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A straightforward and low-cost method for the preparation of low-melting-point powder samples is presented. This simple technique, suitable for materials that are liquid at ambient temperature, involves freezing and subsequent hand-grinding of the material using a chilled stainless-steel mortar, and has enabled high-quality powder samples to be produced from compounds with melting points down to 167 K. By this method, a number of samples have been successfully prepared for detailed structural studies using high-resolution neutron powder diffraction. A recent example of the study of toluene, melting point 177 K, is given.

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