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 -

  • Introduction of Fundamental Parameters
  • Mathematical Derivation of Fundamental Parameter Method
  • Fundamental Parameter Method for Bulk Sample Analysis
  • Fundamental Parameter Method for Thin Film Analysis
  • Fundamental Parameter Method for Multi-Layered Sample Analysis
  • Monte Carlo Method for Single Layer Analysis of Irregular Shaped Sample
  • Total Reflection XRF and Thin Film Analysis
  • Applications

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

Also from this web page:

Registration

XRF2011 Short Course

Sample Prep Workshop

Portable XRF Analyzer Workshop

Contact

Course Coordinator:

Charles Wu (ctwu@uwo.ca)