Accuracy and Error Sources of the Rietveld Full Pattern Fitting Method in Quantitative Analysis of Illite Ores

CHEN Aiqing; ZHANG Lixue; LI Qiang; ZHU Jianxi; LI Shangying; HE Hongping

doi:10.15898/j.cnki.11-2131/td.202103310046

Rock and Mineral Analysis > 2022 > 41(2): 291-299. > DOI: 10.15898/j.cnki.11-2131/td.202103310046

CHEN Aiqing, ZHANG Lixue, LI Qiang, ZHU Jianxi, LI Shangying, HE Hongping. Accuracy and Error Sources of the Rietveld Full Pattern Fitting Method in Quantitative Analysis of Illite Ores[J]. Rock and Mineral Analysis, 2022, 41(2): 291-299. DOI: 10.15898/j.cnki.11-2131/td.202103310046

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Accuracy and Error Sources of the Rietveld Full Pattern Fitting Method in Quantitative Analysis of Illite Ores

1.
Analysis and Testing Center, China Three Gorges University, Yichang 443002, China
2.
Guangzhou Marine Geological Survey, China Geological Survey, Guangzhou 510075, China
3.
Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China
4.
School of Environmental Science and Engineering, Southern University of Science and Technology, Shenzhen 518055, China

More Information

Received Date: March 30, 2021
Revised Date: December 05, 2021
Accepted Date: January 23, 2022
Published Date: March 27, 2022

Abstract

HIGHLIGHTS
(1) Mixed samples with different content and composition were prepared by pure minerals.

(2) The Rietveld method showed high accuracy and its errors were mainly affected by structural model, thermal vibration, and preferred orientation.

(3) The Rietveld quantitative results of natural illite samples were in good agreement with those of the XRF measurements.

ABSTRACT

BACKGROUNDIllite is an important mineral resource. It is of great theoretical and practical significance to accurately obtain the mineral composition and content of illite ores. The Rietveld full pattern fitting method uses the whole diffraction pattern for analysis and shows high accuracy. However, due to the lack of pure illite samples, the accuracy and error sources of this method for analyzing the content of illite ores are not clearly known at present.
OBJECTIVESTo understand the accuracy and error sources of the Rietveld full pattern fitting method in quantitative analysis of illite ores.
METHODSThe Rietveld full pattern fitting method was used to quantitatively analyze artificial and natural illite ore samples. The results of X-ray fluorescence spectrometry (XRF) of natural illite ores were compared with the chemical compositions calculated from the mineral contents by the Rietveld method.
RESULTSThe results showed that the maximum absolute error ranges of illite-quartz binary mixtures, illite-quartz-albite ternary mixtures, and illite-quartz-albite-calcite-kaolinite multiple mixtures were -0.9%-0.9%, -1.9%-1.6%, and -2.3%-1.6%, respectively. The chemical compositions of natural illite ores calculated by Rietveld method were in good agreement with the results of XRF. This indicated that the Rietveld method had high accuracy in the quantitative analysis of mineral contents of natural illite ore samples. The error sources were mainly affected by the illite structural model, atomic thermal displacement parameters U_iso, and preferred orientation.
CONCLUSIONSA reasonable structural model of illite should be chosen according to the actual samples. The values of atomic thermal vibration U_iso should be reasonably set according to the references. Preferred orientation should be decreased as much as possible during the sample preparation.
- illite,
- the Rietveld full pattern fitting method,
- accuracy,
- error sources,
- X-ray diffraction,
- structural refinement

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Accuracy and Error Sources of the Rietveld Full Pattern Fitting Method in Quantitative Analysis of Illite Ores

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