ICTAC Kinetics Committee recommendations for collecting experimental thermal analysis data for kinetic computations

This paper reviews the best-known differential scanning calorimetries (DSCs), such as conventional DSC, microelectromechanical systems-DSC, infrared-heated DSC, modulated-temperature DSC, gas flow-modulated DSC, parallel-nano DSC, pressure perturbation calorimetry, self-reference DSC, and high-performance DSC. Also, we describe here the most extensive applications of DSC in biology and nanoscience.

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Differential Scanning Calorimetry Techniques: Applications in Biology and Nanoscience

Differential scanning calorimetry (DSC) is a powerful tool to address some of the most challenging issues in glass science and technology, such as the nonequilibrium nature of the glassy state and ...

Understanding Glass through Differential Scanning Calorimetry

A compendium of phase change enthalpies published in 2010 is updated to include the period 1880–2015. Phase change enthalpies including fusion, vaporization, and sublimation enthalpies are included for organic, organometallic, and a few inorganic compounds. Part 1 of this compendium includes organic compounds from C1 to C10. Part 2 of this compendium, to be published separately, will include organic and organometallic compounds from C11 to C192. Sufficient data are presently available to permit thermodynamic cycles to be constructed as an independent means of evaluating the reliability of the data. Temperature adjustments of phase change enthalpies from the temperature of measurement to the standard reference temperature, T = 298.15 K, and a protocol for doing so are briefly discussed.

Phase Transition Enthalpy Measurements of Organic and Organometallic Compounds. Sublimation, Vaporization and Fusion Enthalpies From 1880 to 2015. Part 1. C1-C10

Ice nucleation was investigated experimentally in water droplets with diameters between 53 and 96 micrometres. The droplets were produced in a microfluidic device in which a flow of methyl-cyclohexane and water was combined at the T-junction of micro-channels yielding inverse (water-in-oil) emulsions consisting of water droplets with small standard deviations. In cryo-microscopic experiments we confirmed that upon cooling of such emulsion samples ice nucleation in individual droplets occurred independently of each other as required for the investigation of a stochastic process. The emulsion samples were then subjected to cooling at 1 Kelvin per minute in a differential scanning calorimeter with high temperature accuracy. From the latent heat released by freezing water droplets we inferred the volume-dependent homogeneous ice nucleation rate coefficient of water at temperatures between 236.5 and 237.9 Kelvin. A comparison of our newly derived values to existing rate coefficients from other studies suggests that the volume-dependent ice nucleation rate in supercooled water is slightly lower than previously thought. Moreover, a comprehensive error analysis suggests that absolute temperature accuracy is the single most important experimental parameter determining the uncertainty of the derived ice nucleation rates in our experiments, and presumably also in many previous experiments. Our analysis, thus, also provides a route for improving the accuracy of future ice nucleation rate measurements.

The homogeneous ice nucleation rate of water droplets produced in a microfluidic device and the role of temperature uncertainty

DSC studies on organic melting point temperature standards

Studies on the ageing of a magnesium-potassium nitrate pyrotechnic composition using isothermal heat flow calorimetry and thermal analysis techniques

The pyrotechnic and thermal properties of a range of binary magnesium-strontium nitrate compositions containing from 10% to 90% by mass of magnesium have been determined. The burning rate and light output were measured after consolidating the compositions into cardboard tubes. The exothermicity, temperature of ignition and time to ignition of the compositions were also determined and the products of combustion were characterized

Pyrotechnic and Thermal Studies on the Magnesium-Strontium Nitrate Pyrotechnic System

This paper describes the concepts of resolution in the time and temperature domains and illustrates the principles using two new sample controlled thermal analysis (SCTA) techniques. The use of SCTA, where the sample temperature is determined by the rate of reaction, offers a number of advantages over conventional (linear heating) thermal analysis methods. The operation, advantages, and disadvantages of the two new techniques are discussed with examples.

New Concepts in Sample Controlled Thermal Analysis: Resolution in the Time and Temperature Domains

This article describes the design and operation of a new thermal analysis instrument which uses microwaves to simultaneously heat and detect thermally induced transformations in samples with masses in the range of 50 mg to 0.5 g. The data acquisition and control software developed for the instrument support a range of experimental techniques including constant power, linearly ramped power, linearly ramped temperature, and various modulated methods. Microwave thermal analysis utilizes the fact that physical or chemical alterations in a material, caused by processes such as melting, decomposition, or solid-solid phase changes, cause variations in its dielectric properties. These can be revealed by a variety of means including changes in the sample temperature, the differential temperature, or the shape of the power profile during linear heating experiments. The scope of the instrument is demonstrated with the decomposition of basic copper carbonate. The large temperature increase (∼100 °C) observed on the formation of the strongly coupling oxide indicates the potential sensitivity of using the thermal effects of dielectric changes as a means of detection. Further fine detail can be revealed by the use of derivative plots of either the applied power or the temperature.

Edward L. Charsley

Papers

DSC studies on organic melting point temperature standards

Studies on the ageing of a magnesium-potassium nitrate pyrotechnic composition using isothermal heat flow calorimetry and thermal analysis techniques

Pyrotechnic and Thermal Studies on the Magnesium-Strontium Nitrate Pyrotechnic System

New Concepts in Sample Controlled Thermal Analysis: Resolution in the Time and Temperature Domains

Development of a new instrument for performing microwave thermal analysis