Two Salt Analysis PDF

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Never rinse the conical flask with experimental solutions.

Remove the air gaps from the burette.


Do not boil the solution.

Experiment No. 3

Aim : To detect Acid and Basic Radical In given Unknown Inorganic


Sample.

SAMPLE 1

Experiment Observation Inference


1. PHYSICAL EXAMINATION
Colour of the sample is noted White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+
are absent
A little amount of the sample is Pungent smell evolved NH4+ may be present
rubbed between thumb and
finger.
2.Dry Test Tube Heating : Pungent gas evolved along NH4+ ,Cl- may be present
Heated small amount of the with formation of white
sample in a dry test tube. sublimate
3.Flame test was performed. No characteristic colour in Ca2+,Sr2+,Ba2+and Cu2+ may be
the flame absent.

4.Small amount of the sample is Effervescence with S2-, NO2-,may be absent.


treated with dilute H2SO4 and evolution of colourless, CO32- may be present.
and pass the gas through lime odourless gas
water
5.Small amount of the solid Colourless and odourless NO3-, Cl-, Br- may be absent.
sample is treated with gas evolved with CO32- may be present.
concentrated H2SO4. effervescence.
Confirmatory test for acid radicals :
8.Small amount of the solid Effervescence with CO32- is present and
sample is treated with Dilute evolution of colourless, confirmed.
H2SO4 and the evolved gas is odourless gas which turns
passed through lime water. lime water milky.
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for acid radical was
performed.
9. Small amount of the sample is Lime water turns milky and CO32- is present and
treated with dilute H2SO4 and milkiness disappears on confirmed.
and pass the gas through lime passing excess lime water.
water
10. To the aqueous solution of White precipitate was CO32- is present and confirmed
sample MgSO4 solution was formed
added.
Confirmatory test for basic
radicals :

11. Heated the solid sample with Colourless gas with pungent NH4+ (Group 0) may be
NaOH solution in a test tube. smell evolves. present.
Following test was performed
with the evolved gas:
12.A glass rod dipped in HCl White dense fumes NH4+ (Group 0)is present and
was brought near the mouth of produced confirmed.
the test tube.
13.Salt solution + nesslar reagent reddish brown ppt. obtained NH4+ (Group 0) is present and
confirmed.

The given salt contains :


Basic Radical : NH4+
Acid Radical : CO32-

Experiment No. 4

Analysis of Acid and Basic radical in given inorganic


salt.
Aim : To detect Acid and Basic Radical In given Unknown Inorganic
Sample.
SAMPLE 2

Experiment Observation Inference


1. PHYSICAL EXAMINATION
Colour of the sample is noted White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+
are absent
A little amount of the sample is No pungent smell evolved NH4+, S2- may be absent
rubbed between thumb and
finger.
2.Dry Test Tube Heating : Formation of white sublimate NH4+ may be present
Heated small amount of the
sample in a dry test tube.
3.Flame test was performed. No characteristic colour in the Ca2+,Sr2+,Ba2+and Cu2+ may be
flame absent.

4.Small amount of the sample is No gas evolves S2-, NO2-, CO32- may be absent.
treated with dilute H2SO4 .
5.Small amount of the solid Pungent smelling gas evolved . Cl- may be present
sample is treated with It gives dense white fumes with
concentrated H2SO4. rod dipped in NH4OH.
6. When this gas comes in contact Blue Litmus paper turns red Cl- may be present
with blue litmus paper

Confirmatory test for acid radicals :

7.Acidified the solution with Curdy White precipitate Cl - is present and confirmed.
dilute HNO3 and AgNO3 formed which dissoved in
solution was added. excess NH4OH
Confirmatory test for basic
radicals :
13. Heated the solid sample with Colourless gas with pungent NH4+ (Group 0) may be
NaOH solution in a test tube. smell evolves. present.

Following test was performed


with the evolved gas:
14.A glass rod dipped in HCl White dense fumes produced NH4+ (Group 0)is present and
was brought near the mouth of confirmed.
the test tube.
13.Salt solution + nesslar reagent reddish brown ppt. obtained NH4+ (Group 0) is present and
confirmed.

The given salt contains:


Basic Radical : NH4+
Acid Radical : Cl-

Experiment No. 5
Preparation Of Ferrous Ammonium Sulphate (Mohr Salt)
Aim : To Preparare Ferrous Ammonium Sulphate (Mohr Salt)
Materials Required:
Beaker, Conical flask(250ml), Funnel, Glass rod, Tripod Stand, Bunsen Burner

Chemical Required :
Ferrous Sulphate, Ammonium Sulphate, Dilute H2SO4, Distilled water

Theory: When a mixture containing equimolar proportions of ferrous sulphate and ammonium sulphate
is crystallised from its solution, a double salt is formed. The formation of double salt may be
shown as follows:
FeSO4 + (NH4)2 SO4 + 6H2O → FeSO4 . (NH4)2 SO4 . 6H2O
Ferrous ammonium sulphate (Mohr’s salt)
2+
Fe and ions undergo hydrolysis, therefore, while preparing aqueous solutions of ferrous sulphate in
water, 2-3 mL dilute sulphuric acid is added to prevent the hydrolysis of these salts.

Procedure :
➢ Dissolve 3.5 g of ferrous sulphate and 1.7 g of ammonium sulphate (weighed separately), in 5 mL of
distilled water contained in a 50 mL conical flask by heating.
➢ Add about 5 mL of dilute sulphuric acid to the flask and concentrate the solution by heating till the
crystallization point is reached.
➢ Allow the mixture to cool to room temperature slowly.
➢ On cooling, light green crystals of ferrous ammonium sulphate separate out.
➢ Decant the mother liquor and wash the crystals by shaking with very small amounts of 1:1 cold water
and alcohol mixture to remove sticking mother liquor.
➢ Separate the crystals by filtration wash with alcohol, dry between the folds of a filter paper and record
the yield.

Result : Yield of potash alum/Mohr’s salt is 3.8 g.

Precaution:
➢ Cool the solution slowly to get good crystals. Avoid rapid cooling.
➢ Do not disturb the solution while cooling.
➢ Avoid prolonged heating while preparing crystals of ferrous ammonium sulphate, as it may oxidise
ferrous ions to ferric ions and change the stoichiometry of the crystals.

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