

Conclusion: pH of strong acid HCl is less than weak acid CH3COOH

having same concentration. This is because the degree of ionization of
strong acid (eg HCl) is mote than that of weak acid (eg CH3COOH).
 EXPERIMENT No. 6
THE pH CHANGE DUE TO COMMON ION EFFECT
RELATED TO WEAK ACIDS AND WEAK BASES

Theory:
The common ion effect is the shifting of equilibrium of weak acid
(or weak base) by the addition of strong electrolyte having one ion
common with the weak acid (or weak base).

The equilibrium of weak acid gets shifted to left when some

electrolyte having common ion is added. This results in decrease in
[H+] ion concentration and increase in pH. eg

CH3COOH
CH3COO- + H+
CH3COONa
CH3COO- + Na+

Similarly the equilibrium of weak base gets shifted to left when some
electrolyte having common ion is added. This results in decrease in
[OH] ion concentration and increase in pOH or decrease in pH. eg

NH4OH
NH4+ + OH-

NH4Cl
NH4+ + Cl-

Aim: To study the changes in pH of weak acid under the

influence of common ion effect.

Requirement: 0.2 N Acetic acid, 0.2 N sodium acetate, 2 N sodium,

acetate, 0.2 N NH4OH, 0.2 N NH4Cl, 2N NH4Cl, universal indicator,
measuring pipette, test tube, test tube stand etc.

Procedure: Part-I: Effect of common ion on weak acid, CH3COOH

1) Take three test tubes, rinse with distilled water and mark them as
T-1, T-2 and T-3.

2) In T-1 take 1 ml of 0.2 N CH3COOH + 1 ml H2O. Add 1 drop of

universal indicator, record the pH after matching with colour chart.

3) In T-2 take 1 ml 0.2 N CH3COOH + 1 ml 0.2 N CH3COONa. Add 1

drop of universal indictor, record the pH after matching with colour
chart.

4) In a test tube take 1 ml 0.2 N CH3COOH + 10 ml 2 N CH3COONa.

Out of these 11 ml solution, take 2 ml in T-3. Add 1 drop of universal
indicator, record the pH after matching with colour chart.
Part-II: Effect of common ion on weak base, NH4OH.

1) Take three test tubes, rinse with distilled water and mark them as
T-1, T-2 and T-3.

2) In T-1 take 1 ml of 0.2 N NH4OH + 1 ml H2O. Add 1 drop of

universal indicator, record the pH after matching with colour chart.

3) In T-2 take 1 ml of 0.2 N NH4OH + 1 ml 0.2 N NH4Cl. Add 1 drop of

universal indicator, record the pH after matching with colour chart.

4) In a test tube take 1 ml 0.2 N NH4OH + 10 ml N NH4Cl. Out of

these 11 ml solution, take 2 ml in T-3. Add 1 drop of universal
indicator, record the pH after matching with colour chart,

Observation Table:
Part-I: Effect of common ion on weak acid, CH3COONa.

No. Test Colour pH Conc. Of Remark

tube CH3COONa
1 T-1 Zero No common ion
effect
2 T-2 Equal to pH increased,
CH3COOH common ion effect
observed.
3 T-3 100 times more pH increased,
than CH3COOH common ion effect
further observed.
Observation Table:
Part-I: Effect of common ion on weak base, NH4OH.

No. Test Colour pH Conc. Of Remark

tube NH4OH
1 T-1 Zero No common ion
effect
2 T-2 Equal to NH4OH pH decreased,
common ion effect
observed.
3 T-3 100 times more pH decreased,
than NH4OH common ion effect
further observed.
 EXPERIMENT No. 7
PREPARATION OF STANTARD SOLUTION OF OXALIC
ACID

Theory: In volumetric analysis ie titration, to know the strength

(concentration) of unknown solution we require a solution of known
concentration. The solution of known concentration is called as
‘standard solution’.

Aim: To prepare a standard solution of oxalic acid. (Say 100 ml

0.1 N)

Requirement: Crystalline oxalic acid H2C2O4.2H2O, distilled water,

100 ml volumetric flask, watch glass, glass rod, 250 ml beaker etc.

Procedure:
1) Weight empty clean dry watch glass.

2) Place the crystals of oxalic acid on the watch glass and weigh again
so as to get 0.63 g substance.

3) Transfer the weighed oxalic acid to a beaker.

4) Pour distilled water over the watch glass to transfer all the crystals
into beaker.

