XRF and XRPD data sets in ternary mixtures with high level micro-absorption and/or preferred orientations problems...

Area of Science:

• Materials Science
• Analytical Chemistry
• Crystallography

Background:

• Quantitative phase analysis (QPA) using X-ray Powder Diffraction (XRPD) is hindered by micro-absorption (MA) and preferred orientations (PO) in industrial samples.
• Elemental analysis via X-ray Fluorescence (XRF) is often coupled with XRPD for phase identification, especially for elements heavier than sodium.
• Industrial commodities like graphite and urea present significant analytical challenges for QPA due to their physical properties.

Purpose of the Study:

• To develop a standardized methodology for creating complex XRPD and XRF data sets.
• To provide a benchmark for evaluating different QPA approaches and software performance.
• To establish a foundation for an open-access repository of standardized analytical data.

Main Methods:

• Utilized a simplex-centroid design augmented approach for experimental design to ensure homogeneous exploration of ternary domains.
• Prepared sample mixtures of graphite, zinc acetate, and urea with controlled preferred orientation (PO) in graphite via sieving.
• Collected comprehensive XRF and XRPD data across four experimental domains, ranging from pure phases to equal-weighted mixtures.

Main Results:

• Successfully generated diverse data sets with increasing analytical difficulty for QPA testing.
• Demonstrated the feasibility of controlling preferred orientation (PO) in graphite through physical methods like sieving.
• Established a repository on Mendeley Data containing the collected XRF and XRPD data.

Conclusions:

• The developed recipe provides a reliable method for producing standardized data crucial for QPA validation.
• The open-access data repository facilitates reproducible research and advancement in analytical techniques for industrial materials.
• This approach enables the creation of a comprehensive, expandable dataset for benchmarking QPA software and methodologies.