Unit IV Gravimetric Analysis

1.

Gravimetric Analysis
Gravimetric methods – are quantitative methods in which the mass of the analyte or some compound that is
chemically related to the analyte is determined.

PRINCIPLE :
Gravimetric analysis is the process of isolating and weighing an element or a definite compound of the
element in as pure a form as possible. The element or compound of the element is separated from a weighed
portion of the substance being examined. A large portion of the determinations in gravimetric analysis is
concerned with the transformation of the element or radical to be determined into a pure stable compound
which can be readily converted into a form suitable for weighing. The weight of the element or radical may
then be readily calculated from a knowledge of the formula of the compound and the relative atomic masses
of the constituent elements.

The separation of the element or of the compound containing it may be effected in number of ways, the most
important of which are

1. Precipitation Methods
2. Volatilisation or evolution methods
3. Electro analytical methods - Electro Gravimetry

1. Precipitation Methods

The most important is the precipitation method in gravimetric analysis, which is explained in detail below.

A weighed sample of the substance to be analysed is brought into solution by a suitable method, and the
element to be determined is then precipitated as an insoluble compound. The precipitate is filtered off,
washed throughly, ignited (or dried) and weighed accurately. The content of the element is calculated from
the weight of the precipitate and its formula and expressed as a percentage of the sample taken. The
precipitate may be collected on a filter paper or in a Gooch crucible.

2. Volatilisation or evolution methods

In addition to precipitation, the other methods are also used. This Volatilisation or Evolution method depends
essentially upon the removal of volatile constituents. This may be effected in several ways.
(i) By simple ignition in air or in a current of an indifferent gas.
(ii) By treatment with some chemical reagent whereby the desired constituent is rendered volatile and
(iii) By treatment with a chemical reagent whereby the desired constituent is rendered non-volatile.

The volatilised substance may be absorbed in a weighed quantity of a suitable medium when the estimation
is a direct one, or the weight of the residue remaining after volatilisation of a component is determined, and
the proportion of the constituent calculated from the loss in weight.

3. Electro analytical methods - Electro Gravimetry

In electro-gravimetric analysis, the element to be determined is deposited electrolytically upon a suitable

electrode. Filtration is not required, and provided the experimental conditions are carefully controlled, the
co-deposition of two metals can often be avoided.

In each of these analytical methods, the amount of a given component is found from the results of
weighing . These methods can therefore be regarded as different varieties of gravimetric analysis.
Unit IV Gravimetric Analysis
2.
Steps Involved in Gravimetric Analysis

1. Preparation of the solution

2. Precipitation
3. Digestion
4. Filtration
5. Washing of the Precipitate
6. Drying or igniting
7. Weighing
8. Calculation

1. PREPARATION OF THE SOLUTION

This may involve several steps including adjustment of the pH of the solution in order for
the precipitate to occur quantitatively and get a precipitate of desired properties, removing
interferences, adjusting the volume of the sample to suit the amount of precipitating agent to
be added.

2. PRECIPITATION or NUCLEATION
Gravimetric precipitation are usually made in beakers. Except during the actual precipitation, the beaker is
covered with the clock-glass. A thin stirring rod, rounded at each end, is also required.

NUCLEATION

In practice, supersaturation influences one of the mechanisms of precipitation, namely nucleation and crystal
growth. Nucleation is the first stage of precipitation and consists in the formation of stable microcrystals that
can grow spontaneously, i.e. crystallization nuclei. Further precipitation leads to competition between new
and existing nuclei (particle growth). If nucleation predominates, then a crystal will form that is easy to filter.
Low supersaturation encourages the growth of existing microcrystals rather than the formation of new nuclei.
Higher temperatures also favour the formation of crystalline precipitates, because they increase the solubility
of the precipitate (S), and other factors that encourage crystal growth are diluting the solution (Q), and
adding the precipitation agent slowly while shaking energetically.

