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2003 | Buch | 2. Auflage

Introduction Kapitel lesen Erstes Kapitel lesen

Differential Scanning Calorimetry

verfasst von: Dr. G. W. H. Höhne, Dr. W. F. Hemminger, Dr. H.-J. Flammersheim

Verlag: Springer Berlin Heidelberg

Enthalten in: Professional Book Archive

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Über dieses Buch

In this updated and fully revised second edition, the authors provide the newcomer and the experienced practitioner with a balanced and comprehensive insight into all important methods and aspects of Differential Scanning Calorimetry (DSC), including a sound presentation of the theoretical basis of DSC thermal analysis and temperature-modulated DSC (TMDCS). Emphasis is placed on modern evaluation techniques, instrumentation, the underlying measurement principles, metrologically correct calibrations, factors influencing the measurement process, and on the exact interpretation of the results. The information enables the research scientist, the analyst and experienced laboratory staff to choose the most suitable equipment, to apply DSC methods successfully, to interpret the measurement curve, and thus to measure key properties precisely. In addition, the new edition includes improved instrumental techniques such as Tzerotm and StepScantm, new evaluation techniques, more applications, and the latest references.

Inhaltsverzeichnis

Frontmatter
1. Introduction
Abstract
The objective of calorimetry is the measurement of heat. To measure heat means to exchange heat. The exchanged heat tends to effect a temperature change in a body that can be used as a measure of the heat exchanged, or the process of heat exchange creates a heat flow which leads to local temperature differences along its path which again serve as a measure of the flowing heat.
G. W. H. Höhne, W. F. Hemminger, H.-J. Flammersheim
2. Types of Differential Scanning Calorimeters and Modes of Operation
Abstract
Two basic types of Differential Scanning Calorimeters (DSCs) must be distinguished:
  • The heat flux DSC,
  • The power compensation DSC.
G. W. H. Höhne, W. F. Hemminger, H.-J. Flammersheim
3. Theoretical Fundamentals of Differential Scanning Calorimeters
Abstract
In all DSCs, a temperature difference ...T — given as a voltage — is the original measurement signal. In almost all instruments a heat flow rate Φ m (differential heat flow rate) is internally assigned to ...T (cf. Chapt. 2). Independent of whether the user obtains ...T or Φ m from the respective DSC, knowledge of the functional relation between the measured signal (...T, Φ m) and the quantity searched for (the real heat flow rate Φ r consumed/produced by the sample) is important for
  • the time-related assignment of Φ r to ...T or Φ m (investigation into the kinetics of a reaction),
  • the determination of partial heats of reaction,
  • the evaluation and assessment of the influences of operating parameters and properties of the measuring system with regard to this relation,
  • the estimate of the overall uncertainty of measurement.
G. W. H. Höhne, W. F. Hemminger, H.-J. Flammersheim
4. Calibration of Differential Scanning Calorimeters
Abstract
“Calibration means the set of operations that establish, under specified conditions, the relationship between values of a quantity indicated by a measuring instrument or measuring system ... and the corresponding values realised by standards” (from International Vocabulary of Basic and General Terms in Metrology, 1994). “Standards” stands for Certified Reference Materials, or for otherwise calibrated measuring instruments like temperature sensors, standard resistors and the like, which are connected to international fixed quantities. Calibration needs well defined and tested procedures suitable to be done by well trained users in the laboratory.
G. W. H. Höhne, W. F. Hemminger, H.-J. Flammersheim
5. DSC Curves and Further Evaluations
Abstract
A Scanning Calorimeter measures heat flow rates in dependence of temperature or time. Modern DSCs are nowadays always connected with a data acquisition system and a powerful computer (PC). This allows one to present the measured data online on a monitor in form of a curve. Normally the heat flow rate versus the program temperature (or time) is plotted, but it is also possible to calculate other quantities from the originally measured values and draw the respective graphs on the screen as well. Modern computer techniques make it possible to do even complicated evaluations of the just measured values in the background while the measurement runs.
G. W. H. Höhne, W. F. Hemminger, H.-J. Flammersheim
6. Applications of Differential Scanning Calorimetry
Abstract
The output signal from a DSC, the heat flow rate as a function of temperature, and any derived quantity, such as the heat of transformation or reaction or any change of the heat capacity of the sample, may be used to solve many different problems. The work required to evaluate the measured curve may differ greatly from one case to another. This will become clear from the following text. Sometimes the required information can be obtained from only a qualitative evaluation of the DSC curve. But most of the examples described in this section demand precise measurements and critical, very often special, evaluation procedures of the measured curve. In every case the basis of reliable results is a careful calibration of the DSC (see Chapter 4). As a rule the separately measured zeroline (see Sect. 5.1) has to be subtracted from the measured curve before evaluation. In every case, the relationship between uncertainties in the measurements and the quantities to be determined must always be borne in mind.
G. W. H. Höhne, W. F. Hemminger, H.-J. Flammersheim
7. Evaluation of the Performance of a Differential Scanning Calorimeter
Abstract
DSC furnishes information on temperature and heat flow rates (or respectively, heat). Whether it is suited to solve the respective problem depends on the efficiency of the instrument. The characteristic data of the DSC which describe the instrument unambiguously must therefore be known. They allow a decision to be taken as to whether the DSC will be suitable for the intended use, and they also make a comparison with other DSCs possible.
G. W. H. Höhne, W. F. Hemminger, H.-J. Flammersheim
Backmatter
Metadaten
Titel
Differential Scanning Calorimetry
verfasst von
Dr. G. W. H. Höhne
Dr. W. F. Hemminger
Dr. H.-J. Flammersheim
Copyright-Jahr
2003
Verlag
Springer Berlin Heidelberg
Electronic ISBN
978-3-662-06710-9
Print ISBN
978-3-642-05593-5
DOI
https://doi.org/10.1007/978-3-662-06710-9