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TS XRF Lab eBook 2015May04

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10 views

TS XRF Lab eBook 2015May04

Uploaded by

ThePandiux
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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kooBe siht erahS

XRF Technology in the Lab

XRF Technology for


Non-scientists
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Table of Contents

1 2 3
What is XRF? XRF Analyzers in the XRF Analyzers in the
Lab: Technology Lab: Applications
Overview...................................................... 3 Overview...................................................... 14 Metals and Alloys Manufacturing................... 29
How XRF Works............................................ 4 Lab-based XRF Systems................................15 Geology, Mining and Minerals........................ 30
The X-ray Fluorescence Process....................6 EDXRF...........................................................16 Cement Manufacturing..................................31
The Periodic Table.........................................7 WDXRF......................................................... 19 Petroleum Industry........................................ 32
List of Periodic Table Elements.......................8 EDXRF vs WDXRF.......................................... 24 Precious Metals and Gemstones....................33
Interpretation of XRF Spectra......................... 9 General Use Guidelines..................................25 Polymers and Plastics................................... 34
Examples of an XRF Spectra..........................10 Sample Preparation.......................................26 Glass and Ceramics, Refractories...................35
Rayleigh/Compton Scatter Peaks................... 11 Analysis........................................................27 Semiconductor, Thin Films, Coatings.............. 36
Limitations................................................... 12 Environment, RoHS and WEEE screening........37
Calibration....................................................13 Paints and Chemicals....................................38
Forensics......................................................39
Food............................................................ 39

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Overview
X-Ray Fluorescence (XRF)
XRF occurs when a fluorescent (or secondary) x-ray is emitted from a sample that is
being excited by a primary x-ray source. Because this fluorescence is unique to the
elemental composition of the sample, XRF is an excellent technology for qualitative

1 and quantitative analysis of the material composition. XRF spectrometry has a broad
range of applications in industry, which we will discuss later in this ebook.

What is XRF?
X-rays
X-rays are simply light waves that
we can’t see. Other light waves that Properties of X-Rays
X-ray fluorescence (XRF):
a non-destructive analytical
X-rays Are:
we can’t see include ultraviolet (UV)
technique used to determine the • Propagated in straight lines at speed of light
chemical composition of materials. light (which gives you a sun tan), • Absorbed while passing through matter,
infrared light (which warms you up), depending on composition and density
of the substance
and radio waves. X-rays have a very • Emitted with energies characteristic of
short wavelength, which the elements present

corresponds to a very high energy. They:


• Affect the electrical properties of
liquids and solids
• Cause biological reactions such as cell
damage or genetic mutation
• Darken photographic plates
• Ionize gases

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How XRF Works


Fingerprints
Each of the elements present in a sample produces a unique set of
characteristic x-rays that is a “fingerprint” for that specific element.

It All Starts With the Atom


Atoms are the extremely small particles of which we, and everything around us, are made. There
are 92 naturally occurring elements and scientists have made more, bringing the total to 114
confirmed and at least 4 more claimed. Atoms are the smallest unit of an element that
chemically behaves the same way the element does.

Atoms bond
with other atoms to
form a molecule. If two
hydrogen atoms bonded with
an oxygen atom, they
would form a WATER
molecule.

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How XRF Works NOT a c


is is i
Anatomy of the Atom*
T h rcl
In the center of the atom is the nucleus, made up of protons and neutrons. e
Each proton carries a positive electrical charge, but neutrons carry no electrical

!
charge, so the nucleus of an atom is positively charged because of its protons.

Electrons are particles that orbit the nucleus at a high speed and carry a negative
charge, which balances the positive electrical charge of the protons in the nucleus.
Since the total negative charge of electrons is equal to the positive charge of the
nucleus, an atom is neutral.

