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Salt Analysis

The document outlines a systematic approach for anion and cation analysis using various reagents and confirmatory tests to identify specific ions in a salt sample. It details the observations and inferences for each ion tested, including carbonate, sulfate, chloride, and others, along with their respective confirmatory tests. Additionally, it describes the preparation of the original solution and the procedures for identifying unknown salts through gas evolution and precipitation reactions.

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aanya rustagi
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0% found this document useful (0 votes)
32 views8 pages

Salt Analysis

The document outlines a systematic approach for anion and cation analysis using various reagents and confirmatory tests to identify specific ions in a salt sample. It details the observations and inferences for each ion tested, including carbonate, sulfate, chloride, and others, along with their respective confirmatory tests. Additionally, it describes the preparation of the original solution and the procedures for identifying unknown salts through gas evolution and precipitation reactions.

Uploaded by

aanya rustagi
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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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 May be CO32-


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

Sulphide S2- Colourless gas with May be S2-.


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

Sulphite SO32- Colourless gas with May be SO32-


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

Chloride Cl- Colourless gas with May be Cl-.


Preliminary Test: To small pungent smell is evolved.
amount of salt in a test
tube, add a small amount
of conc. H2SO4. White ppt soluble in aq.NH3. Cl-is confirmed.
Confirmatory test: To 1mL
of salt solution (aqueous)
add 1mL AgNO3 solution.

Bromide Br- Reddish brown gas with May be Br-.


Preliminary Test: To small pungent smell is evolved.
amount of salt in a test
tube, add a small amount
of conc.
H2SO4. Off-white ppt partially Br-is confirmed.
Confirmatory test: To 1mL soluble in aq.NH3.
of salt solution (aqueous)
add 1mL AgNO3 solution.

Iodide I- Violet gas is evolved. May be I-.


Preliminary Test: To small
amount of salt in a test
tube, add a small amount
of conc. H2SO4. Pale Yellow ppt insoluble I-is confirmed.
Confirmatory test: To 1mL in aq.NH3is formed.
of salt solution (aqueous)
add 1mL AgNO3 solution.

Nitrate NO3- Pungent brown gas is evolved. May be NO3-.


Preliminary Test: To small
amount of salt in a test
tube, add a small amount
of conc. H2SO4. Heat and
add half Brown ring is formed at NO3-is confirmed.
spatula Copper turnings. the junction of two
Confirmatory test: To 1mL of solutions.
salt solution (aqueous) add
2-3 mL freshly prepared
FeSO4 solution. Add conc.
H2SO4 along sides.

May be CH3COO-.
Acetate CH3COO-:
Preliminary Test: To small Colourless, pungent gas
amount of salt in a test with vinegar like smell is
tube, add a small amount evolved.
CH3COO is confirmed.
of conc. H2SO4.
Confirmatory test: To 1mL
of salt solution (aqueous) Red Colouration
add 1mL FeCl3 solution.

Oxalate C2O42-: Colourless gas with May be C2O42-.


Preliminary Test: To small brisk effervescence is
amount of salt in a test evolved.
tube, add a small amount
of conc. H2SO4. C2O42-is confirmed.
Confirmatory test: To 1 mL White ppt. insoluble in
of salt solution(aqueous) acetic acid.
add 1 mL CaCl2 solution.

Sulphate SO42- White ppt. insoluble in dil. SO42-is confirmed.


Confirmatory Test: HCl is formed.
To 1 mL salt
solution(aqueous), add 1 mL
BaCl2 solution.
Phosphate PO43-:
Confirmatory Test:

To 1 mL aqueous salt Canary yellow ppt is formed. PO43-is confirmed.


solution, add 1-2 mL conc.
HNO3 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 Sulphides


in 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. HNO 3in 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 NH4+ Colourless gas with May be NH4+


Preliminary Test: To small ammoniacal smell is
amount of salt in a test tube, evolved.

add a small amount of NaOH. Dense white fumes. NH4+ confirmed.

Bring a glass rod dipped in


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

Group I:Lead Pb+2 White ppt. is formed. May be Pb2+.


Preliminary Test: To small
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 Yellow ppt. Pb2+ confirmed.
parts: a. To part 1 add KI. Yellow ppt. Pb2+ confirmed.
b. To part 2 add K2CrO4. White ppt. soluble in Pb2+ confirmed.
c. To part 3 add dil. H2SO4. Ammonium acetate.

Group II: Lead Pb+2 Black ppt. May be Pb2+.


Preliminary Test: To small
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 Black ppt. is formed. May be Cu2+.
Preliminary Test: To small
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: White ppt. is formed which Cu2+ confirmed.
a. To part 1 add excess dissolves in excess NH4OH
NH4OH. to give a deep blue solution.

Chocolate brown ppt. is Cu2+ confirmed.


b. To part 2 add formed.
Potassium
ferrocyanide.

Group III: Aluminium Al3+ Gelatinous white ppt. May be Al3+.


Preliminary Test: To small
amount of O.S in a test tube,
add NH4Cl(s) and
NH4OH(aq). Bluish white ppt. in Al3+ confirmed.
colourless solution.
Confirmatory Test:
Lake Test: Dissolve the
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+ Reddish brown ppt. May be Fe3+.
Preliminary Test: To small
amount of O.S in a test tube,
add NH4Cl(s) and
NH4OH(aq).

Confirmatory Test:
Dissolve the ppt. in dil HCl Prussian Blue Solution. Fe3+ confirmed.
and divide the solution into 2
parts: a. To part 1 add
Blood red solution. Fe3+ confirmed.
Potassium ferrocyanide.
b. To part 2 add
Potassium
thiocyanate.
Dirty white ppt. May be Zn2+.
Group IV: Zinc Zn+2
Preliminary Test: To small
amount of O.S in a test tube,
add NH4Cl(s), NH4OH(aq) and
H2S.

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

Group IV: Manganese Mn+2 Buff ppt. May be Mn2+.


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

Confirmatory Test: White ppt. which turns brown Mn2+ confirmed.


Dissolve the dirty white ppt. in
on standing.
dil HCl and to this add NaOH
solution.

Group IV: Nickel Ni+2 Black ppt. May be Ni2+.


Preliminary Test: To small

amount of O.S in a test tube, Rose red ppt. Ni2+ confirmed.


add NH4Cl(s), NH4OH(aq) and
H2S.

Confirmatory Test:
Dissolve the black ppt. in
aqua regia and add water. To
this add 1 mL of NH4OH
followed by Di-
methylglyoxime solution.
Group IV: Cobalt Co+2 Black ppt. May be Co2+.
Preliminary Test: To small
amount of O.S in a test tube,
add NH4Cl(s), NH4OH(aq) and
H2S.

Confirmatory Test: A yellow precipitate is Co2+ confirmed.


Dissolve the black ppt. in
aqua regia and add water. To formed.
this add NH4OH followed by
potassium nitrite. Acidify the
solution with acetic acid
solution.

Group V: Ba+2, Sr2+, Ca2+ White ppt. May be Ba2+/Sr2+/Ca2+.


Preliminary Test: To small
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 Crimson red flame. Sr2+ confirmed.
on glass rod/ Platinum wire
and heat in blue zone of Brick red flame. Ca2+ confirmed
flame.

Group VI: Mg+2

To small amount of O.S in a White ppt. is obtained on Mg2+ confirmed.


test tube, add NH4Cl(s), scratching the inner walls of
NH4OH(aq) 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 CO32-, S2-, SO32- 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
2-
SO or PO43-
4

Note: if no gas is evolved on adding conc. H2SO4to the salt, to this add Cu turnings and heat to check for
evolution of brown gas for NO3-.

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