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AMRITA VIDYALAYAM, NALLAMPALAYAM


CHEMISTRY- SYSTEMATIC PROCEDURE FOR INORGANIC QUALITATIVE ANALYSIS
I. PRELIMINARY TESTS

EXPERIMENT OBSERVATION INFERENCE

1 Appearance: Crystalline May be sulphate, nitrate or chloride

Appearance of the salt is noted Powdery May be sulphide or carbonate

Blue or green Presence of copper

Clourless Absence of copper and iron salts


2 Solubility
May be sulphate, nitrate or chloride
Salt + water Soluble or ammonium chloride or ammonium
carbonate

Insoluble May be sulphide or carbonate

3 Action of heat : Colourless and odourless gas May be carbonate


A small amount of the salt is which turns lime water milky
heated gently and then strongly Reddish brown vapours evolve May be nitrate - Ba(NO3)2
in a dry test tube with crackling sound or Pb(NO3)2

Salt sublimes with evolution of May be Ammonium


pungent smelling gas giving
dense white fumes with a glass
rod dipped in con.HCl .

The salt turns yellow when May be zinc


hot and white when cold

The salt fuses or melts May be magnesium


Absence of carbonate, Ba(NO3)2,
No characteristic change Pb(NO3)2, Ammonium, zinc and
magnesium,
4 Flame test :
Salt + conc. HCl is made into a Brick red flame Presence of calcium
paste and introduced the paste
with the help of the glass rod
into the non luminous part of Apple or glassy green flame Presence of barium
the bunsen flame.
Bluish green flame Presence of copper

No characteristic coloured Absence of Calcium, Barium and


flame Copper
5 Ash test : Blue ash Presence of Aluminium
Green ash Presence of Zinc
Salt + conc. HNO3 + Cobalt
Presence of Magnesium
nitrate taken in watch glass. A
Pink ash
filter paper is soaked into the
Absence of Al, Zinc and Magnesium
solution and burnt
No characteristic coloured ash

IDENTIFICATION OF ACID RADICALS


6 Action of dil Hcl:
Colourless, odourless gas with May be carbonate
Salt + dilute HCl brisk effervescence turning
lime water milky is obtained.

Colourless gas with rotten egg May be sulphide


smell turns lead acetate paper
black is obtained

No characteristic gas evolved Absence of carbonate and sulphide.


7 Copper turnings test:

Salt + Copper Turnings +


conc.H2SO4 + heated Reddish brown gas is evolved. Presence of Nitrate.

No reddish brown gas Absence of Nitrate

Evolution of ammonia gas


Action of NaOH: with pungent smell which
8. gives dense white fumes when
. a glass rod dipped in conc. HCl Presence of Ammonium.
Salt + NaOH + heated is brought near to the mouth of
the test tube and also turns
moist red litmus paper blue.

No pungent smelling gas Absence of ammonium.

9. Chromyl chloride test:


Salt + a pinch of K2Cr2O7
crystals + conc. H2SO4 + Red orange vapours are
heated. evolved.

Pass the vapours through the Solution becomes yellow


test tube contains NaOH Presence of chloride is conformed.
solution. Yellow precipitate is obtained
No red orange vapours are Absence of chloride.
To the yellow solution add evolved
dilute acetic acid and lead
acetate solution.

PREPARATION OF SODIUM CARBONATE EXTRACT


A small amount of salt is mixed with twice the amount of sodium carbonate in a 100 ml beaker. 20ml of distilled water
is added, boiled for 10 minutes, cooled and filtered. The filtrate is known as “Sodium carbonate extract”.

EXPERIMENT OBSERVATION INFERENCE


1 Silver nitrate test:
. Extract + dilute Nitric acid is
added until the effervescence A curdy white precipitate soluble in Presence of chloride is
ceases + few drops of Silver NH4OH is obtained. confimed
Nitrate solution. No curdy white precipitate Absence of chloride

2 Lead acetate test: A white precipitate soluble in Presence of sulphate is


. Extract + dilute acetic acid is added ammonium acetate solution is confirmed.
until the effervescence ceases + few obtained.
drops of lead acetate solution. A black precipitate is obtained. Presence of sulphide is
confirmed.
No characteristic coloured Absence of sulphate and
precipitate sulphide
3 Barium chloride test: A white precipitate insoluble in Presence of Sulphate is
. Extract + dil. HCl is added until the con.HCl conformed.
. effervescence ceases + few drops of is obtained.
barium chloride solution.
No white precipitate Absence of sulphate
4 Brown ring test:
. Extract + dil. H2SO4 is added until A dark brown ring is formed at the Presence of Nitrate is
the effervescence ceases + freshly junction of the two layers. confirmed.
prepared FeSO4 + conc.H2SO4 is
added along the inner side of the No dark brown ring. Absence of Nitrate.
test tube.
5 Test for Phosphate: Presence of phosphate is
. Ammonium molybdate test: Deep yellow precipitate is obtained. confirmed.
Extract + con.HNO3 + the mixture No deep yellow precipitate Absence of phosphate
is boiled + excess of ammonium
molybdate + boiled.
6 Test for Ester:
.a Test for oxalate: Pleasant sweet smelling ester is Presence of oxalate or
Salt + conc.H2SO4 is added until obtained. acetate
the effervescence ceases + ethyl
alcohol No pleasant sweet smelling ester Abesence of oxalate or
acetate
Test for oxalate: Purple colour of KMnO4 Presence of oxalate is
b. Salt + dil. H2SO4 + the mixture is disappears. confirmed.
heated + few drops of KMnO4 No decolourisation Absence of oxalate
solution.