PRECIPITATION

The solution of the precipitating reagents is usually added

slowly from a teat pipette or burette. with efficient stirring,
to a suitably diluted solution of the sample. Efficient
stirring. is necessary to avoid the possible high local
concentrations of precipitating reagent which would tend to
give contamination of precipitate due to co-precipitation.
The reagent is introduced down the side of the beaker to
avoid splashing. Precipitation is usually made from hot
dilute solutions, a procedure which tends to give an easily
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3.
filterable precipitate and reduces the possibility of co-precipitation. The formation of coarse particles is
favoured by slow addition of the precipitant. vigorous stirring of the solution during precipitation and by
carrying out the precipitation from hot solutions. Only a moderate excess of precipitating reagent is required.
When the precipitate has settled somewhat. a few more drops of precipitant should be added to test for the
completeness of precipitation; if further precipitation occurs. then the process of addition of precipitant,
stirring and allowing the precipitation settle and testing again must be carried out until there is no doubt
about completeness of precipitation. The stirring rod should not come into contact with the sides or bottom of
the beaker during stirring in order to avoid scratching particles of glass from the surfaces. Also, a scratched
surface is difficult to wash clean. Reagents should be examined for the clarity before use and filtered if
necessary.

Before filtration, precipitates may need to be digested by allowing them to stand overnight, or by heating the
precipitate and its supernatant liquid nearly to boiling point for some time. Digestion in this manner increases
the degree of coarseness of the precipitate: A further check for completeness of precipitation should be
carried out when the supernatant liquid becomes clear during the period of digestion. No further precipitate
should be produced when a few drops of the must be added as described above.

If the precipitate is much more soluble in hot water than in cold, the solution is allowed to cool to room
temperature, before filtration. Otherwise, solutions are filtered hot to speed up the filtration.

(i) CO-PRECIPITATION

When a precipitate separates from a solution, it is not always perfectly pure: it may contain varying amounts
of impurities dependent upon the nature of the precipitate and the conditions of precipitation. The
contamination of the precipitate by substances which are normally soluble in the mother liquor is termed co-
precipitation.

Hence the term co-precipitation is a phenomenon in which the soluble compounds are removed from solution
during precipitate formation. It is important to understand that the solution is not saturated with the co-
precipitated species. Moreover, contamination of a precipitate by a second substance whose solubility
product has been exceed does not constitute co-precipitation.

Types of Co-precipitation
There are four types of co-precipitation:
(i) Surface adsorption
(ii) Mixed crystal formation
(iii) Occlusion
(iv) Mechanical entrapment.

Surface adsorption and mixed crystal formation are equilibrium processes., where as occlusion and
mechanical entrapment arise from the kinetics of crystal growth.

(i) Surface adsorption:

Adsorption is a common source of
co-precipitation that is likely to
cause significant contamination of
precipitates with large specific
surface areas i.e., coagulated
colloids.

Note the extensive internal

surface area exposed to solvent

Although adsorption does occur in

crystalline solids, its effect on
purity are usually undetectable
because of the relatively small,
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4.
specific surface area of these solids. Coagulation of a colloid does not significantly decrease the amount of
adsorption because the coagulated solid still contains large internal surface areas that remain exposed to the
solvent which can be seen in the figure.

The co-precipitated contaminant on the coagulated colloid consists of the lattice ion originally adsorbed on
the surface before coagulation and the counter ion of opposite charge held in the film of solution
immediately adjacent to the particle. The net effect of surface adsorption is therefore the carrying down of an
otherwise soluble compound as a surface contaminant.

For example

The coagulated silver chloride formed in the gravimetric determination of chloride ion is contaminated with
primarily adsorbed silver ions along with nitrate or other anions in the counter-ion layer. As a consequence,
silver nitrate, a normally soluble compound, is co-precipitated with the silver chloride.

(ii) Mixed - Crystal formation

Mixed-crystal formation is a type of co-precipitation in which a contaminant ion replaces an ion in the lattice
of crystal.

In mixed-crystal formation, one of the ions in the crystal lattice of a solid is replaced by an anion of another
element. For this exchange to occur, it is necessary that the two ions have the same charge and that their sizes
differ by no more than about 5% furthermore, the two salts must belong to the same crystal class.

EXAMPLE

Barium sulphate formed by adding barium chloride to a solution containing sulphate, Lead and acetate ions
is found to be severely contaminated by Lead sulphate even though acetate ions normally prevent
precipitation of Lead sulphate by complexing the lead. Here. Lead ions replace some of the barium ions in
the barium sulphate crystals other examples of co-precipitation by mixed-crystal formation include,
MgKPO4 in MgNH4PO4 and MnS in Cds.

When mixed-crystal formation occurs, separation of the interfering ion may have to be carried out before the
final precipitation step. Alternatively, a different precipitating reagent that does not give mixed crystals with
the ions in question may be used.

