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SALT ANALYSIS

Physical appearance of salt

EXPERIMENT OBSERVATION INFERENCE


1. Colour of the salt is White colour Pb2+,Al3+, Zn2+ ,Ca2+,Mg2+,NH4+
noted salts
Bluish of bluish green colour Cu2+ or Ni2+ salts
Light green colour Fe2+,Ni2+ salts
Yellowish colour Fe3+ salts
Light pink/ buff colour Mn2+ salts
Smell of ammonia NH4+ salt
Deliquescent nature Cl- or NO3-
2. Nature (i) Amorphous May be carbonate
(ii) Crystalline May be nitrate,sulphate and
chlorides

3. Action of heat i) Colourless, odourless gas is evolved May be salt contains carbonate
Pinch of salt is heated which turns lime water milky ion.
in a dry test tube ii) Colourless pungent gas, turns May be salt contains sulphite
acidified potassium dichromate paper ion.
in to green.
iii) Reddish brown gas is evolved, May be salt contains nitrate ion.
which turns ferrous sulfate solution
into brown or black. Zn2+
i) Yellow when hot, white
when cold. Pb2+
ii) Brown when hot, yellow
Residue is observed when cold. Fe2+
after heating. iii) Original light green salt
changes into reddish brown.
iv) Pale brown changes to Fe3+
black.
v) Green changes to yellow. Ni2+
vi) Residue is black in colour. May be Cu2+, Fe3+ Mn2+, Co 2+
vii) Decrepitating sound Lead nitrate or barium nitrate.
viii) Condensation of water May be hydrated salts like
vapours copper sulfate, nitrate etc.,

4. Flame test: i) Brick red Ca2+


ii) Crimson red Sr2+
Salt is mixed with conc. iii) Light green/apple green Ba2+
HCl and made in to iv) Bluish green Cu2+
paste which is subjected v) Green flashes ZnSO4, MnCl2
to flame test vi) Bluish white Pb2+, Sn2+
vii) No characteristic colour Absence of the above mentioned
cations.

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EXPERIMENT OBSERVATION INFERENCE
5. Solubility test
Salt mixture + water i) Soluble May be nitrate, sulfate and
chloride salts
ii) Insoluble May be carbonate sulfide and
sulfite(except amm.carbonate).
Salt mixture + dill HCl Soluble May be carbonate or sulfite or
sulfide

Preparation of sodium carbonate extract: Take 0.5 g of the given salt mixture + 5g sodium carbonate + 20
ml of distilled water and boil this content for about 10 minutes and then filter. The filtrate is used for the
anion analysis and also for the confirmatory test. The filtrate is sodium carbonate extract
Group –I anions
Anions identified by using dilute H2SO4 ( CO3 , SO32- NO2- CH3COO-and S2-)
2-

EXPERIMENT OBSERVATION INFERENCE


Little salt mixture is i) Colourless, odourless gas May be CO32-,
treated with dilute H2SO4, is released
observed in cold and after ii) Vinegar like smell May be CH3COO –
warming.
 The liberated gas is Limewater turns milky. CO32- is confirmed.
passed thorough
limewater.
May be SO32-
ii) Colourless, pungent selling gas is
evolved.
 The liberated gas is Pink colour of pot. SO32- is confirmed.
checked with acidified Permanganate disappears and
pot dichromate and pot dichromate paper turns to green.
permanganate paper.
May be NO2-
iii) Reddish brown gas is evolved
 Gas is passed though
Ferrous sulphate solution turns to dark NO2- is confirmed.
ferrous sulphate solution.
brown or black.

iii) Rotten egg smell gas is May be S2-


 Liberated gas is evolved.
checked with lead acetate
paper Lead acetate paper turns to silvery
S2- is confirmed.
black.

 W.E or S.E + sodium Purple or violet colour formation. S2- is confirmed.


nitroprusside solution is
added
iv) vinegar smell May be acetate

Blood red colour solution CH3COO – is confirmed


 S.E or W.E + dil.
HCl is added till all formation.

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carbonates are removed
then add neutral FeCl3.

Group II anions;
Identified by using conc. H2SO4 (Cl , Br , I , NO3-, CH3COO-).
- - -

EXPERIMENT OBSERVATION INFERENCE


Little salt mixture is i) Colourless gas with May be Cl-
heated with conc. H2SO4, pungent smell is evolved.
observed in cold and also
after warming.
 Add Greenish yellow coloured gas is May be Cl-
MnO2 and heat it evolved.

