ACID INSOLUBLE ASH by Dr.Ajay

Chavan

Analytical Seminar

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Objective

• Brief discussion to understand regarding Acid Insoluble Ash

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Introduction

• The residue remaining after incineration is ash

content of drug.

• Acid Insoluble Ash values represents detecting

presence of Silica and Oxalates in drugs.

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History

• First used by E.D.Simon the milling engineer in 1928

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COMPOSITION OF ASH

Inorganic: Oxalates, Silica, Carbonates.

Organic:Phosphates, Potassium, Magnesium, Calcium.

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Principle

• The Acid Insoluble Ash as Limit Test is designed to

measure the amount of ash insoluble to diluted

Hydrochloric acid.

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MATERIALS

Powdered drug.

Silica Crucibles.

Dryer

Desiccators.

Weighing Machine.

Muffle furnace.

Beaker

Dil.HCL.(2M)

Water Bath

Ash less filter paper.

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PROCEDURE

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Step І

• Heat the Silica crucible at 1050C for ½ hr in Dryer/Oven.

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Step ІІ

• After taking out form the dryer keep crucible in Desiccator, and allow to cool it

• Weigh accurately about 2gm of powdered drug in crucible.

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Step ІІІ

• Incinerate Crucible at 450 °C in muffle furnace for

not less than 4 hours to incinerate until it is free

from charred matter and cool in a desiccator

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Step IV

• Add carefully 25 ml of dilute hydrochloric acid to

the ash, boil gently for 5 minutes on water bath

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Step V

• Filter the solution through ash less filter paper (Whatman No. 41)

• Collect the insoluble matter on ash less filter paper.

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Step VI

• Wash thoroughly with hot water, and dry the

residue together with the filter paper

• Ignite it for 3 hours in a crucible in muffle furnace

at 4500C

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Step VII

• Cool the crucible in a desiccator (silica gel) and

weigh accurately

• Calculate the % of Acid Insoluble Ash

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CALCULATION

Percentage Acid Insoluble Ash - Weight of the acid insoluble residue Weight of the Sample

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X 100

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Precaution

• Sometimes heating a low temperature does not

give a carbon free Ash, because carbon particles

are trapped.

• If the measured amount is larger than the

specified value, ignite until a constant weight is

obtained.

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Applied Aspect

• To detect adulteration with exhausted drugs.

• To ensure percentage of Silica and Oxalates which

are introduced accidently at the time of

collection or capacity of drug reacting with clay

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STANDARDS

• Pharmacopoeial limits for Acid insoluble Ash vary

from 0.5% (agar) to 12% (hyosumus)

• Drug hyosumus plant have capacity to reacting

with clay

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Contd…

Standard acc to P.S.A.F

• Churna: N.M.T. 0.5% w/w

• Vati & Guggulu: N.M.T. 1-16% w/w

• Ghana & Satva: N.M.T. 1-16%w/w

• Bhasma: N.M.T. 2%w/w

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Contd…Some Drug and their Acid Insoluble Ash

• Swarna Bhasma: between 2.12 to 3.18% w/w

• Lauha Bhasma : between 0.101 to 2.803% w/w.

• Arka (Lf) : N.M.T. 5% w/w

• Adraka (Rz): N.M.T. 1%w/w

• Kamala(Fl): N.M.T. 3%w/w

• Bhallataka (Fr): N.M.T. 0.5% w/w01/08/2011

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Contd…

• Ikshu (St): N.M.T. 2.5% w/w

• Dattura (Sd): N.M.T. 1% w/w

• Trivuta (Rt):N.M.T. 1.5% w/w

• Guggulu (Exudute): N.M.T.1% w/w

• Tvaka (St bk) : N.M.T. 2% w/w

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Conclusion

• Validate the prepared drug compared with the

standard drug.

• Important parameters to detect the adulteration

found in the crude and powdered drugs.

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THANK YOU 01/08/2011 24Acid Insluble Ash