5) Dissolve the substance completely in distilled water, taking care

that the volume should not exceed 100 ml.

6) Transfer the solution from beaker to 100 ml volumetric flask and

dilute very carefully to 100 ml mark. Stopper the flask and shake; it
gives standard solution of oxalic acid having concentration 0.1 N and
volume 100 ml.

Calculation:
1) Molecular weight of crystalline oxalic acid H2C2O4.2 H2O = 63 g.

2) Thus 63 g oxalic acid dissolved to final volume 1 dm3 would be 1 N

solution.

3) ... 6.3 g oxalic acid dissolved to final volume 1 dm3 would be 0.1 N
solution.

4) 63 g oxalic acid dissolved to final volume 100 ml would be 0.1 N

solution.
Observation:
1) Weight of empty watch glass = W1=……g

2) Weight of watch glass + oxalic acid = W2=……g

3) Weight of oxalic acid = W2 - W1=……g

 EXPERIMENT No. 8
VOLUMETRIC ESTIMATION OF SODIUM HYDROXOIDE
BY STANDARD SOLUTION OF OXALIC ACID

Aim: To determine the strength in normal terms and gram per

dm3 of sodium hydroxide by using standard solution of oxalic
acid.

Given: 0.1 N H2C2O4, Oxalic acid.

Requirement:
Burette, 10 ml pipette, conical flask, NaOH, H2C2O4.2 H2O,
phenolphthalein.

Procedure:
1) Wash burette, pipette and conical flask with water.

2) Rinse the burette with NaOH solution and fill with it up to zero
level after removing air bubbles if present.

3) Rinse the pipette with oxalic acid. Pipette out 10 ml of the oxalic
acid in the conical flask.

4) Add two drops of phenolphthalein indicator into conical flask,

Titrate slowly against NaOH solution with constant shaking till pink
colour is just obtained. Record the reading. Take three readings. All
the readings must be same or nearly same.

Equation:

H2C2O4 + 2NaOH  Na2C2O4 + 2 H2O

Observation: Given 0.1N H2C2O4

No. Burette Pipette Mean Indicator End Point

NaOH ml H2C2O4 burette
ml reading
1 -- 10 ----- = V1 Phenolphthalein Colourless
2 -- 10 to pink
3 --- 10
Calculation:
(i) NaOH : H2C2O4

N1V1 = N 2 V2

0.1 x 10
N1 = --------------
V1

... NaOH = -----------N

(ii) Strength of NaOH solution = N x Eq. wt. of NaOH

= N x 40

= ----- g dm-3

Result:
1) Normally of NaOH Soln. = ------------ N

2) Strength of NaOH soln. = ------------- g dm-3

 EXPERIMENT No. 9
QUALITATIVE ANALYSIS OF INORGANIC COMPOUND

Qualitative analysis of inorganic compound involves detection of one

‘Basic’ and ‘Acidic’ radical. It is carried out in three steps.
A) Preliminary Examination:
B) Detection of Basic Radical (Cation):
C) Detection of Acidic Radical (anion):

A) PRELIMINARY EXAMINATION:

Test Observation Inference

1) Colour: a) Colourless Ca2+, Pb2+, NH4+,
Al3+, Zn2+
b) Blue Cu2
c) Green Ni2+
d) Pink Co2+
2) Nature: a) Crystalline Soluble salts
b) Hygroscopic CaCl2, Ca(NO3)2,
(moist) Cu(NO3)2
3) Dry Test: a) Decrepitation Pb(NO3)2
Heat a little (crackling noise)
substance in b) Fusion Ca(NO3)2, Pb(NO3)2
a clean dry c) Condensation of Salts containing
test tube. water on cooler part water of
of test tube crystallization
d) White sublimation NH4+
e) Brown fumes NO3-, Br-
f) Violet fumes I-
g) Colour of the
residue left
Yellow Pb2+
White Ca2+
Coloured mass Cu2+, Ni-2+,Co2+
4) NaOH Test: Smell of NH3 NH4+
Sus. + dil. NH3 gas turns moist
NaOH, boil turmeric paper brown
(do not touch the
paper with mouth of
test tube)

5) Dry Test for

Acidic Redical:
i) Dil. H2SO4 Test. a) Effervescence Ca32-
Sub. + dil. H2So4
b) Light brown gas NO2-
ii) Conc. H2SO4
Test. a) Brown fumes NO3-, Br-
(Take cautiously)
Sub.+ Conc. H2So4 b) Violet fumes I-

c) Yellowish green gas Cl-

iii) Phosphate
test: Yellow ppt, soluble in PO43-
Sub.+ Conc. HNO3 NaOH
+

Ammonium
molybadate

B) DETECTION OF BASIC RADICAL:

PREPARATION OF SOLUTION:
Take ¼ spoon substance + 2 test tube distilled water, stir, heat if
necessary. Filter only if solutions is turbid ie not clear. Use it as
original solution, (O.S.)

