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Scheme of Salt and Organic Analysis

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0% found this document useful (0 votes)
33 views9 pages

Scheme of Salt and Organic Analysis

Uploaded by

mohammed shaik
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Rules to be followed in the laboratory:

1. A student must have an observation notebook.


2. Always come prepared for the experiment. This will help you understand the
experiment better.
3. Always listen to the teacher's instruction and always note down the important
points and precautions
4. Thoroughly clean the apparatus after use.
5. Do only experiments assigned, unallotted experiments should not be done.
6. Be economical with reagents. Only a small quantity of reagents should be used. Excess use
of reagents not only leads to wastage but damages the environment by polluting water , soil
and air.
7. Handle glassware carefully and report any damage to the teacher.
8. Dispose chemicals into the zinc and allow water to run for some time by opening the tap.
9. In case of injury or accident, report it to the teacher.
10. Wash your hands with soap solution after completion of experiment.
Some important precautions
• Always wear a lab coat, eye protector, and gloves while working in chemistry laboratory.
• Should not touch corrosive chemicals by hand.
• Before using any chemical, read the label carefully.
• Do not put any object into the reagent bottle.
• Do not bring inflammable liquid near to the flame.
• Cracked apparatus should not be used for heating.
• Be careful while heating the test tube. The test tube should never point towards yourself or
your neighbours while heating or adding reagents.
• Do not heat beakers or china dishes directly on flame. Always make use of wire gauge.
• Be careful while smelling chemicals or vapors.
• Never apply more pressure on glass apparatus there is a chance of breakage. Be gentle.

SCHEME OFSALT ANALYSIS


S.N Experiment Observation Inference
o

I. PRELIMINARY EXAMINATION
1. Colour and appearance of the (a) White (a) Absence of Cu2+,Mn2+
salt is noted. (b) Blue (b) Presence of Cu2+
(c) Light pink (c) Presence of
manganese ion

2. To a little of the salt in the watch (a) Brick red (a) Presence of Ca2+
glass, add Con. HCl and make (b) Apple green (b) Presence of Ba2+
a paste . Introduce a little of this (c) No characteristic (c) Absence of Ca2+,,
paste into a non-luminous flame observation Ba2+,, Sr2+
using a glass rod and flame
colour is noted.
3. To a little of the salt add (a) Blue ash (a) Presence of Aluminium ion
Con. HNO3 and Cobalt (b) Green ash (b) Presence of Zinc ion
nitrate and boil .Dip a filter (c) pink ash (c) Presence of Magnesium
paper in this solution and burn to (d) No characteristic ion
ashes observation (d) Absence of Zinc,
Magnesium and Aluminium
ions.

II. IDENTIFICATION OF ANIONS


1 To a little salt add Dil. HCl (a) Brisk (a) Presence of Carbonate
effervescence
(b) no characteristic (c) Absence of
observation carbonate ion

2 A little salt is taken in a (a) Smell of Vinegar (a) Presence of


watch glass and rubbed with (b) No Characteristic acetate(CH3COO- ion)
Dil. H2SO4 observation (b) Absence of acetate

3 To a little salt add Conc. (a) Colourless (a) Presence of Cl- ion
H2SO4 Pungent gas is (b) Absence Chloride ion
evolved
(b) No characteristic
observation

A glass rod dipped in NH 4OH is Dense white fumes Presence of Chloride ion
shown in above formed gas

4 Above solution is heated (a) Plenty of brown (a) Presence of NO3-


strongly and a paper ball is gas is evolved (b) Absence of NO3-
dropped into it (b) No characteristic
observation

5 To a little salt solution add (a) White precipitate (a) Presence of SO42-
Dil. HCl and BaCl2 soluble in Con. (b) Absence of SO42-
HCl
(b) No characteristic
observation

III. CONFIRMATORY TEST FOR ANION

NOTE: ONCE THE PRESENCE OF ANION IS IDENTIFIED, PROCEED TO DO THE


CORRESPONDING CONFIRMATORY TEST:
1 CARBONATE: 1. Lime water turns milky. 1. Presence of carbonate
1. To a little of the salt add Dil. is confirmed.
HCl. The gas evolved is passed
through lime water which is
taken in another test tube
2. To a little salt solution a few
2. A white precipitate 2. Presence of carbonate
drops of BaCl2 is added.
soluble in excess NH4OH

2 ACETATE: 1. A red colour solution is Presence of Acetate


1. To a little salt solution add obtained. confirmed.
neutral Ferric Chloride
solution.
2. Take a small quantity of salt 2. Smell of vinegar. Presence of Acetate

in a watch glass . Mix it with confirmed.


solid oxalic acid and prepare a
paste with a few drops of water.