The negative electrons are attracted to the positive protons, so the electrons stay K
around the nucleus in discrete shells.
L
When two chemicals react with each other, the reaction takes place between
individual atoms at the atomic level. The outermost or covalent electrons are
The electrons
reside in discrete
M
quanta or shells, and
involved in this bonding. these shells are labeled
K, L, M, N, from
N
inner to outer.
The processes that cause materials to be radioactive occur at the atomic Atoms are not really combined of
concentric circles of electrons...
level, generally within the nucleus.
we just draw them that way to
understand how the electrons
orbit around the nucleus.

thermoscientific.com/XRF *this section site reference: http://www.epa.gov/radiation/understand/atom.html 5


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The X-Ray Fluorescence Process


A solid or a liquid sample is irradiated

1 with high energy x-rays from a controlled


x-ray tube.

When an atom in the sample is struck

2 with an x-ray of sufficient energy (greater


than the atom’s K or L shell binding energy),
an electron from one of the atom’s inner
orbital shells is dislodged.

The atom regains stability, filling the

3 vacancy left in the inner orbital shell with


an electron from one of the atom’s higher
energy orbital shells.

The electron drops to the lower energy

4 state by releasing a fluorescent x-ray.


The energy of this x-ray is equal to
the specific difference in energy between
two quantum states of the electron. The
measurement of this energy is the basis of
XRF analysis.

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The Periodic Table


What is an Element?
Number An element is a chemically pure substance composed of atoms.
of protons = 1 2
Atomic Number Elements are the fundamental materials of which all matter is composed.
(different for each H He
element). 3 4 5 6 7 8 9 10
Number The elements are arranged in increasing order of their atomic
of electrons Li Be B C N O F Ne
typically = number weight (the number of protons in the nucleus of an atom).
11 12 13 14 15 16 17 18
of protons (so
that the atom is Na Mg Al Si P S Cl Ar
neutral). 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34
Number 35 36
of neutrons K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
is variable and is what
allows some atoms to 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54
have isotopes. Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
55 56 57 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86
Cs Ba *La Hf Ta W Re Os Ir Pt Au Hg TI Pb Bi Po At Rn
87 88 89
Electrons in shells
closest to the nucleus are Fr Ra +Ac 58 59 60 61 62 63 64 65 66 67 68 69 70 71
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
most strongly bound to the atom.
90 91 92 93 94 95 96 97 98 99 100 101 102 103
Binding energy increases with
atomic number. The higher
Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
the number, the higher
Standard elements for Not measurable by XRF Unstable elements Ultra-light elements requiring Element requiring Primary Rare gases
the weight. both EDX and WDXRF specific crystals and WD-XRF beam filter to be analyzed with
Rh anode tube

An isotope of an element has the


same number of protons but a
different number of neutrons. Did you know?
The Periodic Table was created in 1869 by Dmitry I. Mendeleev.

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List of Periodic Table Elements


1 Hydrogen H 21 Scandium Sc 41 Niobium Nb 61 Promethium Pm 81 Thallium Tl 101 Mendelevium Md
2 Helium He 22 Titanium Ti 42 Molybdenum Mo 62 Samarium Sm 82 Lead Pb 102 Nobelium No
3 Lithium Li 23 Vanadium V 43 Technetium Tc 63 Europium Eu 83 Bismuth Bi 103 Lawrencium Lr
4 Beryllium Be 24 Chromium Cr 44 Ruthenium Ru 64 Gadolinium Gd 84 Polonium Po 104 Rutherfordium Rf

