|
1.0
|
NAME : 1.0 M HYDROCHLORIC ACID
|
|
2.0
|
REAGENTS :
1.0
Hydrochloric Acid.
2.0
Anhydrous sodium Carbonate
3.0
Methyl
red
|
|
3.0
|
METHOD OF PREPARATION:
Dilute
85.0 ml of concentrate hydrochloric acid with purified water to
produce 1000 ml.
|
|
4.0
|
METHOD OF STANDARDIZATION:
Weigh
accurately about 1.5 g of anhydrous sodium carbonate, previously heated at about
270° for 1 hour. Dissolve it in 100 ml of distilled water and add 0.1 ml of methyl red solution
Add
the acid slowly from a burette, with constant stirring, until the solution
becomes faintly pink. Heat the solution to boiling, cool and continue the
titration.
Heat
again to boiling and titrate further as necessary until the faint pink colour
is no longer affected by continued boiling.
Each ml of 1 M hydrochloric acid is equivalent
to 0.05299 g of Na2CO3.
|
|
5.0
|
CALCULATION:
=
Wt. of Na2CO3
(gm)x 1.0x Assay of Na2CO3
B.R. X 0.05299 X 100
B.R.:
Burette Reading in ml
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 1 M SODIUM HYDROXIDE.
|
|
2.0
|
REAGENTS :
1.0
Sodium hydroxide
2.0
Potassium hydrogen phthalate.
3.0
Phenolphthalein
solution.
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
42 g of sodium
hydroxide in sufficient carbon dioxide-free distilled water to
produce 1000 ml.
|
|
4.0
|
METHOD OF STANDARDIZATION
:
Weigh
accurately about 2.0 g of potassium hydrogen phthalate, previously powdered and
dried at 120o for 2 hours, and dissolve in 75 ml of carbon dioxide-free
distilled water.
Add
0.1 ml of phenolphthalein
solution and titrate with the sodium hydroxide solution until a
permanent pink colour is produced.
Each
ml of 1M
sodium hydroxide is equivalent to 0.2042 g of C8H5KO4.
|
|
5.0
|
CALCULATION:
=
Wt. of KHP (gm)x 1.0x Assay
of KHP
B.R. X 0.2042 X 100
B.R.:
Burette Reading in ml
|
|
6.0
|
REFERENCE: Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M SODIUM HYDROXIDE
|
|
2.0
|
REAGENTS :
1.0
Sodium hydroxide
2.0
Potassium hydrogen phthalate
3.0
Phenolphthalein
solution.
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
4.2 g of sodium
hydroxide in sufficient carbon dioxide-free distilled water to
produce 1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Weigh
accurately about 0.5 g of potassium hydrogen phthalate, previously powdered and
dried at 120o for 2 hours, and dissolve in 75 ml of carbon dioxide-free
distilled water.
Add
0.1 ml of phenolphthalein
solution and titrate with the sodium hydroxide solution until a
permanent pink colour is produced.
Each
ml of 0.1M
sodium hydroxide is equivalent to 0.02042 g of C8H5KO4.
|
|
5.0
|
CALCULATION:
= Wt.
of KHP (gm)x 0.1 x Assay of KHP
B.R. X 0.02042
X 100
B.R.:
Burette Reading in ml
|
|
6.0
|
REFERENCE: Indian Pharmacopoeia
|
|
1.0
|
NAME : 1.0 M SULPHURIC ACID (H2SO4)
|
|
2.0
|
REAGENTS :
1.0
Concentration H2SO4.
2.0
Anhydrous
sodium Carbonate
3.0
Methyl red
|
|
3.0
|
METHOD OF PREPARATION
:
Take
54 ml of conc. H2SO4 in about 600 ml of H2O
in 1000 ml of volumetric flask; cool & finally make the volume to 1000 ml
with distilled water.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Take
about 3.0 gm of anhydrous Na2CO3 dried previously at
270ºC for one hour.
Dissolve it in 100 ml of distilled water,
add 0.1 ml of methyl red as indicator & titrate with 1 M H2SO4
with constant stirring until the solution becomes faintly pink.
Heat
the solution to boiling cool & continue the titration until the faint
pink colour is no longer affected by continue boiling.
