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Classical method of analysis based on

measurements of mass of the analyte or a related


compound.

May be Precipitation Gravimetry or Volatilization


Gravimetry
Precipitation Gravimetry- involves the conversion of
analyte to a sparingly soluble precipitate
Volatilization Gravimetry- converts analyte to a gaseous
product
1. Conversion of the analyte to a sparingly soluble
precipitate
2. Separation of Precipitate from Supernatant
3. Washing of Precipitate
4. Drying or ignition of precipitate to a known
composition
5. Weighing
6. Calculations
Analytical Balance
An instrument for determining mass with a maximum
capacity that ranges from 1 g to a few kilograms with a
precision of at least 1 part in 105 at maximum capacity

Types of Analytical Balance


Macrobalance- maximum capacity from 160 to 200 g with
s= +/- 0.1 mg
Semimicroanalytical balance- maximum loading of 10 to
30 g with s= +/- 0.01 mg
Microanalytical balance capacity of 1 to 3 g and s= +/-
0.001 mg
Buoyancy Error
Affects the data if the density f the object being weighed
significantly differs from that of the standard masses
Arises from the difference in buoyant force exerted by the
medium (air) on the object and on the masses.

Temperature Effects
Difference of the temperature of the object being weighed with
that of the surroundings
Has two sources:
(1) convection currents within the balance exert buoyant effect
on the pan and object;
(2) warm air trapped inside a closed container weigh less than
the same volume at low temperature
Porcelain or glass objects acquiring static charge
which occurs when relative humidity is low.
Relieved by using a photographers brush to relieve the
charge
are used to minimize the uptake of moisture as
dried materials undergo cooling.

Uses a chemical drying agent (desiccants) which


may be anhydrous calcium chloride, calcium
sulfate, anhydrous Mg(ClO4)2, or phosphorus
pentoxide.
Heated objects increase the temperature of
trapped air inside the desiccator. This increases
pressure, breaking the seal between the lid and
the base.

If the object and air inside the desiccator cools, a


partial vacuum is developed.
The steps involved in filtering an analytical
precipitate are decantation, washing, and transfer.

In decantation, most of the clear supernatant liquid


is passed through the filter without disturbing the
beaker where it was formed.
Why? This delays the time by which the pores
of the filter is clogged by the precipitate
The last traces of precipitate clinging to the inside
of the beaker are collected using a rubber
policeman.

Filters are never filled to more than three quarters


of their capacity?
Why? Many precipitates are capable of creeping.
Are made from cellulose fibers which are treated
with HCl and HF to remove metallic impurities and
silica. The paper then undergoes washing with a
volatile base such as ammonia.

Why use ashless filter papers in gravimetry?


Upon ignition, it leaves a residue with a mass of no more
than 0.1 mg which is negligible compared to the mass of
the precipitate to be weighed.
Why use fluted filter papers over conical filter
papers?
Fluted filter papers have larger surface area exposed for
filtration, hastening the process of filtration.
May be done using an oven, Meker burners, Tirril
burners, Bunsen types, or a Muffle furnace.
Analyte: SO3

Precipitant: Barium Chloride

Electrolyte: 6 M HCl

Reaction: Ba2+ + SO4-2 = BaSO4


Figure 4-4 The electric double layer
of a colloid consists of a layer of
charge adsorbed on the surface of
the particle (the primary
adsorption layer) and a layer of
opposite charge (the counter-ion
layer) in the solution surrounding
the particle. Increasing the
electrolyte concentration has the
effect of decreasing the volume of
the counter-ion layer, thereby
increasing the chances for
coagulation.
What Factors Determine Particle Size?
The particle size is related to relative supersaturation,
where

Q is the concentration of the solute at any instant and S


is its equilibrium solubility.
Large supersaturation ratio yields a large amount of
colloidal precipitates
Small supersaturation ratio gives a small amount of
crystalline precipitates
Using dilute solutions- minimizes Q
Using hot solutions- increases S
Slow addition of reagents- minimizes Q
Vigorous stirring- increases S
Control of pH for analyte whose precipitation is pH
dependent