CHAPTER 2
GRAVIMETRIC METHODS OF
ANALYSIS
Instructor- Misikir Milkias (Msc)
Lecture 2
2017/2018 Academic year
For 2nd year chemical Engineering students
Semester I
OUTLINE
Gravimetric Methods of Analysis
Particulate Gravimetry
Electro Gravimetry
Volatilization Gravimetry
Precipitation Gravimetry
GRAVIMETRIC METHODS OF ANALYSIS
Gravimetry refers to any method which measures mass
or change in mass as a signal
Measuring mass is the most fundamental of all analytical
measurements, and gravimetry is one of oldest analytical
technique
There are at least two ways to use mass as an
analytical signal:
Direct measurement - by measuring the mass of the
analyte directly by placing it on a balance
Indirect measurement – By measuring the mass of the matrix
after removing the analyte and subtracting it from the sample
mass gives the analyte mass
samples’ initial mass = analyte + matrix
PARTICULATE GRAVIMETRY
Particulate gravimetry is type of gravimetry where the analyte
is determined following its removal from the sample matrix by
filtration or extraction
Total suspended solid in water
PARTICULATE GRAVIMETRY
Particulate Gravimetry is commonly encountered
Environmental analysis of water, air, and soil
samples.
Grain size distributions for sediments and soils are used to
determine the amount of sand, silt, and clay present in a
sample.
Microbiological testing of water also is accomplished by
particulate gravimetry.
Several standard methods for the quantitative analysis of food
samples are based on measuring the sample’s mass following a
selective solvent extraction
PARTICULATE GRAVIMETRY
EXAMPLE
A 200.0-mL sample of water was filtered through a pre-
weighed glass fiber filter. After drying to constant weight at
105oC, the filter was found to have increased in mass by 48.2
mg. Determine the sample’s total suspended solids (Wt/V%).
VOLATILIZATION GRAVIMETRY
Volatilization Gravimetry is a technique where the analyte is
being evaporated by using thermal or chemical energy and
the analytes’ mass is determined directly or indirectly.
The most common gravimetric methods based on
volatilization are those for determining water and carbon
dioxide.
Food’s moisture content by a direct analysis.
EXAMPLE
The water content of an 875.4-mg sample of cheese was
determined with a moisture analyzer. What is the %w/w H2O in
the cheese if the final mass was found to be 545.8 mg? (5%)
ELECTRO GRAVIMETRY
Electrogravimetry is type of gravimetry where the analyte is
deposited as a solid film on one electrode in an electrochemical
cell.
What if the analyte we want to determine is ion (like Pb2+? Pb2+(aq)
+ 4H2O(l) PbO2(s) + H2(g) + 2H3O+(aq)
to go to completion.
The Pb2+ ion in solution oxidizes to PbO2 and deposits
on the Pt (Platinum) electrode serving as the anode.
If we weigh the Pt anode before and after applying the
potential, the difference in the two measurements gives
the mass of PbO2 and, from the reaction’s stoichiometry,
the mass of Pb2+.
PRECIPITATION GRAVIMETRY
Precipitation gravimetry where the signal is the mass of a
precipitate. Precipitant is a reagent that causes the
precipitation of a soluble species
Quantitative and qualitative determination of organic and
inorganic components in a sample.
For example, phosphite, PO3-, reduces Hg2+ to Hg22+.
In the presence of Cl– a solid precipitate of HgCl forms.
2HgCl2(aq) + PO33–(aq) + 3H2O(l) = Hg2Cl2 (s) +
2H3O+(aq) + 2Cl–(aq)+ PO43–(aq)
The most important precipitants for inorganic cations are
chromate, the halides, hydroxide, oxalate, sulfate, sulfide, and
phosphate.
