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Qualitative Analysis

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0% found this document useful (0 votes)
33 views7 pages

Qualitative Analysis

Uploaded by

Pravvin J
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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NAME:

VEL’S PUBLIC SCHOOL, SANKARANKOVIL


Practical Materials – Chemistry – Class XI & XII

Inorganic salt analysis - General Procedure

S.No EXPERIMENT OBSERVATION INFERENCE

1. a. Colour:
Colour of the salt is noted Colourless Absence of Copper and Iron salts.

b. Appearance:
Appearance of the salt is noted Crystalline May be Sulphate, nitrate, or chloride.

Powdery May be carbonate or sulphide. (except


ammonium carbonate)

2. Solubility: Soluble May be Sulphate, nitrate or chloride.


Add distilled water to the salt
May be carbonate or sulphide.
Insoluble (except ammonium carbonate)

3. Action of heat :
Colourless, odourless gas, which turns May be carbonate
Take a small quantity of the salt in a dry lime water milky, evolves
test tube, heat it gently.
Decripitation (cracking noise) occurs; May be nitrate
Reddish brown gas evolves

Salt sublimes. Colourless, pungent


smelling gas giving dense white fumes May be ammonium salt
with a glass rod dipped in con. HCl
evolves

The salt turns yellow when hot, and May be Zinc salt
white when cold.
Absence of carbonate, nitrate,
No characteristic change
ammonium and zinc.

4. Flame test:
Brick red colour flame Presence of calcium
Add a drop of Conc. HCl to a small amount
of salt in watch glass made into paste. Small Grassy green colour flame Presence of Barium
amount of paste is introduced into non
No characteristic coloured flame Absence of calcium and Barium
luminous part of Bunsen Flame with a help
of glass rod

5. Ash test: Blue ash Presence of aluminium


A filter paper is soaked into the mixture of Green ash Presence of Zinc
salt + con. HNO3 + cobalt nitrate solution
and is burnt
Pink ash Presence of magnesium

No characteristic coloured ash Absence of aluminium, Zinc and


magnesium

1
IDENTIFICATION OF ACIDIC RADICALS

6. Action of dil. HCl: Colourless, odourless gas evolves with Carbonate is confirmed
brisk effervescence turning lime water
To a small amount of salt ,dil HCl acid is milky.
added
Colourless, rotten egg smelling gas
Sulphide is confirmed
turning lead acetate paper black
evolves.

Absence of carbonate and


No characteristic gas is evolved
sulphide

7. Action of Copper turnings: Reddish brown gas evolves Presence of nitrate is confirmed
A small amount of the salt is heated with
copper turnings and con. H2SO4 No reddish brown gas Absence of nitrate

8. Action of NaOH: Pungent smelling gas giving, dense Presence of ammonium salt
white fumes with a glass rod dipped in
A small amount of salt is heated with con. HCl evolves.
sodium hydroxide solution
No pungent smelling gas Absence of ammonium salt

9. Chromyl chloride test:


Red orange vapours evolved which Chloride is confirmed
To a small amount of the salt a pinch of when passed through lead acetate
solution give a yellow precipitate
solid potassium dichromate is added and
heated with a few drops of Con.H2SO4 No red orange vapours evolved Absence of chloride

Preparation of sodium carbonate extract:

Salt + twice the amount of sodium carbonate + 20 ml distilled water, boiled, cooled and filtered.
The filtrate is called sodium carbonate extract.

10. Silver nitrate test: A curdy white precipitate completely Presence of chloride
soluble in excess of ammonium
Sodium carbonate extract + dil. nitric acid hydroxide is obtained.
(till the effervescence ceases) and add 2 ml Presence of sulphide
A black precipitate is obtained
of silver nitrate solution is added
No characteristic precipitate is obtained Absence of chloride and sulphide

11. Lead acetate test: A white precipitate soluble in Presence of sulphate


ammonium acetate and sodium
To a few drops of Sodium carbonate extract hydroxide mixture is obtained.
add dil. acetic acid (till the effervescence Presence of sulphide
A black precipitate soluble in hot dil.
ceases) and lead acetate solution is added nitric acid is obtained.

No characteristic precipitate is obtained. Absence of sulphate and sulphide.