5 Boron B 25 Manganese Mn 45 Rhodium Rh 65 Terbium Tb 85 Astatine At 105 Dubnium Db

6 Carbon C 26 Iron Fe 46 Palladium Pd 66 Dysprosium Dy 86 Radon Rn 106 Seaborgium Sg

7 Nitrogen N 27 Cobalt Co 47 Silver Ag 67 Holmium Ho 87 Francium Fr 107 Bohrium Bh

8 Oxygen O 28 Nickel Ni 48 Cadmium Cd 68 Erbium Er 88 Radium Ra  108 Hassium Hs

9 Fluorine F 29 Copper Cu 49 Indium In 69 Thulium Tm 89 Actinium Ac 109 Meitnerium Mt
10 Neon Ne 30 Zinc Zn 50 Tin Sn 70 Ytterbium Yb 90 Thorium Th 110 Darmstadtium Ds
11 Sodium Na 31 Gallium Ga 51 Antimony Sb 71 Lutetium Lu 91 Protactinium Pa 111 Roentgenium Rg
12 Magnesium Mg 32 Germanium Ge 52 Tellurium Te 72 Hafnium Hf 92 Uranium U 112 Copernicium Cn
13 Aluminum Al 33 Arsenic As 53 Iodine I 73 Tantalum Ta 93 Neptunium Np 113 Ununtrium 113
14 Silicon Si 34 Selenium Se 54 Xenon Xe 74 Tungsten W 94 Plutonium Pu 114 Flerovium Fl
15 Phosphorus P 35 Bromine Br 55 Cesium Cs 75 Rhenium Re 95 Americium Am 115 Ununpentium 115
16 Sulfur S 36 Krypton Kr 56 Barium Ba 76 Osmium Os 96 Curium Cm 116 Livermorium Lv
17 Chlorine Cl 37 Rubidium Rb 57 Lanthanum La 77 Iridium Ir 97 Berkelium Bk
18 Argon Ar 38 Strontium Sr 58 Cerium Ce 78 Platinum Pt 98 Californium Cf
19 Potassium K 39 Yttrium Y 59 Praseodymium Pr 79 Gold Au 99 Einsteinium Es
20 Calcium Ca 40 Zirconium Zr 60 Neodymium Nd 80 Mercury Hg 100 Fermium Fm

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Interpretation of XRF Spectra


Spectral Peaks
As we learned in the previous pages, each of the elements
present in a sample produces a set of characteristic
fluorescent x-rays that is unique for that specific element,
which is why XRF spectroscopy is especially useful for Primary
elemental analysis. This elemental “fingerprint” is best
Pt
X-ray Radiation Au
illustrated by examining the x-ray energy spectrum and its
“scattering peaks.” Au
Pt Au
Pt
Most atoms have several electron orbitals (K shell, L shell,
M shell, for example). When x-ray energy causes electrons
to transfer in and out of these shell levels, XRF peaks with
varying intensities are created and will be present in the
spectrum. The peak energy identifies the element, and the
peak height / intensity is indicative of its
concentration.

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Examples of an XRF Spectra


Energy Dispersive XRF (EDXRF)

Wavelength Dispersive XRF (WDXRF)

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Rayleigh/Compton Scatter Peaks


Overview hv Compton Scattering
Scattering occurs when incoming x-rays do not In Compton scattering, the x-ray strikes an electron of the
produce fluorescence, but rather “collide” with sample. Since some energy is transferred to the electron in
the atoms of the sample which results in a hv the collision, the x-ray leaves the collision with less energy.
change in the direction of motion of a particle. That’s why we see the Compton peak at an energy lower
than the source excitation energy.
Rayleigh Scattering
e1
In Rayleigh scattering, electromagnetic radiation is dispersed
hv1
by particles having a radius less than approximately 1/10 the e

wavelength of the radiation.


hv

During the Rayleigh scattering process, photons are scattered by tightly bound electrons in which
the atom is neither ionized nor excited. The incident photons are scattered with (essentially) an
unchanged energy. Rayleigh scattering occurs mostly at low energies and for high atomic weight.

Rayleigh scattering can be compared


to the cue ball (the incoming x-ray) bouncing
off the side of the table without loss of energy.
Did you know?
Rayleigh scattering is named after the British physicist
Lord Rayleigh, who discovered the process.

