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QUALITATIVE INORGANIC ANALYSIS

SALT ANALYSIS PROCEDURE

I. PRELIMINARAY OF THE SALT

EXPERIMENT OBSERVATION INFERENCE


2+
1. Colour and appearance Blue or bluish green Cu or Ni2+
of salt is noted
Greenish Ni2+

Light green
Fe2+
Dark brown
Fe3+
Pink violet
Co2+
Light pink, flesh colour
or dull
earthy colour Mn2+

Colourless Absence of Cu2+ ,


Ni2+, Fe2+,
Fe3+, Co2+
Presence of NH4+
Ca2+ Sr2+ Ba2+ Zn2+
2+
Pb2+ Al3+ , Mg
2. Odour test: Take a pinch of salt between the Ammoniacal smell NH4+
fingers and rub with a drop of water.
Vinegar like smell CH3COO-

Smell of rotten eggs


S2-
3. Flame Test: Dip a glass rod in conc.HCl and dip Brick red (not Ca2+ might be
the same in a small quantity of the given salt. persistent) present
Introduce this to the non-luminous Bunsen
flame Crimson red Sr2+ might be
(persistent) present

Persistent grassy-green Ba2+ might be


(appears present
after prolonged
heating)

Bright bluish green Cu2+ might be


present
Green flashes Mn2+ might be
present
Light blue flashes Zn2+ might be
present
Dull bluish white Pb2+ might be
present
No characteristic flame Absence of Ca2+,
colouration is Sr2+, Ba2+ , Cu2+ ,
observed
Mn2+ , Zn2+ , Pb2+
(Or) presence of
+ 2+
NH4 , Al3+ , Mg
Green ash 2+
4. Ash Test Zn

To a small quantity of salt in a China dish, add few 2+


Pink ash Mg
drops of cobalt nitrate solution and con.HNO3 heat,
soak a filter paper and burn to ashes
Blue ash Al
3+

II. ANION ANALYSIS


EXPERIMENT OBSERVATION INFERANCE
1. A pinch of the salt in a test Colourless, odourless gas with brisk Presence of
tube is treated with 1-2 effervescence, turns lime water milky. carbonate
ml of dilute sulphuric acid

Colourless vapours, vinegar smell. Presence of acetate

2. A pinch of salt crystals in Colourless gas with pungent smell is Presence of chloride
a test tube +2ML conc. evolved which gives dense white fumes
sulphuric acid. when a glass rod dipped in ammonium
hydroxide is shown at the mouth of the
test tube

Reddish brown vapours with pungent Presence of bromide


smell, turns starch paper yellow. It does
not turn FeSO4 solution black.

Deep violet vapours with pungent smell, Presence of Iodide


turns starch paper blue. A sublimate is
formed on the sides of the tube.

Reddish brown gas with pungent smell, Presence of nitrate


turns FeSO4 solution black.
0r
Evolution of brown fumes on addition of
paper ball ( Salt+Con H2SO4+ Paper ball+
heat)
No characteristic gas or Absence of Cl- , Br- , I- ,
vapour evolution is observed NO3- ,
CH3COO-

3. Salt solution+BaCl2 White ppt Sulphate or


solution. phosphate is
suspected.

No White ppt Absence of Sulphate


or phosphate

III. CONFIRMATORY TESTS FOR ANIONS:

Carbonates (CO32-)
EXPERIMENT OBSERVATION INFERENCE
1. To salt solution, add Formation of white precipitate Presence of soluble carbonate
magnesium sulphate in the solution is confirmed
solution + ammonium
hydroxide

2. A pinch of the salt in a Brisk effervescence of CO2 Presence of soluble carbonate


test tube is treated which turns lime water milky. is confirmed
with 1-2 ml of dilute
sulphuric acid

Chloride (Cl-)
EXPERIMENT OBSERVATION INFERENCE
1. Acidify a portion of the A white precipitate is formed Presence of chloride is
aqueous solution with which is soluble in ammonium confirmed
dil.Nitric acid, boil, cool hydroxide
and add silver nitrate
solution.
2. Chromyl chloride test. To A yellow precipitate is obtained Presence of chloride confirmed
a mixture of the salt and solid
potassium dichromate, add
conc. Sulphuric acid heat and
pass the red vapours through
NaOH solution. To the yellow
solution thus obtained, add
dil.acetic acid and lead acetate
solution.

