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Analysis Seminar

The document discusses different types of X-ray fluorescence spectroscopy techniques including EDXRF, WDXRF, and TXRF. EDXRF uses an energy dispersive detector to analyze the full spectrum of emitted X-rays allowing for both qualitative and quantitative analysis. WDXRF uses a wavelength dispersive crystal to detect specific wavelengths, providing higher resolution but requiring knowing the element first. TXRF uses total reflection of X-rays at low angles to reduce background noise and matrix effects, enabling ultra-trace analysis down to parts-per-trillion concentrations. PIXE is also discussed as using proton beams rather than X-rays for excitation, allowing surface analysis of samples.

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Emad Behdad
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181 views

Analysis Seminar

The document discusses different types of X-ray fluorescence spectroscopy techniques including EDXRF, WDXRF, and TXRF. EDXRF uses an energy dispersive detector to analyze the full spectrum of emitted X-rays allowing for both qualitative and quantitative analysis. WDXRF uses a wavelength dispersive crystal to detect specific wavelengths, providing higher resolution but requiring knowing the element first. TXRF uses total reflection of X-rays at low angles to reduce background noise and matrix effects, enabling ultra-trace analysis down to parts-per-trillion concentrations. PIXE is also discussed as using proton beams rather than X-rays for excitation, allowing surface analysis of samples.

Uploaded by

Emad Behdad
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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EDXRF

WDXRF

TXRF

PROVIDED BY
EMAD BEHDAD

SPECIALIZED PROTECTION AND CORROSION OF MATERIALS

LECTURERS
H.MONAJATI,PHD JAFARI,PHD ISLAMIC AZAD UNIVERSITY OF NAJAFABAD BARANCH OF MATERIAL SCIENCE ENGINEERING

Atoms in the sample are excited and emit characteristic x-rays

x-ray source x-ray detector

Energy of characteristic x-rays

Types of elements present (qualitative analysis)

Number of x-rays for each element concentration (quantitative analysis)

Based on the excitation

Tube excited XRF


Radio-isotope excited XRF Secondary target Synchrotron,

Total reflection of x-ray florescence

Based on the detection


Wavelength dispersive (WD-XRF)

Energy dispersive (ED-XRF)


Filter instruments (proportional counter)

*Energy dispersive X-ray spectroscopy (EDS or EDX)

*Analytical technique used for the elemental analysis


*Technique used for chemical characterization of a sample *Investigation of a sample *Analyzing X-rays emitted by the matter *Full quantitative analysis showing the sample composition

HOW EDX WORKS ?


A high-energy beam of charged particles is focused into the sample Ground state(unexcited) electrons in sample are stimulated Electrons are excited from lower energy shells to higher energy shell The difference in energy between the shells may be released in the form of an X-ray The number and energy of the X-rays emitted from a specimen can be measured by an energy dispersive spectrometer

SCHEMATICS OF EDX

What is the principle behind ED spectrometers?

The heart of an ED-spectrometer is a semi-conductor crystal (Si, Ge) a high voltage is applied over the crystal (bias -600V) and the crystal is cooled (e.g. at liquid nitrogen temperature) When x-rays enter the crystal electron-hole pairs are formed the number is proportional to the energy of the x-ray

because of the bias the electrons are swept out of the crystal
For each photon an electric pulse is produced with an amplitude proportional to the energy. Measuring the amplitude and counting produces the ED-spectrum.

WHY EDX
Fast

(Non)-destructive
Sample Area Good precision, accuracy Fair sensitivity Multi-element analysis

Generally not portable Some sample preparation required Experienced staff Moderately expensive

Wavelength dispersive X-ray spectroscopy (WDXRF or WDS)

A method used to count the number of X-rays


Reads or counts only the x-rays of a single wavelength Element must be known Often used in conjunction with EDS

Identification of spectrally overlapped elements


Detection of low concentration species (10-100 ppm)

Analysis of low atomic number elements Oxidation and corrosion of metals

The WDX operates in much the same way as EDX.

Unlike the related technique of Energy dispersive X-ray spectroscopy (EDX)WDX reads or counts only the x-rays of a single wavelength, not producing a broad spectrum of wavelengths or energies.
The crystal structure of sample diffracts the photons in principles of Bragg's law. Diffractions are then collected by a detector.

(Non)-destructive High accuracy

Some sample preparation Qualified, experience staff Expensive

Excellent precision & long term stability


Good resolution & sensitivity Multi-element analysis Well-established technique

Comparison of WD and ED X-ray Detectors



Most important advantages of WD: Higher resolution, sensitivity Most important advantages of ED: Cheaper, faster (except for multichannel WD) Other differences (more detailed comparison):

DIAGRAM AND CURVES WDS V.S EDS

TOTAL REFLECTION X-RAY FLUORESCENCE (TXRF)


Total reflection X-ray fluorescence analysis (TXRF) is basically an energy dispersive

analytical technique in special excitation geometry.

USAGE AREAS OF TXRF


Total reflection X-ray fluorescence (TXRF) has become increasingly popular in micro and trace elemental analysis. It is being used in geology, biology, materials science, medicine, forensics, archaeology, art history, and more.

Unlike the high incident angles (~ 40 ) used in traditional XRF, TXRF involves very low incident angles.
These low angles allow the X-rays to undergo total reflection.

Background reduced.

Double excitation of sample by both the primary and the reflected beam.
No matrix effects. Calibration and quantification independent from any sample matrix. Simultaneous multi-element ultra-trace analysis. Several different sample types and applications. Excellent detection limits (ppt or pg) for all elements from sodium to plutonium. Excellent dynamic range from ppt to percent. Possibility to analyses the sample directly without chemical pretreatment. Non destructive analysis. Low running cost.

EXPERIMENTAL ANALYSIS RESULTS

Spectrum of a 3 L mineral water sample, spiked with 1 ng/L Ga as internal standard element. Excitation in TXRF geometry with a multilayer monochromator by a Mo X-ray tube (50 kV, 10 mA, 1000 s measuring time).

PROVIDED BY ZABIH ALLAH KHANSHA

PIXE

Proton Induced X-ray Emission

MATERIAL SURFACE. PROCESSES RELEVANT TO ION BEAM ANALYSIS

PROTON INDUCED X-RAY EMISSION


Detector Si(Li)

X-rays

2-3 MeV sample

REACTION PIXE BOX

PIXE USAGE 2004

16% 27% 24%

33%

Environmental & Atospheric Archaeology & Arts Biomedical material & Earth Science

JAME MOSQUE SLIMES PIXE ANALYSIS

SPECTRUMES PIXE SAMPLES LIVER BIOPSY

TYPICAL PIXE SPECTRUM OF NORMAL AND VARICOSE VEINS WITH 175MM MAYLAR ABSORBER IN FRONT OF SI(LI) DETECTOR

QUESTIONS ?
THANKS FOR YOUR ATTENTION

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