IGNITION OF THE

PRECIPITATE:

THERMOGRAVIMETRIC
METHOD OF ANALYSIS
Water in precipitate :
(a)adsorbed water, present on al1 solid surfaces in amount
dependent on the humidity of the atmosphere;
(b)occluded water, present in solid solution or in cavities
within crystals;
(c)sorbed water, associated with substances having a large
interna1 surface development, e.g. hydrous oxides; and
(d)essential water, present as water of hydration or
crystallisation [e.g.CaC204,H20 or Mg(NH4)P04,6H20] or
as water of constitution
[the water is not present as such but is formed on
heating, e.g.
Ca(OH), +Ca0 + H20].
Direction of ignition :

•To bring the precipitate

to a constant composition
before it can be weighed.
Treatment :
• The treatment consists in drying or
igniting the precipitate

• The further treatment will depend both

upon the nature of the precipitate and
upon that of the filtering medium;

• Drying : untill 200 -250 degree Celcius

• Ignition : up to 1200 degree Celcius
Remember…..

• Precipitates that are to be dried should be

collected on filter paper, or in sintered-
glass or porcelain filtering crucibles.

• Precipitates that are to be ignited are

collected on filter paper, porcelain filtering
crucibles, or silica filtering crucibles.
Incineration of the filter
paper

• A silica crucible is first ignited to

constant weight (i.e. to within 0.0002
g) at the same temperature to which
the precipitate is ultimately heated.
• The well drained filter paper and
precipitate are carefully detached from
the funnel;
• The filter paper is folded to enclose the
precipitate completely
• The packet is placed point-down in the
weighed crucible, which is supported on a
silica triangle resting on a ring stand.
• The crucible is slightly inclined, and
partially covered with the lid, which should
rest partly on the triangle.
• A very small flame is then placed under
the crucible lid; drying thus proceeds
quickly and without undue risk
• When the moisture has been
expelled, the flame is increased
slightly so as to carbonize the paper
slowly.
• The paper should not be allowed to
inflame, as this may cause a
mechanical expulsion of fine particles
of the precipitate owing to the rapid
escape of the products of combustion
• If the paper does catch fire, the flame
should be extinguished by momentarily
placing the cover on the mouth of the
crucible with the aid of a pair of crucible
tongs.
• When the paper has completely
carbonized and vapors are no longer
evolved, the flame is moved to the back
(bottom) of the crucible and the carbon
slowly burned off while the flame is
gradually increased.*
• After all the carbon has been burned
away, the crucible is covered
completely (if desired, the crucible
may be placed in a vertical position
for this purpose) and heated to the
required temperature by means of a
Bunsen burner.
• Usually it takes about 20 minutes to
char the paper, and 30-60 minutes to
complete the ignition
After ignition …..
• When the ignition is ended, the flame is
removed and, after 1-2 minutes,
thecrucible and lid are placed in a
desiccator containing a suitable desiccant
and allowed to cool for 25-30 minute
• The crucible and lid are then weighed.
• The crucible and contents are then ignited
at the same temperature for 10-20
minutes, allowed to cool in a desiccator as
before, and weighed again.
• The ignition is repeated until
constant weight is attained. Crucibles
should always be handled with clean
crucible tongs and preferably with
platinum-tipped tongs.
• It is important to note that 'heating
to constant weight' has no real
significance unless the periods of
heating, cooling of the covered
crucible, and weighing are
duplicated.