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‡ Gravimetric methods are quantitative methods

based on determining the mass of a pure
compound to which the analyte is chemically
related.
‡ gravimetric analyses are highly accurate and
precise because they use the analytical balance
as measurement tool.
‡ Gravimetric methods do not require a calibration
or standardization step because the results are
calculated directly from the experimental data
and molar masses.
 



 
 

  

 
 
 
‡ The analyte is converted to a sparingly soluble
precipitate and then separated from the
supernatant.
‡ The precipitate is washed free of impurities, and
converted to a product of known composition
(usually by heating to obtain a more stable form).
‡ Finally, the product is weighed and its weight is
related back to the amount of analyte in the
original sample via a gravimetric factor (GF).
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 ï
‡ The analyte or its decomposition products are
volatilized and the volatile product is collected and
weighed.
‡ Or the weight of the product can be determined
indirectly by determining the weight loss of the
sample.
 




‡ Colloidal suspensionï diameterï



cm; not to settle from solution; nor can be
filtered.
‡ Crystalline suspensionï diameterï tenths of
a millimeter or greater; settle from solution;
readily filtered.
‡ Large crystals (but, not a chunk) are
preferable because they are readily
filterable, have less surface area to react
with atmosphere or adsorb impurities.



  
 

‡  is the concentration of the solute at any time and  is

the equilibrium solubility.
‡ A supersaturated solution is an unstable solution that
contains more solute than a saturated solution
‡ To increse particle size of a precipitate, minimize the
relative supersaturation during precipitate formation.
‡ When (Q)/ is large, the precipitate tends to be
colloidal; when (Q)/ is small, a crystalline solid is
more likely.
 sow do precipitates form?
‡  
   



 

‡ ! 
 results in large number of fine
particles,
‡ 
 
results in a relatively
small number of large particles.
 s" 
 

‡ low addition of precipitant with frequent

stirring (decrease Q)
‡ Use of dilute solutions of analyte and
precipitant (decrease Q)
‡ Elevated temperatures increase solubility
(increase )
Why are the colloidal particles relatively stable?
sow to let colloidal particles precipitate?
 Treatment of colloidal precipitates

‡ seating and stirring

‡ Increasing the electrolyte concentration
‡ Digestion (a process in which a precipitate
is treated for an hour or more in the
solution from it was formed)
 Coprecipitation
‡ urface adsorption
‡ Mixedcrystal formation
‡ Occlusion
‡ Mechanical entrapment

What are the characteristics of each type of coprecipitation?

sow to minish the minus effect caused by coprecipitation?
 somogeneous precipitation
‡ A process which a precipitate is formed by slow
generation of a precipitating reagent
homogenously throughout a solution
‡ olids formed by homogenous precipitation are
generally purer and more easily filtered than
precipitates generated by direct addition of a
reagent to the analyte solution

‡ Why do the results obtained?

Drying and Ignition of Precipitates

‡ seating removes
the solvent and
volatile species
‡Igniting decompose
the precipitate and
form a compound
named weighting
form


 
   
 


 Calculating results from gravimetric data

‡ Example 8 , 8, 8.

The Gravimetric Factor
Calculation of weight percent of analyte
Example
The Gravimetric Factor
     
 
 



  

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$
  


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‡ . readily filtered and washed free of contaminants
‡ . of sufficiently low solubility so that no significant loss
of the analyte occurs during filtration and washing
‡ . unreactive with constituents of the atmosphere
‡ . of known composition after it is dried or, if necessary,
ignited
Applications of gravimetric methods
‡ Inorganic precipitating agents
‡ Organic precipitating agents

‡ What are advantages by using Organic

precipitating agents?
  
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%  

  
ï
‡ . Find a stable, insoluble form of the analyte
‡ . eparate the analyte from the other matrix
components in this form
‡ . Wash the precipitate containing the analyte free
of any impurities
‡ . Convert the precipitated form of the analyte to a
more reliable weighing form (usually by heating)
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 Gravimetric method overview
‡ Simple
‡ Cheap
² Glassware
² Reagents
² ovens, etc.
² Balances
‡ Specific
‡ Timely
‡ Accurate
‡ Precise
‡ Sensitive
 ummary
‡ Colloidal and crystalline suspension
‡ Relative supersaturation (Q)/
‡ Nucleation and particle growth
‡ Controlling particle size
‡ Coprecipitationï surface adsorption, mixed
crystal formation, occlusion and mechanical
entrapment
‡ somogenous precipitation
‡ Gravimetric Factor
‡ Applications