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STEP 1: PREPARING SAMPLE

Factors to be considered while preparing sample solution are;

Volume of solution during precipitation:


o Solution condition (volume) must be adjusted to maintain low solubility of precipitate
o Excess volume of solution during precipitation
o Leads to precipitate will be coagulate

Ph: - Influence the solubility of the analytical precipitate


- Possibility of interference from other substance
- Example: During Calcium oxalate preparation

Temperature:

Increase the temperature


Increase solubility of precipitate
dissolved or coagulated & Difficult to filter

Precipitate will

STEP 2: PRECIPITATION
Precipitation method is a process of weighing an element in form of precipitates which is separated by filtration from solution.
Factors affecting on precipitation method:
Precipitates must be free from soluble impurities
Precipitates must be insoluble in solution
Precipitates must be readily separated from the solution by filtration
Precipitates must be convertible into a pure compound by ignition or by simple evaporation
Example: Gravimetric analysis of a sulphate or halides
Na2SO4 + BaCl2 BaSO4 + NaCl
NaCl + AgNO3 AgCl + NaNO3

STEP 3: FILTRATION

Filtration is a process of separating precipitates from the mother liquor. The media employed for filtration are:
Filter paper
Gooch crucible
Porous fritted plates of resistance glace (Pyrex sintered crucible)
Vitreosil filtering crucibles (Silica)
Porcelain filtering crucibles (Porcelain)
The choice of filtering medium depends on nature of the precipitates and by cost factor.
Properties of filter paper:
It should be Ash-less
Size and diameter of filter paper should be according to the bulk of the precipitates
Pores of filter must be smaller than the size of the particle of the precipitates.
Example: Bulky precipitates like aluminium hydroxide need a larger filter paper than dense precipitates like barium sulphate.
Washing:
Precipitates must be washed with liquid to remove all soluble impurities sticking with the precipitates.
Properties of Ideal washing liquids:
Having no solvent action on precipitates but must removes all foreign impurities
Should not form any volatile product with precipitates
Should easily volatile on ignition
Should have no dispersive action on the precipitates
Should not interfere with precipitates

- If precipitates get colloid during filtration the solution used for washing must contain electrolytes e. g.

ammonium nitrate
solution is used for washing iron (III) hydroxide.
- If precipitates tends to oxidize during filtration, then solution used for washing must reconvert the oxidise form to its
original one e. g. acidified hydrogen sulphide water for copper sulphide.
- If precipitates settles rapidly or is gelatinous by nature, then washing is done by decantation. Gelatinous precipitates require
more washing than crystalline ones e. g. aluminium hydroxide requires more washing than calcium oxalate.

STEP 4: DRYING AND IGNITION

After washing, precipitates are dried or ignited depending on the nature of precipitates and on the filtering medium.
Precipitates that are dried (below 250C) or ignited (above 250C) should be collected on filter paper, porcelain filtering
crucibles or silica filtering crucibles. The temperature at which precipitates are dried or ignited can be determined by a study of
thermogravimetry.
Thermogravimetry is a technique in which a change in the weight of a substance is recorded as a function of temperature or
time. It is used in conjunction with other techniques like differential thermal analysis (DTA), gas chromatography and mass
spectrometry.
Crystalline precipitates absorb water or solvent can be easily removed by heating the precipitates e. g. cuprous thiocyanate.

EXAMPLE:
AgCldrying in over 100 -1300C to remove physically-bound water.
Higher temp. is necessary if water is trapped in crystals / chemically-bound water / or ensure
appropriate chemical changes
Mg2P2O7--> MgNH4PO 900oC
CaC2O4--> CaO 1100oC
STEP 5: WEIGHING & CALCULATION
Ignited sample is cooled for a few minutes and then kept in a desicator to avoid moisture adsorption and then weighed on a
chemical balance.

Advantages:
Extensive numbers of inorganic ions are determined with excellent precision and
accuracy.
Routine assays of metallurgical samples.
Relative precision 0.1 to 1%
Good accuracy
Disadvantages:
v Careful and time consuming.
v Scrupulously clean glassware.
v Very accurate weighing.
v Coprecipitation.