Chemistry Salt Analysis Manual by Savitri

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Chemistry Salt analysis

Estimation of acid radicals (anions)


Classification of anions
Radicals Reaction with dil.H2SO4 Reaction with conc.
H2SO4
Group 1 No reaction
Carbonate CO32- Evolve gas
Acetate CH3COO-
Group 2 Evolve a gas
Chloride Cl- No reaction
Nitrate NO32-
Group 3 No reaction No reaction
Sulphate SO42-

Dil H2SO4

Test Observation Inference


Take about 0.5 g of salt in a Brisk effervescence and Carbonate CO32- may be
clean dry test tube and add evolution of colourless present
dil.H2SO4. odourless gas (CO2)
Take about 0.5 g of salt in a Evolution of acetic acid Acetate CH3COO- may be
clean dry testtube and add dil. vapours with characteristic present
H2SO4. warm the contents if vinegar like odour
no evolution of gas.

Conc. H2SO4

Test Observation Inference


Take about 0.5 g of salt in a Dense white fumes seen Chloride Cl- may be present
clean dry test tube and add
conc.. H2SO4.
Bring a glass rod dipped in
NH4OH near the mouth of
testtube.
Take about 0.5 g of salt in a Evolution of brown fumes. Nitrate NO3- may be present
clean dry test tube and add
conc. H2SO4. add copper
turnings and heat

If no anions are detected with dil. H2SO4 and conc. H2SO4 then the anion is SO4 2-
Salt analysis/savitri/ 2021
Wet test for anions (confirmatory test for anions )
Preparation of sodium carbonate extract
Mix 1 spatula of salt with 2 spatula of solid sodium carbonate in an evaporating dish. To this add
one test tube of water and boil for 10 mins. Cool then filter. This filtrate is sodium carbonate
extract.
Confirmatory Test for CO32-
Test Observation
Take small quantity of salt. To this add dil. Lime water turns milky
H2SO4 pass the gas evolved through lime
water

Confirmatory Test for CH3COO-


Test Observation
Ferric chloride test : Reddish brown ppt seen.
Sodium carbonate extract is acidified with dil
H2SO4and then add freshly prepared neutral
FeCl3 solution and heat if required

Confirmatory Test for Cl-


Test Observation
Silver nitrate test: White ppt which is insoluble in nitric acid and
Neutralize the sodium carbonate extract with soluble in NH4OH
dil. HNO3 till no effervescence is seen. Add
AgNO3 solution.

Confirmatory Test for NO3-


Test Observation
Neutralize the sodium carbonate extract with Brown ring forms just above heavier
dil. H2SO4 till no effervescence is seen. Add sulphuric acid
freshly prepared neutral FeCl3 solution. Pour
conc. H2SO4 gently along the sides of testtube

Salt analysis/savitri/ 2021


Confirmatory Test for SO42-
Test Observation
Neutralize the sodium carbonate extract with White ppt formed which is insoluble in HCl
dil. HCl till no effervescence is seen. Add and HNO3
barium chloride solution to this

Identification of cations
Preparation of original solution (OS)
To maximum quantity of salt add minimum quantity of water to make OS

Classification of cations into groups


Group 0
Salt + NaOH. Pass the gas evolved through Nesslers reagent : Reddish brown ppt seen

Cation group Cation Group reagent Colour of ppt with


group reagent
Group 0 NH4+
Group 1 Pb2+ Dil. HCl PbCl2 (white)
Group 2 Cu2+ H2S in presence of Black (Cu2S)
dil.HCl
Group 3 Al3+ Solid NH4Cl + excess Dirty white
NH4OH (Al(OH)3)
Group 4 Zn2+ H2S in presence of Dirty white (ZnS)
Solid NH4Cl + excess
NH4OH
Group 5 Ba2+ (NH4)2CO3 Solid BaCO3 (White)
Sr2+ NH4Cl + excess SrCO3 (white)
Ca2+ NH4OH CaCO3 (white)

Group 6 Mg2+ Na3(PO4)/ (NH4)3PO4 Mg3(PO4)2 (white)


Solid NH4Cl + excess
NH4OH

Salt analysis/savitri/ 2021


Group 1
Test Observation Inference
To the OS add dil.HCl White ppt Group 1 present

Filter the solution to obtain


ppt.
Dissolve the ppt in hot water
and divide into 3 parts White crystalline ppt Pb2+ present and confirmed
Part 1: cool under tap water Yellow ppt
Part 2: add potassium Yellow ppt
chromate
Part 3: add potassium iodide

If the salt is insoluble in dil HCl check for Pb2+


Group 2
Test Observation Inference
To the OS add dil.HCl. pass Black ppt Group 2 present
H2S gas.
Filter the solution to obtain Bluish green solution
ppt.
Dissolve the ppt in 50%
HNO3and divide into 2 parts Blue colour or ppt Cu2+ present and confirmed
Part 1: add excess conc.
NH4OH Reddish brown ppt
Part 2: add potassium
ferrocyanide solution

Group 3
Test Observation Inference
To the OS add solid NH4Cl White ppt Group 3 present
and excess NH4OH
Filter the solution to obtain
ppt. Blue lake obtained
Dissolve the ppt in dil.HCl
and then add few drops of Al3+ present and confirmed
blue litmus solution. To this
add excess NH4OH solution.

Salt analysis/savitri/ 2021


Group 4
Test Observation Inference
To the OS add solid NH4Cl Dirty White ppt Group 4 present
and excess NH4OH. Pass H2S
gas
Filter the solution to obtain
ppt.
Dissolve the ppt in dil.HCl
and divide the solution in two Zn2+ present and confirmed
parts
Part 1: add NaOH dropwise White ppt formed which
dissolves in excess NaOH

Part 2: add potassium


ferrocyanide solution Bluish white ppt formed

Group 5
Test Observation Inference
To the OS add solid NH4Cl White ppt Group 5 present
,excess NH4OH and
(NH4)2CO3
Filter the solution to obtain
ppt.
Dissolve the ppt in acetic acid
to obtain clear solution.
Divide it into 3 parts

Test for Ba2+ :


Add potassium chromate Yellow ppt Ba2+ present and confirmed

If Ba2+ is absent then


Test for Sr2+
Add (NH4)2SO4 White ppt Sr2+ present and confirmed

If Ba2+ and Sr2+ is absent


then
Test for Ca2+
Add ammonium oxalate and White ppt Ca2+ present and confirmed
allow it to stand for some
time

Salt analysis/savitri/ 2021


Group 6
Test Observation Inference
To the OS add solid NH4Cl White ppt Group 6 present
,excess NH4OH and Mg2+ confirmed
ammonium phosphate or
disodium hydrogen
phosphate. Scratch the inner
side of the testtube
To the OS add few drops of Blue colour or ppt Mg2+ confirmed
magneson reagent and few
drops of NaOH

Salt analysis/savitri/ 2021

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