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Limitations
Overview Spectral Effects
Light element analysis with XRF can be Some elements have lines that overlap other elements. Fortunately the software will strip out and correct most
challenging depending on what type of system of these overlaps (as long as the interfering element is in the model being used), but limits of detection may be
you’re using because the fluorescent x-rays worse when two overlapping elements are present. WDXRF produces fewer spectral overlaps because of its
from lighter elements (Z<18) are less energetic higher resolution.
and are greatly attenuated as the x-rays pass
through air. Wavelength Dispersive XRF (WDXRF)
Matrix Effects
instruments tend to be more successful with The matrix is any other element present in or on the sample other than the one element being considered.

light element analysis than Energy Dispersive Enhancement and absorption effects are typically taken care of in the software if you are using a fundamental

XRF (EDXRF) instruments. The differences parameters based calibration with all the necessary elements present.

between WDXRF and EDXRF will be explained Enhancement Effects


further in chapter 2. Some fluorescent x-rays have more energy than the binding energy of other elements present in
the sample, and so their energy will excite those other elements. These elements will give a
greater signal return to the detector, i.e. “enhancing” the reading.

Absorption Effects
The fluorescent x-ray does not reach the detector as it is scattered or absorbed by other elements
present in the sample, so the signal is weaker.

Sample Effects
The surface of the material being analyzed is not representative of the entire sample (particle size,
inhomogeneity, surface contamination, etc.). XRF is a surface analysis technique, so inhomogeneity
or contamination will skew the results.
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Calibration
Common calibration routines include the following:

Empirical Calibration Fundamental Parameters


In empirical calibration, the user must first analyze known samples to For measuring samples of unknown chemical composition in which
obtain the count intensity, which is then plotted using off-line software concentrations of light and heavy elements may vary from parts per
to generate the calibration curve. This curve data is then put back onto million (ppm) to high percent levels, Fundamental Parameters (FP)
the analyzer which can then be run to give immediate results. Empirical analysis is used to simultaneously compensate for a wide variety of
testing modes are only suited for measuring samples for which chemical geometric effects (including small and odd-shaped samples), plus x-ray
compositions will fall within the narrow calibration range, and absorption and enhancement effects as well as spectral overlaps. FP is
interferences (spectral and matrix) must be taken into consideration the preferred analysis tool when no reference samples are available.
within the calibration. This method is the most accurate and widely used
in process control where similar, well known reference samples are
available.

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Overview
2
Lab-based XRF analysis can be used in tandem with handheld XRF analysis to provide
confirmatory data, but its analytical range and applications are wider.

XRF Analyzers
Handheld XRF analyzers are designed to provide instant elemental analysis in
situations where immediate feedback is needed to determine the next course of

in the Lab:
action.

Laboratory-based XRF systems provide qualitative and quantitative analysis for

Technology process and quality control. WDXRF is the standard test method for analytical
laboratories serving applications as diverse as cement manufacturing, metallurgy,
mining, geology and geochemistry, petroleum, polymers, glass and ceramics,
Energy Dispersive XRF = EDXRF
Wavelength Dispersive XRF = WDXRF semiconductors, paints and chemicals, forensics investigations, and environmental
applications.

Lab-based XRF can evaluate all kinds of materials and sample types including
conductive or non-conductive solids, liquids, loose powders, pressed pellets, fusion
beads, pastes, granules and coatings.

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Lab-based XRF Systems


Overview
The two primary types of lab-based XRF systems are EDXRF and
WDXRF. Each has a different detection system.
WDXRF
WDXRF technology is well established
for high sensitivity down to low atomic
number elements, high repeatability and
element selectivity in order to achieve the
performance needed for routine industrial
EDXRF applications. WDXRF is also exploited for
EDXRF instruments may be either handheld for
its wide dynamic range and extremely
use in the field or benchtop for use in a lab.
good reliability for laboratory applications.
EDXRF is a convenient technology to screen
all kinds of materials for quick identification
and quantification of elements with little or no
sample preparation. Low cost of ownership and
rapid elemental analysis of regular or irregular
samples make EDXRF an attractive front-end
analysis tool.

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EDXRF
How It Works
EDXRF is designed to analyze groups of elements simultaneously. This type of XRF
instrumentation separates the characteristic x-rays of different elements into a
complete fluorescence energy spectrum which is then processed for qualitative or
quantitative analysis. Filters positioned between sample and detector are used to
improve signal, background reduction, and focus on certain regions of the spectra.