Each
ml of 1 M H2SO4 is equivalent to 0.10598 gm of Na2CO3
(Sodium Carbonate).
|
|
5.0
|
CALCULATION:
=
Wt. of Na2CO3
(gm)x 1.0x Assay of Na2CO3
B.R. X 0.10598 X 100
B.R.:
Burette Reading in ml
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.5 M SULPHURIC ACID (H2SO4)
|
|
2.0
|
REAGENTS :
1.0
Concentration H2SO4.
2.0
Anhydrous
sodium Carbonate
3.0
Methyl red
|
|
3.0
|
METHOD OF PREPARATION
:
Take
30 ml of conc. H2SO4 in about 600 ml of H2O
in 1000 ml of volumetric flask; cool & finally make the volume to 1000 ml
with distilled water.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Take
about 1.50 gm of anhydrous Na2CO3 dried previously at
270ºC for one hour.
Dissolve
it in 100 ml of distilled water, add 0.1 ml of methyl red as indicator &
titrate with 1 M H2SO4 with constant stirring until the
solution becomes faintly pink.
Heat
the solution to boiling cool & continue the titration until the faint
pink colour is no longer affected by continue boiling.
Each
ml of 0.5 M H2SO4 is equivalent to 0.05299 gm of Na2CO3
(Sodium Carbonate).
|
|
5.0
|
CALCULATION:
=
Wt. of Na2CO3
(gm)x 1.0x Assay of Na2CO3
B.R. X 0.05299 X 100
B.R.:
Burette Reading in ml
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M DISODIUM EDETATE (EDTA)
|
|
2.0
|
REAGENTS :
1.0
Disodium Edetate.
2.0
Calcium
Carbonate
3.0
Eriochrome black – T
4.0
Ammonia –ammonium Chloride Buffer pH10
(Dissolve 5.4 gm of NH4Cl + 35ml of 10M NH3 solution
& dilute to 100 ml with distilled water.)
5.0
Hydrochloric Acid.
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
37.2 g of disodium
edetate in sufficient distilled water to produce 1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Take
about 200 mg of CaCO3 dried previously at 110ºC for Two hour, Dissolve in
minimum -
Quantity
of hydrochloric acid, and add 50 ml of purified water and 10 to 15 ml Ammonia
–ammonium hydroxide Buffer.
Titrate
against 0.1M EDTA.
End
point Violet to bluish black.
Each
ml of 0.1 M EDTA is equivalent to 0.010009 gm of CaCO3.
|
|
5.0
|
CALCULATION :
= Wt
of CaCO3 (gm) X 0.1x Assay of CaCO3
B.R. x 0.010009 X 100
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE: Indian Pharmacopoeia
/ United state Pharmacopoeia
|
|
1.0
|
NAME : 0.05 M DISODIUM EDETATE (EDTA)
|
|
2.0
|
REAGENTS :
6.0
Disodium Edetate.
7.0
Calcium
Carbonate
8.0
Eriochrome black – T
9.0
Ammonia –ammonium Chloride Buffer pH10
(Dissolve 5.4 gm of NH4Cl + 35ml of 10M NH3 solution
& dilute to 100 ml with distilled water.)
10.0
Hydrochloric Acid.
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
18.6 g of disodium
edetate in sufficient distilled water to produce 1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Take
bout 100 mg of CaCO3 dried previously at 110ºC for Two hour, Dissolve in
minimum -
Quantity
of hydrochloric acid, and add 50 ml of purified water and 10 to 15 ml Ammonia
–ammonium hydroxide Buffer.
Titrate
against 0.05M EDTA.
End
point Violet to bluish black.
Each
ml of 0.05 M EDTA is equivalent to 0.0050045 gm of CaCO3.
|
|
5.0
|
CALCULATION :
= Wt of CaCO3 (gm) X 0.05 x Assay of CaCO
B.R. X 0.0050045 X 100
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE: Indian
Pharmacopoeia / United state Pharmacopoeia
|
|
1.0
|
NAME : 0.05 M IODINE
|
|
2.0
|
REAGENTS :
1.0
Iodine.
2.0
Potassium Iodide
3.0
Arsenic Trioxide
4.0
Hydrochloric Acid
5.0
Sodium Hydroxide
6.0
Methyl orange.
