This post is for those who might be new to sample preparation using a top-loading zero background sample holder (with a well for sample material), or for those who are looking to benchmark sample preparation practices.
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This project started with a phone call several months ago from a Canadian government lab. They had a very specific application so the design was driven much more by their requirements than most zero-background holder designs. A 1mm deep well with a zero-background plate at the bottom was a key specification. We tried several options for creating this, but settled on a two-part design with a solid “floor” plate and a ring above it. As it turns out, cutting a ring out of monocrystalline Si was more challenging than I’d expected.
It took a few months of experimenting with various fixtures to settle on a design that had a low failure rate and excellent cut quality, but with that done, the sample holders came out beautifully. Making these with a traditional, solid, plate would certainly be much easier, but this kind of project is always an opportunity to try something new.
KS Analytical Systems now offers custom sample holders for Rigaku Miniflex systems. The 6-position autosamplers and rotation stages (and even some fixed stages) make use of the magnetic disk design for holding powder without taking up much extra room in the diminutive benchtop.