TGA课件.pptVIP

热重分析(TGA) Theory Applications Mechanisms of Weight Change in TGA Weight Loss: Decomposition: The breaking apart of chemical bonds. Evaporation: The loss of volatiles with elevated temperature. Reduction: Interaction of sample to a reducing atmosphere (hydrogen, ammonia, etc). Desorption. Weight Gain: Oxidation: Interaction of the sample with an oxidizing atmosphere. Absorption. All of these are kinetic processes (i.e. there is a rate at which they occur). TGA: Purge Gas Flow TGA: Accurate Residuals Effect of Sample Size Effect of Heating Rate Mass Effect – Semi-crystalline PE Pan Shape Effect – Amorphous PMMA Sample Morphology Effects – PET Shift in Onset with Ramp Rate Time to Complete Degradation Q5000 IR – High-Heating Rate TGA Analysis Thermal Stability of Polymers Thermal Stability of an Explosive Material Thermal Stability of an Explosive Material TGA of an Adhesive Inset View Shows Strange Result Aberration in Heating Rate TGA of Drug A TGA of Drug A Monohydrate TGA of Drug A Microspheres TGA Analysis of Cold/Allergy Tablet DSC-TGA Sodium Tungstate Dehydration Sensitivity TGA-DSC Soda Ash EVA Copolymer PET w/ Carbon Black Filler PET Comparison of Filled Un-Filled PET Resolution Enhancement by Changing Purge Decomposition Kinetics Background Includes isothermal and constant heating rate methods. Constant heating rate method is the fastest and will be discussed here. Based on method of Flynn and Wall – Polymer Letters, 19, 323, (1966). Requires collection of multiple curves at multiple heating rates. Ultimate benefit obtained in ‘Life-Time’ plots. Kinetic Analysis The rate at which a kinetic process proceeds depends not only on the temperature the specimen is at, but also the time it has spent at that temperature. Typically kinetic analysis is concerned with obtaining parameters such as activation energy (Ea), reaction order (k), etc. and/or with generating predictive curves. Kinetic Analysis, con’t. Mass-Spectrom