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Salt Analysis Method

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29 views8 pages

Salt Analysis Method

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Anion Analysis:

Dil H2SO4 Group: CO32-, S2-, SO32-


Conc.H2SO4 Group: Cl-, Br-, I-, CH3COO-, NO3-, C2O42-
Independent Ions: SO42-, PO43-

Experiment Observation Inference

Carbonate CO32- Colourless, odourless gas is May be CO32-


Preliminary Test: To small evolved with brisk
amount of salt in a test tube, effervescence.
add a small amount of dil.
H2SO4.
Confirmatory test: To small Lime water turns milky. CO32- confirmed.
amount of salt in a test tube,
add a small amount of dil.
H2SO4,pass the evolved gas
through lime water.

Sulphide S2-
Preliminary Test: To small Colourless gas with rotten May be S2-.
amount of salt in a test tube, eggs smell is evolved.
add a small amount of dil.
H2SO4.
Confirmatory test: To 1mL of Purple coloured solution is S2- is confirmed.
salt solution (aqueous) add formed.
1mL Sodium Nitroprusside
solution.

Sulphite SO32-
Preliminary Test: To small Colourless gas with burning May be SO32-
amount of salt in a test tube, Sulphur smell is evolved.
add a small amount of dil.
H2SO4.
Confirmatory test: To 1mL of Green coloured solution is SO32- is confirmed.
salt solution (aqueous) add 1 formed.
mL Potassium dichromate
solution.

Chloride Cl-
Preliminary Test: To small Colourless gas with pungent May be Cl-.
amount of salt in a test tube, smell is evolved.
add a small amount of conc.
H2SO4.
Confirmatory test: To 1mL of White ppt soluble in aq.NH3. Cl- is confirmed.
salt solution (aqueous) add
1mL AgNO 3 solution.

Bromide Br-
Preliminary Test: To small Reddish brown gas with May be Br-.
amount of salt in a test tube, pungent smell is evolved.
add a small amount of conc.
H2SO4.
Confirmatory test: To 1mL of Off-white ppt partially soluble Br- is confirmed.
salt solution (aqueous) add in aq.NH3.
1mL AgNO 3 solution.

Iodide I-
Preliminary Test: To small Violet gas is evolved. May be I-.
amount of salt in a test tube,
add a small amount of conc.
H2SO4.
Confirmatory test: To 1mL of Pale Yellow ppt insoluble in I- is confirmed.
salt solution (aqueous) add aq.NH3 is formed.
1mL AgNO 3 solution.

Nitrate NO3-
Preliminary Test: To small Pungent brown gas is evolved. May be NO3-.
amount of salt in a test tube,
add a small amount of conc.
H2SO4. Heat and add half
spatula Copper turnings.
Confirmatory test: To 1mL of Brown ring is formed at the NO3- is confirmed.
salt solution (aqueous) add 2-3 junction of two solutions.
mL freshly prepared FeSO 4
solution. Add conc. H 2SO4
along sides.

Acetate CH3COO-:
Preliminary Test: To small Colourless, pungent gas with May be CH3COO-.
amount of salt in a test tube, vinegar like smell is evolved.
add a small amount of conc.
H2SO4.
Confirmatory test: To 1mL of Red Colouration CH3COO- is confirmed.
salt solution (aqueous) add
1mL FeCl 3 solution.

Oxalate C2O42-:
Preliminary Test: To small Colourless gas with brisk May be C2O42-.
amount of salt in a test tube, effervescence is evolved.
add a small amount of conc.
H2SO4.
Confirmatory test: To 1 mL of White ppt. insoluble in acetic C2O42- is confirmed.
salt solution(aqueous) add 1 acid.
mL CaCl 2 solution.

Sulphate SO42-
Confirmatory Test:
To 1 mL salt solution(aqueous), White ppt. insoluble in dil. HCl SO42- is confirmed.
add 1 mL BaCl 2 solution. is formed.

Phosphate PO43-:
Confirmatory Test:
To 1 mL aqueous salt solution, Canary yellow ppt is formed. PO43- is confirmed.
add 1-2 mL conc. HNO 3 and
boil. To this add 1mL
ammonium molybdate solution.