Direct Excitation vs. Indirect Excitation


Overview
EDXRF instruments can have one of two types of excitation geometry; direct
excitation, or 2D optics, and indirect excitation, also called 3D optics. The purpose of
these geometries is to remove the background below the characteristic element lines
in the spectrum and to increase the peak-to-background ratio (peak-to-noise). Both
types rely on an energy dispersive detector and an x-ray tube; the difference is in the
optic path.

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EDXRF
Direct Excitation Geometry (2D optics) Indirect Excitation (3D optics)
In direct excitation geometry, the detector, sample and x-ray tube are positioned in the Indirect excitation features a 3D geometry with the x-ray tube,
same plane. Primary x-rays from the tube are filtered according to which elements secondary target and sample in one plane, and the detector in a
are being detected. The filtered primary radiation excites the sample elements and the perpendicular plane.
resulting secondary radiation is detected by the detector.
Instruments with 3D optics direct the primary x-rays first to a secondary
target in the sample-target-tube plane, and then to the sample outside
Sample the plane. If reflections happen at exactly 90°, the primary radiation
Cassette
coming from the tube, which produces the background in the spectrum,
is completely eliminated. However, irradiating the secondary target
produces almost monochromatic radiation which is used to excite the
sample elements.

For EDXRF instruments with a tube power up to 50 Watts, the analytical


Detector
performance of 2D and 3D are very similar.

X-ray Tube

2D Optics

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EDXRF
Detectors
The resolution and elemental range achieved by EDXRF analyzers depends on the type of detector used.

Si(Li) Solid State Silicon Drift


PIN Diode
Semiconductor Detectors (SDDs)

• Highest stopping power (efficiency) • High detection efficiency but lower • Most popular thanks to better resolution,
• Resolution as good as silicon drift resolution higher count rates, and faster results than
detectors, but lower count rate • Silicon semiconductor detector material Si(Li) detectors
• Silicon or germanium chip detector • Peltier cooled (requires -20°C) • Peltier cooled (requires -20°C)
material • No longer used in new instruments • Silicon chip detector material
• Liquid nitrogen or Peltier cooled • Lower efficiency, especially for heavy
(requires -90°C) elements

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WDXRF
How It Works
WDXRF uses crystals to disperse the fluorescence spectrum into individual WDXRF systems are based on Bragg’s law, which states that
wavelengths of each element, providing high resolution and low background spectra crystals will reflect x-rays of specific wavelengths and
for accurate determination of elemental concentrations. incident angles when the wavelengths of the scattered x-rays
interfere constructively. While the sample position is fixed,
The types of crystals used in WDXRF include minerals, metallic, organic and synthetic the angles of the crystal and detector can be changed in
multi-layers. Synthetic thin film multilayer crystals are increasing in popularity because compliance with Bragg’s law so that a particular
they offer higher sensitivity and resolution for enhanced light element analysis. Some wavelength can be measured. Only x-rays that satisfy
traditional crystals are sensitive to instrument temperature changes and Bragg’s law are reflected.
x-ray exposure and will degrade over time.
Collimators further improve resolution by providing different

Sample Collimator angular divergences to restrict unwanted secondary x-rays


Detector
Cassette from reaching the detector. Larger collimators can be used
when high intensity is favored over resolution.

X-ray Tube
Did you know?
In 1912, William Lawrence Bragg and William Henry Bragg won a
Nobel Prize in Physics for their discovery.

Detector
Crystal

Optical Encoder Optical Encoder


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WDXRF
Detectors Sample
Two types of detectors can be used in WDXRF instruments. Sealed or
flow gas detectors are best for measuring lower energies (light elements,
below iron [Fe]), while scintillation detectors are better for measuring
higher energies. Both have poor resolution, which is compensated for by
the crystals.

WDXRF analysis can be performed either sequentially using


goniometers or simultaneously using monochromators.