(iii) Occlusion and Mechanical entrapment

When a crystal is growing rapidly during precipitate formation, foreign ions in the counter- ion layer may
become trapped or occluded, Within the growing crystal. Because supersaturation, and thus growth rate
decrease as a precipitation progresses, the amount of occluded material is greatest in that part of a crystal that
forms first:

Mechanical entrapment occurs when crystals lie close during growth. Here, several crystals grow together
and in so doing trap a portion of the solution in a tiny pocket.

Both occlusion and mechanical entrapment are at a minimum when the rate of precipitate formation is low-
that is, under conditions of low super saturation. In addition, digestion is often remarkably helpful in
reducing these types of co-precipitation. Undoubtedly, the rapid solution and re precipitation that goes on at
the elevated temperature of digestion opens up the pockets and allows the impurities to escape into the
solution.

(ii) POST PRECIPITATION

Post-precipitation is the precipitation which occurs on the surface of the first precipitate after its formation. It
occurs with sparingly soluble substances which form supersaturated solutions-, they usually have an ion in
common with the primary precipitate. Thus in the precipitation of calcium as oxalate in the presence of
magnesium. magnesium oxalate separates out gradually upon the calcium oxalate; the longer the precipitate
is allowed to stand in contact with the solution, the greater is the error or mercury (II) sulphide in 0.3 M
hydrochloric acid in the presence of zinc ions; zinc sulphide is slowly post-precipitated.
Unit IV Gravimetric Analysis
5.

Post - precipitation differs from Co-precipitation in the following

(a) The contamination increases with the time that the precipitate is left in contact with the mother
Liquor in post-precipitation, but usually decreases in co-precipitation.

(b) With post-precipitation, contamination increases the faster the solution is agitated by either mechanical or
thermal means. The reverse is usually true with co-precipitation.

(c) The magnitude of contamination by post-precipitation maybe much greater than in co- precipitation.

It is convenient to consider now the influence or digestion. This is usually carried out by allowing the
precipitate to stand for 12-24 hours at room temperature, or sometimes by warming the precipitate for some
time in contact with the liquid from which it was formed; the object is, of course, to obtain complete
precipitation in a form, which can be readily filtered. During the process of digestion or of the ageing of
precipitates, at least two changes Occur. The very small particles, which have a greater solubility than the
larger ones, will, after precipitation has occurred, tend to pass into,solution, and will ultimately re-deposit
upon the larger particles; co-precipitation on the minute particles is thus eliminated and the total co-
precipitation the ultimate precipitate reduced. The rapidly formed crystals are probably of irregular shape and
possess a comparatively large surface; upon digestion these tend to become more regular in character and
also more dense, thus resulting, in a decrease in the area of the surface and a consequent reduction of
adsorption. The net result of digestion is usually to reduce the extent of co-precipitation and to increase the
size of the particles rendering filtration easier.

3. DIGESTION
The particle size of the coagulated colloid can be further increased by a process called digestion. In this
context, digestion refers to letting the precipitate stand in its “mother liquor” (the solution in which it is
formed), usually at elevated temperatures. The smaller precipitate particles tend to dissolve faster than large
ones and re precipitate onto larger particles. This relatively slow dissolution/re-precipitation process also
tends to remove foreign ions that have been trapped inside rapidly growing precipitate particles. Letting the
AgCl precipitate stand at room temperature between lab periods will generally result in a complete settling of
the AgCl and a clearing of the supernatant (the liquid above the precipitate).

4. FILTRATION
The separation of the precipitate from the solution by filtration is carried out either by
filter paper or sintered crucible or Gooch crucible.

1. Filter Papers

Different grades of filter-paper have

to be used for different precipitates.
Ash-less filter- papers are used
routinely. The size of the filter paper
is selected, according to the bulk of
the precipitate. The filter paper must
be selected in such a way, that the
pores of the filter paper must be
smaller than the size of the particles
of the precipitate.

The precipitate is separated by filtration either through crucibles

or Whatman's No. 40, 41, or 42 filter papers. The diameter of filter
paper may vary according to the bulkiness of precipitate. Bulky precipitate like aluminium hydroxide needs a
large filter paper than dense precipitate, i.e. barium sulphate. The folded filter paper is kept in a funnel
moistened with water and pressed to expel the air. Then , precipitate is transferred in a usual way and gets
separated.

Apparatus used in filtration

Unit IV Gravimetric Analysis
6.

Various types of filtering, apparatus are used in gravimetric analysis.

(a) Gooch crucible of either porcelain or silica in which ready-made, disposable glass filter mats may only
due used for precipitates at temperatures below 200°C.

