When and how to use XRF for

Analysis of Soil /Ceramics/& Mud Rocks

Based on fundamental physics, which we have not yet found a way to violate:
1. One should never determine the weight percent of a non-uniform material
using XRF. You must convert it to a uniform material first.
2. Nor can one ever use XRF to report content it cannot measure like C, O and H
unless the compound it is bound to is known and part of the compound is
measurable. So the content listed in this calibration is only the weight
percent of the elements that are measured. It does not add up to 100 percent.
3. The Tracer spot size is approximately 3 by 4 mm, if your substance has a
mixture of particles smaller than 0.2 mm and they are well mixed then you
will get a reasonable result.
4. Mud rock is Mother Nature’s fine grain ceramic/soil (both in content variation
and density) and Dr. Harry Rowe at the UT Bureau of Economic Geology
selected those that cover a large range of elements found in natural soil and
ceramic materials.
5. If your material is a conglomerate then it is not uniform and the only way to
get a reasonable estimate of its average elemental content is to grind a large
quantity of it and then press it into a pellet, there is no other method that will
work.
6. How did Bruker check / correct for any matrix effect due to material
containing heterogeneous particles with size larger than mud (silt/clay)?
Actually you have to do this by grinding your material up and pressing it to
pellets. See item 5 
7. Bruker provided a calibration that is very accurate on uniform fine grain rocks,
soil and ceramics without preparation and non-uniform material ground and
pressed in to pellets.
8. Note ceramics of other material with paint, slip, and glaze or any covering like
dirt on them are VERY non-uniform!
9. Your sample also has to be infinitely thick relative to the range of the emitted
photon from each element of interest. See table 1. below. Your sample must
be thicker than the values listed for each element noted. Oxygen is listed for
reference; we do not measure it directly with a Tracer.

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 When and how to use XRF for
Analysis of Soil /Ceramics/& Mud Rocks
For analysis on uncleaned or surfaces that are known to be “covered”, ie the surface has not been aggressively
cleaned or the plating or any other material covering the bulk metal has not been removed; you would want to
do the analysis using no filter the Vacuum and 15 kV and then the yellow filter no vacuum and 40 kV.
Note as well what you see is what you measure! So if the surface is covered with patination, corrosions products,
paint, dirt or any material foreign to the original object, or the surface has been modified in any way by a
chemical process, natural or man induced etc. you are measuring that and some of the underlying bulk material
and to some extent that overlying material adds to the elements in your bulk and does masks or completely
masks the underlying material depending on the thickness.
While you will learn a great deal, be very careful as to what to attribute which elements to which layers you are
measuring( your measurement is exponentially sensitive to the layer thickness variation) and if you want to know
what the bulk material is exactly you MUST REMOVE any and all overlaying material.

You can use the Artax software on the raw photon spectra and determine the presence and relative amount of
any and all elements in the non-uniform material, note you CANNOT DO QUATITATIVE ANALYSIS OF NON
UNIFORM MATERIAL.

Note the Tracer can see coatings or residual coatings that are not apparent when using I to 3 eV photons (your
eye or microscope)

Negative numbers (photons or ppm or weight percent) are not an error! They are the result of the mathematical
process and are an indication of the level of detection and the statistical variation in the process for THAT
particular measurement. So let us say you get significant numbers of As photons in several measurements as
calculated (by the Artax software or the calibration software) that just means that when you subtracted the
interference and the back ground photons form the As k alpha peak there was statistical variation that resulted in
a negative result indicating that you have no detectable As. So in every number there is a plus and minus
uncertainly and when you get close to 0 that uncertainty will lead, mathematically, to negative numbers.
Certainly you cannot have a negative number of photons. So whenever you see a negative number you can be
certain that is essentially 0 photons or weight percent or ppm whatever your units are. Note that means when
you have a positive number equal to the negative numbers that also means those readings are also essentially 0
since any given value is always that value plus or minus the uncertainly!!!!

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 When and how to use XRF for
Analysis of Soil /Ceramics/& Mud Rocks

Element Photon Emitted energy (keV) Analysis depth in Ceramic(cm)

O 0.53 0.000001
Na 1.04 0.0007
Mg 1.2 0.00096
Al 1.47 0.0017
Si 1.74 0.0027
P 2.01 0.0013
Ca 3.69 0.0064
Cr 5.41 0.0192
Fe 6.4 0.03
Cu 8.01 0.058
Zn 8.64 0.077
Pb 10.55 0.113
Zr 15.78 0.384

Note
• This calibration is located in the instrument folder.
• It is a two-part calibration:
o GL1.cfz* is a 15kV calibration used for the major elements. Run your unknowns without a filter
and with the vacuum at 15 kV and current evident in the Calibration *.PDZ files.
o GL2.cfz* is a 40kV calibration used for trace elements. Run your unknown analysis using the
yellow filter, no vacuum, at 40 kV and current evident in the Calibration *.PDZ files.

1) To calculate the concentration of a spectrum, OPEN the S1PXRF program

2) OPEN the spectrum file.

3) SELECT Setup > Select Coef (SRZ, CFZ or PMZ file).

4) SELECT the appropriate file from the calibration folder:

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 When and how to use XRF for
Analysis of Soil /Ceramics/& Mud Rocks
a) GL1.CFZ for the majors
b) GL2.CFZ for the trace element analysis
5) CLICK the CONC button and a inset table of the weight percent will pop up.
6) If you wish to save the data in a spread sheet then CLICK On the name block under the word copy, this will
highlight the entire table. Then CLICK on copy and you can then past the entire table in and excel table.
NOTE: Use the numbers in the popup that are on the right of the box; the units are in weight percent.
7) For large data sets see “How to Perform a Chemistry Analysis of Large Data Sets.pdf”.

030.0077.01.0

www.bruker.com/hhxrf hhinfo@Bruker-Elemental.net Tel. +1 (509) 783-9850