DSC and TGA analysis.pdfVIP

EYP 2006 Differential Scanning Calorimetry Clare Rawlinson School of Pharmacy University of Bradford “Cooking with Chemicals” EYP 2006 Outline Brief history of thermal analysis Theory of thermal analysis techniques – Thermal Gravimetric Analysis (TGA) – Differential Scanning Calorimetry (DSC) Generating valid data – Calibration – Sample preparation Interpreting data and Applications – Real events – Artefacts Recent advances EYP 2006 Calorimetry Calorimetry – The study of heat transfer during physical and chemical processes Calorimeter – A device for measuring the heat transferred Lavoisier and Laplace (1782-1784): oil was burned in a lamp (Fig 9) held in a bucket (Fig. 8) held in a wire mesh cage (f) surrounded by ice in spaces b and a of the double walled container a foot in diameter lid (F) was topped with ice, as was a mesh lid (not shown) beneath it that covered the inner volume b EYP 2006 Oil lamps to Guinea Pigs… Measured heat production of the metabolic processes in the ice bath calorimeter Outer jacket prevented conduction of heat from the external environment which would have also melted the ice From latent heat of fusion for ice (334 J/gram ice at 0 oC) Lavoisier converted the rate of water formation to heat production In 10 hours 370 grams of ice melted Guinea pig produced 12,358 J per hour of heat (12.4 kJ/hr) EYP 2006 Basic Principles of Thermal Analysis Modern instrumentation used for thermal analysis usually consists of four parts: sample/sample holder sensors to detect/measure a property of the sample and the temperature an enclosure within which the experimental parameters may be controlled a computer to control data collection and processing EYP 2006 TGA and DSC Thermogravimetric Analysis (TGA) – mass change of a substance measured as function of temperature whilst the substance is subjected to a controlled temperature programme1 – mass is lost if the substance contains a volatile fraction Differential Scanning Calorim