(b) Sintered glass or sintered silica ( vitreosil) crucibles,

Gooch or sintered crucibles have now almost completely superseded the use. of filter paper, largely because
filtration and washing of the precipitates. can be carried out so much more rapidly and efficiently with their
aid. The ignition of precipitates in crucibles also avoids the necessity of first drying and then burning off the
filter paper. Filtration through paper. may, however. occasionally be advantageous with gelatinous
precipitates.

2. Gooch Crucibles

A Gooch crucible should be supported by

a soft rubber collar in a glass adapter
which passes through a rubber bung fitting
into a Buchner flask.

The rubber collar should not project below

the bottom or above the top of the
crucible. The tip of the adapter should
project below the side arm of the Buchner
flask to avoid the risk of the filtrate being
sucked out of the flask. A trap is required
to prevent any back flow from the pump
contaminating the filtrate. Furthermore, it
reduces the effects of changes in water
pressure which may cause the filter pod to
lift from the base of the crucible.

Disposable glass fibre filter discs

Standard glass filter discuss are available. (whatman; 2.1 cm diameter) for use as filtration beds in Gooch
crucibles. These filter discs are cheap, easy to handle, stable upto temperatures of atleast 180° and, like the
asbestos filter beds formerly used, are readily removed for cleansing and disposal at the end of the analysis.

They very coarse grades (0 and 1) are used for such purposes as dispensing as gases in wash-bottles or
gas absorption apparatus, and for sintered glass funnels for collecting solid material in preparative work. The
very fine grade 5 is designed for the collection of precipitates in gravimetric analysis, but for fine precipitates
(such as barium sulphate or silver chloride) grade 4 should be used. The rate of filtration is naturally slower
the finer the porosity.

Sintered glass crucibles are easiest and more convenient to use than Gooch crucibles which require some
skill and experience in preparation. They can be safely heated at temperature upto 400°, and are resistant to
all reagents except hydrofluoric acid and strong alkalis.

One disadvantage is that they are much more difficult to clean than Gooch crucibles. The following is the
recommended procedure;

1. Brush out as much of the dry material as possible with a hard brush.
2. Wash the crucible out by water drawn through it backwards (this is why sintered glass crucibles have a
glass Rim or skirt below the sintered plate).
3. Soak the crucible for several hours in a solvent appropriate to the material to be removed (but not in
solutions of caustic alkalis).
4. Wash the crucible well with water, and dry it.
Unit IV Gravimetric Analysis
7.
Preparation of the Gooch crucible for filtration

Place the crucible in the suction filtration

apparatus, sit a glass fibre filter disc gently
on top of the porous base of the crucible.
Gently wash the crucible and filter disc
with water to remove any loose fibers, and
apply gentle suction to drain off excess
water. Such the pad as dry as possible,
covering the mouth of the crucible during
the suction to prevent dust particles being
drawn in Dry (or ignite) the prepared
Gooch crucible under the conditions
specified for the drying (or ignition) of the
precipitate, cool in a desiccator and weigh.
Reheat, cool, and weigh; repeat until
constant weight is attained.

3. Sintered glass or Sintered Silica Crucibles:

Sintered glass crucibles are made of resistant glass and have a porous
bottom of sintered .ground glass which is fused in so as to be an
integral part of the crucible. The filtering beds are fused-in sintered
discs of the same material as the crucible. The sintered glass type of
crucible is most frequently used, they are available in various degrees
of porosity numbered 1, 2, 3, 4 and 5 indicating decreasing pore
diameter with increasing number. A number 3 crucible is suitable for
precipitates of medium particle size, such as silver chloride, while a
number 4 is necessary for fine precipitates, such as barium sulphate.
Sintered glass crucibles should not be heated at temperatures above
400°.If the precipitate has to be ignited, or requires drying at
temperatures above 400°, Sintered silica Crucible (vitreosil) should
be used.

Sintered Crucibles are prepared for use in filtration by washing and

passing water through under suction and then drying (or igniting) to
constant weight under the conditions which are specified for the
drying (or ignition) of the filtered precipitate.

5. WASHING THE PRECIPITATE:

USING A GOOCH CRUCIBLE
Care must be taken to avoid dislodging the filter disc. Suction must, therefore, be applied before pouring
liquid into the crucible and should be adjusted, before filtration is commenced, to a low level just sufficient
to draw liquid through the filter at a conveniently steady rate.

