Clearly divided into three parts, this practical book begins by dealing with all fundamental aspects of calorimetry. The second part looks at the equipment used and new developments. The third and final section provides measurement guidelines in order to obtain the best results. The result is optimized knowledge for users of this technique, supplemented with practical tips and tricks.
Stefan Sarge is working for the Physikalisch-Technische Bundesanstalt (PTB) in Braunschweig, which is the national institute for natural and engineering sciences and the highest technical authority for metrology and physical safety engineering in Germany. He is e.g. head of the working group caloric quantities. 1990 and 2004 he received the Netzsch-GEFTA awards. G?nther H?hne, born 1937 in Berlin (Germany) studied chemistry, physics and mathematics at the Technical Universit?t Berlin. In 1997 he was appointed Privatdozent after his habilitation in experimental physics. 1970 - 1999 he was head of the section for calorimetry of the University of Ulm, including academic teaching in physics. Since 1999 he is visiting professor at the Eindhoven University of Technology. In 2002 he received the science award of German Society of Thermal Analysis (GEFTA). He published 115 articles and 2 monographs on calorimetry and DSC. Wolfgang Hemminger was working at the University of Braunschweig as well as for the PTB, the national institute for natural and engineering sciences and the highest technical authority for metrology and physical safety engineering in Germany. He is author of numerous journals and book publications. In 2006 he received the science award of the GEFTA and 1981 the Netzsch-GEFTA award.
Table of Contents
PART 1: CALORIMETRY - Definition, Examples, Units 1 Methods of Calorimetry Compensation of the Thermal Effect Compensation by a Phase Transition Compensation by Electric Effects Compensation by Chemical Heat of Reaction Measurement of Temperature Differences Measurement of Time-dependent Temperature Differences Measurement of Local Temperature Differences Summary of Measuring principles Classification of Calorimeters Different Approaches as Drawn from Literature 2 Fundamentals of Calorimetric Measurements Auxiliary Measuring Instruments Measurement of Material Quantities Measurement of Electric Quantities Measurement of Temperatures Measurement of Mass Measurement of Time Concept of Traceability Fundamental Basic Measurements Calibration The Role of (Certified) Reference Materials Uncertainty of Measurement Approach of the Guide to the Expression of Uncertainty in Measurement Application to Simple Problems Uncertainty of an Experiment by Bomb Combustion Calorimetry 3 Fundamentals of Thermodynamics States and Processes Thermodynamic Variables (Functions of State) Forms of Energy, Fundamental Form, Thermodynamic Potential Function Equilibrium Reversible and Irreversible Process The Laws of Thermodynamic Measurement of Thermodynamic State Functions Phases and Phase Transitions Multiphase Systems Phase Transitions Gibbs Phase Rule Measurement of Variables of State in Phase Transitions Calorimetry as the Art of Applied Thermodynamics 4 Heat Transport Phenomena Heat Conduction Free Convection Forced Convection Heat Radiation Heat Transfer 5 Surroundings and Modes of Operation Isothermal Operation Isoperibol Operation Adiabatic Operation Scanning Operation Combinations Found in Reality 6 The Measured Curve and its Evaluation Consequences of Temperature Relaxation within the Sample Measured Curves of Different Types of Calorimeters Adiabatic Calorimeter Isoperibol Calorimeter Differential Scanning Calorimeter (DSC) Reconstruction of the True Heat Exchange Function from the Measured Curve Special Evaluations Determination of Specific Heat Capacity Determination of the Kinetic Parameters of a Chemical Reaction Determination of Phase Transition Temperatures Determination of Heats of Transitions Determination of Purity PART 2: CALORIMETERS 7 Calorimeters with Compensation of the Thermal Effect Phase Transition Calorimeters Ice Calorimeter Calorimeters with Liquid-Gas Transition Calorimeters with Thermoelectric Compensation General Considerations Isothermal Calorimeters Isoperibol Calorimeters Scanning Calorimeters Calorimeters with a Contactless Energy Supply 8 Calorimeters Involving the Measurement of a Temperature Difference Measurement of a Time-dependent Temperature Difference General Considerations Calorimeters with Liquid Calorimeter Substance Calorimeters with Solid Calorimeter Substance (Aneroid Calorimeters) Calorimeters for the Measurement of Specific Heat Capacities Measurement of a Local Temperature Difference Heat Flux Calorimeters Flow Calorimeters 9 Commercial Calorimeters Types of Commercial Calorimeters (non exhaustive but representative) Advantages/Disadvantages Uncertainty Claims of the Manufacturers Calorimetry as a Commercially Available Service 10 New developments Nanocalorimetry (Chip calorimeters) Extreme Ranges of State (temperature, pressure, radiation,...) Calorimeters for Biological Applications Calorimeters for Space Research
PART 3: GUIDELINES FOR CALORIMETRIC MEASUREMENTS Definition of the Problem to be Investigated Selection of the Proper Calorimeter Calibration of the Calorimeter Performing the Measurement Preparation of the Sample The Calorimetric Experiment Evaluation of the Results Interpretation of the Result Uncertainty Estimation Detailed Example 11 Glossary