X-ray Tube Flow Gas


Detector
Scintillation
Detector

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WDXRF
Goniometers
Detectors can be mounted on a goniometer and moved through a range of angles to
measure the intensities of different wavelengths in sequential fashion. This system
offers flexibility and optimum performance across the periodic table. However, the
sequential nature of WDXRF instruments and the need to readjust the geometry
between measurements make them operate slowly. Monochromators
X-ray Tube When monochromators are used, the crystal and detector combination is in a fixed
geometry. Each monochromator measures a single element but they all work
simultaneously. This set-up offers speed and precision for a given set of elements.

Sample
Detector

Did you know?


The term goniometry is derived from two Greek
words, gonia, meaning angle, and metron,
meaning measure.

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WDXRF
Small Spot Analysis
Some instruments feature small masks that restrict the analyzed area on the sample. Combined
with appropriate sample movement, this allows the measurement of an individual spot of the sample.

When samples present a defect, the ability to analyze a small


area in isolation can help determine the source of the defect.
XRF instruments with a spotting capability are used for this
purpose in various industries like glass and metal
production.

Only an instrument equipped with spotting can effectively


measure a small defect as shown here. Knowing this was
Copper helped pinpoint the source of the problem.

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WDXRF Y [mm] Ca Ka 1,2 [cps]


Elemental Mapping
XRF Mapping is a great tool to measure the homogeneity of a sample in a sub-millimeter size
range. This can help validate sample preparation or indicate problems in a process.

Geologist’s use XRF elemental mapping to select or screen samples for more in-depth
analysis with a scanning electron microscope (SEM), which requires highly controlled sample [cps]
preparation and provides information in the sub-micrometer size range.

Al Ka 1,2 [cps]

X [mm]

Elemental mapping of a rock gives


understanding to its genesis. X [mm] [cps]

Y [mm]
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EDXRF vs. WDXRF

EDXRF WDXRF
From Sodium (Na) to Uranium (U), very From Beryllium (Be) to Uranium, preferred
Elemental Range: accurate and sensitive for heavy metal analysis. method for light elements and rare earths.

• Poor energy resolution: ~150 eV • Better energy resolution: ~15-150 eV


• More efficient, less costly. • Less efficient, more costly.
• Fewer optical components. • More optical components, benefits from

Pros and Cons: • Acquires an entire spectrum of elements a higher power x-ray tube.
within seconds. • Wide range of instruments to suit various
• No moving parts, more compact, performance needs.
energy-efficient and has lower • Moving parts under vacuum, larger
operating costs. footprint.

Accommodates almost any sample size. Accommodates powder or liquid samples

Samples: in standardized holders and placed in a


sample loading system.

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General Use Guidelines


Radiation
When operating any type of instrumentation that emits x-rays, reasonable effort should be made
to maintain exposures to radiation as far below dose limits as is practical. This is known as the
ALARA (As Low as Reasonably Achievable) principle. For any given source of radiation, three
factors will help minimize your radiation exposure: Time, Distance, Shielding.

Time Distance Shielding


Did you know?
All modern lab XRF instruments are very safe. You would receive
more radiation dose travelling in an airplane than by working next
to a modern XRF lab instrument.

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Sample Preparation
XRF analysis is significantly improved by proper sample There is a trade-off between the time and effort spent in
preparation. This is especially true for strongly altered and sample preparation versus the accuracy of the analytical
mineralized samples. result. Sometimes it’s better to do limited sample preparation
in order to get rough results very quickly. Other applications
A sample must represent all of the material being analyzed; require higher accuracy and hence careful sample
non-homogenous samples contain different concentrations preparation.
of elements at different points across the sample, so the
analysis may not indicate what is really in the material of
interest.

Sample preparation creates a homogeneous sample, which


is extremely important because sample composition and
sampling techniques can greatly impact results. Powdered
samples are fine-grained and contain more consistent
particle sizes. A fused bead is even more representative of
the sampling media and will produce consistent and
repeatable assay data.