7.0
Sodium bicarbonate
8.0
Starch solution
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
about 14 g of iodine
in a solution of 36 g of potassium iodide in 100 ml of distilled water , add three
drops of hydrochloric
acid and dilute with distilled water
to 1000 ml
(Note
:- Dissolve Iodine in 100 ml KI solution then make up volume to 1000 ml )
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Weigh
accurately about 0.15 g of arsenic trioxide, previously dried at 105° for 1 hour,
and dissolve in 20 ml of 1M sodium hydroxide by warming, if necessary.
Dilute
with 40 ml of distilled
water, add 0.1 ml of methyl orange solution and add drop
wise dilute
hydrochloric acid until the yellow colour is changed to pink.
Add
2 g of sodium bicarbonate
dilute with 50 ml of distilled water and add 3 ml of starch solution.
Titrate with 0.05 M iodine until a permanent blue colour is produced.
Each
ml of 0.05 M
iodine is equivalent to 0.004946 g of As2O3
|
|
5.0
|
CALCULATION :
= Wt. of As2O3 (gm) X 0.05 X Wt. of As2O3
B.R. x 0.004946 X 100
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE: Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M CERIC AMMONIUM SULPHATE
|
|
2.0
|
REAGENTS :
1.0
Ceric
Ammonium sulphate
2.0
Arsenic
trioxide
3.0
Sodium
hydroxide (8.0 % w/v)
4.0
Sulphuric
Acid
5.0
Ferroin
sulphate solution
6.0
Osmic
acid (1 %w/v)
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
65 g of ceric
ammonium sulphate, with the aid of gentle heat,
in a mixture of 30.0 ml of sulphuric acid and 500 ml of distilled water.
Cool,
filter the solution, if turbid, and dilute to 1000 ml with distilled water.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Weigh
accurately about 0.2 g of arsenic trioxide, previously dried at 105 ° for 1 hour,
and transferred to a 500- ml conical flask.
Wash
down the inner walls of the flask with 25 ml of a 8.0% w/v solution of sodium hydroxide,
swirl to dissolve, add 100 ml of distilled water and mix. Add 30 ml of
dilute
sulphuric acid, 0.15 ml of osmic acid solution, 0.1 ml of ferrroin sulphate
solution and slowly titrate with the ceric ammonium sulphate
solution until the pink colour is changed to a very pale blue, adding the
titrant slowly towards the end- point.
Each
ml of 0.1 M
ceric ammonium sulphate is equivalent to 0.004946 g of As2O3.
|
|
5.0
|
CALCULATION :
= Wt. of As2O3 (gm) X 0.1 X Wt. of As2O3
B.R. x 0.004946 x 100
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE: Indian
Pharmacopoeia
|
.
|
1.0
|
NAME : 0.1 M SODIUM NITRITE
|
|
2.0
|
REAGENTS :
1.0
Sodium nitrite
2.0
Sulphanilic acid.
3.0
Potassium bromide.
4.0
2M Hydrochloric Acid
5.0
Starch
iodide paper
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
7.5 g of sodium
nitrite in sufficient distilled water to produce 1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Dissolve
0.3 g of
sulphanilic acid in 50 ml of 2 M hydrochloric acid, add 3 g of potassium bromide, cool
in ice and titrate with the sodium nitrite solution using starch iodide paper
as indicator.
Each
ml of 0.1 M
sodium nitrite is equivalent to 0.01732 g of C6H7NO3S.
|
|
5.0
|
CALCULATION :
= Wt. of C6H7NO3S.
(gm) X 0.1
B.R. x 0.01732
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M SILVER NITRITE
|
|
2.0
|
REAGENTS :
1.0
Silver Nitrate
2.0
Acetic acid.
3.0
Sodium
chloride
4.0
Methanol
5.0
Eosin
solution
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
17.0 g of Silver Nitrate in sufficient double distilled water to produce
1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Weigh
accurately about 0.1 g of sodium chloride, previously dried at 110o for
2 hours and dissolve in 5 ml of distilled water.
Add
5 ml of acetic
acid, 50 ml of methanol and 0.15 ml of eosin solution.
Stir,
preferably with magnetic stirrer, and titrate with the silver nitrate
solution.
