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Overview
The most common questions we get from visitors concern
sample preparation. These questions are generally in three areas: sample
mounting, polishing, and coating.
Sample
Mounting The UCLA Cameca IMS 1270 holds up to three
1" diameter samples with maximum thickness of ~1/2". Samples are typically
polished grain mounts, thick sections, or thin sections although other
samples can be accommodated. Note: only a 0.8" diameter circular area can
be analyzed (see figure). In addition, the field inhomogeneity caused by
the finite thickness of the tantalum cover plate prevents analyzing within
~0.05" of the plate, reducing the useful sample area to ~0.7" in diameter.
Diagram courtesy
of Rick Hervig, ASU SIMS Laboratory
Grain assemblages
should be mounted in epoxy resin. The resin should be of low viscosity
to reduce risk of air bubbles being trapped next to the grains, and should
be hard when cured to facilitate polishing. Thick sections are preferred
over thin sections, especially when the samples are porous and where the
mounting medium (epoxy) may interfere with the analysis (e.g. C-isotopes
in carbonates). Epoxy out-gasses a significant volume of water vapor in
the vacuum of the analysis chamber. For work where hydride interferences
are a concern (e.g. 17O measurements) the following steps should be taken
to minimize out-gassing. For grain mounts, thin the 1" epoxy disc using
a lathe or cut-off saw, to between 3/16" - 1/4" thick. Store samples in
a warm oven (50°C), a desiccator or, if possible, a vacuum oven. If
samples can be left in the instrument overnight before analysis begins,
hydride background will be further reduced.
Sample
Polishing The primary objective of polishing is to
produce a flat analysis surface. Prolonged polishing with sub-micron polishing
compound may yield a fine polish but will also tend to "round" grains in
grain mounts and excavate trenches around them, hindering analysis near
grain boundaries or the analysis of small (<50mm) grains. Diamond, alumina,
or silica polishing media may be used. Typically, a brief, final polish
with 1mm diamond yields an adequate polish without compromising flatness.
Do not use a polishing medium which will contaminate the sample with the
elements to be studied.
Sample
Coating For almost all work in the geological sciences,
samples must have an electrically conductive coating which makes contact
with the tantalum cover plate on the sample holder. Either gold or carbon
coats are used. Gold is preferred, being more conductive and more easily
sputtered than carbon. Clearly, carbon should be avoided if C-isotopes
are to be measured. The carbon coat thickness should be similar to that
used for electron probe microanalysis; gold coats should be 20-40nm.
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