3 CHLORIDE: 1.White curdy precipitate Presence of Chloride is


1. To a little of the salt solution soluble in excess NH4OH. confirmed.
add Dil HNO3 and AgNO3
solution.
2.To salt solution add a few 2. Purple colour Presence of chloride
drops of dilute H2SO4 and boil decolourises. confirmed.
then add KMNO4 drop wise.

4 NITRATE: 1. A brown ring is formed Presence of Nitrate is


1. To a little salt solution equal at the junction of the two confirmed.
volume of freshly prepared layers.
FeSO4 is added to the test tube
through its side without shaking
add Con. H2SO4 is added to the
test tube through its sides
without shaking.
2. Copper chips test : To a little
salt solution, small quantity of 2. Dark brown fumes of Presence of Nitrate confirmed.
salt and Con. H2SO4 and nitrogen dioxide are
Copper chips are added. evolved

5 SULPHATE: A white precipitate soluble Presence of Sulphate is


To a little salt solution add in ammonium acetate is confirmed.
acetic acid and lead obtained
acetate.

ANALYSIS OF CATION:

IV. IDENTIFICATION OF GROUP OF CATION:


1 To a little of salt solution add (a) No precipitate (a) Presence of zero
Na2CO3 solution (b) White precipitate group (NH4+)
is formed (b) Absence of ammonium
ion.

2 To a little salt solution add (a) A white precipitate (a) Presence of group I
Dil. HCl (b) No white (b) Absence of group I
precipitate

3 To a little salt solution add Dil. (a) A black precipitate (a) Presence of group II
HCl and then pass H2S gas. (b) No precipitate (b) Absence of group II

4 To a little of the solution add (a) A white gelatinous (a) Presence of group III
solid NH4Cl and shake well add precipitate (b) Absence of group III
excess of NH4OH solution (b) No precipitate

5 To a little of salt solution add (a) A dirty white (a) Presence of Zinc

solid NH4Cl and then add precipitate (group IV)


NH4OH. Pass H2S through the (b) A flesh coloured (b) Presence of
above solution precipitate manganese (group VI)
(c) No precipitate (c) Absence of group IV

6 To a little of the salt solution add (a) White precipitate (a) Presence of group V
solid NH4 Cl followed by (b) No precipitate (Barium/Calcium)
NH4OH and (NH4)2CO3 (b) Absence of group V
solution. (Barium/Calcium)

7 To a little of the salt solution add (a) White precipitate (a) Presence of group VI,
solid NH4 Cl followed by excess magnesium ion
of NH4OH and disodium
hydrogen phosphate solutions
Scratch the inner side of the test
tube with a thin glass rod

V) CONFIRMATORY TESTS FOR CATIONS


1 Group Zero ( NH 4+ ) 1. A brown precipitate Presence of NH 4+ confirmed
1. Few drops of Nessler's
reagent is added to
the salt solution and
made alkaline with Presence of NH4+confirmed
2. Ammonia gas is
NaOH
evolved.
2. To solid salt add .
NaOH solution and
Dense White fumes
warm.A glass rod dipped
evolved
in Con.HCl is shown in the
above formed gas
2 Group-I ( Pb2+) 1. Yellow spangles 1. Presence of Lead ,
1. To a little salt solution KI disappear on ( Pb2+) is confirmed
solution is added. heating and
reappears as
golden spangles on
cooling

2. Yellow precipitate
2. To a little of salt solution 2. Presence of Lead
add acetic acid and (Pb2+) is confirmed
potassium chromate

4 GROUP III 1. Blue coloured ash .Presence of Al 3+confirmed


1. To a little of the salt formed.
solution add Conc.HNO3 and
Cobalt nitrate solution and
boil. A filter paper is dipped in
the solution and burn to
ashes
2. Blue precipitate floats
in colourless solution
2. To a little of salt solution
add 3-4 drops of blue litmus
solution and then add
NH4OH till a blue
colour develops

