ACID INSOLUBLE ASH by Dr.Ajay Chavan Analytical Seminar
ACID INSOLUBLE ASH by Dr.Ajay
Chavan
Analytical Seminar
Acid Insluble Ash 2
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