ANALYTICAL METHOD FOR MINERALS IDENTIFICATION

Minerals are naturally occurring, solid inorganic compounds with a definite physical, chemical
composition and an orderly internal arrangement of atoms. This orderly internal arrangement of
structure is what makes it crystalline. The crystal lattice of a mineral are held in place by atomic
bonds. There are various methods for the identification of soil minerals, example; differential
thermal analysis.

Differential Thermal Analysis (DTA)

Differential thermal analysis (DTA) is a technique for identifying and quantitatively analyzing
the chemical composition of substances by observing the thermal behavior of a sample as it is
heated. The technique is based on the fact that as substance is heated, it undergoes reactions and
phase changes that involve absorption or emission of heat. In DTA the temperature of the test
material is measured relative to that of an adjacent inert material (Jose, 2017). The sample and
the reference material (sample) are heated in one furnace. The difference of the sample
temperature and the reference material temperature is recorded during programmed heating and
cooling cycles (Höhne et al., 2003). The result is a DTA curve. DTA curve is a curve of
temperature difference between the sample material and the reference material versus
temperature or time.

DTA consists of simultaneously heating a test sample and a thermally inert substance at constant
rate (usually about 10 °C/min) to over 1000 °C and continuously measuring the differences in the
temperature between the sample and the inert material. The amount of heat involved and
temperature at which these changes take place are characteristic of individual elements or
compounds; identification of a substance, therefore, is accomplished by comparing DTA curves
obtained from the unknown with those of known elements or compounds. The DTA technique is
widely used for identifying minerals and mineral mixtures. Differential thermal analysis (DTA)
was constructed soon after the development of the thermocouple (1887, Le Chatelier). Most of
the research efforts were made on clay and carbonate materials. A Differential Thermal Analyzer
is composed of three major components;

1. Sample holder comprising thermocouples, sample containers and a ceramic or metallic block.
2. Furnace (a controlled source of heat).

3. Recording system (a device for the measurement of the heats of reaction).

Fig. 1: Schematic illustration of a DTA cell.

Differential Thermal Analysis (DTA) is a "fingerprinting" technique that provides information

on:

 The chemical reactions,

 Phase transformations, and

 Structural changes that occur in a sample during a heat-up or a cool-down cycle.

Thermal Reactions

1. Dehydration: water is present as adsorbed water or water of hydration driven off at 100
to 3000C (reversible process). Crystal lattice water in form of (OH) ion removal is called
dehydroxylation. It is not reversible and it destruct mineral structure. Endothermic reaction.

2. Crystallization: new crystals can form from amorphous material. All crystals destroyed
at a lower temperature. It is an exothermic reaction.
3. Phase Changes: Some crystal structures change from one form to another at a specific
temperature. Quartz changes from α to β form at 573°C (reversible) peak appears during cooling.
Endothermic

4. Oxidation: Combustion of organic matter (250-450 °C), Oxidation of Fe 2+ to Fe3+.

Exothermic

Characteristic Thermograms

Clay minerals:

 Endothermic reaction at 100-200°C absorbed water is lost.

 Endothermic reaction at 500-1000 °C dehydroxylation

 Exothermic reaction at 800-1000 °C Recrystallization.

Non-clay minerals

 Quartz: Endothermic at 573 °C

 Carbonates: Endothermic (very large peaks) at 800 °C -1000 °C

 Oxides (such as gibbsite, brucite and geothite) Endothermic reaction at 250-450 °C .

 Organic matter Exothermic reaction at 250-450 °C .

Quantitative Analysis: Area of the reaction peak can be considered as indicating the amount of
mineral present.

Conclusion
The DTA measures the differences in energies released or absorbed, and the changes in heat
capacity of materials as a function of temperature. All materials behave in certain, predictable
ways when exposed to certain temperatures, so the resulting DTA curve is an indication of the
materials and phases present in the sample. The DTA technique is widely used for identifying
minerals (such as clay) and mineral mixtures.
References

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Höhne, G. W. H., Hemm inger, W. F., Flamm ersheim, H. J. (2003): Differential Scanning
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Jose, C. C., Abraham, J. Kumar, M. R., George, S. C., and Thomas, S. (2017). Instrumental
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