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Volatilization Grav

Volatilization gravimetry involves changing the chemical state of a sample through thermal or chemical decomposition, allowing for the measurement of volatile products or remaining residues. Thermogravimetry continuously monitors the mass of a sample as temperature increases, helping identify decomposition products and enabling analytical procedures. Derivatization modifies compounds to make them suitable for analysis by techniques like gas chromatography, focusing on reactions such as silylation, alkylation, and acylation.

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Volatilization Grav

Volatilization gravimetry involves changing the chemical state of a sample through thermal or chemical decomposition, allowing for the measurement of volatile products or remaining residues. Thermogravimetry continuously monitors the mass of a sample as temperature increases, helping identify decomposition products and enabling analytical procedures. Derivatization modifies compounds to make them suitable for analysis by techniques like gas chromatography, focusing on reactions such as silylation, alkylation, and acylation.

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Volatilization Gravimetry

The aim of volatilization is to cause the change in chemical state of the sample.
Volatilization of the sample can be carried out either by heating the sample or by using the
certain types of chemical reagents (Derivatization). In volatilization gravimetry; the solid
sample is thermally or chemically decomposed. The volatile products of the decomposition
reaction may be trapped and weighed to provide quantitative information. Alternatively, the
residue remaining when decomposition is complete may be weighed. Volatilization is done
by two methods.
1. Through heating the Sample → Thermogravimetry
2. Derivatization (used in chromatographic techniques; specially for GC and GC/MS*)

1. Thermogravimetry

Thermogravimetry is one of the type of volatilization gravimetry in which sample’s


mass is continuously monitored while the applied temperature is slowly increased. In
thermogravimetric analysis, the sample is placed in a small weighing bottle attached to one
arm of a specially designed electromagnetic balance and placed inside an electric furnace.
The temperature of the electric furnace is slowly increased at a fixed rate of a few degrees
per minute, and the sample’s mass is monitored.

Theory
Thermogravimetry requires that the products of the decomposition reaction be
known. This requirement is rarely a problem for organic compounds for which volatilization
is usually accomplished by combustion and the products are gases such as CO2, H2O, and N2.
For inorganic compounds, however, the identity of the volatilization products may depend on
the temperature at which the decomposition is conducted.
In thermogravimetry, the products of a
thermal decomposition can be deduced
by monitoring the sample’s mass as a
function of applied temperature. The
loss of a volatile gas on thermal
decomposition is indicated by a step in
the thermogram. The change in mass
at each step in a thermogram can be
used to identify both the volatilized
species and the solid residue.
Once the products of thermal
decomposition have been determined, an analytical procedure can be developed.

*GC= Gas Chromatography


GC/MS= Gas Chromatography/ Mass Spectrometry

1
For example, the given thermogram shows that a precipitate of CaC2O4 .H2O must be heated
at temperatures range of 250°C to 400°C if it is to be isolated as CaC2O4. Alternatively, by
heating the sample to 1000 °C, the precipitate can be isolated as CaO. Knowing the identity
of the volatilization products also makes it possible to design an analytical method in which
one or more of the gases are trapped. Thus, a sample of CaC2O4 .H2O could be analyzed by
heating to 1000 °C and passing the volatilized gases through a trap that selectively retains
H2O, CO, or CO2.
Each volatilization gravimetric procedure has its own unique characteristics, for
example Silicon is determined by dissolving the sample in acid. Dehydration of the resulting
solution precipitates silicon as SiO2. Because a variety of other insoluble oxides also form,
the precipitate’s mass does not provide a direct measure of the amount of silicon in the
sample. Treating the solid residue with HF results in the formation of volatile SiF4. The
decrease in mass following the loss of SiF4 provides an indirect measure of the amount of
silicon in the original sample.

2. Derivatization

Often compounds cannot be analyzed by a particular method because they are not in a
form that is amenable to the analytical technique. Examples of this problem are nonvolatile
compounds for gas chromatographic analysis and insoluble compounds for high performance
liquid chromatography (HPLC) analysis. Many materials that are not stable under the
conditions of the technique also fall into this category. The derivatization procedure modifies
the chemical structure of the compounds so that they can be analyzed by the desired
technique.

Types of Derivatization

The bulk of analytical derivatization reactions used for gas chromatography (GC) fall into
three general reaction types: silylation, alkylation and acylation. For GC analysis,
compounds containing functional groups with active hydrogens (e.g., -COOH, -OH, -NH and
-SH) are of primary concern. The tendency of these functional groups to form intermolecular
hydrogen bonds affects the inherent volatility of compounds containing them, their tendency
to interact deleteriously with column packing materials and their thermal stability. Silylation,
alkylation and acylation all are used to modify these classes of compounds.

Suggested Readings

1. Handbook of Analytical Derivatization Reactions by Daniel R. Knapp.


2. Silylation of Organic Compounds by Alan E. Pierce

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