XRS
Introduction to X-Ray Emission Spectrometry
Table of Contents
1.
Introduction
2.
X-rays physics
3.
Instrumentation for x-ray emission spectroscopy
4.
EDXRS spectra
5.
XRS emission techniques and methodologies
6.
Quantitative analysis in EDXRF
7.
Method validation in EDXRF
8.
Final recommendations
Table of Contents
1.
Introduction
1.1
Audience
1.2
Instructions for following the course
2.
X-rays physics
2.1
The nature of x-rays
2.2
Energy and wavelength
2.3
X-rays properties
2.4
Mechanisms of x-ray production
2.4.1
Production of continuous radiation
2.4.2
Production of characteristic emission
2.5
Characteristic radiation
2.6
Interactions of x-rays with matter
2.6.1
Photoelectric absorption
2.6.2
Scattering
2.6.3
Total sample attenuation
2.6.4
X-ray total reflection
2.6.5
X-ray diffraction
2.6.6
The use of different interactions in XRS
3.
Instrumentation for x-ray emission spectroscopy
3.1
Excitation sources
3.1.1
Radioisotope sources
3.1.2
X-ray tubes
3.1.2.1
Direct excitation
3.1.2.2
Use of filters for excitation
3.1.2.3
Secondary targets and scatter devices
3.1.2.4
Comparison of performance: Direct tube, Filtered and ST excitation
3.1.2.5
Capillary lenses
3.1.3
Electrons
3.1.4
Charged particles
3.1.5
Synchrotron light
3.2
Detectors
3.2.1
Efficiency
3.2.2
Energy resolution
3.2.3
Types of x-ray detectors and main applications
3.2.4
Gas filled detectors
3.2.4.1
Ionization chambers
3.2.4.2
Proportional counters
3.2.5
Scintillation detectors
3.2.6
Semiconductor detectors
3.2.6.1
Intrinsic semiconductors: Si(Li) and Ge detectors
3.2.6.2
PIN diode detectors
3.2.6.3
SDD
3.2.6.4
CCD detectors
3.3
Signal processing
3.3.1
Analogic signal processing (ASP)
3.3.2
Digital signal processing (DSP)
4.
EDXRS spectra
4.1
EDXRS spectra evaluation
4.1.1
Probability distribution
4.1.2
Detection limits
4.2
Characteristic emission peaks
4.3
Spectrum continuum
4.4
Escape and sum peaks
4.5
Scatter peaks
4.6
Estimation of peak area by basic fit procedure
4.6.1
Advanced peak fitting models
4.6.2
Continuum fitting models
4.6.3
Available software for spectrum deconvolution
5.
XRS emission techniques and methodologies
5.1
Emission techniques
5.1.1
XRF spectrometry
5.1.1.1
WDXRF spectrometry
5.1.1.2
EDXRF spectrometry
5.1.2
Synchrotron XRF analysis
5.1.3
Electron microprobe analysis (SEM-EDS)
5.1.4
Particle induced x-ray emission (PIXE)
5.2
Spatially resolved elemental distribution: element mapping
5.2.1
Micro-XRF
5.2.2
Confocal XRF
5.2.3
Full Field XRF
6.
Quantitative analysis in EDXRF
6.1
Fundamentals: the Shermann equation for Intermediate thickness samples
6.1.1
Enhancement effects
6.1.2
Thick samples
6.1.3
Thin samples
6.2
Sample preparation
6.3
Common quantification approaches
6.3.1
Thin sample analysis
6.3.2
Sample dilution to facilitate linear regression
6.3.3
Influence coefficients
6.3.4
Scatter normalization
6.3.5
Fundamental parameters
7.
Method validation in EDXRF
7.1
Selectivity
7.2
Working interval
7.3
Detection limits
7.4
Trueness and recovery
7.5
Precision
7.6
Accuracy
7.7
Uncertainty estimation
7.7.1
Type A evaluation
7.7.2
Type B evaluation
7.8
Robustness
7.9
External quality control
8.
Final recommendations