Contai n ct uform s fo
at r mion oreSample preparation
for XRF analysis ofmetallic materials

Linishing (grinding) or milling are the two mostcommonly used sample preparation methods for
X-ray analysis of metallic materials. After the sample
preparation procedure, the sample surface should
be as homogeneous as possible (clean and that
almost all imperfections have been removed). Chips
and drillings of hard metals can also be measured if
remelted to form a solid sample. For soft metals, you
can press the loose material into a stable pellet.

Remelting
You can remelt bulk or loose metal particulates to form
a solid piece. You can then directly measure such metal
samples or prepare them further according to one of
the techniques below before analyzing them. Remelting
may be combined with diluting. It is not always possible
to remelt ferroalloys as fine granules without getting
segregation. In this case diluting with metallic iron may
result in a homogeneous melt. However, there is a risk oflosing volatile elements in this process.

Linishing
The sample top layer of hard metallic samples (likesteel) is removed by using a linishing belt or disk grinder(comparable to sandpaper) to ensure that measurements
are carried out on a flat and non-oxidized surface. Be
careful to avoid cross-contamination when using thesame area of the sandpaper. It is a very fast and cheap
method. Soft alloys (Al- and Cu-based) are usually
not suited for linishing as parts of the sample may besmeared out or ripped away from the sample.

Grinding
This is very similar to linishing, but instead of sandpaper,
it is a solid abrasive (like a rotating stone or circularsander) that is used. The same restriction with regard tosoft metals apply.

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Milling and turning
Milling and turning are techniques usually based on
hard-metal tooltip(s) that cut metal away from thesample surface. In a milling machine, the fixed sample isdriven towards the usually rotating cutter head that may
involve many tool tips. In a lathe, the sample is spun anddriven towards a single-bladed cutter head. Mills andlathes will grind laboratory samples at low cost and witha high degree of reproducibility. The rapid machiningof laboratory samples is suitable for both XRF and XRD
sample preparation. Tool tips are used and for both
hard and soft grinding materials when appropriate (hardmetal).
This technique produces a clean and flat surface,eliminates cross-contamination and fine-tunes theroughness of the analytical surface.

Pressing
Chips and drilling residues from sufficiently malleable
alloys can be pressed using a hydraulic press to forma pellet. You can use either a manual or an automatedpress for this purpose.

FusionYou can prepare powdered metal alloys (e.g. FeSi, FeCr,etc.) as fused borate beads if they are properly oxidized.
This offers improved accuracy and reproducibility incomparison to lose powder or pressed pellet analysis.
Malvern Panalytical fusion instruments can be very
helpful in this situation.

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