ash content

determination

exercise 4
objectives
1. to determine the total ash and acid-insoluble ash
as content of plant material

2. to understand the purpose of the ash content

determination of plant sample

3. to be familiarized with the different laboratory

equipment used in the determination of ash
content
ash content
is the inorganic residue remaining
after the water and organic matter
have been removed by heating in
the presence of oxidizing agents

the most widely used methods are

based on the fact that minerals
are not destroyed by heating
ash content
why measure the ash content?

1. provides a measure of the total amount of minerals

within a sample
2. furnishes a basis for judging the identity and
cleanliness of a drug
3. gives information relative to its adulteration with
inorganic matter
total ash content
residue remaining after incineration
allows to quickly and easily identify the physiological and
non-physiological materials contained in the vegetable
physiological ash derived from the plant tissue itself
non-physiological ash often from environmental
contaminations such as sand and soil
the total ash usually contains CO3, PO4, SO4, Cl, oxides of
Ca, Mg, K, Na, Al, Fe and other metallic elements
acid-insoluble ash
another index to measure the purity and quality of
plant samples
refers to part of the total ash that is insoluble in
dilute inorganic acids
the diluted HCl dissolves the CaCO3, alkali Cl, etc.,
leaving an acid insoluble residue that consists
almost entirely of silica derived from soil adhering
to the drug
laboratory apparatus
crucible & cover

used to contain compounds

when heated to extremely
high temperatures
quartz crucible & cover

satisfies high-
temperature
requirements up to
1050C (1922F)
crucible tongs

used to grasp a hot crucible

or evaporating dishes
clay triangle

supports a crucible when it

is being heated over the
Bunsen burner
muffle furnace

used in research to
incinerate samples to ash
muffle furnace
Temperature range (C) Description
500-550 Very dull red heat
550-700 Dull red heat
800-1000 Bright red heat
1000-1200 Yellow red heat
1200-1600 White heat
ash content determination
careful control of temperature is the most important
analytical factor to be regulated in making ash
determinations
careful selection of crucible is important
the ash consists largely of CaCO3 formed from Ca(C2HO4)2
contained in the drug
when incineration is carried out as a:
dull red heat Ca(C2HO4)2 is converted to CaCO3
bright red heat varying amounts of the CaCO3 are
converted to the CaO with consequent variable results
ash content determination

if the ash contains alkali chlorides which frequently

does, there may be a loss of some chloride by
volatilization when a high ignition temperature is
used
when the ignition is not heated above dull redness, it
is frequently difficult to burn off all the carbon
computation
total ash = weight of the crucible and ash weight of the
crucible

% total ash = 100

% acid-insoluble ash = 100

end of discussion

exercise 4