Cation Analysis:
Group Cations Group Reagent Precipitated As

0 NH4+ - -

I Pb2+ Dil. HCl Chlorides

II Pb2+, Cu2+ Dil HCl, H2S (H2S in acidic Sulphides


medium)

III Al3+ NH4Cl(s), NH4OH(aq) Hydroxides

IV Zn2+, Mn2+, Ni2+, Co2+ NH4Cl(s), NH4OH(aq), H2S(H2S in Sulphides


basic medium)

V Ba2+, Sr2+, Ca2+ NH4Cl(s), NH4OH(aq), (NH4)2CO3 Carbonates

VI Mg2+ - -

Preparation of Original Solution (O.S)


To prepare the original solution, following steps are followed one after the other in a systematic order. In
case the salt does not dissolve in a particular solvent even on heating, try the next solvent. The
following solvents are tried:

1. Take a little amount of the salt in a clean boiling tube and add a few mL of distilled water and shake
it. If the salt does not dissolved, heat the content of the boiling tube till the salt completely dissolves.

2. If the salt is insoluble in water as detailed above, take fresh salt in a clean boiling tube and add a few
mL of dil.HCl to it. If the salt is insoluble in cold, heat the boiling tube till the salt is completely dissolved.

3. If the salt does not dissolve either in water or in dilute HCl even on heating, try to dissolve it in a few
mL of conc. HCl by heating.

4. If salt does not dissolve in conc. HCl, then dissolve it in dilute nitric acid.

5. If salt does not dissolve even in nitric acid then a mixture of conc. HCl and conc. HNO3 in the ratio
3:1 is tried. This mixture is called aqua regia. A salt not soluble in aqua regia is considered to be an
insoluble salt.

Experiment Observation Inference

Group 0: Ammonium NH 4+
Preliminary Test: To small Colourless gas with May be NH4+
amount of salt in a test tube, ammoniacal smell is evolved.
add a small amount of NaOH.

Bring a glass rod dipped in Dense white fumes.


conc HCl near the mouth of test
tube.
Confirmatory test: To small Chocolate brown ppt. is NH4+ confirmed.
amount of salt in a test tube, formed.
add a small amount of NaOH,
pass the evolved gas through
Nessler’s reagent.

Group I:Lead Pb+2


Preliminary Test: To small White ppt. is formed. May be Pb2+.
amount of O.S in a test tube,
dil. HCl.

Confirmatory test: Dissolved the


white ppt. in hot water and
divide the solution into 3 parts:
a. To part 1 add KI. Yellow ppt. Pb2+ confirmed.
b. To part 2 add K2CrO4. Yellow ppt. Pb2+ confirmed.
c. To part 3 add dil. H2SO4. White ppt. soluble in Pb2+ confirmed.
Ammonium acetate.

Group II: Lead Pb+2


Preliminary Test: To small Black ppt. May be Pb2+.
amount of O.S in a test tube,
dil. HCl, H2S.

Confirmatory test: Dissolve the


black ppt in dil.HNO3. To this
add dil H2SO4 and few drops of
alcohol.
White ppt. dissolves in
ammonium acetate on boiling.
Divide the solution into 2 parts:
a. To part 1 add KI. Yellow ppt. Pb2+ confirmed.
b. To part 2 add K2CrO4. Yellow ppt. Pb2+ confirmed.

Group II: Copper Cu+2


Preliminary Test: To small Black ppt. is formed. May be Cu2+.
amount of O.S in a test tube,
dil. HCl and H2S.

Confirmatory test: Dissolved the


black ppt in 50% nitric acid, a
blue colour solution is formed;
divide it into 2 parts:
a. To part 1 add excess White ppt. is formed which Cu2+ confirmed.
NH4OH. dissolves in excess NH4OH to
give a deep blue solution.

b. To part 2 add Potassium Chocolate brown ppt. is Cu2+ confirmed.


ferrocyanide. formed.
Group III: Aluminium Al 3+
Preliminary Test: To small Gelatinous white ppt. May be Al 3+.
amount of O.S in a test tube,
add NH4Cl(s) and NH4OH(aq).

Confirmatory Test: Bluish white ppt. in colourless Al3+ confirmed.


Lake Test: Dissolve the solution.
gelatinous white ppt. in dil HCl,
to this add 1-2 drops of blue
litmus solution and then add
NH4OH dropwise.