Confirmatory test
S.E or W.E + dil White curdy ppt, soluble in excess Cl- is confirmed.
HNO3 till effervescence of ammonium hydroxide solution.
ceases + AgNO3 solution.
ii) Violet vapours appear. May be I-,
May be I-,
Violet vapours intensify
May be I-,
Turns to blue-black

Yellow ppt is formed which is I- is confirmed.


insoluble in excess of
amm.hydroxide

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 Add MnO2 iii) Reddish brown gas is May be NO3-, Br-
and heat it. evolved.
. Check the Reddish brown gas intensifies May be NO3-
gas with starch paper. Reddish brown gas does not May be Br-
intensify
Confirmatory test
S.E or W.E + dil
HNO3 till effervescence Yellow ppt, dissolves in excess of Br – is confirmed.
ceases + AgNO3 solution. amm.hydroxide solution.

 Add
piece of copper turning or
paper ball. Brown ring at the junction of two NO3- is confirmed.
liquids.
Confirmatory test
S.E or W.E + dil
HNO3 till effervescence
ceases + AgNO3 solution
iv) Smell of vinegar. May be CH3COO –

Confirmatory test Pleasant odour CH3COO – is confirmed.


S.E or W.E + dil
H2SO4 is added till all
carbonates are removed
then add freshly prepared
FeSO4 solution, then add Blood red colour solution
con H2SO4 through the formation.
sides of the test tube. CH3COO – is confirmed.
Red- brown ppt
 Add
about 1ml of ethyl
alcohol.

Confirmatory test
S.E or W.E + dil
HCl is added till all
carbonates are removed
then add neutral FeCl3.
-- Heat the red
colour solution.

SO42- is the 10th anion in the syllabus


W.E / SE acidified with White ppt insoluble in dil HCl SO42- confirmed
dil HCl .Boil off to expell
CO2 .Add BaCl2 soln

Note : In all CT for anions the order should be WE or SE ,as only SE has to be acidified with acid (to
remove the CO32- which would otherwise give ppt with any reagent ) .if WE is used you do not need to
acidify

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CATION ANALYSIS

Preparation of original solution for cation analysis: original solution is prepared by dissolving the salt
mixture in any one of the following solvent.1. Water 2. dil. HCl 3. dil. HNO3 4. conc. HCl
EXPERIMENT OBSERVATION INFERENCE
0. Salt mixture + NaOH Gas evolved turns moist red litmus Group 0 present. NH4+
solution and heat. blue and gives dense white fumes may be present.
with glass rod dipped in conc.HCl
Confirmatory
test Reddish brown precipitate. NH4+ is confirmed.
Salt + NaOH, pass the gas
evolved through Nessler’s
reagent.

EXPERIMENT OBSERVATION INFERENCE


1 O.S + excess dill HCl White ppt Group I present.
Cations of Pb2+ or Ag+
may be present.

No ppt Absence of group I


radicals.
Confirmatory test for Pb2+ Precipitate dissolves Pb2+ may be present
Boil the precipitate with the
distilled water and divide in
to two parts
Part I of the hot filtrate + KI Yellow precipitate. Pb2+ is confirmed.
solution.

Part II of the hot filtrate + Yellow precipitate. Pb2+ is confirmed.


K2Cr2O7 it should be
K2CrO4 solution.(This is a
common mistake seen during
correction )
2 Filtrate of group I +H2S Black colour ppt Group II present.
Brown colour ppt Cu2+, Pb2+, Hg2+
Sn2+ may be present.

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Confirmatory test for Cu2+
Boil the precipitate with 5 ml
of 50% nitric acid. Blue colored solution is formed Cu2+ may be present
Divide the solution in to two
parts.
Part I + NH4OH soln. little Pale blue ppt, dissolves in excess Cu2+ is confirmed.
and then in excess. of amm.hydroxide solution.

Part II + potassium Chocolate brown ppt. Cu2+ is confirmed.


ferocyanide solution
Confirmatory test for Hg2+ Ppt does not dissolve. Hg2+ may be present
Boil the precipitate with 5ml
of 50% nitric acid.
Treat the ppt with aqua regia
and heat to dryness then
dissolve it in water. Divide
the content in to two parts.
Part I + excess of KI Red ppt of HgI2, which dissolves Hg2+ is confirmed.
solution. in excess of KI solution.

Part II +freshly prepared White ppt formed which turns Hg2+ is confirmed.
stannous chloride (SnCl2) black.
solution.

Confirmatory test for Sn2+ Brown ppt dissolves Sn2+ may be present
Boil the ppt with yellow
ammonium sulphide
solution.(NH4)2S
Divide in to two parts

Part I + mercuric chloride White ppt Sn2+ is confirmed.


(HgCl2).

Part II + dil HCl +H2S Brown ppt Sn2+ is confirmed.

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Boil the filtrate of group II to Precipitate colour: Group III present.
expel H2S. Add few drops Gelatinous white Al3+,Fe2+, Fe3+
conc. HNO3 + pinch of Brown Cr3+
NH4Cl(s) +NH4OH solution Bluish green or grey green
in excess.