First, moisten the pad with a few drops of water from a teat Pipette. Apply suction, add more water and then
pour the liquid gently down a stirring rod on to the central portion of the filter mat. Pour the supernatant
liquid above the precipitate down the glass rod into the filter without-disturbing the precipitate more than is
necessary. Keep the lower end of the glass rod close to, but not touching the filter pad. Do not allow the
liquid to rise above a level of 1 cm from the top edge of the crucible. Keep the beaker inclined and a stream
of liquid passing into the filter as long as the liquid filters freely. Wash the precipitate in the beaker by
decantation as follows. Add about 10 mL of the wash liquid to the precipitate, stir the mixture, allow the
precipitate to settle and pour off the supernatant liquid down the glass rod onto the filter paper. Repeat this
procedure three or four times, then Stir the precipitate with about 20 ml or wash liquid transfer as much of
the solid as possible to the filter. Wash the traces of precipitate which adhere to sides and bottom of the
Unit IV Gravimetric Analysis
8.
beaker into the filter with a jet of water from a wash-bottle. Hold the wash-bottle in the right hand and the
beaker in the left hand, with the stirring rod pressed firmly against the lip of the beaker with the left thumb.
Incline the beaker and direct a stream of wash liquid against the precipitate to wash it down the stirring rod
into the filter. Small amounts of precipitate which adhere tenaciously to the walls of the beaker and the rod
should be dislodged by rubbing with a 'policeman' (a glass rod covered at one end with a small piece of
rubber or plastic tubing). When all the precipitate has been dislodged, rinse the 'policeman' with wash liquid
and transfer the trace of precipitate down the rod to the filter. Finally, hold the beaker and stirring rod up to
the light and examine carefully for traces of precipitate; repeat the treatment if necessary. (Note; a
'policeman' should not be used during precipitation or the early stages of filtration and should be removed
from the beaker immediately after use).

When the precipitate has been transferred quantitatively to the filter. it should be washed immediately with
was liquid from a wash-bottle. Unwashed precipitate should not be allowed to stand for any length of time.
because it will dry out and the mass will crack and. in this form. it cannot be washed properly. The jet of
liquid should be directed onto the side of the crucible. The filter should be allowed to drain completely
between each washing. From time to time. test for the completeness of washing by collecting small samples
of the washings in a test-tube as the pass through the funnel, applying appropriate qualitative tests. When
negative test are obtained. the precipitate and crucible are ready for drying.

In some determination, it is advantageous to wash the precipitate finally with ethanol to remove most of the
water and thus reduce the time require: for subsequent drying of the precipitate.

Using of sintered glass or sintered silica crucibles. The technique is similar to that described for Gooch
crucibles except that a filter mat is not used.

Some general theoretical consideration in washing the precipitate

Most precipitates are produced in the presence of one or more soluble compounds, and it is t0he object of the
washing process to remove these as completely as possible. It is evident that only surface impurities will
depend upon the solubility and the chemical properties of the precipitate upon its tendency to undergo
peptisation, the impurities to be removed, and the influence of traces of the wash liquid upon the subsequent
treatment of the precipitate before weighing. Pure water cannot, in general, be employed owing to the
possibility of producing partial peptisation of the precipitate and, in slight solubility of the precipitate; a
solution of some electrolyte is employed. This should posses a common ion with the precipitate in order to
reduce solubility errors, and should easily be volatized in the preparation of the precipitate for weighing. For
these reasons, ammonium salts, ammonia solution, and dilute acids are commonly employed. If the filtrate is
required in a subsequent determination, the selection is limited to substances which will not interfere in the
sequel. Also, hydrolysable substances will necessitate the use of solutions containing an electrolyte which
will depress the hydrolysis whether the wash liquid is employed hot or at some other temperature will
depend primarily upon the solubility of the precipitate: if permissible, hot solutions are to be preferred
because of the greater solubility of the foreign substances and the increased speed of filtration.

It is convenient to divide wash solutions into three classes:

1. Solutions which prevent the precipitate from becoming colloidal and passing through the
filter. This tendency is frequently observed with gelatinous or flocculated precipitates but rarely with well-
defined crystalline precipitates. The wash solution should contain an electrolyte. The nature of electrolyte is
immaterial, provided it is without action upon the precipitate either during washing or ignition. Ammonium
salts are therefore widely used. Thus dilute ammonium nitrate solution of employed for washing iron (III)
hydroxide [hydrated iron (III) oxide], and 1% nitric acid for Washing silver chloride.

