
Thermal methods were used as instrumental methods for drug analysis. The learner is able to study the determination of different properties such as physical and chemical of the materials as they change with temperature. When the matter is heated, it undergoes certain physical and chemical changes. These physical and chemical changes take place over a wide temperature range.
It is necessary to characterize materials and their behavior over a range of temperatures to determine what materials are suitable for specific uses and to determine what temperature range materials or chemicals can withstand without changing.
Thermal methods are divided into several types such as TGA (Thermo gravimetric analysis), DTA (Differential Thermal Analysis), DSC (Differential Scanning Calorimetry), TT (Thermometric Titration), DMA (Dynamic Mechanical Analysis), TMA (Thermo Mechanical Analysis).
Students will understand the principle of the Thermogravimetric method in analytical chemistry and what is the type of TGA method. The main function of the TGA method is to determine the weight loss of the substance by applying heat or by changing the temperature. The principle of TGA is based on the fact that the sample is continuously weighed as it is heated to elevated temperatures. An instrument that is used for this purpose is called a Thermobalance. Modern TGA equipment has a sensitive balance, usually a microbalance, for continuously measuring sample weight, a furnace surrounding a sample holder, and a purge gas system for providing inert or reactive atmospheres. A computer generally controls the furnace and the data (weight vs. sample temperature) is collected and processed by the computer.
Students will be able to understand the parts of the instrument with their function which is used in the TGA method. The instrument also known as thermobalance is divided into four compartments such as a recording balance ( Thermobalance), A furnace, a Furnace controller, and A recording device. Several modern analytical microbalances are commercially available - torsion balances, spring balances, and electro balances. In general, the balance is designed so that a change in sample weight generates an electrical signal proportional to the weight change. The electrical signal is transformed into weight or weight loss by the data processing system and plotted on the y-axis of the thermal curve.
In this lecture, students will understand the factors which affect the TGA curve and the applications of the TGA method in the analysis of drugs. As per the previous lecture, the TGA curve shows the graph of weight loss versus temperature so that we can determine the decomposition of substances at different temperatures.
Students understand the function of the DTA method. Differential thermal analysis is a technique in which the temperature of the substance under investigation is compared with the temperature of thermally inert material. This differential temperature is then plotted against time, or against temperature (DTA curve, or thermogram). The method is used to determine the endothermic or exothermic changes of the material when undergoes heat.
In this lecture, students will learn about the instrumentation of the DTA apparatus. The instrumentation of the DTA method includes the different compartments and their function for the identification of different properties of the substance by applying the increasing temperature.
DTA is the type of thermal method that is used to determine or record the endothermic as well as exothermic changes that occur in the substance when it undergoes heat or by increasing the temperature. Thermal methods are used in different areas such as pharmaceuticals, forensics, to study of archaeological materials, etc.
Thermal analysis is a branch of materials science where the properties of materials are studied as they change with temperature. When the material is heated, it undergoes certain physical and chemical changes. Physical changes include phase changes such as melting, vaporization, crystallization, transitions between crystal structures, changes in microstructure in metal alloys and polymers, volume changes (expansion and contraction), and changes in mechanical behavior. Chemical changes include reactions to form new products, oxidation, corrosion, decomposition, dehydration, chemisorption, etc.
These physical and chemical changes take place over a wide temperature range. It is necessary to characterize materials and their behavior over a range of temperatures to determine what materials are suitable for specific uses and to determine what temperature range materials or chemicals can withstand without changing.
TGA (Thermogravimetric analysis) measures the amount and the rate of weight change of a material with respect to temperature or time in controlled environments. The change in the weight of the substance is recorded as a function of temperature or time. The temperature is increased at a constant rate for a known initial weight of the substance and the changes in weights are recorded as a function of temperature at different time intervals. This plot of weight change against temperature is called the Thermogravimetric curve. From TGA, we can determine the purity and thermal stability of both primary and secondary standards. Used for the determination of the composition of complex mixture and decomposition of the complex. For studying the sublimation behavior of various substances.TGA is used to study the kinetics of the reaction rate constant. Used in the study of catalysts.
DTA (Differential Thermal Analysis) is a technique in which the temperature between sample & thermally inert reference substance is continuously recorded as a function of temperature /time. This differential temperature is then plotted against time, or against temperature (DTA curve, or thermogram). The area under a DTA peak is the enthalpy change and is not affected by the heat capacity of the sample. DTA is based on changes in heat flow into the sample. Using DTA, we can detect the decomposition or volatilization of the sample, just as we can with TGA. In addition, however, physical changes that do not involve weight changes can be detected by DTA. Such changes include crystallization, melting, changes in solid crystal phases, and homogeneous reactions in the solid state. In each of these changes, there is a flow of heat between the sample and its surroundings caused by endothermic or exothermic transitions or by changes in the heat capacity. DTA is widely used in the pharmaceuticals and food industries.