Thermal Methods of Analysis Wilkes University威尔克斯大学热分析方法.pptVIP

Thermal Methods of Analysis Background and Continued Evolution into Hyphenated Methods of Chemical Analysis Thermal Methods of Analysis Properties are measured as a function of temperature, time, or both Heat flow – direction and magnitude Mass change – loss / gain Mechanical properties Sheer Strain Dynamic loading Gas evolution Traditional Thermal Analysis Calorimetric Methods of Analysis Coffee cup calorimetry (constant P) Bomb calorimetry (constant V) Gravimetric Methods of Analysis Heating until constant weight loss Traditional C / H analysis Differential Thermal Analysis (DTA) Analysis of heat flow direction (endo vs. exo) as a function of temperature as a function of time at a given temperature Coffee Cup Calorimetry Bomb Calorimetry Heat to constant mass Loss of waters of hydration CuSO4?5H2O(s) ? CuSO4(s) + 5 H2O(g) Decomposition of Oxalates CaC2O4(s) + ? O2(g) ? CaCO3(s) + CO2(g) Carbonates CaCO3(s) ? CaO(s) + CO2(g) Combustion Analysis a known mass of a compound (with an unknown formula but known elemental makeup) is burned in an excess of O2 CuO oxidizes traces of C and CO into CO2. It also ensures that all of the H2 is oxidized completely to H2O H2O is collected in an absorber filled Mg(ClO4)2 CO2 is collected in a separate absorber filled with NaOH The change in mass of the absorbers is used to determine the amount of CO2 and H2O produced and thus the initial amount of C and H in the compound Differential thermal analysis (DTA) DTA involves heating or cooling a test sample and an inert reference under identical conditions, while recording any temperature difference between the sample and reference. This differential temperature is then plotted against time, or against temperature. Changes in the sample which lead to the absorption or evolution of heat can be detected relative to the inert reference. Evolution of Thermal Analysis ThermoGravimetric Analysis (TGA) Analysis of mass change as a function of temperature as a function of time at a giv