Group III: Ferric Fe3+


Preliminary Test: To small Reddish brown ppt. May be Fe3+.
amount of O.S in a test tube,
add NH4Cl(s) and NH4OH(aq).

Confirmatory Test:
Dissolve the ppt. in dil HCl and
divide the solution into 2 parts:
a. To part 1 add Potassium Prussian Blue Solution. Fe3+ confirmed.
ferrocyanide.
b. To part 2 add Potassium Blood red solution. Fe3+ confirmed.
thiocyanate.

Group IV: Zinc Zn+2


Preliminary Test: To small Dirty white ppt. May be Zn2+.
amount of O.S in a test tube,
add NH4Cl(s), NH4OH(aq) and
H2S.

Confirmatory Test:
Dissolve the dirty white ppt. in
dil HCl and divide it into 2 parts:
a. To part 1 add Potassium Bluish white ppt. Zn2+ confirmed.
ferrocyanide solution.
b. To part 2 add NaOH
solution.
White ppt. soluble in excess Zn2+ confirmed.
NaOH.

Group IV: Manganese Mn+2


Preliminary Test: To small Buff ppt. May be Mn2+.
amount of O.S in a test tube,
add NH4Cl(s), NH4OH(aq) and
H2S.

Confirmatory Test:
Dissolve the dirty white ppt. in White ppt. which turns brown Mn2+ confirmed.
dil HCl and to this add NaOH on standing.
solution.

Group IV: Nickel Ni+2


Preliminary Test: To small Black ppt. May be Ni2+.
amount of O.S in a test tube,
add NH4Cl(s), NH4OH(aq) and
H2S.

Confirmatory Test:
Dissolve the black ppt. in aqua Rose red ppt. Ni2+ confirmed.
regia and add water. To this add
1 mL of NH4OH followed by
Di-methylglyoxime solution.

Group IV: Cobalt Co+2


Preliminary Test: To small Black ppt. May be Co2+.
amount of O.S in a test tube,
add NH4Cl(s), NH4OH(aq) and
H2S.

Confirmatory Test:
Dissolve the black ppt. in aqua A yellow precipitate is formed. Co2+ confirmed.
regia and add water. To this add
NH4OH followed by potassium
nitrite. Acidify the solution with
acetic acid solution.

Group V: Ba+2, Sr2+, Ca2+


Preliminary Test: To small White ppt. May be Ba2+/Sr2+/Ca2+.
amount of O.S in a test tube,
add NH4Cl(s), NH4OH(aq) and
(NH4)2CO3.

Confirmatory Test:
Dissolve the white ppt. in acetic
acid and divide it into 3 parts:
a. To the first part add Yellow ppt. Ba2+ confirmed.
potassium chromate
solution.
b. If barium is absent, take White ppt. Sr2+ confirmed.
second part of the
solution and add
ammonium sulphate
solution.
c. If both barium and White ppt. Ca2+ confirmed.
strontium are absent,
take the third part of the
solution. Add
ammonium oxalate
solution and shake well.

Flame Test: Make a paste of Grassy green flame. Ba2+ confirmed.


given salt in conc.HCl on a
watch glass. Take the paste on Crimson red flame. Sr2+ confirmed.
glass rod/ Platinum wire and
heat in blue zone of flame. Brick red flame. Ca2+ confirmed

Group VI: Mg+2


To small amount of O.S in a test White ppt. is obtained on Mg2+ confirmed.
tube, add NH4Cl(s), NH4OH(aq) scratching the inner walls of
and disodium test tube with glass rod.
hydrogenphosphate solution.

Unknown Salt Analysis:

Anion Analysis:

Salt
+ dil. H2SO4

Gas is evolved No gas evolved


May be CO , S2-, SO32-
3
2-
Salt + conc. H2SO4
Identify the gas and do corresponding
Confirmatory.

Gas evolved No gas evolved

May be Cl-, Br-, I-, NO3-, CH3COO-, C2O42-


Identify the gas and do the corresponding
Confirmatory.
Test for
SO42- or PO43-

Note: if no gas is evolved on adding conc. H2SO4 to the salt, to this add Cu turnings and heat to check for
evolution of brown gas for NO3-.

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