DETECTION GROUP: (Gr. I, II, IIIA, III B, IV, V, VI)

Test Observation Inference
Test for Gr. I
O.S. + dil. HCl a) ppt obtained a) Gr. I Present
b) No ppt b) Gr. I Absent
Test for Gr. II
O.S. + dil. HCl, warm + H2S a) ppt obtained a) Gr. II Present
b) No ppt b) Gr. II Absent
Test for Gr. III A
O.S. + NH4Cl + NH4OH a) ppt obtained a) Gr. III A Present
b) No ppt b) Gr. III A Absent
Test for Gr. III B
O.S. + NH4Cl + NH4OH + a) ppt obtained a) Gr. III B Present
H2S b) No ppt b) Gr. III B Absent
Test for Gr. IV
O.S. + NH4Cl + NH4OH + a) ppt obtained a) Gr. IV Present
(NH4)CO3 b) No ppt b) Gr. IV Absent
Test for Gr. V
O.S. + NH4Cl + NH4OH + a) ppt obtained a) Gr. V Present
Na2HPO4 b) No ppt b) Gr. V Absent

Test for Gr. VI

No particular test a) If no ppt to Gr. a) Gr.VI must be
 vi Present

Note: After detecting the Group find the ‘Basic Radical’ in the group
detected only. Once basic radical is detected, confirm it by taking
Confirmatory Test (C.T.)
GROUP – I
If Gr.I is present, then the basic radical is Pb2+
Confirmatory Test (C.T.):

Test Observation Inference

2+
Pb
1) O.S. + Kl Yellow ppt Pb2+ Confirmed
2) O.S. + dil. H2SO4 White ppt Pb2+ Confirmed
3) O.S. + dil. K2CrO4 Yellow ppt Pb2+ Confirmed

GROUP – II

Radicals of Gr.II: Pb2+, Cu2+ any one radical is present.

Test Observation Inference

O.S. + dil. H2SO4 a) White ppt Pb2+ Present
b) No ppt, and O.S. Cu Present
2+

blue

Confirmatory Test (C.T.):

Test Observation Inference

2+
Pb
1) O.S. + Kl Yellow ppt Pb2+ Confirmed
2) O.S. + dil. H2SO4 White ppt Pb2+ Confirmed
3) O.S. + dil. K2CrO4 Yellow ppt Pb2+ Confirmed
Cu2+
1) O.S. + Kl Brown colour Cu2+ Confirmed
(with white ppt)
2) ) O.S. + dil. K4[Fe(CN)6] Reddish brown ppt Cu2+ Confirmed
 GROUP – III A
Radicals of Gr. III A: Al3+, Fe3+ any one radical is present.

Test Observation Inference

O.S. + NH4Cl + a) Reddish brown ppt Fe3+ Present
NH4OH
b) White gelatinous Al3+ Present
ppt
Confirmatory Test (C.T.):

Test Observation Inference

3+
Fe
1) O.S. + NH4CNS Blood red colour Fe3+ Confirmed

2) O.S. + K4[Fe(CN)6] Blue colour Fe3+ Confirmed

Al3+
1) O.S. + NaOH White gelatinous ppt Al3+ Confirmed

2) ) O.S. + Na2HPO4 White ppt Al3+ Confirmed

GROUP – III B
Radicals of Gr. III B: Ni2+, Co2+, Zn2+, Mn2+ any one radical is present.

