1.

Grind the sample to a talc-like powder (<0.062 mm).

2.

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.

3.

Add 2–3 drops of acetone, isopropyl alcohol, or distilled water to the sample.
Note: Acetone and Isopropyl dry faster than water.

4.

Create a thin layer of sample material using a glass rod (rolling it over the sample works well).

5.

Place sample in desiccator to dry.

1.

Place undried sample on a glass slide or quartz disk.

2.

Using a pastuer pipette, slowly drop 2 M HCl on the sample until bubbling/fizzing stops.

3.

Desiccate and transfer sample to sample holder for analysis.

1.

Place ~2 cm3 of undried sample into a centrifuge tube with 25 mL of acetic acid (10% solution).

2.

Mix well, and let sit until the reaction ceases.

3.

Shake well again to ensure the reaction has stopped (i.e., no more bubbles).

4.

Spin sample in the centrifuge (15 min at 1500 rpm)

5.

Decant the acetic acid solution and dispose of the acid solution properly.

6.

Add 25 mL of DI to the centrifuge tube and centrifuge again for 15 min at 1500 rpm.

7.

Decant the clear water.

8.

Repeat the "wash cycle" (Steps 5 and 6) with DI.

9.

Place washed sample in a large beaker with some distilled water and a little 1% Calgon.

10.

Suspend the clay material by placing the beaker in a sonic dismembrator for ~1 min.
Note: Do not let the sample heat up.

11.

Transfer the sample to a clean centrifuge tube and spin for 5 min at 1000 rpm to remove the >2 µm size fraction from suspension

12.

Remove the <2 µm size fraction by collecting the top 1 cm of solution with an eye dropper.
Note: If it is necessary to re-suspend flocculated clay particles using the dismembrator add more Calgon solution. 15 min at 1500 rpm in the centrifuge may not settle the <2 µm particle size. Increase the speed to as much as 5000 rpm to remove the clay from the Calgon solution.

13.

Make an oriented clay mount by placing 2–3 drops (enough to cover the quartz disk) of clay suspension onto a glass slide and let dry in a desiccator.

1.

In centrifuge tube, mix a small amount of bulk sample (~5 mL) (fresh, not dried) with 1% Calgon solution. Use an ultrasonic bath or dismembrator, if necessary.

2.

Centrifuge the Calgon solution/sample mix at 1000 rpm for 5 min to remove the >2 µm particle-size fraction.

3.

Decant the Calgon solution (containing suspended clays) into a new centrifuge tube, and spin it at 1500 rpm for 15 min to remove the remaining <2 µm clay-size fraction.

4.

Decant the Calgon solution and wash the clay residue with distilled water.

5.

Spin-down again at 1500 rpm for 15 min.

Note:Repeat steps 4 and 5 as necessary to remove the Calgon.

6.

Make an oriented clay mount by placing 2–3 drops (or enough to cover the quartz disk) of solution onto the quartz disk and let dry in the desiccator.

1.

Find the "Glycolator" container stored in the ICP prep sink cupboard.

2.

Pour ethylene glycol to a depth of ~1 cm in the bottom of the container.

3.

Place the samples onto the shelf

4.

Place glycolator (with samples) in oven at 60°–70° overnight.

5.

Keep samples in glycolator until ready to analyze.

1.

Using a glass rod or eye dropper, apply a drop of ethylene glycol directly to the surface of the sample mount.

2.

Samples are ready to be analyzed as soon as the glycol is uniformly absorbed.
Note: Excess ethylene glycol may be gently mopped up with a lab tissue.

1.

Open XRD Commander > Jobs tab > Create jobs.

2.

Under Positions, enter the position of the sample (A1–A6 up to K1–K6).

3.

Use the Text ID. Use the barcode scanner to enter the Sample ID.

4.

Select the appropriate instrument.dql file under Parameter. If needed, use the XRD Wizard to set up a new parameter file (2θ span between 2.5°2θ and 80°2θ).
Note: Several .dql files are already created under C:\Documents and Settings\daq\Desktop\XRD Expedition Files\.

5.

Specify the path to save the raw results file, for example C:\data\xrd\in. Use the sample's Text ID as the file name.

6.

Select the appropriate instrument settings:

–Script: measure.vbs, located in the DIFFPLUS folder (should open automatically)

–Mode: QL(qualitative)

–Time Scale: 1.0

7.

Check that the samples are loaded correctly and nothing is blocking the sample handler.

8.

Click Start.

1.

Double-click on the .raw file, which automatically opens the file in the DIFFRAC.EVA software.

2.

Go to File > Print.

3.

Export as a .PNG file.

4.

In the save window, name the file with the Text_ID and Save.