Each
ml of 0.1 M
silver nitrate is equivalent to 0.005844 g of NaCl.
|
|
5.0
|
CALCULATION :
= Wt. of
NaCl (gm) X 0.1 X Assay of NaCl
B.R. x 0.005844 x 100
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M POTASSIUM HYDROXIDE (KOH)
|
|
2.0
|
REAGENTS :
1.0
Potassium
hydroxide
2.0
Hydrochloride Acid.
3.0
Phenolphthalein
solution
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
6.0 g of potassium hydroxide in sufficient carbon dioxide (CO2) free double
distilled water to produce 1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Titrate
20 ml of the solution with 0.1 m Hydrochloride Acid using 0.5 ml of phenolphthalein
solution as indicator until colour changes from pink to colourless.
Each ml of 0.1 M Hydrochloride Acid is equivalent
to 0.005611 g of Potassium hydroxide (KOH).
|
|
5.0
|
CALCULATION :
= Molarity of Hydrochloride Acid x Volume of Hydrochloride Acid
Volume taken of KOH
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M SODIUM THIOSULPHATE (Na2S2O3)
|
|
2.0
|
REAGENTS :
1.0
Sodium Thiosulphate
2.0
Sodium Carbonate
3.0
Potassium Bromate
4.0
Potassium Iodide
5.0
Hydrochloric Acid
6.0
Starch Solution
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
25 g of sodium
thiosulphate and 0.2 g of sodium carbonate in carbon dioxide-free
distilled water and dilute to 1000 ml with the distilled water
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Dissolve 0.200 g of potassium
bromate, weighed accurately, in sufficient distilled water to produce 250.0 ml.
To 50.0 ml of this solution add 2 g of
potassium iodide and 3 ml of 2M hydrochloric acid and titrate with the sodium
thiosulphate solution using starch solution, added towards the end of the
titration, as indicator until the blue colour is discharged.
Each ml of 0.1M sodium thiosulphate
is equivalent to 0.002784 g of KBrO3.
Re-standardize
the solution frequently.
|
|
5.0
|
CALCULATION :
= Wt. of
KBrO3. (gm) X 0.1 X Assay of KBrO3.
B.R. x 0.002784 X 100
Burette
Reading in ml.
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M AMMONIUM THIOCYANATE (NH4SCN)
|
|
2.0
|
REAGENTS :
1.0
Ammonium Thiocyanate
2.0
0.1 M Silver Nitrate
3.0
Nitric Acid
4.0
Ferric
ammonium Sulphate
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
7.612 g of ammonium
thiocyanate in 1000 ml volumetric flask, add 500 ml distilled water
mixed thoroughly & make up to 1000 ml. with distilled water.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Pipette 30.0 ml of 0.1 M silver nitrate into
a glass-stoppered flask, dilute with 50 ml of distilled water, add 2 ml of nitric acid
and 2 ml of ferric
ammonium sulphate solution and titrate with the ammonium thiocyanate
solution to the first appearance of a red-brown colour.
Each ml of 0.1 M silver nitrate is
equivalent 0.007612 g of NH4SCN.
|
|
5.0
|
CALCULATION :
= Molarity of 0.1 M silver nitrate x 30
B.R.
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M FERROUS AMMONIUM SULPHATE
|
|
2.0
|
REAGENTS :
1.0
Ferrous ammonium sulphate
2.0
Sulphhuric acid
3.0
1,10-phenanthroline solution
4.0
0.1 M
ceric ammonium
sulphate
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
40 g of ferrous
ammonium sulphate in a previously cooled mixture of 40 ml of sulphuric acid and
200 ml of distilled
water, dilute with sufficient freshly boiled and cooled distilled water to
produce 1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Measure accurately 25.0 ml of the
solution into a flask, add 2 drops of 1,10-phenanthroline solution and
titrate with 0.1
M ceric
ammonium sulphate until the red colour is changed to pale blue.
Each ml of 0.1 M ceric ammonium
sulphate is equivalent to 0.03921g of Fe(NH4)2(SO4)2,
6H2O.
|
|
5.0
|
CALCULATION :
= Molarity of 0.1 M ceric ammonium
sulphate x T.R. of ceric ammonium sulphate
Vol.of
Solution ferrous ammonium sulphate
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M ZINC SULPHATE
|
|
2.0
|
REAGENTS :
1.0
Zinc Sulphate.