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Analysis
XRF instruments are calibrated with a set of reference standards for a list of selected
elements. Once the reference list is stored, analysis of incoming samples is
straightforward. Just prepare the new sample in the same way as the reference ones
were prepared and run the analysis. Instruments are automated and display results on
a screen which can then be exported and sent to remote locations.

Whenever possible, a quantitative calibration will provide more accurate and faster
results than a standard-less analysis. However, obtaining enough known standards to
create a calibration isn’t always possible. Standard-less analysis techniques provide
quantitative data when reference material can’t be procured, for example, waste
processing, or unstable materials.

The strength of standard-less analysis is that it can directly analyze all elements in
any type of sample in about 15 minutes and provide fairly accurate results, down to
ppm levels. This is a great tool when someone comes in the lab with some exotic
material and asks “could you analyze this, please?”

Did you know?


Automated XRF systems are available that combine sample
thermoscientific.com/XRF preparation and analysis in one integrated system. 27
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Metals and Alloys Geology, Mining Cement Manufacturing


Manufacturing and Minerals

3
XRF Analyzers Petroleum Industry Precious Metals and
Gemstones
Polymers and Plastics

in the Lab:
Applications Lab XRF analyzers have many applications
for elemental analysis. Here are a few Glass and Ceramics, Semiconductor, Thin Environment, RoHS and
industries putting XRF technology to work Refractories Films, Coatings WEEE screening
in daily operations.

Paints and Chemicals Forensics Food

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Metals and Alloys Manufacturing


XRF instrumentation is used to verify the quality and composition of metals used in fabrication to ensure Special alloys are made by adding expensive elements
final product integrity. This analysis prevents incorrect or out-of-specification metal alloys caused by material to steel. XRF is the only technique that can measure
mix-ups, incorrect weld chemistry and dilution, or even counterfeit materials from entering the manufacturing high concentrations of the alloying element directly in
process. the solid metal. This allows large cost savings by
preventing overuse of the expensive alloying agents.

Slag, a by-product of the metallurgical smelting


process, can contain environmentally hazardous
materials and must be analyzed for elemental
composition before reuse. Quick and reproducible
analyses of all the oxides in the slag are needed to
control slag quality as well as alloy quality during the
smelting process. WDXRF is an excellent technology
to accomplish this analysis.

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Geology, Mining and Minerals


WDXRF instruments are employed in geology laboratories to evaluate materials and products with wide
elemental coverage, wide concentration ranges and varied samples matrices.

Some examples include the analysis of samples at various stages during mineral processing for quality
control, and optimization of the recovery rate.

XRF also has important applications in detecting penalty and waste elements in iron ore that dilute the
overall grade of the ore, change the physical properties of iron and, impede the proper operation of the
smelting facility.

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Cement Manufacturing
XRF is used to perform elemental analysis on cement-making raw materials to ensure the
concentrations for the major oxides are correct. If the raw materials are inappropriate, or
if they are blended improperly, buildings and roads made from the concrete will have poor
strength and durability.

Oxide CaO SiO2 Al2O3 Fe2O3 MgO Na2O K2O SO3


Concentration 67.4 22.1 5.32 1.88 1.69 0.12 0.66 0.49
Typical clinker analysis result

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Petroleum Industry
The demand for analysis of sulfur in fuels and oils is increasing as environmental regulations worldwide
continue to tighten. Current fuel sulfur standards in some countries are already as low as 10 ppm, and other
countries are likely to follow suit. WDXRF instrumentation can achieve these low levels of quantification with
excellent precision. WDXRF is commonly used to validate the formulation of oil additives and to control for wear
metals in the running process.

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Precious Metals and Gemstones


EDXRF is a nondestructive tool to test the purity and composition of all precious metals. It can
provide the exact karat weight and percentage of all elements within an item.