Bromide (Br-)
EXPERIMENT OBSERVATION INFERENCE
1. Acidify a portion of the A light yellow precipitate is Presence of bromide is
aqueous solution with obtained which is partially confirmed
dil.nitric acid, boil , cool soluble in NH4OH
and silver nitrate
solution
2. Heat a small quantity of Evolution of yellowish brown Presence of Bromide is
the salt with solid vapours of bromine which turn confirmed
MnO2 and conc. Sulphuric starch paper yellow
acid

Iodide (I-)
EXPERIMENT OBSERVATION INFERENCE
1. Acidify a portion of the A yellow precipitate is formed Presence of Iodide is confirmed
aqueous solution with which is insoluble in NH4OH
dil.Nitric acid, boil, cool
and add silver nitrate
solution
2. Heat a small quantity of Evolution of violet vapours of Presence of iodide is confirmed
the salt with solid MnO2 iodine which turns starch paper
and conc.Sulphuric acid blue
Nitrate (NO3-)
EXPERIMENT OBSERVATION INFERENCE
1. Heat a small quantity of Dark brown fumes of nitrogen Presence of Nitrate is
the salt with conc. peroxide are evolved confirmed
Sulphuric acid and a few
copper chips.
2. Brown ring test: Add a A dark brown ring is formed at Presence of nitrate is confirmed
small quantity of freshly the junction of the layers of the
prepared solution of acid and the solution
ferrous sulphate to a
part of the aqueous salt
solution and then pour
conc.sulphuric acid
slowly along the sides
of the test tube.

Acetate (CH3COO-)
EXPERIMENT OBSERVATION INFERENCE
1. Salt solution+ neutral Red colour solution Presence of acetate is
FeCl3 confirmed

3. Prepare a paste of the Smell like that of vinegar Presence of acetate is


salt with a pinch of confirmed
oxalic acid and a few
drops of water in a
watch glass. Rub the
paste and smell
2. Take a small quantity of the Pleasant fruity smell of ester. Presence of acetate is
salt in a test tube . Add conc. confirmed.
Sulphuric acid and heat. Now
add a few drops of ethanol and
shake. Pour the contents of
the test tube in a beaker half-
filled with water and stir.
Sulphate (SO42-)
EXPERIMENT OBSERVATION INFERENCE
1. To a part of a aqueous A white precipitate is formed Presence of sulphate is
solution of salt add lead which is soluble in excess of hot confirmed
acetate solution. ammonium acetate solution

2. To a part of the aqueous A white precipitate is formed Presence of sulphate is


solution of salt and which is insoluble in dil.HCl confirmed.
barium chloride
solution
IV. CATION ANALYSIS (GROUP WISE ANALYSIS)
SL.NO. EXPERIMENT OBSERVATION INFERENCE
1. A pinch of salt+ dil. NaOH No characteristic gas Absence of group zero
and heat, show a moist red evolution. (NH4+)
litmus paper at the mouth
of the test tube Evolution of a colourless gas
with the smell of ammonia, Presence of group zero
red litmus paper turns blue (NH4+)

