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Gravimetric Methods - 3

Gravimetric analysis methods determine the quantity of a substance by measuring its mass. There are three main types: precipitation gravimetry forms a precipitate whose mass is measured, electrogravimetry measures the mass of an electrodeposit, and volatilization gravimetry measures the mass lost upon volatilization. For precipitation gravimetry, the precipitate should react specifically with the analyte, be insoluble, pure, and easy to separate from the reaction mixture. Particle size and filterability of precipitates also impact accuracy. Examples show calculations for determining percentages of substances from measured precipitate masses.

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105 views34 pages

Gravimetric Methods - 3

Gravimetric analysis methods determine the quantity of a substance by measuring its mass. There are three main types: precipitation gravimetry forms a precipitate whose mass is measured, electrogravimetry measures the mass of an electrodeposit, and volatilization gravimetry measures the mass lost upon volatilization. For precipitation gravimetry, the precipitate should react specifically with the analyte, be insoluble, pure, and easy to separate from the reaction mixture. Particle size and filterability of precipitates also impact accuracy. Examples show calculations for determining percentages of substances from measured precipitate masses.

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Gravimetric Methods of Analysis

Aliya Nur Hasanah


Analytical Chemistry Laboratory
2016
Fig 12-5, p.324
Gravimetric
Any method in which the signal is a mass
or change in mass.
Gravimetric Analysis
• Formation and growth of crystals are very important
in analytical chemistry and other areas of science.
• Gravimetric methods are based on determining mass
of a pure compound to which the analyte is
chemically related.
Types of Gravimetric Methods
• precipitation gravimetry
A gravimetric method in which the signal is the mass of a precipitate.
• electrogravimetry
A gravimetric method in which the signal is the mass of an electrodeposit on
the cathode or anode in an electrochemical cell.
• volatilization gravimetry
A gravimetric method in which the loss of a volatile species gives rise to the
signal.
Gravimetric Analysis
• Precipitation gravimetry:

A precipitating agent should react specifically or at


least selectively with the analyte.

Spesific : DMG to Ni
Selective : 8-hydroxyquinoline with pH control
The attributes of the precipitate
• must be of low solubility,
• high purity,
• known composition if its mass is to accurately reflect the
analyte’s mass.
• must be in a form that is easy to separate from the reaction
mixture.
Gravimetric Analysis
• Particle Size & Filterability of Precipitates:

– Larger particles generally more desirable.


– Factors that determine Particle Size:

1. Colloidal vs. Crystalline suspensions


2. Relative supersaturation
3. Mechanism: Nucleation & Particle Growth
Example
An ore is analyzed for the manganese content by converting the
manganese to Mn3O4 and weighing it. If a 1,52 g sample yields Mn3O4
weighing 0,126 g, what would be the percent Mn2O3 in the sample ?

% Mn2O3 = 0,126 g Mn3O4 x (3Mn2O3/2Mn3O4)(BM Mn2O3/ BM Mn3O4) x100%

1,52 g

= 0,126 x 3 (157,9)/2(228,8)

1,52 g

= 8,58 %
Example
The calcium in a 200 mL sample of natural water was determined by
precipitating the cation as CaC2O4. the precipitate was filtered, washed, and
ignited in a crucible with an empty mass of 26.6002 gram. The mass of the
crucible plus CaO (56.077g/mol) was 26.7134 gram. Calculate the
concentration of Ca (40.078 g/mol) in water in units of grams per 100 mL of
the water
Example
A sample contain Na2SO4 were determined gravimetrically using BaCl2 as
precipitating agent to formed BaSO4 precipitated. If 25 gram of sample was
used to formed 5.342 g BaSO4. calculate how much Na2SO4 (%) on the sample
and how much SO4 (%) on the sample ?

BM BaSO4 : 233,4
BM Na2SO4 : 142.05
BM SO4 : 96.07
Fig 12-6, p.325
p.331

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