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There are two techniques for XRD analysis to mount small amount of material depending on the volume of material available.

Preparing Mount for Small Amount of Material

Note: Sample mounting on Figure 1 is for backloading sample holder of the Aeris XRD. Similar technique should be used for frontloading sample holder of the Bruker XRD.

  1. Freeze dry the sample prior to analyses (for about 12 h). It helps to collect sample material of interest (e.g., mineral vein in hard rock samples) (Figure 1, Step 1).
  2. If enough material, grind the sample to a talc-like powder (<0.062 mm) (Figure 1, Step 2).
  3. Place a small amount of sample powder in the center of a sample holder (Figure 1, Step 3). Spread evenly and as flat as possible. Place a cardboard spacer on top of the sample (Figure 1, Step 4).

Preparing Smear Slurry/Smear Slide

Sample Slurry/Smear Slide Mounting for Small Sample Amounts

The following technique is modified from the U.S. Geological Survey Open-File Report 01-041, A Laboratory Manual for X-Ray Powder Diffraction. For a very small amount of sample material (i.e., end of a tooth pick), samples may be ground to a fine talc-like powder and smeared onto one of the quartz disk or zero background inserts. Although not useful for semi-quantitative analysis, this method is useful for rapidly determining bulk mineralogy.

  1. Freeze dry the sample prior to analyses (for about 12 h). It helps to collect sample material of interest (e.g., mineral vein in hard rock samples).
  2. Use tools to scratch the surface of interest.
  3. Place a small amount of sample powder in the center of a quartz or single crystal quartz disk. Place a small amount of sample in the center of the quartz disk. Two quartz disks will adequately fill the sample holder. The upper quartz disk will be used for the slurry.
  4. Add 2–3 drops of acetone, 70 % isopropyl alcohol or distilled water to the sample. Note: Isopropyl dries faster than water.
  5. Spread the sample to a thin layer using a glass rod. The slurry should be spread evenly across the disk. If there is not enough material to cover the entire disk, concentrate the sample in the middle of the disk where the X-rays will contact the sample. You can also use a piece of tape, stick it to the sample holder and sprinkle the ground sample onto it.
  6. Place the sample in the dessicator to dry before running in the XRD.

Figure showing preparation steps

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