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salt analysis for zero and first group

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List of Common Anions (Acidic Radicals) for Salt Analysis

Group Anions
Group 1 (Dil H2SO4 Group) CO32- , NO2 - , SO3 2- , S2-
Group 2 (Conc. H2SO4 Group) Cl- , Br- , I- , CH3COO- , NO3 - , C2O4 2-
Group 3 (Independant Group) SO4 2-, PO4 3-

List of Common Cations (Basic Radicals) for Salt Analysis

Group Cation
Group 0 NH4+
Group 1 Pb2+
Group 2 Cu2+
Group 3 Fe3+, Fe2+, Al3+
Group 4 Co 2+, Ni 2+, Mn 2+, Zn 2+
Group 5 Ba 2+, Sr 2+, Ca2+
Group 6 Mg 2+

The first essential step is to prepare a clear and transparent solution of the
salt. This is called original solution. It is prepared as follows:
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 14

Aim: To identify the acidic and Basic radical from the given inorganic salt.

Procedure:

Preliminary Test for Anion(Dil . group)


Experiment Observation Inference
Add a few drops of dilute H2SO4 (sulfuric NO OBSERVATION dilute H2SO4 (CO32- , NO2 - , SO3 2- , S2)
acid) to a small quantity of the salt in a ABSENT
test tube
Preliminary Test for Anion(Conc. . group)
Experiment Observation Inference
Take a small chunk of the salt in a test White, pungent-smelling fumes that Chloride (Cl-) May be present
intensify when a glass rod dipped in
tube and add a few drops of concentrated ammonium hydroxide is brought to the
H2SO4 (sulfuric acid) to it. mouth of the test tube
Confirmatory Test for Anion
Experiment Observation Inference
Add silver nitrate (AgNO3) to the water Formation of a white precipitate which Chloride (Cl-)confirm
extract is soluble in ammonium hydroxide
(NH4OH)
chromyl chloride test
Mix a little amount of salt and an Chloride (Cl-)confirm
equal amount of solid potassium Formation of a yellow precipitate of
dichromate (K2Cr2O7) in a test tube lead chromate
and add conc. H2SO4 to it. Heat the
test tube and pass the evolved gas
through sodium hydroxide solution.
If a yellow solution is obtained,
Acidify the solution with acetic acid
and then add lead acetate solution.
Preliminary Test for Cation (zero group)
Experiment Observation Inference
Take 0.1 g of salt in a test tube and White fumes are observed NH4+ may be present
add 1-2 mL of NaOH solution to
it and heat. If there is a smell of
ammonia, this indicates the
presence
of ammonium ions. Bring a glass
rod dipped in hydrochloric acid
near the mouth of the test tube.
Confirmatory Test for NH4+
On passing the above gas through brown colouration or a NH4+ Confirm
Nessler’s reagent solution precipitate of basic mercury(II)
amido-iodine is formed.

Result: The acidic radical is Chloride (Cl-) (anion) and basic is NH4+

Reaction involved
Anion
Reaction involved

NaCl + AgNO3 NaNO3 + Ag Cl


Silver chloride
(White precipitate
AgCl + 2NH4OH [Ag(NH3)2 ]Cl + 2H2O
Diammine silver (I) chloride (soluble)

4NaCl + K2Cr2O7 + 6H2SO4 2KHSO4 + 2CrO2Cl2 + 4NaHSO4 + 3H2O


(Chromyl chloride)
CrO2Cl2 + 4NaOH Na2CrO4 + 2NaCl + 2H2O
(CH3COO)2Pb + Na2CrO4 PbCrO4 + 2CH3COONa
Sodium chromate Lead chromate (Yellow precipitate)
Cation
(NH4)2 SO4 + 2NaOH Na2SO4 + 2NH3 + 2H2O
NH3 + HCl NH4Cl (white fumes)
2K2HgI4 + NH3 + 3KOH HgO.Hg(NH2)I + 7KI + 2H2O
Basic mercury (II)amido-iodine (Brown precipitate)

Experiment 15
Note: If no positive test is obtained for zero group than proceed for next group by showing
previous groups absent

Aim: To identify the acidic and Basic radical from the given inorganic salt.

Procedure:

Preliminary Test for Anion(Dil . group)


Experiment Observation Inference
Add a few drops of dilute H2SO4 (sulfuric NO OBSERVATION dilute H2SO4 (CO32- , NO2 - , SO3 2- , S2-)
acid) to a small quantity of the salt in a ABSENT
test tube
Preliminary Test for Anion(Conc. . group)
Experiment Observation Inference
Take a small chunk of the salt in a test Brown fumes with a pungent smell Nitrate (NO3-) May be present
tube and add a few drops of concentrated
H2SO4 (sulfuric acid) to it.
Confirmatory Test for Anion
Experiment Observation Inference
Brown Ring Test
Take 1 mL of an aqueous solution Nitrate (NO3-) confirm
of the salt and add 2 mL add A dark brown ring is formed at the
freshly prepared ferrous sulphate junction of the two solutions due to
solution. Mix the solutions the formation of nitroso ferrous
thoroughly and cool the test tube sulphate
under the
tap. Now, add conc. H2SO4
slowly along the sides
of the test tube dropwise so that it
forms a layer on the top of the
liquid
already present in the test tube.
Preliminary Test for Cation (zero group)
Experiment Observation Inference
Take 0.1 g of salt in a test tube and No smell of ammonia NH4+ group absent
add 1-2 mL of NaOH solution to
it and heat.
Preliminary Test for Cation (first group)
Take small quantity of original solution White Precipitate apper Pb2+ May be present
and add Dil HCl to it
Confirmatory Test for Pb2+
Dissolve the precipitate in hot water .
and divide the hot solution into two
parts.
Add potassium iodide solution to the yellow precipitate is obtained. Pb2+ Confirm
first part.
To the second part add potassium A yellow precipitate is obtained which Pb2+ Confirm
chromate solution. is soluble in NaOH and insoluble in
ammonium acetate solution.

Result: The acidic radical is (NO3-) (anion) and basic is Pb2+

Reaction involved
PbCl2 + 2KI PbI2 + 2KCl
(Hot solution) Yellow precipitate
PbCl2 + K2CrO4 PbCrO4 + 2KCl
(Hot solution) Lead chromate
(Yellow precipitate)

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