International
Tables for
Crystallography
Volume C
Mathematical, physical and chemical tables
Edited by E. Prince

International Tables for Crystallography (2006). Vol. C, ch. 3.2, p. 156

Section 3.2.1.1. General precautions

P. F. Lindleyb

3.2.1.1. General precautions

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Meticulous temperature control is essential for the highest precision. The allowable temperature fluctuation will depend on the thermal coefficient of expansion of the material and on the required accuracy of the measurement. The utmost care must be taken to avoid air bubbles and inclusions. In those techniques that require immersion of the solid in a liquid, it is assumed that no chemical or physical interaction occurs between the liquid and the solid, and that the volume of the liquid displaced represents the true volume of the solid. For most hard crystalline materials, liquids can easily be found for which these assumptions are valid. However, for amorphous powders, porous structures such as zeolites, crystalline proteins, and natural and synthetic fibres, the measured `density' may depend markedly on the particular liquid chosen and on the details of the method applied. In these cases, penetration or swelling of the solid will depend on a variety of factors such as interfacial tension, the relation of pore size to molecular dimensions, adsorption, and electrostrictive forces. The structural unit to which the measured density applies may be very difficult to specify. Even with materials not subject to these difficulties, variability in the measured density is frequently found. Such variations may arise from differences in trace impurities or in the previous history of the sample (Johnston & Adams, 1912[link]).

References

Johnston, J. & Adams, L. H. (1912). On the density of solid substances, with especial reference to permanent changes produced by high pressures. J. Am. Chem. Soc. 34, 563–584.








































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