12. Barium Chloride test: A white precipitate insoluble in con. Sulphate is confirmed
HCl is obtained
Sodium carbonate extract + dil. HCl (till the
effervescence ceases) + Barium Chloride is No white precipitate is obtained Absence of sulphate
added

2
13. Brown ring test:

Sodium carbonate extract + dil. H2SO4 (till Brown ring is formed at the junction of Nitrate is confirmed
two layers.
the effervescence ceases) + freshly prepared
FeSO4 + con. H2SO4 is added is added in
No brown ring is formed Absence of nitrate.
drops along the inner side of the test tube.

Confirmatory Tests for Acetate:

14. To a little of the salt sol., add one or two drops A deep red colourisation Presence of acetate
of neutral ferric chloride solution

15. A mixture of salt and ethanol is heated with Pleasant fruity smell Acetate anion is confirmed
little con. H2SO4 in a dry test tube. It is
poured into excess of water

IDENTIFICATION OF BASIC RADICALS


Preparation of Original Solution:

Crystalline Salt : The original solution is prepared by dissolving the salt in distilled water.

Powder Salt : The original solution is prepared by dissolving the salt in dil. HNO3.

Zero Group

16 To a few drops of the Original solution Reddish brown precipitate is obtained. Ammonium is confirmed

Nessler’s reagent and NaOH solution is


No reddish brown precipitate is obtained Absence of Ammonium
added
Group separation

17. White precipitate soluble when boiled Presence of first group (Lead)
To a few drops of the Original solution 2 ml
with water is obtained
of dil. HCl is added
No white precipitate is obtained Absence of first group (Lead)

18. To a few drops of Original solution 1 ml of Gelatinous white precipitate is obtained Presence of III group (Aluminium)

NH4Cl and 2 ml of NH4OH are added


No Gelatinous white precipitate is Absence of III group (Aluminium)
obtained

19. To a few drops of Original solution + NH4Cl Dirty white precipitate is obtained Presence of IV group (Zinc)

and NH4OH and H2S are added No Dirty white precipitate is obtained. Absence of IV group (Zinc)

20. To a few drops of Original solution 1 ml of White precipitate is obtained Presence of V group
(Calcium or Barium)
NH4 Cl and NH4 OH + ammonium
carbonate solutions are added Absence of V group
No white precipitate is obtained
(Calcium or Barium)

21. To a few drops of Original Solution 2 ml of White precipitate is obtained Presence of VI group ( Magnesium)
NH4Cl + NH4OH + disodium hydrogen
No white precipitate is obtained Absence of VI group (Magnesium)
phosphate are added

3
Confirmatory tests for Basic Radicals:

22. Lead (I group) : Yellow Precipitate soluble in Hot water


and reappears as golden yellow spangles Lead is confirmed
To a few drops of Original solution added KI
on cooling is obtained
solution

23. Aluminium (III group) :


A bright red lake is obtained Aluminium is confirmed
To a few drops of Original solution added
ammonium hydroxide and aluminon reagent

24. Zinc (IV group):


White precipitate soluble in excess of Zinc is confirmed
To a few drops of Original solution added
NaOH but insoluble in dilute acids is
potassium ferro cyanide solution obtained

25. Barium (V group):


Yellow precipitate is obtained Barium is confirmed
To a few drops of Original solution added
potassium chromate

26. Calcium (V group):

To a few drops of Original solution added White precipitate insoluble in acetic acid Calcium is confirmed
Ammonium hydroxide and ammonium is obtained
oxalate solutions

27. Magnesium (VI group):

To a few drops of Original solution added Blue precipitate is obtained Magnesium is confirmed
magneson reagent

Result:

The given Simple salt contains i) Acid radical: __________________

ii) Basic radical: __________________

The given simple salt is _______________________________________

4
Organic Sample Analysis - General Procedure
Preliminary Tests

EXPERIMENT OBSERVATION INFERENCE

Colour and appearance is noted Colourless liquid Absence of phenol & aniline

Brown liquid May be phenol or aniline

Odour is noted Carbolic smell May be phenol

Bitter almond smell Maybe an aldehyde

No characteristic smell Absence of phenol, aniline, aldehyde.

