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After the grinding jars are secured in the clamps, the pin is in the closed position and the clear cover is closed it is time to select grinding settings (Figure 19). Program 1 (A) is currently set for 12 min at 25 1/s. This setting is good for clay rich material. Softer sediments such as CaCO3 typically need less time. It is important to only grind soft sediments in the agate jars and hard material should be ground in the shatter box. After Grinding cycle has completed turn knob counter clockwise and pull pin up and into its open position (Figure 19A). Unscrew clamp and open jar to verify grind size. If sediment is still too coarse regrind.
Figure 18. A) Preset programs. B) The shaker frequency C) The time grinder is set for D) The start and stop.
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There are three ways to load a sample holder: front load, side load, and backload. Front and side loading methods uses the same sample holders and back-loading uses unique holders. Front Loading is the most common method. Back and side-loading are ideal for reducing preferred orientation and should be used over frontloading if preparing samples for semi quantitative analysis.
Collect Enough Material to Fill a Sample HolderMake sure the sample from the sampling table is enough material to fill a sample holder - sample size for bulk powder is generally a 1-2 cm QRND (Quarter Round) from the section half. This will produce more than enough material to fill a sample holder. You do not want more than this as it will be wasted.
Front-Load Samples
- Unless the sample material is very small, select the appropriate sample holder (see Sample Slurry/Smear Slide Mounting for Small Sample Amounts).
- Label the sample holder with a unique identifier to keep the samples organized (e.g., text ID or 14H2 77-78)
- Place enough powder from the labeled sample bottle to fill an empty sample holder. Gently press the powder flush with the sample holder using a glass slide. Roll the glass slide over the powder to fill any gaps in material and smooth the surface of the powder. The surface of the powder must be smooth. Remove excess powder from the sample holder edges and carefully place the holder in the D4 sample magazine.
The sample material needs to be flush with the sample holder. The beam is set to focus on the height of the sample holder. If the sample is above or below that focal point, the geometry of the beams do not converge properly, the peak resolution decreases, and the peaks are shifted.
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Side-loading samples is a preparation method to reduce mineral orientation. This method may be desirable for quantitative XRD.
- Take a 2mm or 1.8mm sample holder and hold it on its side.
- Tape a piece of cover glass across the well leaving a very small gap at the top
- Keep the holder on its side and pour powder into the open gap.
- Tap the holder while filling in power to evenly distribute it
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Back-loading samples is a preparation method to reduce mineral orientation. This method may be desirable for quantitative XRD.
There are 10 back-loading holders. The holder has an empty ring and backing piece that snaps in from behind (Figure 1619). There are also two loading pieces. One piece helps funnel the powder in and the other taps down the powder into a flat surface.
Figure 1619. Back-loading sample holder pieces. A. Sample Ring B. Back piece C. Funneling piece D. Tapper
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- Take a front-loading holder and put a clean glass slide over it.
- Take the ring, flip it upside down and put it on the slide (Figure 1720). Now the powder will fall on a smooth flat surface that will be easy to flip over.
Figure 1720. Ring upside down on glass. Funnel piece next to unit.
3. Take the funneling piece and put It inside the ring (Figure 1821).
Figure 1821. Funnel inside ring.
4. Load powder into the ring. Try to load the powder evenly across the well.
5. Take the tapping piece and lightly tap down the powder. The idea behind this method is not applying pressure to the measuring face will reduce mineral orientation. Do not tap the powder to too firmly or you may unnecessarily orient the minerals.
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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 semiquantitative semi-quantitative analysis, this method is useful for rapidly determining bulk mineralogy.
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There are various methods for separating clay from coarser material involving a series of centrifuging or gravity settling. Those listed below are methods used on-board.
If you removed carbonates first, start here after your water washes are finished and the water has been decanted. If you did not remove carbonates, take approximately 5 mL of sample material and put into a centrifuge tube.
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The dismembrator setup is shown in Figure 1922. The power source is connected to the probe. The probe fits into the case through a hole in the top. Put the probe into the top clamp and the sample tube into the bottom clamp. Adjust the positions so the probe goes into the tube. The probe should be about half-way into the sample material without touching the sides of the tube. The probe releases a lot of energy, and if it is touches the sides it will heat up the tube and the sample. 
Figure 19 (above)22: The dismembrator set up. Included is the soundproof box and the Probe with power source.
Figure 2023: Dismembrator power source control Panel. (A) On/Off switch (B) Start button (C) Set button (D) Mode button
The probe power source is shown in Figure 2023. Flip the "ON" Switch (Figure 20A23A). The settings are already set to our needs. To run as is, press the "Start" button (Figure 20B23B). If you need to change a setting, see the "Set" button (Figure 20C23C) and the "Mode" button (Figure 20D23D). From these two panels, you have access to the power, time, and displayed units. For more information, reference the Manufacturer Manual located in the side pocket of the dismembrator case.
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