Validation of Sample Surface Temperatures Using Solid - Solid Phase Transition and Melting Point
In-situ studies of phase transition and melting point to evaluate the extent of deviation between actual sample surface temperatures and the measured value of non-ambient XRD devices.
Several parameters lead to a deviation of temperatures measured inside a heater of a non-ambient X-ray diffraction attachment and those which can actually be reached on the sample surface. The most important ones are the heating mechanism itself (heater with the heat source directly underneath the sample or environmental heater with heating source which surrounds the sample), the atmosphere within the sample compartment, the sample itself (thermal properties, thickness, emission coefficient) as well as the contact between the heater and sample.
Hence a certain amount of deviation is normal and can´t be avoided. With a change of experimental conditions a validation of the sample surface temperature is recommended due to different heat transfer properties.
A simple method of temperature validation is done by observing solid – solid phase transitions and solid – liquid transitions (melting points) of well-known reference samples. A number of compilations with applicable substances and their transition temperatures exist.
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