EXERCISE NO. 19
15
TOTAL AND ACID-INSOLUBLE ASH
CONTENT
DETERMINATION OF ACACIA LEAVES
Questions :
1. From what different sources may the
ash of a drug be derived ?
- ash maybe derived from the drug
itself natural from the inorganic
matter that comes from external
sources.
2. Why should the incineration residue
not be heated above a dull redness ?
- when incineration is carried out at
a bright red heat, the calcium
oxalate is converted into
carbonate, but when the
incineration is carried out in a
bright red heat, varying amounts
of the carbonate are converted to
the oxide with consequent
variable results.
3. Name the important inorganic plant
constituents that will not be found in the ash.
- this total ash, which usually
contains carbonate, phosphate,
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,
are volatilized or converted to
carbonate.
4. What does the quantity of
acid-insoluble ash in a drug indicate ?
- diluted HCl dissolves the calcium
carbonate, alkali chlorides,
leaving an acid insoluble residue
that consists almost entirely of
silica derived from the soil
adhering to the drug.
EXERCISE NO.
ASSAY OF CUPRIC SULFATE
indicator : starch Ts
Primary: potassium iodide
Secomd: sodium thiosulfate
End point: yellow
Reaction involved:
● 2CuSO4+ 4KI—-----> 2CuI2+ 2K2SO4
● 2 CuI2—------> CU2I2+ I2
● 2Na2S2O3+I2—-------> Na2S4O6 + 2NaI
● 2CuSO4 + 4 KI —----> 2CuI 4 K2SO4 + I2
EXPERIMENT NO. 17
ASSAY OF SODIUM CHLORIDE (GRAVIMETRIC
METHOD)
Primary: silver nitrate
Endpoint: cloudy
Reaction Involved :
NaCl + HNO3—----> HCl+ NaNO3
6HCl+ 2HNO3—-----> 3CL2+ 4H2O+ 2NO
AgNO3+ NaCl—------> AgCl+ NaNO3
Questions :
1. Why should the solution be acidified with
nitric acid ?
- All metallic nitrates are water soluble.
Thus, in reactions involving metallic ions
in solution that need to be acidified,
nitric acid is used in order to prevent
metallic salts precipitating out of the
solution.
2. Why add silver nitrate in excess in the
precipitation of the chloride ?
- Slightly excess silver nitrate is added
and also nitric acid is added to raise the
concentration of the nitrate ion in the
solution for two reasons. The first
reason is to prevent the solubility of the
silver chloride precipitates that are
formed as precipitate.
3. Why is the precipitate washed with water
slightly acidified with nitric acid ?
- If you wash with nitric acid, a high
electrolyte concentration is maintained
and the silver chloride particles stay
 clotted together. When you dry the
precipitate, the acid decomposes and
volatilizes, so it should not have a strong
effect on the precipitate mass.

4. Why is it best to wash the precipitate by

decantation before it is transferred to Gooch
crucible ?
- When the Gooch method is used, a
gentle pressure from the mouth on the
water in the bottle must be maintained,
and care must be taken that the
precipitate is not splashed up the sides
of the glass funnel, or that the layer of
asbestos in the Gooch crucible is not
disturbed.

5. Why should this determination be carried out

away from direct sunlight ?
- To avoid the presence of impurities
- The precipitation must be performed
away from strong sunlight , since silver
chloride is decomposed by sunlight with
loss of chlorine, while in diffused light
the error from this source is negligible

6. When is a crucible considered to have been

heated to constant weight ?
- If the two weighings do not agree within
0.04 g, you must heat the crucible and its
contents a third time for an additional 5
minutes. Cool and reweigh again. This
procedure is called “ heating to constant
weight “ only the anhydrous salt is left in
the crucible.