Sample preparation and loading

XRD analysis relies on diffracting x-rays from randomly-oriented crystals.

For results that best match scans in the Powder Diffraction File, use a power form of the material that you want to analyze.

A detailed set of instructions for preparing power specimens can be found at this site.

The top surface of the power will need to be flush with the top surface of the specimen holder.

A glass slide can be used to create a flat surface.

Beware that the glass slide can introduce a preferred crystal orientation if the power particles are not equiaxed.

This will show up as unexpected intensity ratios of the peaks (some peaks may be larger or smaller than expected).

Locate the specimen stage at the center of the XRD goniometer.

Locate the brass stage lock that is directly beneath the specimen stage.

Pull stage release toward you

With release engaged, drop stage plunger to lower specimen stage.

The stage for the specimen is an aluminum disk.

The stage sits on a ball joint that will rotate without warning.

Set specimen on stage.

With stage release engaged, raise the specimen stage by pressing the plunger upward.

Ensure that the specimen top surface is contacted by the three planar positioning pins.

Disengage the stage release.

You are ready to take analyze the specimen. Go to Standard Operating procedures.