Chemistry Lab

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CHEMISTRY

ACID RADICAL(ANION) ANALYSIS

BASIC METHOD
Dil H2SO4 - Carbonate(CO32-)
Conc H2SO4 - Acetate(CH3COO-),Chloride(Cl-),Nitrate(NO3-)
Special Case - Sulphate(SO42-)

Carbonate(CO32-)
● To the given salt add dil H2SO4 . Brisk effervescence. Pass
through lime water. Turns lime water milky.
Acetate(CH3COO-)
● To the given salt add conc H2SO4 . Vinegar smell.
Chloride(Cl-)
● To the given salt add conc H2SO4 . Bubbles are seen.
Nitrate(NO3-)
● To the given salt add conc H2SO4 . Heat the contents of
beaker. Reddish brown fumes are seen.
Sulphate(SO42-)
● Dilute the given salt by adding water. To the solution add
BaCl2. A white coloured ppt is formed that is insoluble in all
mineral acids.

CONFIRMATORY TEST:
Experiment Observation Inference
2-
CO3 To the salt add dil H2SO4 A colourless, odourless CO32- is confirmed
gas is evolved that turns
lime water milky
CH3COO- To the salt add neutral A vine red colour is CH3COO- is
FeCl3(neutral ferric chloride) observed confirmed
Cl- To the salt add Silver Nitrate A white ppt is formed Cl- is confirmed
solution (AgNO3) which is soluble in
excess NH4OH
NO3- To the salt add freshly A brown ring is formed NO3- is confirmed
prepared ferrous sulphate at the junction of the
(FeSO4) and then add conc layers.
H2SO4 along the sides of the
test tube.
SO42- Dilute the given salt by A white coloured ppt is SO42- is confirmed
adding water. To the solution formed that is insoluble
add BaCl2. in all mineral acids.

SODIUM CARBONATE EXTRACT(SE)Only for insoluble salts

It converts insoluble salts to soluble extract. Without SE there


will be a ppt, hence low visibility of brown ring.
Formation:
● In a beaker add 1 spatula of the given salt,1/2 spatulas of
Sodium carbonate, 20 ml of water
● Boil the solution using a burner until bubbles are seen
● Filter the contents of beaker. The extract formed is Sodium
Carbonate Extract
● Split the extract to do experiment

Carbonate(CO32-)
Same as confirmatory test.
Acetate(CH3COO-)
● To the SE add dil HCl till effervescence ceases. To convert all the CO 32- to
CO2.
● To the solution add neutral FeCl3(reagent)
Observation: A vine red colour is formed
Chloride(Cl-)
● To the SE add dil HNO3 till effervescence ceases.
● To the solution add AgNO3(reagent)
Observation: A curdy white ppt is obtained which is soluble in excess NH4OH

Nitrate(NO3-)
● To the SE add dil H2SO4 till effervescence ceases.
● Add freshly prepared ferrous sulphate (FeSO4) and then add conc H2SO4
along the sides of the test tube.
Observation: A brown ring is formed at the junction of the layers.

Sulphate(SO42-)
● To the SE add dil HCl till effervescence ceases.
● To the solution add BaCl2(reagent)
Observation: A white ppt is formed insoluble in all mineral acids.

BASIC RADICAL(CATION) ANALYSIS

GROUP ION
Group 0 NH4+
Group 1 Pb2+
Group 2 Cu2+ (not general cause coloured
salt)
Group 3 Al3+ Fe2+ (not general cause
coloured salt)
Group 4 Zn2+
Group 5(BSC) Ba2+, Ca2+, Sr2+
Group 6 Mg2+

⮚ GROUP 0 (All ammonium salts are soluble in water)


Salt (direct)+ NaOH + Heat ( ∆ ) → Gas(ammonia )evolved mosit redlitmus paper blue (Basic )

