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Gravimetric Analysis
Precipitation Method
Volatilization Method

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Gravimetric Analysis
Gravimetric analysis is the quantitative analysis
by weight.

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Gravimetric analysis involves weighing an analyte
or a compound of known composition containing
the analyte to determine the amount of one of the
substances present.

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Principle
The principle behind gravimetric analysis is that the
mass of an ion in a pure compound can be

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determined and then used to find the mass
percent of the same ion in a known quantity of
an impure compound.

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Types of Gravimetric Analysis
There are two (2) general types of gravimetric
analysis:

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1. __________________
2. __________________

BOTH methods involve changing the phase of the

analyte to separate it from the rest of the mixture,
causing a change in mass.
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Types of Gravimetric Analysis
There are two (2) general types of gravimetric
analysis:

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1. Precipitation Method
2. Volatilization Method

BOTH methods involve changing the phase of the

analyte to separate it from the rest of the mixture,
causing a change in mass.
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Precipitation Method
The precipitation method uses a precipitation
reaction to separate ions from a solution.

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Precipitation Method cont’d
To ensure accurate analysis, the following
conditions must be met.

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The precipitate must:
• Be a pure substance, ie. Have high purity
• Be easily filtered
• Have low solubility
• Must not react with the atmosphere
• Must be of known composition
• Must be readily washed free of impurities 7
Precipitation Method cont’d
Undesired precipitation may occur with the desired
product, that is, _____________ may occur.

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Coprecipitation is minimized by washing and slow
precipitation.
Coprecipitation – simultaneous precipitation of
more than one compound from a solution.

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Precipitation Method cont’d
Undesired precipitation may occur with the desired
product, that is, coprecipitation may occur.

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Coprecipitation is minimized by washing and slow
precipitation.
Coprecipitation – simultaneous precipitation of
more than one compound from a solution.

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Apparatus Set-up

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Summary of Precipitation Method
Analyte

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Precipitate

Washing

Drying/Igniting

Weighing
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Calculations
Method
• Precipitant or precipitating agent is added to
the solution containing the analyte.

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Precipitant – substance that causes the
precipitation of a desired substance.

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Method cont’d
• A Büchner funnel (or suction funnel) is fitted
unto a vacuum flask (or filter flask or suction

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flask) with a rubber adaptor.

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Method cont’d
• A sheet of filter paper is placed in the Büchner
funnel and all holes in the funnel covered.

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holes in Büchner funnel

• The filter paper is moistened with the solvent to

be used in the filtration.
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Method cont’d
• The flask is connected to a
vacuum source, can be a

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mechanical vacuum pump
or water aspirator pump,
and turned on.
• The mixture containing the
analyte is poured unto the
filter paper in the Büchner
funnel. Or directed into the
Büchner funnel via a glass 15
rod.
Method cont’d
• Remaining precipitate is transferred to the
funnel using water and the filtrate is collected

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into the suction flask.

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• Then washing occurs.
Method cont’d
The precipitate is washed while it is still in the filter
funnel. Water CANNOT dissolve the precipitate, but it can
wash off any remaining soluble impurities. A small amount

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of solvent may be also be used to wash the precipitate.

Filtration washing is carried out by the leaching of the

wash liquid through the precipitate layer on a filter screen;
the pore liquid is partially displaced and
replaced by the wash liquid.

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Method cont’d
• The precipitate is allowed to dry by sucking air
through the precipitate via the vacuum.

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• After adequate drying, the Buchner funnel is
removed to break the vacuum and the aspirator 18
turned off.
 Method cont’d
• The filter paper with the product it
transferred to a weighed crucible

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and ignited.
• Drying (or ignition) is done
REPEATEDLY until a constant Oven
mass is obtained. This is achieved
by cooling the sample at room
temperature in a desiccator after
heating, then weighing. It is again
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heated, cooled and weighed until
the constant mass is obtained. Analytical Balance
Method cont’d
There are two (2) types of crucibles:
1. Silica crucible – high resistance

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to heat shock due to its small
coefficient of expansion; tolerate
temperatures higher than 200°C.
2. Sintered glass crucible – porous
disc of sintered glass fused in the
body so mixtures can be filtered,
dried and weighed directly;
tolerate temperatures below 20

200°C.
Method cont’d
• The precipitate is dried in an oven at about
120-150◦C or ignited in a furnace between 600-

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1200◦C.
• If the compound decomposes upon heating, the
damp solid is air dried instead for a day. Eg.
Hydrated salts.

• A dessicator may also be used to

dry solids. Dessicator will contain
phosphorus (v) oxide, silica gel or 21
soda lime.
 Volatilization Method
• Involves separating components of the mixture
via heating or chemically decomposing the

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sample.

• Heating and chemical

decomposition
separates out volatile
components leading to
a change in mass.
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Volatilization Method
• To obtain the mass of the product, the gas
given off may be collected and weighed, or

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can be indirectly determined from the loss in
sample mass.

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Volatilization Method
• The amount of water of
crystallization in a hydrated

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salt and the moisture
content in soils and food
stuffs may be obtained by
heating the sample until
sample weight is constant.

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Example 1
The treatment of a 0.800g sample of impure
potassium chloride with aqueous silver

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nitrate resulted in precipitation of 1.460g of
silver chloride. Calculate the percentage of
potassium chloride in the sample.

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 The treatment of a 0.800g sample of impure
potassium chloride with aqueous silver nitrate

Example 1 resulted in precipitation of 1.460g of silver

chloride. Calculate the percentage of
potassium chloride in the sample.

•
Number of moles in 1.46g of AgCl = = 0.01mol
Ag+(aq) + Cl-(aq)  AgCl(s)

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KCl  K+ + Cl-
Since 1mol of AgCl is formed from 1 mol of Cl- ions,
and 1 mol of Cl- ions is formed from 1 mol of KCl, the
number of moles of KCl that reacted = 0.01mol

Mass of 0.01 mole of KCl = 0.01 x 74.5 = 0.745g

Thus, % KCl in the sample = = 93.13% 26
Example 2
A 2.5g sample of impure calcium carbonate
was decomposed with excess hydrochloric

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acid. The liberated carbon dioxide collected
in an absorbent was found to weigh 0.88g.
Calculate the percentage of calcium
carbonate in the sample.

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 A 2.5g sample of impure calcium carbonate
was decomposed with excess hydrochloric

Example 2 acid. The liberated carbon dioxide collected in

an absorbent was found to weigh 0.88g.
Calculate the percentage of calcium carbonate
in the sample.
•
Number of moles in 0.88g of CO2 = = 0.02mol
CaCO3+ 2HCl CaCl2 + CO2 + H2O

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1mol of CO2 is formed from 1 mol of CaCO3 therefore
0.02mol of CaCO3 was used in the rxn
Mass of CaCO3 used = 0.02 x 100 = 2g
Thus, % CaCO3 in the sample = = 80%

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References
• Maraj, Susan. 2011. Chemistry For CAPE. La Romaine,
Trinidad: Caribbean Educational Publishers.
• Jacobs, Helen, Novelette Sadler-McKnight, Stewart McLean,

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Patrice Piggot-Cumberbatch, Graeme Corbin, and Mike Taylor.
2014. Chemistry For CAPE Examinations. 1st ed. London:
Macmillan Publishers Limited.
• Videos retrieved from https://youtube.com
• https://www.youtube.com/watch?v=dERZhN-01f8
• https://www.youtube.com/watch?v=7odndKXhJgw
• https://www.youtube.com/watch?v=1E4YmuSY4Ek
• https://www.youtube.com/watch?v=r1IzC6PlSaw
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