2. Solutions which reduce the solubility of the precipitate. The wash solution may Contain a moderate
concentration of a compound with one ion in common with the precipitate use being made of the fact that
substances tend to be less soluble in the presence of a slight excess of a common ion. Most salts are insoluble
in ethanol and similar solvents, so that organic solvents can sometimes be used for washing precipitates.
Sometimes a mixture of an organic solvent eg.,ethanol) and water or a dilute electrolyte is effective in
reducing the solubility to negligible proportions. Thus 100 mL of water at 25°C will dissolve 0.7 mg calcium
oxalate, but the same volume of dilute ammonium oxalate solution dissolves only a negligible weight of the
salt. Also 100 ml of water a room temperature will dissolve 4.2 mg of lead sulphate, but dilute sulphuric acid
or 50 per cent aqueous ethanol has practically no solvent action on the compound.
Unit IV Gravimetric Analysis
9.

3. Solutions which prevent the hydrolysis of salts of weak acids and bases. If the precipitate is a salt of
weak acid and is slightly soluble it may exhibit a tendency to hydrolyse, and the soluble product of
hydrolysis will be a base; the wash liquid must therefore be basic. Thus (Mg (NH4)PO4 may hydrolyse
appreciably to give the hydrogen phosphate ion HPO42- and hydroxide ion, and should accordingly be
washed with dilute aqueous ammonia. If salts of weak bases, such as hydrated iron (III), chromium (III), or
aluminium ion, are to be separated from a precipitate, e.g. silica, by washing with water, the salts may be
hydrolysed and their insoluble basic salts or hydroxides may be produced together with an acid.

The addition of an acid to the wash solution will prevent the hydrolysis of iron (III) or similar salts: thus
dilute hydrochloric acid will serve to remove iron (III) and aluminium salts from precipitates that are
insoluble in this acid.

Solubility losses are reduced by employing the minimum quantity of wash solution consistent with the
removal of impurities. It can be readily shown that washing is more efficiently carried out by the use of many
small portions of liquid than with a few large portions, the total volume being the same in both instances.

6. DRYING AND IGNITION OF THE PRECIPITATE

When the precipitate has been washed free from excess of the precipitant and other soluble
impurities, it is convered to a substance of constant compositon before it is weighed. The details
of the actual temperature of drying or the temperature of ignition are given in the description of
each determination. General techniques are outlined below.

The funnel containing the washed precipitate is covered with a piece of filter paper (not ashless),
moistened with distilled water. The paper projecting beyond the rim of the funnel is pressed
firmly against the outside of the funnel and turn off. This forms a close-fitting lid which protects
the precipitate against dust, currents of air etc. The funnel with precipitate is then put for 20 - 30
minutes into a drying oven at about 90 — 105°C.

Electric drying ovens are generally used in laboratories. The lower part of the oven contains several heating
coils covered with a perforated metal sheet. The outside of the oven is provided with switches for the

SAMPLE
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10.
separate coils so that the temperature can be regulated. An oven fitted with a thermoregulator, which
maintains the required temperature automatically, is especially convenient. The oven has shelves with holes

into which the funnels containing the precipitates are inserted.

Of course, if the precipitate is not ignited on the same day, there is no need to put it in the drying oven, as it
will dry at room temperature.

Precipitates are ignited in porcelain or platinum crucibles. Before the ignition the weight of the empty
crucible must be known, and it is necessary to be sure that this weight will not alter during the ignition. The
crucible is therefore first heated to constant weight,i.e until its weight ceases to change. The crucible is
heated under the same conditions as in the subsequent ignition of the precipitate. This is done in good time
during the preceding stages of analysis. A clean and absolutely dry crucible is put in a porcelain triangle
resting on a tripe and heated in the burner flame so that the blue cone of the flame is a few millimeters below
the bottom of the crucible.

It will be remembered that when gas burners are used the air supply must be carefully adjusted. With excess
air the flame may `strike back' or go out, while with a deficiency of air a smokey flame at a low temperature
is obtained. After 15 - 20 minutes, the burner is turned out, the hot crucible is allowed to cool in air for 1 -2
minutes and then put into a Desiccator for final cooling so that the crucible does not absorb moisture from
the air and so increase in Weight.

7. WEIGHING
The ignited samples in the crucibles are cooled for a few minutes and then they are kept in a desiccator, so
that the moisture in atmosphere does not get adsorbed by the residue. Then it is accurately weighed on a
chemical balance.

8.CALCULATION