Confirmatory: Pass the gas through Nessler’s reagent. A Reddish


Brown ppt is seen.
Conclusion: Group 0 Cation is confirmed

IF IT IS NOT GROUP 0 PREPARE 0RIGINAL SOLUTION


PREPERATION OF OS
Know if soluble or insoluble in water. (PbCO3 is insoluble). All carbonate
salts are insoluble except for Na2CO3
If soluble in water,
Salt+H20
Dilute the given salt by adding water. Make sure that the solution is
concentrated and fills only 1/4th of a boiling tube. No salt should settle
down.
If insoluble in water (CO32- salts),
Salt+ dil HCl
If salt doesn’t from clear solution with dil HCl then,
Salt+ dil HNO3 usually PbCO3

⮚ GROUP 1 ( Pb2+)

OS +dil HCl →White ppt (Lead chloride)

Confirmatory: Slightly heat the white ppt. The ppt dissolves and ppt
becomes soluble. Take potassium chromate(yellow colour) solution
and a perfect yellow ppt is observed.
Conclusion: Group 1 Cation is confirmed

⮚ GROUP 2(Cu2+)

OS+dil HCl+ ( passthru ) H 2 S ↑ → Black ppt (CuS)

Confirmatory: OS+ potassium ferro cyanide🡪Chocolatey brown ppt


Conclusion: Group 2 Cation is confirmed

⮚ GROUP 3(Al3+)
OS+ N H 4 C l ( s) +excess N H 4 OH →Gelatinous white ppt

Confirmatory: Dissolve the gelatinous white ppt in minimum quantity


of dil HCl. To this add a few drops of blue litmus solution followed by
NH4OH till solution becomes basic. A floating, blue layer is formed on
the surface of the clear solution.
Conclusion: Group 3 Cation is confirmed

⮚ GROUP 4(Zn2+)

OS + N H 4 C l ( s) +excess N H 4 OH + ( pass thru ) H 2 S →White ppt

Confirmatory: Take NaOH and add to salt solution. A white ppt formed.
Add excess NH4OH to ppt. Ppt dissolves.
Salt solution+ Potassium Ferro Cyanide🡪 white ppt of zinc ferro cyanide
Conclusion: Group 4 Cation is confirmed

⮚ GROUP 5(Ba2+, Sr2+, Ca2+)

OS+ N H 4 C l ( s) +excess N H 4 OH + ( N H 4 ) 2 C O 3 →White ppt


Process: First prepare the OS using dil HCl. Make sure completely dissolved
(Very slow process).
To the OS add 1 spatula of N H 4 C l( s) and dissolve completely.
Now take red litmus paper. To the solution add excess N H 4 OH until and unless
the solution becomes basic (red litmus turns blue)
To the basic solution add ( N H 4 ) 2 C O3 . We will get a white ppt.
Filter out the solution and let the ppt remain the filter paper until full soln is
removed. The liquid part is not needed for the further analysis.
Take acetic acid in a test tube and heat it. Pour the hot acetic acid in the filter
paper with the white ppt and collect the filtrate in three test tubes.
(i)The one test tube add potassium dichromate (yellow in colour). On adding, if
we get a yellow colour ppt
Conclusion: Ba2+ cation is confirmed.

(ii)If the (i) doesn’t work split the solution in 2 test tubes and add potassium
dichromate (yellow in colour) to one. On adding, if we do not get a yellow
colour ppt add dil H2SO4 to the second test tube. We will get a white ppt.
Conclusion: Sr2+ cation is confirmed.

(iii)If the above tests don’t work add ammonium oxalate to the solution in the
3rd test tube. On adding, it will either dissolve or a white ppt is formed.
If a white ppt is formed add potassium permanganate. It will decolourize the
potassium permanganate. If it dissolves well done.
Conclusion: Ca2+ cation is confirmed.

⮚ GROUP 6(Mg2+)
OS+ Na H 2 PO 4 → White ppt

(sodium di hydrogen phosphate)


Confirmatory: Add NH4Cl, add excess NH4OH. Add
(NH4)3PO4 (ammonium phosphate) . A white colour ppt is seen .
Conclusion: Group 6 Cation is confirmed

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