Methenamine

Description : A white ,crystalline powder or colorless crystals

Solubility: Freely soluble in water ,soluble in alcohol and in methylen chloride

Identification Test:

Solution S:
Dissolve 10.0 gm in distilled water and make volume upto 100 ml in flask,solion is
clear and colorless.

A:
To 1 ml of solion S add 1 ml of sulfuric acid and immediately heat to boiling .Allow
to cool .To 1 ml of solution add 4 ml of water and 5 ml of acetylacetone reagent heat on a
water bath for 5 min .an intense yellow color is developed

B:
Dissolve 10 mg in 5 ml of water and acidify with dilute hydrochloric Acid .Add 1 ml
of potassium iodobismuthate solution .An orange precipitate is formed immediately.

Acicity or Alkinity:

To 5 ml of solution S add 0.1 ml of phenolphthalein solution .NMT 0.2 ml of 0.1 M HCl

is required to change the color.
Loss on Drying:

NMT 2.0 % ,determined on 1.00 gm by drying in a desicator.

Assay:

Dissolve 0.100 gm in 30 ml of methanol .Titrate with 0.1 M perchloric acid ,determined

the end –point potentiometrically
1 ml of 0.1 M perchloric Acid is equivalent to 14.02 mg of C6H12N4
 Finished Product

Standard Preparation:

Take 100 mg of methenamine Rf std in 100 ml of flask and add 25 ml of methanol in it

.shake it on sonicator until it dissolve and make volume upto 100 ml with same solvent
and sonicate.take 1 ml in 50 ml flask and make volume upto mark with methanol.
Sonicate it for 5 minute.

Sample Preparation:

Take powder containing methenamine equivalent to 100 mg of methenamine Rf std in

100 ml of flask and add 25 ml of methanol in it .shake it on sonicator until it dissolve and
make volume upto 100 ml with same solvent and sonicate.filter it and take 1 ml from
filter in 50 ml flask and make volume upto mark with methanol.
Sonicate it for 5 minute.

Now take reading both standard and sample on U.V at 336 nm

Limits: 90% to 110 %

 Piperazine Adipate

Description : A white ,crystalline powder

Solubility: Freely soluble in water ,practically insoluble in alcohol

Identification Test:

Solution S:
Dissolve 2.5 gm in distilled water and make volume upto 50 ml in flask,solion is
clear and colorless.

A:
To 10 ml of solion S add 5 ml of hydrochloric acid and shake with three quantity
,each of 10 ml of ether ,evaporate the combined ether layer to dryness.the residue
,washed with 5 ml of water and dried at 100 Co

Loss on Drying:

NMT 0.5 % ,determined on 1.00 gm by drying in a desicator.

Assay:

Dissolve 0.100 gm in 10 ml of anhydrous acetic acid with gentle heating and dilute to 70
ml with same solvent .Titrate with 0.1 M perchloric acid ,using 0.25 ml of
naphtholbenzene solution as indicator until the color change from brownish-yellow to
green
1 ml of 0.1 M perchloric Acid is equivalent to 11.61 mg of C10H20N2O4
 Finished Product

Standard Preparation:

Take 100 mg of piperazine hydrate Rf std in 100 ml of flask and add 25 ml of Distill
Water in it .shake it on sonicator until it dissolve and make volume upto 100 ml with
same solvent and sonicate.take 1 ml in 50 ml flask and make volume upto mark with
Distill Water.
Sonicate it for 5 minute.

Sample Preparation:

Take powder containing piperazine hydrate equivalent to 100 mg of piperazine hydrate

Rf std in 100 ml of flask and add 25 ml of Distill Water in it .shake it on sonicator until it
dissolve and make volume upto 100 ml with same solvent and sonicate.filter it and take 1
ml from filter in 50 ml flask and make volume upto mark with Distill Water.
Sonicate it for 5 minute.

Now take reading both standard and sample on U.V at 295 nm

Limits: 90% to 110 %

Phenothiazine

Description : A yellow ,crystalline powder

Solubility: Freely soluble in ether ,chloroform,benzene and sparingly soluble in water

Melting Point: 185Co

Identification Test:

Solution S:
Dissolve 2.5 gm in distilled methanol and make volume upto 50 ml in flask,solion
is clear and colorless.

A:
To 10 ml of solion S add 5 ml of hydrochloric acid and shake with three quantity
,each of 10 ml of ether ,evaporate the combined ether layer to dryness.the residue
,washed with 5 ml of water and dried at 100 Co

Loss on Drying:

NMT 0.5 % ,determined on 1.00 gm by drying in a desicator.

Assay:

Dissolve 0.100 gm in 10 ml of anhydrous acetic acid with gentle heating and dilute to 70
ml with same solvent .Titrate with 0.1 M perchloric acid ,using 0.25 ml of
naphtholbenzene solution as indicator until the color change from brownish-yellow to
green
1 ml of 0.1 M perchloric Acid is equivalent to 19.61 mg of C12H9NS
 Finished Product

Standard Preparation:

Take 100 mg of Phenothiazine Rf std in 100 ml of flask and add 25 ml of Methanol in it

.shake it on sonicator until it dissolve and make volume upto 100 ml with same solvent
and sonicate.take 1 ml in 50 ml flask and make volume upto mark with Methanol.
Sonicate it for 5 minute.

Sample Preparation:

Take powder containing Phenothiazine equivalent to 100 mg of piperazine hydrate Rf

std in 100 ml of flask and add 25 ml of Methanol in it .shake it on sonicator until it
dissolve and make volume upto 100 ml with same solvent and sonicate.filter it and take 1
ml from filter in 50 ml flask and make volume upto mark with Methanol.
Sonicate it for 5 minute.

Now take reading both standard and sample on U.V at 278 nm

Limits: 90% to 110 %