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ANALYSIS
VOLUMETRIC
ANALYSIS
VOLUMETRIC ANALYSIS-1
Aim:
Prepare M/50 solution of oxalic acid. Use this solution to determine
molarity and the strength of the given potassium permanganate
(KMnO4) solution.
Theory:
The quantity of oxalic acid required for the 250ml of the solution
having a molarity of 0.02M can be calculated as follows.
Molar mass of oxalic acid = 126g/mol
Molarity =mass/Molar mass x V(L)
Materials Required:
1. Oxalic acid
2. Potassium permanganate solution
3. 4N sulphuric acid
4. Chemical balance
5. Burette
6. Burette stand
7. Pipette
8. Conical flask
9. Funnel
10. Measuring flask
11. Weighing bottle
12. White tile
13. Burner
14. Wire gauze
Procedure:
(a) Preparation of 0.02M (1/50M) standard solution of oxalic
acid:
Precautions:
1. Clean all the apparatus with distilled water before starting the
experiment and then rise with the solution to be taken in
them.
2. Rinse the pipette and burette before use.
3. Potassium permanganate is dark in colour, so always read
the upper meniscus.
4. Use dilute sulfuric acid for acidifying the potassium
permanganate.
5. Take accurate readings once it reaches the end point and
don’t go with average readings.
6. Use antiparallex card or autoparallex card while taking the
burette readings.
7. Do not use rubber cork burette as it is can be attacked by
KMnO4.
8. The strength of the unknown solution should be taken upto
two decimal places only.
VOLUMETRIC ANALYSIS-2
Aim:
Prepare M/20 solution of ferrous ammonium sulphate (Mohr’s salt).
Using this solution find out the molarity and the strength of a given
potassium permanganate solution.
Theory:
The quantity of Mohr’s salt required for the 250ml of the solution
having a molarityof 0.05M can be calculated as follows.
The molar mass of mohr’s salt = 392 g/mol
Molarity =mass/Molar mass x V(L)
=molarityxmolarmassx250/1000
=0.05x 392 x250 / 1000
=4.9g
For the preparation of 250 mL of M/20 mohr’s salt solution amount
of mohr’s salt required = 4.9g
Materials Required:
1. Mohr’s salt (ferrous ammonium sulphate)
2. Potassium permanganate solution
3. Dilute sulphuric acid
4. Chemical balance
5. Burette
6. Burette stand
7. Pipette
8. Conical flask
9. Funnel
10. Measuring flask
11. Weighing bottle
12. White tile
13. Burner
14. Wire gauze
Procedure:
1. Wash and rinse the burette and pipette with distilled water
and then rinse with the corresponding solution to be filled
in them.
2. Rinse the burette with the potassium permanganate
solution and fill the burette with potassium permanganate
solution.
3. Fix the burette in the burette stand and place the white tile
below the burette in order to find the endpoint correctly.
4. Rinse the pipette and conical flask with standard ferrous
sulphate solution.
5. Pipette out 20ml of 0.05N standard Mohr’s salt solution
into the conical flask.
6. Add a test tube full of sulphuric acid in order to prevent
oxidation of manganese to form manganese dioxide.
7. Note down the initial reading in the burette before starting
the titration.
8. Now start the titration, titrate against potassium
permanganate solution and simultaneously swirl the
solution in the flask gently.
9. Initially, the purple colour of KMnO4 is discharged with
ferrous ammonium sulfate. The appearance of a
permanent pink colour reveals the endpoint.
10. Repeat the titration until concordant values are obtained.
11. Note down the upper meniscus on the burette readings.
Results:
1. Molarity of given KMnO4 solution =
2. The strength of given potassium permanganate solution =
Precautions:
S.No
Experiment Observation Inference
.
1. Absence of
Copper, Iron,
Colourless
Cobalt,
Colour and appearance of the
Manganese
substance are noted
Nickel salts
2.
Action of heat:
No Absence of
A little of the salt is strongly
characteristic carbonate and
heated in a clean dry test tube
reaction acetate
3. Flame test:
Alittle of the salt is made into a
paste with few drops of conc. No Absence of
HCl. The paste is brought close to characteristic calcium, strontium
a non-luminous flame by means flame and barium
of a platinum wire
RESULT:
THE GIVEN SALT IS ZINC SULPHATE (ZnSO4)
SALT ANALYSIS -2
I. Preliminary Examination
2. Action of heat:
A little of the salt is No characteristic Absence of carbonate
strongly heated in a reaction and acetate
clean dry test tube
3. Flame test:
Alittle of the salt is Crimson colour Presence of
made into a paste strontium ion
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire
RESULT:
2. Action of heat:
A little of the salt is A colourless, Presence of
strongly heated in a odourless gas is carbonate
clean dry test tube evolved which turned
lime water milky.
3. Flame test:
Alittle of the salt is No characteristic Absence of calcium,
made into a paste flame strontium and barium
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire
V.RESULT:
2. Action of heat:
A little of the salt is No characteristic Absence of carbonate
strongly heated in a reaction and acetate
clean dry test tube
3. Flame test:
Alittle of the salt is Brick red colour Presence of calcium
made into a paste ion
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire
RESULT:
I. Preliminary Examination
2. Action of heat:
A little of the salt is Pleasant smelling Presence of acetate
strongly heated in a inflammable vapours
clean dry test tube are evolved.
3. Flame test:
Alittle of the salt is No characteristic Absence of calcium,
made into a paste flame strontium and barium
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire
RESULT:
1 Litmus test
Place a drop of the given Colour changes Presence of
compound on a moist to red carboxylic
blue litmus paper group is
confirmed
2 Ester test
Take about 0.1 g of the Fruity smell Presence of
organic compound ,1 ml carboxylic
of ethyl alcohol and 1-2 group is
drops of conc.H2SO4 in a confirmed
test tube. Heat the
reaction mixture on a
water bath for five
minutes. Pour the
reaction mixture in a
beaker containing water.
Result :
Aim:
1 Litmus test
Place a drop of the given Colour changes Presence of
compound on a moist to red phenol is
blue litmus paper confirmed
2 Liebermann’s test
Place sodium nitrite in a A deep blue or
clean dry test tube and green Presence of
add the given organic colouration phenol is
compound in it. Heat develops confirmed
gently for half a minute
and allow it to cool. Then
add conc. H2SO4 and
shake the tube.
Result :
Result :
RESULT:
Aim:
To identify which of the following A and B contain starch and
glucose
Experiment Observation Inference
1 Fehling’s test
Toa little of the given A: Red A may be
samples add Fehling’s precipitate glucose
solution A and B.Heat it
on a water bath B: no B may be
characteristic starch
change
2 Benedict test
To a little of the given
solutions add Benedict A:reddish ppt. A contains
reagent. Keep the test glucose
tubes in a boiling water B: no
bath. characteristic B contains
change starch
3 Iodine test
To the aqueous A: no
suspension of the characteristic A contains
sample,add 1-2 drops of change glucose
iodine solution
B: appearance of
blue colouration B contains
starch
Result :
RESULT:
Sample A contains protein