Analytical Seminar

ACID INSOLUBLE ASH

by Dr.Ajay Chavan

Objective

Brief discussion to understand regarding Acid Insoluble Ash

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Acid Insluble Ash

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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Acid Insluble Ash

History

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

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Acid Insluble Ash

COMPOSITION OF ASH

Inorganic: Oxalates, Silica, Carbonates. Organic: Phosphates, Potassium, Magnesium, Calcium.

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Acid Insluble Ash

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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Acid Insluble Ash

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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Acid Insluble Ash

PROCEDURE

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Acid Insluble Ash

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

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Acid Insluble Ash

STEP
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
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

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: Vati & Guggulu: Ghana & Satva: Bhasma: N.M.T. 0.5% w/w N.M.T. 1-16% w/w N.M.T. 1-16%w/w 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) : Adraka (Rz): Kamala(Fl): Bhallataka (Fr):
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N.M.T. 5% w/w N.M.T. 1%w/w N.M.T. 3%w/w N.M.T. 0.5% w/w

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Contd
Ikshu (St): Dattura (Sd): Trivuta (Rt): N.M.T. 2.5% w/w N.M.T. 1% w/w 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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