Test Observation Inference

O.S. + NH4Cl + a) White ppt Zn2+ Present
NH4OH + H2S b) Buff ppt Mn Present
2+

c) Black ppt Na2+ or Co2+ Present

O.S. Colour a) Green Ni2+ Present
b) Pink Co2+ Present

Confirmatory Test (C.T.):

Test Observation Inference
2+
Zn
1) O.S. + K4[Fe(CN)6] White ppt Zn2+ Confirmed
2) O.S. + NH4OH White ppt soluble in Zn2+ Confirmed
excess of NaOH
2+
Ni
1) O.S. + Dimethyl Red ppt Ni2+ Confirmed
glyoxime + NH4OH
2) O.S. + Na2HPO4 Pale green ppt, Ni2+ Confirmed
soluble in excess of
NH4OH
2+
Co
1) O.S. + NH4CNS Deep blue colour Co2+ Confirmed
2) O.S. + NH4OH Blue ppt Co2+ Confirmed
Mn2+
1) O.S. + NaOH + Br2 Black or brown ppt Mn2+ Confirmed
water
2) O.S. + PbO2 + Pink colouration Mn2+ Confirmed
Conc.HNO3, + boil +
H2O

GROUP – IV
Radicals of Gr. IV: Ca2+, Sr2+,
Ba2+ any one radical is present.

Test Observation Inference

2+
Ca
O.S. + CaSo4 a) White ppt Ba2+ Present
immediately obtained
b) White ppt on Sr2+ Present
warming and waiting
c) No ppt even on Ca2+ Present
warming

Confirmatory Test (C.T.):

Test Observation Inference

2+
Ca
1) O.S. + (NH4)2C2O4 White ppt Ca2+ Confirmed
ammonium oxalate
2) O.S. + NaOH White ppt soluble in Ca2+ Confirmed
excess of NaOH

Ni2+
1) O.S. + Dimethyl Red ppt Ni2+ Confirmed
glyoxime + NH4OH
2) O.S. + NH4OH Pale green ppt, Ni2+ Confirmed
soluble in excess of
NH4OH

Co2+
1) O.S. + NH4CNS Deep blue colour Co2+ Confirmed
2) O.S. + NH4OH Blue ppt Co2+ Confirmed

Mn2+
1) O.S. + NH4OH + Black or brown ppt Mn2+ Confirmed
Br2 water Pink colouration Mn2+ Confirmed
2) O.S. + Pbo2 +
HNO3, + boil + H2O

GROUP – V
If Gr. V is present, then the basic radical is Mg2+.
Confirmatory Test (C.T.):

Test Observation Inference

2+
Mg
1) O.S. + NaOH a) White ppt Mg2+ Confirmed

2) O.S. + Hypoiodide b) Reddish Brown ppt Mg2+ Confirmed

soln *.

* Hypoiodide soln.:
½ ml NaOH + ½ KI +
I2 till solution
becomes yellow

GROUP – VI

If Gr.VI is present, then the basic radical is NH4+

Confirmatory Test (C.T.):

Test Observation Inference

+
NH 4
1) O.S. + NaOH, boil Smell of NH3, turns NH4+ Confirmed
moist turmeric paper
brown.
2) O.S. + Nessler’s Brown ppt NH4+ Confirmed
reagent *

[*Nessler’s reagent:
3 drops HgCl2 + Kl
with shaking till
scarlet red ppt
dissolves in Kl +
equal volume of
NaOH]
C) DETECTION OF ACIDIC RADICAL:

Hint: Take test in serial order. Once ‘Acidic Radical’ is detected do not
take further test. Directly take the C.T. of acidic radical detected.

Test Observation Inference

1) O.S. + dil. HCl Effervescence CO32- present
2) O.S. + FeSO4 + Brown colour NO3- present
Conc.H2SO4 shake
3) O.S. + HgCl2 Scarlet red ppt I- present
4) O.S. + Conc.H2SO4 + Yellowish brown Br- present
Starch soln. (freshly colour
prepared)
5) O.S. + Conc.HNO3 + Yellow ppt PO43- present
Ammonium molybdate
6) O.S. + AgNO3 White ppt, soluble Cl- present
in NH4OH
7) O.S. + BaCl2 or Ba(NO3)2 White ppt, insoluble SO42-present
in dil. HCl
8) O.S. + Kl + Starch soln. Dark blue colour NO2- present
(freshly prepared)
9) O.S. + 1 drop v. dilute Pink colour C2O42- present
KMnO4 warm. (1 drop disappears
KMnO4 + large H2O, Use it
as v.dilute KMnO4)
10) O.S. + FeCl3 Reddish colour CH3COO- present

Confirmatory Test (C.T.):

