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授課教師: Professor 吳逸謨 教授 Warning: Copyrighted by textbook publisher. Do not use outside class. Principles of Instrumental Analysis Section Six Miscellaneous Methods p. 893 Chapter 31 Thermal Methods Contents: TGA, DTA, DSC Time: 3 hrs (1 week) 11 Miscellaneous Methods Chap. 31 Thermal Methods DSC, DTA, TGA The following Chapters are not covered: • Chap. 32 Radiochemical • Chap. 33 Automated analyses • Chap. 34 Particles size determination Laboratory items – 下學期實驗課 DSC – Differential scanning calorimeter [Note: DTA is similar to DSC. DTA is less often used now.] TGA (2008購) – Thermogravimetric analyzer 22 Chapter 31 Thermal Analysis p.894 Thermal Analysis – Definition Techniques in which a physical (thermal) property of a substance is measured as a function of temperature while the substance is subjected to a controlled temperature variation. More than a dozen of such thermal techniques are used. But only three techniques are covered in this chapter: 1. Thermogravimetry analysis (TGA) 2. Differential thermal analysis (DTA) 3. Differential scanning calorimetry (DSC) 33 TGA p. 894 The mass of a sample in a controlled atmosphere is recorded continuously as a function of temperature (or time) as the temperature of the sample is increased. TGA thermogram: - A plot of mass percent as a function of time or temperature. [TGA measures the change in weight of a sample as it is heated, cooled or held at constant (isothermal) temperature.] Instrumentation of TGA includes the following: (1) A sensitive analytical balance Range : up to 100 mg. Sample holder is in furnace. However, the rest of the balance must be thermally isolated from the furnace. (2) furnace Temperature range: up to 1500oC. (3) purge gas system For prevention of oxidation: N2, Ar, He, etc. For oxidation: O2 or air. (4) Temperature control and a computer for data acquisition /display. 44
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