Gravimetric Method

of Analysis

Gravimetric Methods of Analysis

Gravimetric Methods of Analysis are

quantitative methods involving the
measurement of the weight of an
analyte or a compound of known
composition that contains the analyte

Principles of Gravimetry
The main steps in gravimetric analysis are:

1. Preliminary treatment of sample

Sample may be pretreated for example by dissolving in appropriate
solvent or adjusting the pH

2. Isolation of the analyte

Isolate the element (or a definite compound of the element) in as pure a
form as possible for eg. by precipitation

3. Separation
Separate the element (or compound of the element) from a weighed
portion of the substance being examined eg. by filtration

Principles of Gravimetry (contd)

4. Transformation of the analyte
The element (or compound of the element) that was separated is washed,
dried and ignited to convert into a pure stable compound which can be
readily converted into a form suitable for weighing.

5. Weighing
The dry element (or compound of the element) is weighed accurately (on an
analytical balance)

6. Calculation
The weight of the element can be calculated from a knowledge of the
formula of the compound and the relative atomic mass of the constituent
elements

From the mass and known composition of the precipitate, the amount of
the original ion can be determined

Methods of Separation in Gravimetry

Precipitation
Volatilization/evolution method
Electroanalytical method
Extraction
Chromatographic methods

Gravimetric Method of Analysis Types

We will study two types of Gravimetric techniques:

1.

Precipitation

2.

Volatilization

1. Precipitation
Isolation of an ion in solution as a sparingly soluble
precipitate

Known composition or
Converted to a product of known concentration

The precipitate is:

Filtered
Washed free of contaminants
Dried and Ignited
Weighed

The original ion is determined from:

Mass of precipitate
Known composition of the precipitate

Properties of the Precipitate

The precipitate to be isolated must have the following properties:
1. Low solubility (loss of product due to solubility are negligible)
2. A known composition after drying or igniting
3. Easily filtered (should contain large crystals to make
filtration easier)
4. Readily washed free of impurities (larger crystals have
smaller surface areas for adsorption of impurities)

Properties of the Precipitate

5. No reaction with the atmosphere
6. High Purity
High Purity
.Is difficult to obtain
.Requires careful precipitation
.Can be obtained by sufficient washing to reduce impurities
Co-precipitation
.occurs when unwanted precipitation occurs along with desired
product
.minimized by slow precipitation and thorough washing

2. Volatilization
o Volatilization involves heating a sample to drive off
its volatile or gaseous species such as CO2 or H2O
o Gaseous Products
Can be collected and weighed (Direct Method)
Mass can be determined indirectly from the loss in the mass of
the sample (Indirect Method)

o Eg. determination of water, carbon dioxide in a

sample or carbon and hydrogen in organic
compounds

Volatilization Direct method

Determination of water in a sample
1.

Heating the sample and collecting the water vapour in a

solid dessicant

2.

Determine the amount of water from the increase in

mass of the dessicant

CaSO4 (Drierite) may be used as a dessicant

Volatilization Direct Method

Determination of CO2 in carbonate containing
materials
1.

Heat the sample with excess acid to evolve CO2

2.

CO2 is absorbed in an alkaline absorbent e.g. Soda Lime

or Ascarite II

3.

The increase in mass is as due to the CO2

Volatilization Direct Method

Volatilization Direct Method

Determination of carbon and hydrogen in organic
compounds
1.

Combustion of organic compound gives CO2 and

H2O

2.

CO2 and H2O can be collected and weighed

Volatilization Indirect method

Water of Crystallization in Hydrated Compounds
1.

Heat the sample to a sufficient temperature

2.

Weigh the residue the difference between the

weights is used to determine the mass of water
driven off

Apparatus used in
Gravimetric Analysis

Apparatus
Buchner (Filter )
Flask

Buchner Funnel

Vacuum Filtration Set-Up

Vacuum Filtration

Apparatus
Sintered
Crucibles

Silica
Crucibles

Vacuum filtration with sintered

crucible

 Porous disc
Porosity is
labelled from 0-5

Filter, dry and

weigh directly

Cannot
withstand
temperatures
>200 oC

Sintered Crucibles

 Container used
for drying and
igniting sample

Silica Crucibles

Inert
High resistance
to heat shock

Does not suffer

mass changes

Does not
contaminate the
product

Can tolerate
temperatures
>200 oC
http://www.csudh.edu/oliver/demos/heatcruc/heatcruc.htm

Weighing
Analyte is dried to a constant reproducible mass
Q. Why?
Ans. Solids can absorb water from air and increase in
weight. Gravimetric analysis depends on mass,
therefore weights must be accurate

Procedure
Dry sample in crucible in low temperature oven
Cool sample to room temperature in a desiccator then weigh*
Heat again, cool, weigh
Repeat until constant mass is found
* Weigh using analytical balance

Desiccators

stores dried
samples in a dry
atmosphere

hot samples are

cooled in
dessicator in
dry conditions

Contain
dessicant

Apparatus Ovens and Furnaces

Ovens
Drying precipitate under low controlled temperature

Furnaces
Drying precipitates to high temperatures

Advantages and Disadvantages

of Gravimetric Analysis

Advantages
o Very precise and accurate analysis (analytical
balance is use to weigh)
o Possible sources of errors can be easily identified (eg.
filtrate can be tested for completeness of precipitate
and precipitate maybe examined for the presence of
impurities)
o Obtain direct measurement (no calibration curve
needed)

Gravimetric Analysis Advantages

o Cheap to carry out experiment ( no expensive
equipment required just a few exceptions e.g.
crucibles furnaces)
o Used to calibrate other instruments (as an
alternative to reference standards)

Gravimetric Analysis Disadvantages

o Time consuming
o Analysis of a single element, or a limited group of
elements, at a time
o Methods are often complex (slight misstep in a
procedure can often mean disaster for the analysis)

Applications of
Gravimetric Analysis

Applications of Gravimetric Analysis

Gravimetric Analysis is used:
1. To analyze standards used for testing
and/or for calibrating instrumental
techniques
2. In analysis requiring high accuracy but
is limited to small number of
determinants since it is time consuming