Preparing Powder X-ray Diffraction Samples


Wear eye protection

Chemical gloves recommended

Prepare a microscope slide with an aluminum holder.  Take a piece of tape and wrap it TIGHTLY around the slide so that the sticky side is facing out. If the tape is loose the final height of the sample will be off and so will be the measured diffraction angles. Place the aluminum holder on top of the slide with the tape centered in the hole. The longer end of the aluminum must match the end of the slide. Not using double sticky tape means you can slide the tape if necessary.

Since the instrument is a powder x-ray diffractometer your sample should be a powder.  Grind the sample using a rotary motion with a mortar and pestle.  The finer the powder the better the data.

Pour the powder on to the holder. Use another microscope slide to wipe off the excess. Best results are obtained if the sample is level and as deep as the holder. If the height is off, then so will be the measured diffraction angles.

Make sure the plastic tray is under the sample. This container is meant to catch any powder which could otherwise fall to the x-ray source and damage the machine. Hold both the slide and the aluminum holder. Insert the pair together into the clip holder.

Measuring particle size

Rigaku Miniflex Instrument Operating Directions

This page created by George Lisensky, Beloit College. Last modified August 29, 2022 .