Solubility is noted:

1. Water Partially soluble in cold water but soluble in May be an acid or alcohol (fully soluble)
hot water

No characteristic observation Absence of alcohol and acid

2. dil. HCl Soluble Presence of aniline

Insoluble Absence of aniline

3. NaOH Soluble May be acid

Insoluble May not be acid or phenol

4. Red litmus paper test Changes to blue Presence of aniline

No characteristic observation Absence of aniline

5. Blue litmus paper test Changes to red May be acid

No characteristic observation May not be acid

TEST TO FIND OUT WHETHER THE COMPOUND IS

ALIPHATIC / AROMATIC

Ignition test:
Burns with non-smoky flame The compound is aliphatic
A little of the substance is burnt on a pocket
spatula Burns with smoky flame The compound is aromatic

Nitration test:

To a mixture of 1ml of con. HNO3 and 1ml of Yellow precipitate/solution The compound is aromatic
con. H2SO4 in a test tube, a little of compound
is added and heated in a boiling water bath for
No Yellow precipitate / solution The compound is aliphatic
15min and then pour it into cold water taken
in a beaker.

5
TEST TO FIND OUT WHETHER THE COMPOUND IS SATURATED
OR UNSATURATED

1. A little of the compound is shaken with Immediate decolourisation The compound may be unsaturated
water and very dil. KMnO4 is added drop wise
No decolourisation The compound may be saturated

2. A Little of the compound is shaken with Decolourisation The Compound may be unsaturated
water and Br2 water is added drop wise
No decolourisation The compound may be saturated

DETECTION OF FUNCTIONAL GROUP

1. To a little of NaHCO3 salt, a little of the Brisk effervescence Presence of carboxylic acid
compound is added
No observation Absence of carboxylic acid

2. To an aq. Or alc. Solution of the compound Violet colour Presence of phenol


add a few drops of Neutral FeCl3

No observation Absence of phenol

3. To a little of Borche’s reagent, a little of the Orange/Yellow precipitate Presence of aldehyde / ketone
compound is added and shaken
No observation Absence of aldehyde / ketone

4. To a little of Schiff’s reagent, a little of the Pink colour developed immediately Presence of aldehyde
compound is added
Pink colour developed after some time Presence of ketone

No observation Absence of aldehyde/ketone

CONFIRMATORY TESTS

CARBOXYLIC ACID

1. A little of the substance is dissolved in


excess NaOH and boiled until there is no smell
A brown precipitate formed Presence of Carboxylic acid is confirmed
of NH3. Cool the mixture and add few drops of
FeCl3

2. A little of the compound is mixed with


ethanol and few drops of con. H2SO4 and A pleasant fruity smell Presence of Carboxylic acid is confirmed
poured into water taken in a beaker

6
KETONES & ALDEHYDE
No black precipitate or silver mirror Presence of Ketone is confirmed
1. Tollen’s test :

To little of Tollen’s reagent a little of Black precipitate formed and then a bright Presence of aldehyde is confirmed
compound is added and heated in boiling silver mirror
water

2. To a little of the given compound finely


Appearance of violet colour which slowly Presence of ketone is confirmed
powdered m-dinitrobenzene and a little of
fades
NaOH solution is added and shaken

3. To a little of the compound NaOH sol. is


Pink Colour Presence of ketone is confirmed
added and shaken followed by sodium nitro
prusside.

4.Fehlings test:
To the mixture of Fehling A & B soln., few
Red precipitate Presence of aldehyde is confirmed
drops of the given compound is added and
warmed in a test tube in hot water bath.

PHENOLS

1. Liebermann’s nitoso reaction:

A few drops of the substance is mixed with


con. H2 SO4 and added with sodium nitrate and Red turns to blue colour Presence of phenol is confirmed
warmed gently for a minute and poured into
water taken in a beaker. Excess of NaOH is
added to the red solution in the beaker.

2. A few drops of substance is mixed with


phthalic anhydride in a test tube and added few Appearance of blue colour Presence of phenol is confirmed

drops of con H2SO4 heated , cooled and poured


into beaker containing dil. NaOH

Result:

The given organic compound is ______________________ (Aliphatic / aromatic, Saturated / Unsaturated, Ketone / Alcohol / Aldehyde /
Carboxylic acid, etc…)

COSMIC

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