2. Salt solution in water+ No characteristic ppt Absence of group I (Pb2+)


dil.HCl
White ppt Presence of Group I (Pb2+)
3. Salt solution in water+ No characteristic ppt Absence of Group II (Cu2+)
dil.HCl+ammonium
sulphide solution Black ppt. Presence of Group II (Cu2+)
4. Salt solution+solid No characteristic ppt Absence of Group III (Al3+)
ammonium chloride, boil
and cool+excess White gelatinous ppt Presence of Group III (Al3+)
ammonium hydroxide
5. Salt solution+solid No characteristic ppt Absence of Group IV (Zn2+ ,
ammonium chloride, boil Ni2+ , Co2+ , Mn2+)
and cool+excess Dirty white ppt Presence of Zn2+
ammonium hydroxide+3 Flesh coloured ppt Presence of Mn2+
drops of ammonium Black ppt Presence of Co2+ or Ni2+
sulphide
6. Salt solution+solid No characteristic ppt. Absence of Group V
ammonium chloride, boil (Ba2+,Ca2+, Sr2+)
and cool+excess Mg2+ might be present
ammonium hydroxide+
(NH4)2 CO3 soln. White ppt Presence of Group V
(Ba2+,Ca2+, Sr2+)

7 Salt solution is treated


with solid ammonium
chloride,ammonium White ppt on scratching
Presence of Group VI (Mg2+)
hydroxide in slight and the sides of the test tube
excess of disodium with a glass rod
hydrogen phosphate
solution

V.CONFIRMATORY TESTS FOR CATIONS:


For NH4+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. A pinch of salt+dil.NaOH
and heat, show a glass
Formation of dense white
fumes of ammonium
NH4+ IS Confirmed
rod dipped in conc.HCl at chloride
the mouth of the test
tube

Salt solution+ Nessler's Reddish brown ppt


2. reagent NH4+ IS Confirmed

For Pb2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution + KI solution yellow ppt of lead iodide
Pb2+ is confirmed
2. Salt solution + potassium Yellow ppt of lead
chromate solution chromate Pb2+ is confirmed

For Cu2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution + excess of
ammonium hydroxide
Deep blue solution
Cu2+ is confirmed
solution

2. Acidify the above deep


blue solution with
Chocolate brown ppt.
Cu2+ is confirmed
dil.acetic acid and add
potassium ferrocyanide
solution

For Al3+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt + dil HCl+ a few drops A blue lake formation
of blue litmus
Al3+ is confirmed
solution+ammonium
hydroxide solution in
excess

2. Salt + conc.Nitric Blue ash formation


acid+cobalt nitrate
Al3+ is confirmed
solution dip a filter paper
in the solution and show
it to the Bunsen flame

For Zn2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution+sodium
hydroxide solution (drop
White ppt is formed and it
dissolves in excess NaOH
Zn2+ is confirmed
wise addition)
2. Salt solution + potassium White / bluish white ppt
ferrocyanide solution
Zn2+ is confirmed

For Mn2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution+ NaOH White ppt that turns dark
solution, shake with bromine water Mn2+ is confirmed
2. To the dark ppt add few
drops of conc.Nitric
Pink coloured solution
Mn2+ is confirmed
acid+lead peroxide, boil,
cool and allow to settle

For Co2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution+ acetic acid+
a crystal of potassium
Yellow ppt
Co2+ is confirmed
nitrate and warm

2. Salt solution +0.5ml


ether+ one crystal of
Blue colour in ether layer
Co2+ is confirmed
ammonium thiocyanate
and shake and allow to
settle

For Ni2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution + few drops of Bright rose red ppt
ammonium hydroxide +
Ni2+ is confirmed
few drops of dimethyl
glyoxime

2. Salt solution+ excess black ppt


Ni2+ is confirmed
NaOH+bromine water, boil

For Ba2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution+few drops of yellow ppt
potassium chromate Ba2+ is confirmed
solution

2. Flame test (salt+conc.HCl


paste is taken on a glass
Grassy green
Ba2+ is confirmed
rod and shown to flame

For Sr2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution+ammonium White ppt
sulphate solution Sr2+ is confirmed

