Thermogravimetric analysis

Thermogravimetric Analysis
Acronym TGA
Classification

Thermal analysis

Other techniques
Related Isothermal titration calorimetry
Dynamic mechanical analysis
Thermomechanical analysis
Thermogravimetric analysis
Differential thermal analysis
Dielectric thermal analysis

Thermogravimetric analysis or thermal gravimetric analysis (TGA) is a type of testing performed on samples that determines changes in weight in relation to change in temperature. Such analysis relies on a high degree of precision in three measurements: weight, temperature, and temperature change. As many weight loss curves look similar, the weight loss curve may require transformation before results may be interpreted. A derivative weight loss curve can identify the point where weight loss is most apparent. Again, interpretation is limited without further modifications and deconvolution of the overlapping peaks may be required. To determine composition and purity one must take the mass of the substance in the mixture by using thermal gravimetric analysis. Thermal gravimetric analysis is the act of heating a mixture to a high enough temperature so that one of the components decomposes into a gas, which dissociates into the air. It is a process that utilizes heat and stoichiometry ratios to determine the percent by mass ration of a solute. If the compounds in the mixture that remain are known, then the percentage by mass can be determined by taking the weight of what is left in the mixture and dividing it by the initial mass. Knowing the mass of the original mixture and the total mass of impurities liberating upon heating, the stoichiometric ratio can be used to calculate the percent mass of the substance in a sample. TGA is commonly employed in research and testing to determine characteristics of materials such as polymers, to determine degradation temperatures, absorbed moisture content of materials, the level of inorganic and organic components in materials, decomposition points of explosives, and solvent residues. It is also often used to estimate the corrosion kinetics in high temperature oxidation.

Simultaneous TGA-DTA/DSC measures both heat flow and weight changes (TGA) in a material as a function of temperature or time in a controlled atmosphere. Simultaneous measurement of these two material properties not only improves productivity but also simplifies interpretation of the results. The complementary information obtained allows differentiation between endothermic and exothermic events with no associated weight loss (e.g. melting and crystallization) and those that involve a weight loss (e.g. degradation).

Equipment

The analyzer usually consists of a high-precision balance with a pan (generally platinum) loaded with the sample. A different process using a quartz crystal microbalance has been devised for measuring smaller samples on the order of a microgram (versus milligram with conventional TGA).[1] The sample is placed in a small electrically heated oven with a thermocouple to accurately measure the temperature. The atmosphere may be purged with an inert gas to prevent oxidation or other undesired reactions. A computer is used to control the instrument.

Methodology

TGA is a process that utilizes heat and stoichiometry ratios to determine the percent by mass of a solute. Analysis is carried out by raising the temperature of the sample gradually and plotting weight (percentage) against temperature. The temperature in many testing methods routinely reaches 1000°C or greater. After the data are obtained, curve smoothing and other operations may be done to find the exact points of inflection.

A method known as hi-resolution TGA is often employed to obtain greater accuracy in areas where the derivative curve peaks. In this method, temperature increase slows as weight loss increases. This is to more accurately identify the exact temperature where a peak occurs. Several modern TGA devices can vent burnoff to an infrared spectrophotometer to analyze composition.

References

  1. ^ Mansfield, E.; Kar, A.; Quinn, T. P.; Hooker, S. A. (2010). "Quartz Crystal Microbalances for Microscale Thermogravimetric Analysis". Analytical Chemistry 82 (24): 101116152615035. doi:10.1021/ac102030z.  edit