2.0
Acetic acid-Ammonium acetate buffer(77.1 gm Ammonium acetate in
water +57 ml Acetic acid
diluted to 1000 with water).
3.0
Dithiazone solution (25.6 mg in 100 ml alcohol, store in cool
place,
use within 2 month.
4.0
0.05M
disodium edetate(
EDTA)
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve
29 g of zinc
sulphate in sufficient distilled water
to produce 1000 ml.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Pipette
20ml of standard 0.05 EDTA solution in a conical flask.
Add 10ml of Acetic acid-Ammonium acetate buffer,
50ml of alcohol and 2ml of
Dithiazone solution. Titrate with 0.1M ZnSO4
solution to a clear pink colour end point.
1 ml of c is
equivalent to 0.02875 g of ZnSO4,7H2O
|
|
5.0
|
CALCULATION :
Molarity
of 0.05M EDTA x 20
B.R.
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE : United state Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M PERCHLORIC ACID
|
|
2.0
|
REAGENTS :
1.0
Perchloric acid
2.0
Potassium hydrogen phthalate
3.0
Anhydrous
glacial acetic acid
4.0
Crystal
violet solution
|
|
3.0
|
METHOD OF PREPARATION
:
Mix
8.5 ml of perchloric
acid with 500 ml of anhydrous glacial acetic acid and 25
ml of acetic
anhydride,
cool and add anhydrous
glacial acetic acid to produce 1000 ml.
Allow
the prepared solution to stand for 1 day for the excess acetic anhydride to
be combined and carry out the determination of water, If the water content
exceeds 0.05 %, add more acetic anhydride. If the solution contains no titrable water, add
sufficient water
to obtain a content of water between 0.02% and 0.05%.
Allow
the solution to stand for 1 day and again titrate the water content.
The
solution so obtained should contain between 0.02% and 0.05% of water.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Weigh
accurately about 0.35 g of potassium hydrogen phthalate, previously powdered lightly
and dried at 120° for 2 hours and dissolve it in 50 ml of anhydrous glacial acetic
acid.
Add
0.1 ml of crystal
violet solution and titrate with the perchloric acid solution
until the violet colour changes to emerald-green.
Perform
a blank determination and make any necessary correction.
Each
ml of 0.1 M
perchloric acid is equivalent to 0.02042 g of C8H5KO4.
|
|
5.0
|
CALCULATION :
= 0.1 X Wt. of KHP (gm) X Assay of KHP
B.R. x 0.02042 x 100
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M SODIUM HYDROXIDE ( ETHANOLIC)
|
|
2.0
|
REAGENTS :
1.0
Sodium Hydroxide
2.0
Ethanol
3.0
Benzoic Acid
|
|
3.0
|
METHOD OF PREPARATION
:
Add 3.3 g of 10 M Sodium Hydroxide Solution to 250
ml of absolute ethanol.
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Ascertain its exact concentration
immediately before use in the following manner. Dissolve 0.2 g of benzoic
acid in a mixture of 10 ml of ethanol (96%) and 2 ml of water and titrate
with the ethanolic sodium hydroxide solution using 0.2 ml thymolphthalein
solution as indicator until the solution changes colorless to pink.
Each ml of 0.1M ethanolic sodium
hydroxide is equivalent to 12.21 mg of C7H6O2
|
|
5.0
|
CALCULATION :
= Wt. of Benzoic Acid x 0.1 x Assay of
Benzoic Acid
B.R. x
0.01221 x 100
B.R.:
Burette Reading in ml.
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
|
1.0
|
NAME : 0.1 M POTASSIUM HYDROXIDE (
ETHANOLIC)
|
|
2.0
|
REAGENTS :
1.0
Potassium Hydroxide
2.0
Ethanol
3.0
Hydrochloric Acid
4.0
Phenolphthalein
|
|
3.0
|
METHOD OF PREPARATION
:
Dissolve 6 g of potassium hydroxide in 50 ml of
water and diluted to 1000 ml with aldehyde-free ethanol (96%).
|
|
4.0
|
METHOD OF
STANDARDIZATION :
Ascertain its exact concentration
immediately before use in the following manner.