7 Test for acetate: Deep red colour turns into reddish Presence of acetate is
.a Salt + 2 ml neutral ferric chloride brown precipitate when water is confirmed.
and warmed added.
No red colouration Absence of acetate

Salt + 2 ml of oxalic acid Vinegar smell is obtained. Presence of acetate is


b. confirmed
No vinegar smell Absence of acetate

IDENTIFICATION OF THE BASIC RADICALS


PREPARATION OF ORIGINAL SOLUTION:
The original solution is prepared by dissolving 1 gm of the salt in 10 ml of distilled water / Hot water - Pb(NO 3)2 /
dil.HCl- CaCO3 and CuCO3
GROUP ANALYSIS
EXPERIMENT OBSERVATION INFERENCE
1 ZERO GROUP (AMMONIUM) Evolution of ammonia gas with
. Salt + NaOH solution + heated. pungent smell which gives dense
white fumes when a glass rod
dipped in conc. HCl is brought near Presence of Ammonium.
to the mouth of the test tube and
also turns moist red litmus paper
blue.

No pungent smelling gas Absence of ammonium.


1 ml of original solution + few
drops of Nessler’s reagent + excess Reddish brown precipitate is Presence of Ammonium.
of NaOH solution obtained.

No reddish brown precipitate Absence of ammonium.


2 Group – 1 Analysis: ( Pb )
White precipitate is obtained. Presence of group 1 radical
Original solution + dil.Hcl (Pb)

No White precipitate Absence of Lead.


3 Group – 2 Analysis (Pb &Cu)
Original solution + dil.HCl + H2S Black precipitate is obtained Presence of group 2 radical
gas. (Pb / Cu)
Black precipitate becomes
i) Black precipitate + 50% HNO3 colourless solution which turns into Presence of lead
white precipitate when H2SO4 is
added.
ii) Black precipitate + 50% HNO3
+ excess of NH4OH Bluish colour solution Presence of copper

No black precipitate Absence of group 2 radicals


4 Group – 3 Analysis (Al)
Gelatinous white precipitate is Presence of group 3 radical
Original solution + 1 ml NH4Cl + obtained. (Al)
2ml NH4OH
No Gelatinous white precipitate Absence of group 3 radical
(Al)
5 Group – 4 Analysis (Zinc)
Dirty white precipitate is obtained. Presence of group 4
Original solution + 1 ml NH4Cl + 2 radical(Zn).
ml NH4OH + H2S gas.
No dirty white precipitate Absence of group 4
radical(Zn).

6 Group – 5 Analysis (Ca & Ba) White precipitate is obtained. Presence of group 5 radicals
Original solution + 1 ml NH4Cl + 2 (Ca or Ba)
ml
NH4OH + 2 ml of saturated No White precipitate Absence of group 5 radicals
(NH4)2CO3 solutions + warm (Ca and Ba)

Dissolve the white precipitate in hot


acetic acid and divide into 2 parts
Part – 1 + potassium chromate Yellow precipitate is obtained
solution Presence of Barium is
White precipitate is obtained confirmed.
Part – II + ammonium oxalate +
ammonium hydroxide solutions Presence of Calcium is
confirmed.
7 Group – 6 Analysis (Mg)
Original solution + 2 ml disodium white precipitate is obtained Presence of Magnesium.
hydrogen phosphate + ammonia
solution No white precipitate Absence of Magnesium.

CONFIRMATORY TESTS FOR BASIC RADICALS

EXPERIMENT OBSERVATION INFERENCE


1. ZERO GROUP (AMMONIUM)

Original solution + Nessler’s Reddish brown precipitate is Presence of ammonium is


reagent + excess of NaOH solution. obtained. confirmed.
2. Group 1: Lead
Original solution + potassium
chromate (K2CrO4) solution Yellow precipitate is obtained Presence of Lead is
confirmed.
Original solution +KI solution Yellow precipitate is obtained

Yellow precipitate + water + boil Precipitate dissolves and Presence of Lead is


and cool reappears in the form of golden confirmed.
spangles
3. Group 2: (Pb & Cu)
Confirmatory test for copper: Presence of copper is
A pale blue precipitate dissolves in confirmed
Original solution + NH4OH in drops excess of NH4OH to give inky blue
and then in excess. solution.
Original solution + dil.acetic acid +
potassium ferrocyanide solution Chocolate brown precipitate Presence of copper is
K4 [Fe (CN)6] confirmed

4. Group 3 : (Al)
White gelatinous precipitate
dissolves in dil.HCl by boiling and
make it into 2 parts

Part 1 + few drops of blue litmus Formation of a blue floating


solution precipitate in colourless solution
( Lake test)
Aluminium is confirmed.
Part 2 +2 ml of NH4OH + A bright red lake is formed
Aluminon
reagent

5. Group 4 : (Zinc)
Dissolve a part of white
precipitate in dil.HCl. , boil and
pass H2S and divide it into 2 parts

i) Part 1 + potassium Bluish white precipitate Zn is confirmed


ferrocyanide
solution
White precipitate soluble in excess Zn is confirmed
ii) Part 2 + NaOH solution NaOH
6. Group 5 :Ba & Ca

Original solution + K2CrO4 solution Yellow precipitate Barium is confirmed

Original solution + ammonium


oxalate + NH4OH solution and White precipitate Calcium is confirmed
scratch the sides of the test tubes
Group 6 : (Mg)
7. Original solution + solid NH4Cl
and warm to dissolve , cool +
NH4OH solution in slight excess +
ammonium phosphate solution , White crystalline precipitate Magnesium is confirmed
shake well and allow to stand

Original solution + Magneson Blue precipitate Magnesium is confirmed


reagent + excess NaOH solution

RESULT : The given simple salt contains


Anion / Acid Radical :
Cation / Basic Radical :

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