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- Add 25 ml of 1% Borax solution to the clay plug
- Dismembrated sample (machine is auto set on time), to remove the >2 um clay fraction
- Centrifuge for 4 mins at 750 rpm, decant the suspended liquid into a separate centrifuge tube (you should end up with a ~full centrifuge tube of suspended clay)
- Repeat steps 1-3 on the remaining >2 um fraction
- Centrifuge the <2 um fraction for 15 mins at 1500 rpm to remove the Borax solution
- Decanted and add 25 ml of nanno pure water
- Centrifuged for 60 mins at 3000 rpm, the liquid decanted before loading onto a zero background silica disk.
Preparing the Mount
Clay mounts are put onto a zero-background silicon disk that fits into a 2 mm steel sample holder (Figure 21). Only put the disks into sample holders that have a hole drilled in the bottom. The hole allows the disks to be taken out, otherwise they are stuck inside the holder. The disk should sit flush with the sample holder.. Some of the disks are at different depths, so a quartz insert disk can also be put in the bottom of a sample holder with the silicon disk on top.
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- When the muffle furnace has finished its program and is cooling down, wait until the temperature reaches between 100° and 200°C before removing the sample. The sample can be placed in the desiccator until it reaches room temperature. Once it has completely cooled down it can be run in the D4.
Clay Separation Method for removal of Chlorite
For the double peaks of Kaolinite and Chlorite, heating the sample only suggest that one of the minerals is present, it will not give final and complete results for a sample that contains both Kaolinite and Chlorite. In order to determine which mineral is present, an additional treatment is necessary.
- Take the <2um clay fraction, this should be rinsed and free of any treatments, in centrifuge tube add ~20ml of 1N HCl
- Vortex the sample to completely dislodge all material before pouring sample into a 100ml beaker, add stir bar once sample is in place
- Set hotplate to 300C (boiling point of HCl is ~101, but in order to maintain a continuous boil the hotplate needs to be much hotter)
- Set the stir RPM below 100, this is only to keep the material suspended within the HCl
- Start time once the samples have come to a complete boil, leave for 2 hours - add more HCl as necessary (DO NOT, let the sample go dry and burn)
- Once the sample has boiled for 2 hours, centrifuge down for 15 mins at 1500 rpm, decant acid and rinse with 25 ml nannopure (3X)
- After samples has been washed 3X and is free of HCl, centrifuge for 60 mins at 30 rpm
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