Titrate 20 ml of the solution of
0.1 M Hydrochloric Acid with 0.1 M KOH using 0.5 ml of phenolphthalein
solution as indicator. Until the colorless solution appears as pink.
|
|
5.0
|
CALCULATION :
= Volume of HCl x Molarity of HCl
Volume of KOH
|
|
6.0
|
REFERENCE : Indian Pharmacopoeia
|
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1.0
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NAME : 0.1 M TETRABUTYLAMMONIUM
HYDROXIDE
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2.0
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REAGENTS :
1.0
Tetrabutylammonium iodide
2.0
Methanol
3.0
Dimethylformamide
4.0
Thymol Blue
5.0
Benzoic Acid
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3.0
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METHOD OF PREPARATION
:
Dissolve 40 g of Tetrabutylammonium iodide in 90
ml of anhydrous methanol add 20 g of finely powdered Silver Oxide and shake
vigorously for 1 hour.
Centrifuge a few ml of the mixture and test the
supernatant liquid for iodides.
If a positive reaction is obtained, add a further
2 g of silver oxide and shake for 30 minutes.
Repeat this procedure until the mixture is free
from iodides, filter through a fine sintered-glass filter and wash the
reaction vessel and filter with three 50 ml quantities of toluene.
Add the washings to the filtrate and add
sufficient Toluene to produce 1000 ml.
Pass dry carbon dioxide free nitrogen through the
solution for 5 minutes.
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4.0
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METHOD OF
STANDARDIZATION :
Ascertain its exact concentration
immediately before use in the following manner.
To 10 ml of Dimethylformamide add
0.05 ml of a 0.3% w/v solution of Thymol Blue in Methanol and titrate with
Tetrabutyl ammonium hydroxide solution until a pure blue colour is produced.
Immediately add 0.2 g of Benzoic acid,
stir to effect solution and titrate with the tetrabutyl ammonium hydroxide
solution until the pure blue colour is restored.
Protect the solution from
atmospheric carbon dioxide throughout the titration. The volume of titrant
used in the second titration represents the amount of tetrabutylammonium
hydroxide required.
Each ml of 0.1 M tetrabtylammonium
hydroxide is equivalent to 12.21 mg of C7H6O2
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5.0
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CALCULATION : = Volume of HCl x Molarity of HCl
Volume of KOH
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6.0
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REFERENCE : Indian Pharmacopoeia
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1.0
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NAME : 0.01 M SODIUM TETRAPHENYLBORATE
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2.0
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REAGENTS :
1.0
Sodium
Tetraphenylborate
2.0
Sodium Hydroxide
3.0
Aluminium
Hydroxide
4.0
Sodium Chloride
5.0
Cetylpyridinium
Chloride
6.0
Potassium Chloride
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3.0
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METHOD OF PREPARATION
:
Dissolve
3.5 g of sodium tetraphenylborate in a 50 ml of water, shake for 20 minutes
with 0.5 g Aluminium hydroxide gel, add 250 ml of water and 16.6 g of sodium
chloride and allow to stand for 30 minutes. Filter, add 600 ml of water,
adjust the pH to 8.0 to 9.0 with 0.1 M sodium hydroxide and dilute to 1000 ml
with water.
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4.0
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METHOD OF
STANDARDIZATION :
Ascertain
its exact concentration immediately before use in the following manner.
Dissolve
7 mg of potassium chloride, previously dried at 150°C for 1 hour, in 5 ml of
acetate buffer pH 3.7 and 5 ml of water, add 15 ml of the sodium
tetraphenylborate solution, allow to stand for 5 minutes and filter through a
dry, sintered glass filter.
To
20 ml of the filtrate add 0.5 ml of bromophenol blue solution and titrate the
excess of sodium tetraphenylborate with 0.005M cetylpyridinium chloride to
the blue colour of the indicator.
Repeat
the procedure without the potassium chloride.
The
molarity of the solution is given by the expression: aw/[15(a-b)0.07455]
Where
a
is the volume of 0.005 M cetylpyridinium chloride required when the potassium
chloride is omitted, b is the
volume of 0.005 M cetylpyridinium chloride required when the potassium
chloride is present and w is the weight , in g, of
potassium chloride taken.
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5.0
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CALCULATION :
= aw/[15(a-b)0.07455]
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6.0
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REFERENCE : Indian Pharmacopoeia
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