Course Outline

Week I - Fundamentals, Instrumentation and Qualitative Analysis

It is open to all who are working or intend to work in X-ray spectrometric analysis. No previous knowledge or background in X-ray spectrometry is required.

Topics to be covered in the lectures:

Properties of X-rays; Origin of X-ray Spectra
Instrumentation: Wavelength Dispersive (WD) & Energy Dispersive (ED) Spectrometers
Dispersion of X-rays: WD Spectrometer; Collimator; Analyzing Crystals
Detection of X-rays: Flow and Scintillation Counters; Si(Li), PIN Diode, Silicon Drift Detectors
Pulse height Distributions and Pulse Height Selection (and ED equivalent)
Excitation of X-rays: Characteristic Lines in Tube and Sample; Secondary Targets; Radioisotopes; Polarization
Scattering of X-rays: Rayleigh and Compton Scattering; Sum Peak
Matrix Effects: Absorption; Mass Absorption Coefficients
Matrix Effects: Enhancement; Particle Size; Chemical and Mineralogical effects; Surface Effects and Infinite Thickness
Introduction to Quantitative XRF Analysis: Basic Counting Statistics; Figure of Merits; Calibration and Corrections for Inter-element Matrix Effects.
Selection of Instrumental Variables

plus Sample Preparation Workshop -

Sampling and Sample Preparation (in general)
Pressed Powder Briquettes
Sample Preparation for Metals and Liquids
Borate Fusion Technique

Topics to be covered in the laboratory exercises:

Introduction to the WDXRF spectrometer
Introduction to the EDXRF spectrometer
Qualitative Analysis: Interpretation of Wavelength / Energy Scans
Setting Detector Voltages; Determine Detector Resolution; Setting Pulse Height Selector
Determination of Mass Absorption Coefficients by Transmission, Calculation from Major Element Composition and by Compton Peak Measurements
Introduction to Quantitative XRF Analysis: Evaluation and Applications of Influence (alpha) Coefficients; Application of Mass Absorption Coefficients

Week II - Quantitative Analysis and Data Reduction Methods

A continuation from Week I. Because of the intense and demanding nature of the program, prior attendance at Week I (in this or a previous year) is usually required. In exceptional circumstances a participant may be accepted where their background and experience are considered equivalent.

Topics to be covered in the lectures:

Introduction to Quantitative Analysis:
- Choice of Counting Positions
- Determination of Background Intensity
- Peak Deconvolution (EDXRF)
- Correction for Spectral Line Interferences
- X-ray Tube Line Interference Corrections
- Standards and Standardization
- Crystal fluorescence problems and their solutions
Introduction to Influence Coefficients
Mathematical Matrix Correction Techniques
Semi-quantitative to Standardless Quantification Methods
Quality Control and Monitors
Summary of Advantage and Disadvantages of XRF

plus Layered Sample and Thin Film Analysis Workshop

Topics to be covered in laboratory exercises:

Major and Trace Element Data Reduction:
- Methods of Background Determination
- Correction for Peak-on-Peak and Peak-on-Background Spectral Interferences
- Determining of and Correction for X-ray Tube Line Interferences
- Iterative Cross-tail Corrections Procedures
- Standardization
- Calculation of Concentration, Counting Error and Lower Limit of Detection
Applications of Mass Absorption Coefficients; Absorption Edge Problems; Techniques for Crossing Major Element Absorption Edges
Calculations for Influence Coefficients; Application of Different Algorithms Correcting for Matrix Effects