Short Course Outline - XRF2024

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 XRF: WDXRF and EDXRF
• X-Ray Physics
• Instrumentation: WDXRF and EDXRF
• Practical Exercise: Instrumentation and X-ray Source

1. Introduction to WDXRF and EDXRF Spectrometers
2. Live instrument demonstration
   
   

Day 2

• Practical Exercise: Qualitative Analysis, Spectral Identification – WDXRF & EDXRF
• Matrix Effects Part I: Absorption; Mass Absorption Coefficients
• Matrix Effects Part II: Enhancement, Mineralogical, Particle Size, Chemical Effects, & Infinite Thickness
• Practical Exercises: Working with Mass Absorption Coefficients (MACs)

Day 3

• Introduction to Setting Up Analytical Programs
• Simple Net Intensity - Introduction to Background Correction
• 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
  
  

Day 4

• Introduction to Calibration and Matrix Correction Models
• Application Methods Maintenance: Drift Monitors; Drift Correction; Quality Control (QC)
• Introduction to Method Validation
• Best Operation Practice: WDXRF, EDXRF and related Analytical Issues
• 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

• Trace Element Calibration; How to use ratio to Compton Peak Intensity
• Numerical Matrix Correction Approaches: Compensation Methods; Influence Coefficients - Empirical vs Theoretical
• Fundamental Parameter (FP) Method Equation: the Fluorescent Process Explained

Day 4

• Applying Matrix Correction in the Calibration Process
• Practical Exercise: Calculation and Validating the Case Study of a Ternary System
• Testing & Validating the Method; Control Samples, Defining QC Limits
• Q/A and Discussion: Problem encountered in Your Lab

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