Confirmatory test for Al3+


Dissolve the pt with
minimum quantity of dill
HCl and then and divide in to A white ppt formed which Al3+is confirmed.
two parts. dissolves on adding excess of
To the first part add NaOH NaOH.
drop wise
A blue lake floating in clear liquid Al3+ is confirmed.
is seen.
To the second part add blue
litmus solution then add
NH4OH solution. Blood red colouration May be Fe2+or Fe3+
2+
Confirmatory test for Fe
Dissolve the brown ppt with
dil HCl. Then add potassium
thiocyanide (KCNS) Dirty green preciptate Fe2+ is confirmed.

O.S + NaOH. Solution. Pale blue ppt Fe2+ is confirmed.

O.S + pot. Ferricyanide No ppt Fe2+ is confirmed.

O.S + pot. Ferrocyanide

Confirmatory test for Fe3+


Dissolve the brown ppt with
dil HCl. Then add potassium Blood red colouration May be Fe2+or Fe3+
thiocyanide (KCNS)

O.S + NaOH. Solution. Reddish brown ppt Fe3+ is confirmed.

O.S + pot. Ferricyanide No ppt Fe3+ is confirmed.

O.S + pot. Ferrocyanide Blue ppt Fe3+ is confirmed.


Confirmatory test for Cr3+
Treat the ppt with 1ml of Formation of yellow solution. Cr3+ is confirmed.
NaOH and bromine water.

To the yellow solution Formation of yellow ppt of lead Cr3+ is confirmed.


formed add 1 ml of lead chromate.
acetate solution.

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Filtrate of group III + pinch Precipitate formation Group IV is present
of NH4Cl(s) +NH4OH + H2S Grayish white Zn2+,Ni2+,Mn2+ may be
gas. Black present
Buff coloured

Confirmatory test for Zn2+


Dissolve the ppt with dil HCl
, boil the content to remove
H2S. Cool and divide the
solution in to two parts.
White ppt forms which dissolves Zn2+ is confirmed.
st
To the 1 part add NaOH in excess of NaOH
drop wise and then in excess
Bluish white ppt is formed. Zn2+ is confirmed.
To the second part add pot
ferro cyanide solution.

Confirmatory test for Ni2+


Dissolve the ppt in minimum
quantity of aqua regia , and
evaporate to dry mass.
Extract the residue with
water. Add 1-2 ml of A cherry red colouration. Ni2+ is confirmed.
Dimethyl glyoxime (DMG)
solution. Then add NH4OH
solution.

Confirmatory test for Mn2+


Divide the buff ppt into two
parts
Dissolve the 1st part in least
quantity of dil HCl. Boil to White ppt is formed, which slowly Mn2+ is confirmed.
expel H2S. Add NaOH turns to brown on standing.
solution drop wise.
Pink colour developed in solution. Mn2+ is confirmed.
Dissolve the 2nd part in con
HNO3. Add 1 gm lead
dioxide boil the content.
Dilute it with water.

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Boil off H2S from filtrate of
group IV and reduce the
volume of the solution to 1/3 White ppt Group V is present
by heating. Now add pinch May be Ba2+, Sr 2+ , Ca2+
of NH4Cl(s) +NH4OH
solution + excess of
ammonium carbonate
solution.
Dissolve the ppt with
hot acetic acid and divide in
to four parts.
Ba2+ is confirmed.
To the 1st part add Yellow ppt of barium chromate is
pot.chromate. formed.
Ba2+ is confirmed.
nd
To the 2 part add dil H2SO4. White ppt is formed. Insoluble in
all mineral acid.
To the 3rd part add 1ml of Sr2+ is confirmed.
concentrated ammonium Formation white ppt of strontium
sulphate solution and warm. sulfate.

To the 4th part add 1ml of Ca2+ is confirmed.


ammonium oxalate solution. White ppt is formed.
The white ppt is Not to be done or
dissolved in dil HCl and then Pink colour of KMnO4 is written
add few drops of KMnO4 discharged.
solution.

Perform flame test with the


ppt. A brick red flame. Ca2+ is confirmed.
A crimson red flame Sr2+ is confirmed.
A light green/apple green flame Ba2+ is confirmed.
To the filtrate of group V add White ppt is formed Group VI present.
ammonium phosphate or di
sodium hydrogen phosphate Mg2+ is confirmed.
solution + 2ml of ethyl
alcohol. Scratch the wall of
the test tube with glass rod.

Note :
1. In Gp V –if you have to follow the order of Ba2+, Sr 2+ , Ca2+ eg , if your salt contains Sr 2+ , then you have
to write the tests for Ba2+ and say ppt not observed , hence Ba2+absent .Then go on to write test for
Sr 2+ .
2.CT for Mg2+ ----Boil the filtrate of group V to reduce the volume .Filter ,if necessary .To the clear solution
add an excess of disodium hydrogen phosphate and a few drops of ammonium hydroxide. Shake well and
scratch the walls of the test tube with a glass rod → White crystalline ppt on standing