Test Observation Inference
-
1) Cl
i) O.S. + AgNO3 White ppt, soluble Cl- Confirmed
in NH4OH
ii) O.S. + lead acetate White ppt Cl- Confirmed
(CH3COO)2Pb
2) Br-
i) O.S. + AgNO3 Pale yellowish ppt Br- Confirmed

ii) O.S. + MnO2 + Brown fumes Br- Confirmed

conc.H2SO4, heat
3) I-
i) O.S. + CuSO4 Brown colour with I- Confirmed
white ppt
ii) O.S. + HgCl2 Scarlet red ppt I- Confirmed
4) CO32-
i) O.S. + dil. H2SO4 Effervescence CO32- Confirmed
CO32- Confirmed
ii) O.S. + dil. HNO3 Effervescence

5) SO42-
i) O.S. + (CH3COO)2Pb lead White ppt SO42- Confirmed
acetate SO42- Confirmed
White ppt, insoluble
ii) O.S. + BaCl2 or Ba(NO3)2 in HCl
6) NO3-
i) Ring Test: O.S. + FeSO4 + Brown ting at the NO3- Confirmed
conc. H2SO4 slowly from bottom
sides without shaking the
tube NO3- Confirmed
Brown fumes
ii) O.S. + Cu filling conc.
H2SO4, heat
7) NO2-
i) O.S. 1 drop on filter paper Dark blue spot on NO2- Confirmed
+ 1 drop KI + starch filter paper
NO2- Confirmed
ii) O.S. + FeSO4 + dil. Brown colour
H2SO4, shake
8) PO43-
i) O.S. + AgNO3 White ppt PO43- Confirmed
PO43- Confirmed
ii) O.S. + NaOH + BaCl2 White ppt
9) C2O42-
i) O.S. + CaCl2 White ppt C2O42-Confirmed
C2O42-
ii) O.S. + BaCl2 or Ba(NH3)2 White ppt Confirmed
10) CH3 COO- Reddish colour or CH3 COO-
i) O.S. + FeCl3 ppt Confirmed
(To this + dil. HCl 
red colour
ii) O.S. + conc. H2SO4, heat disappears) CH3 COO-
strongly till almost dryness Confirmed
Black clour

Result: The given compound contains:

1) Basic radical………… 2) Acidic radical …………

 EXPERIMENT No. 10
QUALITATIVE ANALYSIS FOR ORGANIC COMPOUND

DETECTION OF NITROGEN, SULPHUR, CHLORINE, BROMINE

AND IODINE IN AN ORGANIC COMPOUND

Caution: ☺ Sodium metal is very active, hence preserved under

Kerosene. Never bring it in contact with water.

Part – I: Preparation of Sodium Extract, (S.E.)

1) Take about two test tube of distilled water in porcelain dish.

2) Take out sodium metal from kerosene, place on filter paper. Cut
the sodium metal with knife into few small pieces. Take 2 or 3 fusion
tube. In each tube take 1 – 2 pieces of sodium metal.

3) Heat gently the fusion tube to melt the sodium metal. Then add the
organic compound and heat again very strongly to red hot, plunge
into water taken in the porcelain dish and cover immediately the dish
with asbestos sheet to avoid splashing. Repeat the same procedure
with remaining fusion tubes.

4) Boil the solution for few minutes along with broken fusion tubes.
Filter the solution and collect the filtrate into small beaker. It is called
as ‘Sodium Extract’ (S.E.)

5) The elements C, N, S and X (X = Cl, Br, I halogens) gets converted

into sodium compounds as.

i) C + N + Na  NaCN
ii) S + 2 Na  Na2S
iii) X + Na  NaX

Part –II: Detection of N, S, halogens in Sodium Extract (S.E.)

No. Test Observation Inference

1 Test for Nitrogen, N:
S.E. 2 ml + 2 drops a) Green or Blue colour N Present
NaOH + 1-2 ml FeSO4, b) No green or Blue N Absent
boil + dil. H2SO4 colour
2 Test for Sulphur, S:
S.E.1- 2 ml + 1 drops a) Violet or purple colour S Present
sodium nitroprusside b) No violet or purple S Absent
colour
3 Test for Iodine, I:
S.E. 1 ml + HgCl2 a) Scarlet red ppt I Present
b) No Scarlet red ppt I Absent
4 Test for Bromine, Br:
S.E. 1 ml + Conc.+ a) Yellowish brown Br Present
H2SO4 + Starch colour Br Absent
b) No Yellow brown
colour
5 Test for Chlorine, Cl:
S.E. 1 ml + AgNO3 a)White ppt soluble in Cl Present
NH4 OH
b) No White ppt Cl Absent

Result: The given organic compound contains ……………

Element/s.