Chapter 11

Ash and Water Determinations

Ash Content
Residue remains after incineration.
Inorganic matter added to the crude drug for the purpose of adulteration.

Ash Determination
A basis for judging the identity and cleanliness of a drug and gives information
relative to its adulteration with inorganic matter.

Total Ash
The residue remaining after incineration.
Usually contains carbonates, phosphates, sulfates, chlorides, oxides, etc., of
calcium, magnesium, potassium, sodium, aluminum, iron, and other metallic
elements, does not necessarily represent all the inorganic constituents of the
drug, since ammonium salts, some alkali iodides and nitrates, etoc., are
volatilized or converted to carbonates, etc.

Acid-insoluble Ash
Part of the total ash which is insoluble in diluted hydrochloric acid.

*The diluted hydrochloride acid dissolves the calcium carbonate, alkali chlorides, etc.,
leaving an acid-insoluble residue that consists almost entirely of silica derived from the
soil adhering to the drug.

Temperature
Very dull-red heat 500 to 550C
Dull-red heat 550 to 700C
Bright-red heat 800 to 1000C
Yellow-red heat 1000 to 1200C
White heat 1200 to 1600C

Residue on Ignition
The ash content of chemicals is determined by ignition to dull redness in the
same manner as in the determination of the ash content of the crude drug.
It is economically impracticable to make ash determinations on large samples of
expensive chemicals.
Neglible is defined as a quantity not exceeding 500 microgram.

Loss on Ignition
These technique provides a means of determining the percentage of test
material which is volatilized and driven off under the conditions specified.
Substances which have a definite limitations on the amounts of volatile matter
they will lose when heated: USP calamine, magnesium sulfate, titanium dioxide,
zinc oxide, NF calcium phosphate, tribasic, kaolin, lime, magnesium hydroxide,
magnesium phosphate.



Water Content
To ensure uniformity in the official drugs, it is necessary that the USP and the NF
specify certain water-content limits in the drug monographs.
Water content is generally determined by one of six methods:
Gravimetric, for drugs containing no constituents, other than water,
volatile at 105C;
Gravimetric, for drugs containing ether-soluble constituents volatile at
105C;
Azeotropic (Xylene USP; Toluene NF);
Titrimetric (Karl Fischer);
Dew point;
Electrolytic hygrometric.
The water content is also the moisture content of the drug.

Formulas:


























Gravimetric Method











Azeotropic Method











Karl Fischer Method
Standard Solution Karl Fischer Solution
Karl Fischer Reagent
o Primary Standard Sodium Tartrate
o Secondary Standard Water-Methanol Solution


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