2. Flame test (salt+conc.HCl


paste is taken on a glass
Crimson red flame
colouration
Sr2+ is confirmed
rod and shown to flame

For Ca2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution+ammonium White ppt
oxalate solution+few drops
Ca2+is confirmed
of ammonium hydroxide
solution

2. Flame test (salt+conc.HCl brick red flame


paste is taken on a glass colouration
Ca2+is confirmed
rod and shown to flame)

For Mg2+
Sl.No. EXPERIMENT OBSERVATION INFERENCE
1. Salt solution +magneson reagent Blue ppt
Mg2+ is confirmed
2. Salt +conc.Nitric acid+cobalt Pink ash formation
Mg2+ is confirmed
nitrate solution, dip a filter
paper and show to
Bunsen flame
RESULT

1. The given salt containing anion=……………………(write formula with charge in bracket)


2. The given salt containing Cation=…………………. ( )
3. The given salt is ……………………( )

NOTES

0
 Heating through test tubes should be 45 angle with respect to the burner.
 All the apparatuses should be washed only after pouring the contents out of it.Never add water directly to the
apparatus.
 Odour test to be conducted without gloves.
 Flame test chemicals should be washed off immediately as the produce volatile chloride fumes.
 If flame colour is absent ash test to be conducted immediately for quick identification of cations such as
Aluminium[Blue ash] , zinc[green ash] and magnesium[pinkish white ash]. Salt+3 drops of con.HNO3+ 3 drops
of cobalt nitrate solution.
 Concentrated acids should not exceed 3 drops. Con.H2SO4 to be added to dry test tube only.
 Carbonate preliminary [lime water] test should be conducted in U shaped gas tube and lime water to be added
first in gas tube before adding the salt.
 Dense white fumes of chloride will appear soon after treating the salt with con.H2SO4.No heating required for
this experiment.
 Nitrate is identified with reddish brown fumes by heating with con.H2SO4 followed by Paper ball addition.
FeSO4 need not be added as they produce poisonous fumes.
 Brown ring test filtrate obtained after adding FeSO4 to be transferred to another test tube followed by slow
addition of con.H2SO4 along the sides of test tube produces clear brown ring. FeSO4 to be added in excess.
 Chromyl chloride and copper chips confirmatory tests ,Bromide and iodide tests are meant for VIVA.
 Acetate can be identified with smell of vinegar which then directly confirmed with oxalic acid test.No
preliminary test required for acetate.
 If Carbonate ,chloride and nitrate are absent sulphate can be tested directly by confirmatory test. Ammonium
acetate to be added in excess to check the solubility of ppt.
 Ammonium salts are identified by heating salt with NaOH followed by ammoniacal smell.
 Never rely on litmus paper test for acetate and ammonium salts as they may change the colour due to the
presence of acid and base taken.
 All cations are identified using flame and ash tests.Therefore kindly avoid using harmful chemicals such as
ammonium sulphide mentioned in preliminary tests for cations.
 Coloured cations are identified directly by noting their colour and are supported directly with respective
confirmatory tests.
 Clues for quick identification
Ammonium carbonate - smelling salt ;has strong smell of ammonia.
Other ammonium salts such as ammonium chloride and ammonium acetate and ammonium sulphate produce
ammonia only after heating with NaOH.
Ammonium nitrate is explosive .so wont be given for analysis.

Insoluble salts are not provided for testing.

Examples of soluble salt combinations


Ammonium - Ammonium carbonate , ammonium chloride ,
and ammonium sulphate

Pb – Pb nitrate , Pb acetate are the possible combinations.

Aluminium - Aluminium sulphate

Ca – Ca chloride , Ca nitrate , Ca acetate

Ba – Ba chloride , Ba nitrate , Ba acetate

Sr – Sr chloride , Sr nitrate , Sr acetate

Zn – Zn chloride , Zn nitrate , Zn acetate

Mg – Mg chloride , Mg nitrate, Mg acetate , Mg sulphate

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