Short Course Outline - XRF2018

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 Week I:

Day 1

  • Introduction to X-rays;Properties of X-rays
  • Origin of X-ray Spectra; Excitation and Characteristic Radiations
  • Instrumentation Part I: Introduction of WDXRF, EDXRF and Detectors
  • Practical Exercise: Instrumentation and X-ray Source
  1. Source Spectra: what will excite our sample?
  2. Introduction to WDXRF and EDXRF Spectrometers
  3. Live instruments demo

Day 2

  • Instrumentation Part II: Dispersion of X-rays; Pulse Height Analysis
  • Practical Exercise: Qualitative Analysis, Spectral Identification – WDXRF & EDXRF
  • Introduction to Matrix Effect Part I: Absorption; Mass Absorption Coefficients
  • Practical Exercises: Working with Mass Absorption Coefficients (MACs)

Day 3

  • Introduction to Matrix Effect Part II: Enhancement; Particle Size, Chemical and Mineralogical Effects; Surface Effects and Infinite Thickness
  • Practical Exercise: Where does the signal come from - Infinite or non infinite thickness?
  • Introduction to Quantitative Analysis: Counting Statistics; Figure of Merits; Correction for Spectral Interferences; Calibration and Standardless Analysis
  • Practical Exercise: Sources of Error; Counting Statistics- Precision/ Accuracy/ Bias
  • Practical Exercise: My first calibration

Day 4

  • Application Methods Maintenance: Drift Monitors; Drift Correction; Quality Control (QC)
  • Practical Exercise: Counting Statistics and SPC Charts
  • Best Operation Practice: WDXRF, EDXRF and related Analytical Issues
  • Group Discussion: Analytical and Calibration issues with Practical Examples
  • Summary of Advantages and Disadvantages of XRF Spectrometry

Day 5 – Sample Preparation Workshop

  • Representative Sampling
  • Specimen Preparation: Crushing & Milling
  • Pressed Powder Briquettes
  • Surface Preparation for Metals Samples
  • Preparation for Liquid Samples
  • Borate Fusion Technique

 

Week II - Quantitative Analysis and Method Development

Week II is in a NEW format, concentrating on the practical Method Development aspect for new applications. The approach is following Good Laboratory Practice (GLP) guidelines and enriched with many real world examples from the experience of the lecturers. The aim is to ingrain the steps, thus giving the participants a framework and successful tools. Once completed, the participants will be more successful in developing methods and able to deliver better methods in a shorter time!

Week II is built on the fundamentals of XRF from Week I. Because of the intense and demanding nature of the program, prior attendance at Week I is required. In exceptional circumstances a participant may be accepted where their background and experience are considered equivalent.


Topics to be covered in Week II:

Day 1

  • What do we know so far: Recalling Week I
  • Quantitative Analysis
    1. Define the Application: Get your specification right at the beginning!
    2. Sample Preparation Method: What is the BEST for your sample (matrix)?
    3. Availability of Standard Reference Materials
    4. Select Instrumental Parameters
    5. Use Figure of Merit and Optimize Pulse Height Analysis
    6. Practical Exercise:
      1. Figure of Merit for WDXRF Instrumental Settings
      2. Figure of Merit for EDXRF Instrumental Settings


Day 2

  • Quantitative Analysis (cont'd)
    1. Measuring Standards and Define the Drift Correction
    2. Getting the Correct Intensities
    3. From Intensity to Concentration: KIM Equation; Matrix Correction Term and Algorithms
    4. Practical Exercise:
      1. Determining Net Intensities, including Background and Spectral Interference Corrections
      2. Trace Element Calibration: How to use ratio to Compton Peak Intensity


Day 3

  • Quantitative Analysis (Matrix Correction)
    1. Fundamental Parameter (FP) Method I: X-ray Fundamental Parameters
    2. Fundamental Parameter (FP) Method II: Algorithms and Derivations
    3. Fundamental Parameter (FP) Method III: Applying the FP Method in Calibration Process
    4. Practical Exercises and Lectures are concurrent to reinforce each FP aspect step by step.


Day 4

  • Introduction to Influence Coefficients
  • Practical Exercise: Calculation and Validating the Case Study of a Ternary System
  • Quality Assurance Samples and their limitations
  • Q/A and Discussion: Problem encountered in Your Lab


Day 5 – Method Development: "Work Smarter, Not Harder"

  • Define the Objective
  • Find Reference Materials & Type Standards
  • Define Sample Preparation Procedures
  • Select Instrument Parameters
  • Define Method Maintenance
  • Perform Calibrations
  • Validate Calibrations
  • Documentation & Backup

 

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