Quantitative Analysis of Calcium Compounds by Rietveld Method
Applications | 2018 | ShimadzuInstrumentation
The accurate determination of crystal phases in calcium-containing materials is essential for applications ranging from biomaterials research to quality control in cement and pharmaceuticals. The Rietveld method enables simultaneous phase identification and quantification without calibration curves, enhancing consistency and throughput in powder X-ray diffraction analysis.
This study demonstrates phase identification using Match!3 software and subsequent crystal structure and quantitative analysis via the FullProf Rietveld refinement program. A multi-component sample containing hydroxyapatite (95 wt%) and calcium carbonate (5 wt%) was analyzed to validate the workflow and assess the accuracy of phase quantification.
The combined Match!3/FullProf approach offers:
Advances in database expansion and automation will streamline phase analysis further. Integration with machine learning for peak deconvolution and real-time monitoring of synthesis processes is anticipated. Expansion to in situ and high-throughput setups will broaden use in materials discovery and process control.
The study validates a reliable, calibration-free protocol for phase identification and quantification of calcium compounds using Match!3 and FullProf. This workflow delivers accurate compositional data and structural insights, supporting a wide range of analytical and industrial applications.
XRD
IndustriesMaterials Testing
ManufacturerShimadzu
Summary
Quantitative Analysis of Calcium Compounds by Rietveld Method
Significance of the Topic
The accurate determination of crystal phases in calcium-containing materials is essential for applications ranging from biomaterials research to quality control in cement and pharmaceuticals. The Rietveld method enables simultaneous phase identification and quantification without calibration curves, enhancing consistency and throughput in powder X-ray diffraction analysis.
Objectives and Study Overview
This study demonstrates phase identification using Match!3 software and subsequent crystal structure and quantitative analysis via the FullProf Rietveld refinement program. A multi-component sample containing hydroxyapatite (95 wt%) and calcium carbonate (5 wt%) was analyzed to validate the workflow and assess the accuracy of phase quantification.
Instrumentation
- Diffractometer: Shimadzu XRD-6100
- Detector: OneSight wide-range high-speed detector
- X-ray source: Cu target, 40 kV, 30 mA
- Monochromator: Ni filter
- Scan range: 5–70° 2θ, step scan at 0.0155° increments, 10°/min
Main Results and Discussion
- Phase Identification: Match!3 identified hydroxyapatite and calcite despite overlapping peaks by matching patterns against the Crystallography Open Database.
- Rietveld Refinement: FullProf provided a high‐quality fit (Rwp = 15.3, Chi² = 1.8), confirming the structural model for hexagonal hydroxyapatite (space group P63/m).
- Quantitative Analysis: The refined weight fractions were 95.1 wt% hydroxyapatite and 4.9 wt% calcite, closely matching the prepared composition.
Benefits and Practical Applications
The combined Match!3/FullProf approach offers:
- Calibration-free quantification of multi-phase samples.
- Robust identification in complex mixtures with overlapping peaks.
- Integration into R&D, QA/QC, and industrial production workflows for biomaterials and cement chemistry.
Future Trends and Potential Applications
Advances in database expansion and automation will streamline phase analysis further. Integration with machine learning for peak deconvolution and real-time monitoring of synthesis processes is anticipated. Expansion to in situ and high-throughput setups will broaden use in materials discovery and process control.
Conclusion
The study validates a reliable, calibration-free protocol for phase identification and quantification of calcium compounds using Match!3 and FullProf. This workflow delivers accurate compositional data and structural insights, supporting a wide range of analytical and industrial applications.
Content was automatically generated from an orignal PDF document using AI and may contain inaccuracies.
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