#ASSAY OF PHENOBARBITONE
Aim:
To determine the
percentage purity of phenobarbitone present in the given powder.
Apparatus:
Burette,
Pipette, Burette stand, conical flask.
Chemicals: Silver nitrate,
phenobarbitone, sodium carbonate, potassium chromate indicator.
Principle:
Assay of phenobarbitone comes under
precipitation titration. Barbiturates when interact with silver nitrate in the
presence of sodium carbonate initially it forms one substituted sodium salt of
phenobarbitone, which reacts with silver nitrate (AgNO3) with the formation
of soluble one-substituted Ag-salt. Then soluble Na-Ag-salt is formed. In
equivalence point excess of titrant AgNO3 destroys Na-Ag-salt and
the insoluble two-substituted Ag-salt of phenobarbitone is formed, that
indicates the end point.
Procedure:
Standardisation
of Silver nitrate: Weigh accurately 0.5g (5ml) of NaCl and
add 10ml of water in to conical flask. Add 0.5ml of indicator and titrate
against AgNO3 solution until brick red colour precipitate was formed.
Each ml of
0.1M AgNO3 ≡
0.005844gm of NaCl
Assay: Weigh accurately about 2.0 g of phenobarbitone, add 30 ml of water
and 3 g of sodium carbonate, stirr to dissolve and titrate with 0.1
M silver nitrate until a distinct turbidity was observed when Viewed against a
black background, the solution being stirred vigorously throughout the
titration.
1 ml of 0.1
M silver nitrate is equivalent to 0.02542 g of C12H11N2NaO3.
Calculations:
Standardisation
of AgNO3:
S. No
|
Contents in
the flask
|
Burette
Reading
|
Volume
Consumed
|
Indicator
|
|
Initial
|
Final
|
||||
|
|
|
|
|
|
1
|
|
|
|
|
|
2
|
|
|
|
|
|
Each ml of 0.1M AgNO3≡
0.005844gm of NaCl
X ml of Y M of AgNO3≡ -----gms of NaCl
Y =
Assay:
S. No
|
Contents of
the flask
|
Burette
reading
|
Volume
consumed
|
Indicator
|
|
Initial
|
Final
|
||||
1
|
|
|
|
|
|
1ml of 0.1M AgNO3≡ 0.02542 gms of C12H11N2NaO3.
X ml of Y MAgNO3≡
Z gm of C12H11N2NaO3.
Z=
Percentage
purity = Estimated amount / Weight of powder taken
Report:
The
percentage purity of phenobarbitone
Sodium
present in given sample is found to be ………………
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