XRD is used for the elemental detection and purity
of the test sample. Specific protocol should be followed to prepare sample for
XRD analysis which includes a few steps prior to be subjected under x-ray
diffraction machine. Minimum requirement of sample to be analyzed through XRD technique
is one gram. The sample should be purified prior to analysis.
Complete procedure to prepare XRD sample is being
discussed in detail in this article. Solid crystalline sample is first manually
grinded thoroughly to obtain smooth and fine sample in the form of powder. Afterwards,
an organic solvent, mostly ethanol is added in small amount and grinned again. The
purpose of addition of ethanol during grinding procedure is to lower the surface
energy of test sample that can otherwise disrupts not only the formation but
also specific position of peaks in XRD pattern. Another edge of using solvent
during grinding is that it significantly reduces the mesh size of the
particles. The mesh size of particles of a test sample should be lower than 10
micrometer. Grinding is then followed by taking the sample is a sample holder. The
sample is spread on a glass slide and packed inside sample container or it can
also be distributed on a sticky tape by spraying it on the tape. A small amount
of reference standard is usually added in the analyzing product which can assist
in elemental identification process. At this stage sample is ready for
analysis.
Related
questions
What
is procedure of sample preparation for XRD analysis?
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