1 GROUP V 1. A yellow precipitate 1. Presence of Ba2+ ion is


confirmed.
1. To a little of the salt
solution add acetic acid
and potassium chromate
solution
2. To a little of salt solution
in a watch glass , add
2. Presence of Ba2+ ion is
Con.HCl and make a
2. Apple green confirmed.
paste. Introduce a little of
this paste into non coloured flame
luminous flame using a
glass rod and flame
colour is noted
(Note: If barium is
present no need to test Ca)
2 1. To a little of the solution 1. A white precipitate 1. Presence of Ca2+ ion is
add solid NH4Cl and then is formed. formed.
add NH4OH and
ammonium oxalate
solution
2. To a little of salt in a
watch glass , add
Con.HCl and make a 2. Brick red coloured 2. Presence of Ca2+ ion is
paste. Introduce a little of flame . formed.
this paste into non
luminous flame using a
glass rod and flame
colour is noted

GROUP VI (a) A pink ash (a) Presence of Mg2+ is


(a) To To a little of the salt confirmed.
solution add con.
HNO3
and Cobalt nitrate then
boil .Dip a filter paper in
this solution and burn it
(b) A white precipitate is (b) Presence of Mg2+ is
into ashes
formed. confirmed.
(b) To a little of the salt
solution NaOH solution
is added.
SCHEME FOR IDENTIFICATION OF FUNCTIONAL GROUP IN AN ORGANIC
COMPOUND
S. Experiment Observation Inference
No.

I. PRELIMINARY TESTS
1. Colour of the substance is noted Brown Presence of amines or phenols

Colourless Presence of aldehydes,


ketones, acids etc.,

2. Smell of substance is noted Fishy smell Presence of amines

Carbolic acid smell Presence of phenols

Smell of bitter and Presence of aldehyde


almond

3. A little of the substance is placed Red litmus turnsblue. Presence of amine


on a moist litmus paper.
Blue litmus turns red. Presence of acid or phenol.

II. IDENTIFICATION TESTS


1. Test with sodium bicarbonate Brisk effervescence Presence of carboxylic acid
solution:
To a little of the substance , add 1
ml of saturated sodium
bicarbonate( NaHCO3) solution.

2. Test with sodium hydroxide: The substance Presence of carboxylic acid


A little of substance is shaken dissolves and and phenol.
well, with NaOH solution reappears on adding
NaOH solution.

3. Test with dil. HCl The substance Presence of amine.


A little of the substance is dissolves and
shaken well with a few drops reappears on adding
of Dil. HCl. NaOH solution

4. Test with neutral ferric Formation of violet Presence of phenol


chloride solution: colour
To a little of the substance , add
1ml of neutral ferric chloride
solution
5. Borsche's reagent test:(2,4 DNP Formation of yellow Presence of aldehyde
Test) precipitate and ketone.
To a little of the substance , add

about 1 ml of borche's reagant


and shake well

6 Ceric ammonium nitrate test: Appearance of red Presence of alcoholic group


colour
To little of the solution add a few
drops of Ceric ammonium
nitrate reagent and shake well.

II. CONFIRMATORY TEST


1. Carboxylic acid- Esterification Pleasant fruity smell. Presence of carboxylic acid
test confirmed.
A little of substance is mixed
with about 1 ml of ethyl
alcohol and a few drops of Con.
H2SO4.
The mixture is warmed, cooled
and poured into cold water taken
in a beaker.

2. Phenol: To a little of the White precipitate Presence of phenol confirmed.


substance , add bromine
water and shake well.

3. Azo-Dye test: Formation of red Confirms the presence of


Test tube 1:Dissolve the dye amine
compound in 2 ml of Dil HCl in a
test tube.
Test tube 2: Prepare
aqueous solution of
Sodium nitrite. Test tube 3:
Dissolve Beta
Naphthol in Dil. NaOH.
Place three test tubes in an
ice bath.

Now add sodium nitrite solution


to test tube 1 and the resulting
solution to test tube 3

5 A little of the substance is shaken Presence of aldehyde


with two drops of schiff's confirmed.
reagent,
Pink colouration
6 Tollens test: A brown precipitate Presence of aldehyde
Take 1 ml of silver nitrate formed. confirmed.
solution in a test tube and add 4-5
ml of NaOH solution ,

To this precipitate add


Ammonium Hydroxide until it
A shining silver mirror
dissolves. To this add 3 or 4
formed
drops of given
substance and warm about
5 minutes

7 Sodium nitroprusside test: Appearance ofred colour Presence of ketonic group


Dissolve crystals of sodium confirmed.
nitroprusside in about 1 ml of
distilled water in a clean test tube
and then add drops of given
substance

Esterification test:
8.
A little of the substance is warmed
with 1 ml of acetic acid and 3 Pleasant fruity smell. Presence of alcohol
drops of Con. H2SO4 in a water confirmed.
bath for 5 minutes and pour it into
20 ml of cold water.

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