EDXRF is also used to determine the authenticity of colored gemstones and their geographical
origin. Identification and quantification of characteristic combination of trace elements at
different concentrations may allow tracking of a gemstone down to its location of origin.
Similarly the presence of certain trace elements also helps to distinguish between a valuable
naturally formed gemstone and a worthless synthetic crystal.

thermoscientific.com/XRF 33
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Polymers and Plastics


XRF is the best method for the analysis of trace elements in polymers. Additives such as
plasticisers, lubricants, stabilizing agents, neutralizers, antioxidants, pigments, as well as catalytic
agents, are used to make polymers. XRF is an important process control tool to evaluate the
presence of these agents in the finished product. Elements, including Al, P, Cl, Ti and Fe are
typically analyzed between 5 and 100 ppm.

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Glass and Ceramics, Refractories


Most glass is composed of silica, carbonate and sulfate, lime, and other types of oxides like alumina or
magnesia. WDXRF analysis can be used to confirm that each ingredient is present in the correct percentage
to impart specific physical properties to the glass.

thermoscientific.com/XRF 35
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Semiconductor, Thin Films, Coatings


XRF can be used to simultaneously measure all the layers in magnetic media for in-line process control and
quality assurance. It also has applications in measuring metal coatings and analyzing layers in glass.

thermoscientific.com/XRF 36
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Environment, RoHS and WEEE Screening


High-resolution EDXRF instruments with large sample changers are ideal for analysis of toxic metals in the air resulting from
leaks or spills of petroleum or other toxic products. EDXRF can be used to evaluate components in waste and sludge for
recycling and reuse.

Restriction of Hazardous Substances = RoHS


Waste Electrical and Electronic Equipment = WEEE

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Paints and Chemicals


Elemental analysis using WDXRF instrumentation validates the integrity,
conformity and homogeneity of paints and coatings to be certain they can
be applied successfully, as well as to test ink and toner quality.

thermoscientific.com/XRF 38
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Forensics
EDXRF is an important tool for the crime lab.
Forensic evidence such as gunshot residue on fabrics can be
identified with elemental analysis. EDXRF is also routinely used
to analyze glass chips, metals, and unknown materials.

Food
Food and chemical products contain major and trace elements and
contaminants which can be detected with XRF. One important application
is monitoring nutritional additives to powdered milk. Milk powder can be
measured directly to confirm minerals are present in the appropriate
quantities for quality control and compliance to local regulations.

thermoscientific.com/XRF 39
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Raphael Yerly works as a Senior Product Specialist at Thermo Fisher Scientific


within the Marketing department of Thermo Scientific Laboratory Analyzers, based in
Ecublens, Switzerland. He was born and educated in Switzerland but worked in
Germany and the USA before graduating.

Raphael has been working with both X-Ray Fluorescence and X-Ray Diffraction
equipment in a variety of application fields, including cement production, ore
beneficiation and food quality control. He has traveled around the world to develop
analytical methods that improve production processes and have a positive impact on
the ecological footprint

About the Author of the industry.

Raphael Yerly Raphael’s motto in life is


to make sure we use our
limited resource in the
best possible way.

Debbie Schatzlein, author of XRF in the Field: XRF Technology


for the Non-scientist, contributed to sections of Chapter 1.

thermoscientific.com/XRF 40
Company Intro Contact Us
About Thermo Fisher Scientific For additional information or to schedule a demo, please click below.

Thermo Fisher Scientific is the world leader in serving science. Our mission is to enable our
customers to make the world healthier, cleaner and safer. With revenues of $17 billion, we
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have approximately 50,000 employees and serve customers within pharmaceutical and biotech
companies, hospitals and clinical diagnostic labs, universities, research institutions and government
agencies, as well as in environmental and process control industries. We create value for our key
stakeholders through four premier brands, Thermo Scientific, Life Technologies, Fisher Scientific,
and Unity Lab Services, which offer a unique combination of innovative technologies, convenient
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purchasing options and a single solution for laboratory operations management. Our products and
services help our customers solve complex analytical challenges, improve patient diagnostics and
increase laboratory productivity.

Thermo Fisher Scientific,


(Ecublens) SARL, Switzerland
is ISO 9001:2008 Certified.

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