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AE 2 Group 03
Explanation Report
SEMESTER 1 2020/2021
There are seven steps involved in the process of precipitation gravimetric analysis.
The first step is the preparation of the solution with a known weight of the sample. Silver
chloride (AgCl) solution is the solution that is usually prepared in this analysis. It can be
prepared from the reaction between magnesium chloride (MgCl2) and silver nitrate
(AgNO3). The solution prepared needs to maintain a low solubility to obtain a more
suitable form for filtration. A few factors need to be considered while preparing the
solution, which are the volume of solution, concentration, temperature, and pH.
The second step is precipitation. Precipitation refers to the formation of a solid from
a solution. When a reaction occurs in a liquid solution and solid formed, the solid formed
is precipitate. Before conducting precipitation, a few significant conditions need to be
considered. The precipitate firstly needs to be insoluble so that it can reduce the amount
of loss due to solubility. It must also be stable under atmospheric conditions. The
precipitation process requires the addition of a precipitating agent solution to the sample
solution. After adding the precipitating agent, supersaturation followed by nucleation and
particle growth occurs. Both nucleation and particle growth are direct functions of
supersaturation.
However, during precipitation, the precipitate often contained ions that were trapped
in it. This causes a problem for the crystalline precipitates. If the trapped ions are not
volatile, their presence will eventually corrupt the weighing. Hence, the concentration of
interfering species is reduced by digestion. The precipitate is redissolved and being
precipitated out to a cleaner environment of a solution during the digestion process. The
precipitate that has been obtained during the separation is placed into a volatile electrolyte
solution and heated. Thus, larger particles are broken down to speed up the digestion
process. This solution is often heated first to increase the kinetic rates of dissolution and
precipitation. All the material will cycle from solid to solution and back since the solid is
in dynamic equilibrium with the solution. This does not speed up the chemical kinetics so
the solution will be cooled after digesting for an hour or more. The precipitate is being
prefiltered (Bialkowski, 2004).
Next step is the filtration steps. To filter the precipitates, sintered glass crucibles are
used. These sintered glass crucibles are marked as fine(f), medium(m) and coarse
porosities(c). First, the crucibles are first cleaned thoroughly and then subjected to the
same regimen of heating and cooling required for the precipitate. This process is repeated
until a constant mass differing by 0.3 mg or less has been achieved. However, colloidal
precipitates that are present cause a filtering problem if the particles are too small. Thus,
filter paper or glass can be plugged and passed right through the filter if they are not
coagulated well. Hydrophobic colloids generally filter better than hydrophilic colloids.
The fifth step is washing. Washing can remove the mother liquor and some of the
coprecipitated compounds but can also cause peptization of colloids. Thus, by diluting the
counter-ion layer causes it to get larger, forcing the coagulated colloidal particles apart.
After diluting it and forcing the particles apart, they will go right through the filter.
Washing it with a solution of a volatile electrolyte and it will be removed in the drying
step.