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It is the process of isolation of element in pure form and weighing of the final product of
reaction.
Advantages
1. precise
2. It has wide range of applications
Disadvantage
Time consuming
pure
The final product must be
stable
of definite chemical structure
1. Precipitation method.
Isolation
Steps:
I. Precipitation
II. Digestion
III. Washing
IV. Filtration
V. Drying
VI. Ignition
VII. Weighing
I. Precipitation
Choice of the precipitant
1. Precipitant should be specific
i.e. Precipitate single substance thus preventing interference.
Usually available precipitant are mostly selective, i.e. precipitate a group of substances
we have to use Ba2+ (not Pb2+ or Ca2+ or Sr2+) as BaSO4 has the lowest KSP.
BaCl2 is better than Ba(NO3)2 as BaSO4 precipitate is contaminated with Ba(NO3)2.
Types of precipitates
1-Colloidal Precipitate
The particle size of this precipitate is small enough to pass through ordinary filter paper, i.e. it
no coagulation.
Coagulation of colloids
Addition of an electrolyte
coagulation
N.B.: The coagulation effect of electrolyte increases with increasing the valence of its ions and
vice-versa.
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Properties of colloids:
a. The solid is dispersed in the form of aggregates of molecules or ions
(while in true solution, solid is dispersed as individual molecules or ions).
b. The solid present in a colloidal suspension has a negligible effect, F.P., B.P and
osmotic pressure.
c. The colloidal suspension has the tendency to scatter visible radiation.
d. The ratio of surface/wt is large due to small particle size.
e. The colloid is stable without coagulation due to the presence of similar electric
charges on its particles (double electric layer).
Peptization
Upon washing a Precipitate with pure water or (distilled water) part of electrolyte (neutralizing
the double electric layer) is removed and falls below the minimum amount necessary for
coagulation leading to recharging of the precipitate again and pass into colloidal state.
2- Amorphous precipitate:
Where addition of precipitant causes rapid formation of numerous no. of very minute nuclei
which grow by joining not by deposition.
adsorbs impurities.
3. Crystalline Precipitate:
Definite crystal shape and large particle size
(small surface area)
2. Occlusion coprecipitation
In this type of contamination, impurities are coprecipitated within the precipitated particles.
N.B. During the growing of crystals impurities are displaced by ions constituting the lattice of
the formed precipitate, however this process is incomplete.
To overcome the problem of occlusion coprecipitation, we have to carry out recrystallisation
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and/ or ageing.
Example:
If we precipitate Ba2+ as BaSO4, the presence of K+ in the medium causes displacement of
In this type of contamination, the Ksp of both of the sample and interfering ion (impurity) are
exceeded at one and the same time.
Examples:
In case of precipitation of Ba2+ as BaSO4 if Pb2+ is present it will be precipitated as PbSO4
together with BaSO4.
In case of precipitation of Fe3+ as Fe(OH)3, if Al3+ & Cr3+ are present, they are precipitated as
Al(OH)3 & Cr(OH)3, together with Fe(OH)3.
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Fine crystals which are formed during precipitation disappear, i.e., crystals tend to perfect
themselves.
After digestion, precipitate becomes of large crystals (i.e. easily filtered) and of low surface
area (i.e. of low adsorption power) leading to minimum contamination by adsorption
coprecipitation.
N.B.: Rise of temperature accelerate ripening, as it increases the rate of dissolution of fine
crystals.
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Post precipitation
It is the precipitation of impurity on the surface of pure precipitate of the sample to be analyzed
after its precipitation
(i.e. Ksp of pure precipitate is exceeded first then Ksp of impurity is exceeded during digestion).
Usually occurrs with sparingly soluble substances which form supersaturated solution containing
ion in common with the precipitated sample.
Example:
During precipitation of Ca2+ as CaC2O4 in Ca2+/Mg2+ mixture, CaC2O4 is precipitated first (being of
lower Ksp), but if it is allowed to stand in contact with the mother liquor, MgC2O4 will be
precipitated on the surface (being of higher Ksp) after complete precipitation of CaC2O4.
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III. Washing
After removal of the mother liquor, final purification of precipitate is carried out by washing
to remove any adherent mother liquor together with any other soluble products of reaction
and excess precipitant present in the medium which may be adsorbed on the precipitate.
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3. Washing liquid should contain volatile electrolyte (e.g.NH4+ Salt, ammonia, dilute acids) to be
easily removed at temperature of drying leaving pure precipitate.
4. It should dissolve impurities without any solvent action or dispersive action on the precipitate.
N.B.: NH4+ salts are the most commonly used as they are volatile on ignition.
Washing must be continued until a portion of the washing liquid (filtrate) gives negative test for
some ions which are known to be present in the original solution, sample or the mother liquor
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IV. Filtration
It is the process of separation of the precipitate from the mother liquor.
The filtering medium used is usually governed by the nature of precipitate and the
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4. According to the nature of precipitate it may be incinerated with or apart from the
filter paper.
a. Incineration apart from filter paper:
This is done in case of precipitate which are easily reduced by the action of carbon (C)
produced on burning the filter paper.
In this case, after drying the precipitate at 100-105C, the precipitate is separated from
filter paper by friction, then the filter paper is incinerated in a crucible until its C is
completely burnt. Transfer the precipitate into a crucible and incineration is completed
until the crucible acquires constant weight.
VI. Weighing
After drying or ignition, the final product is weighed.
Requirements of the weighed form:
1. Has definite chemical composition (chemical formula)
2. The weighed form must have adequate chemical stability, i.e. doesnt absorb
moisture and CO2 e.g. As CaO absorbs moisture & CO2 from the atmosphere.
3. The content of element to be determined should be as low as possible to minimize
error due to incomplete transfer during weighing.
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