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What is XRF ?

Prepared by Lusi Mustika Sari 1


What is XRF ?
X-Ray Fluorescence (XRF) is an analytical
method to determine the chemical
composition of all kinds of materials.
The types of material that can be analyzed
are
Solids
Liquids
Powders
Filters
Fusion beads

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What is XRF?
Analysis as push button method
Precise: 0.1 0.3 % relative
Accurate: LLDs 0.1 ppm to 100%
Easy sample preparation without chemicals
Fast throughput time of analysis (sample
preparation and measuring)
Fit for integration and automation
Quantitative and qualitative analysis of all
elements from Be to U

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What is XRF?
H He

Li Be B C N O F Ne

Na Mg Al Si P S Cl Ar

K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr

Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe

Cs Ba L Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn

Fr Ra A

L La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu

A Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr

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Where is XRF used?
Materials characterization and (process)
monitoring in research, development, engineering
and product and quality control a.o. for:
Chemical and petrochemical
Cement and industrial minerals
Mining
Steel and non-ferrous
Environmental and pollution
Pharmaceutical and cosmetic
Food

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What are X-rays ?
Electromagnetic radiation: Wavelength 0.01 nm - 10.0 nm

hc 1.2396
E (keV )
(nm) (nm)

Energy 124 keV - 0.124 keV


-rays X-rays UV Visual light

0.001 0.01 0.1 1.0 10.0 100 200 nm

1nm = 10 = 10-9m = 10-6mm


X-rays are highly energetic, therefore dangerous for humans etc.
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X-ray sources in XRF spectrometry
In an X-ray spectrometer there are two places
where X-rays are generated
The X-ray tube
In the x-ray tube the excitation is provided by
electrons from the tube filament
The sample
In the sample the analyte elements are excited by
the photons originating from the X-ray tube

(Note: Power off => X-rays off, no radiation possible)

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The X-ray tube
The x-ray tube
filament

acceleration voltage
current
vacuum
anode material
exit window

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X-ray generation in - End Window Tubes
Super Transmission
Sharp Tube Target Tube

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The side window x-ray tube

20..100kV
anode
Current
electrons
filament

Bewindow X-rayphotons

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Production of x-rays in a sample
d

F lu o r e s c e n c e

In c o m in g x - r a y s
P a s s e d x -ra y s

R a y le ig h
S c a tte r
C o m p to n

S c a tte r

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Production of x-rays in a sample

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Characteristic lines: electron shells

Example:

Fe-K1 = Fe K-LIII
= 7.111-0.708
keV
= 6.403 keV

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The X-ray Fluorescence Spectrometer
Schematic System Design

Spectrometers can be divided


into two main groups:
Wavelength dispersive (WD-
XRF)
Energy dispersive (ED-XRF)

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ED-XRF vs WD-XRF
S a m p le S a m p le

P r im a r y
c o llim a to r

S o u rc e S o u rc e

D e te c to r

D e te c to r

A n a ly s in g c r y s ta l
2

Epsilon 3 Axios
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ED-XRF
The voltage of the pulse produced within a
detector is proportional to the x-ray photon
energy that produces it.
Detector may be solid state e.g. Si(Li), a gas-
filled proportional counter or scintillation counter.
Pulses are sorted by energy in a multi-channel
analyser, where the channel number is
proportional to pulse voltage and the number of
pulses in each channel are counted.
Elemental range is Na U, from ppm to 100%

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ED XRF system
channel
counts

sample
energy (KeV)

X-ray tube
amplifier and
multi-channel
detector analyser

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ED-XRF
Advantages
All elements can be measured simultaneously.
Relatively inexpensive.
Simple operation and maintenance

Disadvantages
Poor performance for light elements
Poor resolution for light elements.
Some detectors require liquid N2.

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EDXRF optics: basic differences

Direct excitation (2D) Polarized excitation (3D)

S a m p le
X -ra y tu b e S a m p le

X -ra y tu b e

S e c o n d a r y ta r g e t
D e te c to r
D e te c to r

Epsilon 3 Epsilon
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Simple 2D EDXRF Optics

X-ray tube Detector


Typically a
Rh anode

Primary tube filters


(5 + blank)
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Or sample surface up
Primary tube
filters
(5 + blank)

X-ray tube
Detector Typically a Rh-anode

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Polarized EDXRF
Sample
Polarised optical
Polarized
Fluorescent
design
x-rays
radiation Very low
backgrounds
Tube
High
Non-polarized peak:background
primary radiation ratio
Best LLDs
Targets Detector

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2D vs. 3D optics

Direct excitation (2D) Polarized excitation (3D)

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EDXRF System

Epsilon 3 XLE Epsilon 5


Epsilon 3X
Epsilon 1

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WD-XRF
Uses single crystals or multilayer to
diffract selected wavelength into the
detection system.
High resolution for all elements.
Quantitative and qualitative analyses.
Elemental range is Be U, from ppm to
100%

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WD XRF system
CPS

sample
degrees 2

primary
collimator

X-ray tube
amplifier,
PHS and
detecto counting
r circuitry
analysing crystal
2

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WD-XRF

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The WDXRF Spectrometer
Schematic Diagram Axios
The WDXRF Spectrometer
Schematic Diagram Axios-Fast
The WDXRF Spectrometer

Bragg's law:

2d sin=n
WDXRF System

Axios Family Axios Fast Cubix XRF


Venus 200

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Direct excitation Secondary excitatio
S a m p le S a m p le
X -ra y tu b e S a m p le

P ro m a ry
c o llim a t o r

X -ra y tu b e
D e te c to r
X -ra y tu b e

S e c o n d a r y ta r g e t
A n a ly s in g c r y s ta l D e te c to r
2 D e te c to r

I I
P1 P3 P3
P1 P3 P1
P2 P2 P2
P4
B3
B1 B4 B B
B2
P4
E E E
WDXRF EDXRF Polarized
EDXRF 32
XRD Family

XPert Powder Cubix3 XPert pro MRD EMPYREAN


Global and near
Resourceful
Experienced

Thank
you

The Analytical X-ray


Company 05/07/17 34

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