利用 X 射线衍射法制备塔卡林加矿的黄铁矿精矿粉,以进行定量相分析。

IF 6.1 3区 材料科学 Q1 Biochemistry, Genetics and Molecular Biology
Journal of Applied Crystallography Pub Date : 2022-11-29 eCollection Date: 2022-12-01 DOI:10.1107/S1600576722009888
Hamish McDougall, Monica Hibberd, Andrew Tong, Suzanne Neville, Vanessa Peterson, Christophe Didier
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引用次数: 0

摘要

使用 X 射线衍射法对塔卡林加矿提取的黄铁矿精矿样品进行定量相分析存在问题,原因是颗粒统计、微吸收和优先取向较差。对样品制备对这些问题的影响进行了评估,发现球磨粉末最适合进行准确和精确的定量相分析。对研磨持续时间和样品制备的其他方面进行了探讨,结果表明,当颗粒尺寸小于 5 微米时,相反射强度非常准确。对这些样品进行的定量相分析得出了精确的相分数,标准偏差低于 0.3 wt%。利用 X 射线粉末衍射数据获得的元素组成与利用波长色散 X 射线荧光测定的元素组成之间存在一些差异,这可能是由于未考虑晶相置换以及可能存在无定形相造成的。本研究提供了对塔克林加矿黄铁矿精矿的 X 射线粉末衍射数据进行精确定量相分析的方法,并讨论了该方法的局限性。优化过程揭示了在确认新样品的可重复性时尽可能事先了解情况的重要性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Preparation of pyrite concentrate powder from the Thackaringa mine for quantitative phase analysis using X-ray diffraction.

Preparation of pyrite concentrate powder from the Thackaringa mine for quantitative phase analysis using X-ray diffraction.

Preparation of pyrite concentrate powder from the Thackaringa mine for quantitative phase analysis using X-ray diffraction.

Preparation of pyrite concentrate powder from the Thackaringa mine for quantitative phase analysis using X-ray diffraction.

The quantitative phase analysis using X-ray diffraction of pyrite ore concentrate samples extracted from the Thackaringa mine is problematic due to poor particle statistics, microabsorption and preferred orientation. The influence of sample preparation on these issues has been evaluated, with ball milling of the powder found most suitable for accurate and precise quantitative phase analysis. The milling duration and other aspects of sample preparation have been explored, resulting in accurate phase reflection intensities when particle sizes are below 5 µm. Quantitative phase analysis on those samples yielded precise phase fractions with standard deviations below 0.3 wt%. Some discrepancy between the elemental composition obtained using X-ray powder diffraction data and that determined using wavelength-dispersive X-ray fluorescence was found, and is thought to arise from unaccounted for crystalline phase substitution and the possible presence of an amorphous phase. This study provides a methodology for the precise and accurate quantitative phase analysis of X-ray powder diffraction data of pyrite ore concentrate from the Thackaringa mine and a discussion of the limitations of the method. The optimization process reveals the importance of confirming reproducibility on new samples, with as much prior knowledge as possible.

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来源期刊
CiteScore
10.00
自引率
3.30%
发文量
178
审稿时长
4.7 months
期刊介绍: Many research topics in condensed matter research, materials science and the life sciences make use of crystallographic methods to study crystalline and non-crystalline matter with neutrons, X-rays and electrons. Articles published in the Journal of Applied Crystallography focus on these methods and their use in identifying structural and diffusion-controlled phase transformations, structure-property relationships, structural changes of defects, interfaces and surfaces, etc. Developments of instrumentation and crystallographic apparatus, theory and interpretation, numerical analysis and other related subjects are also covered. The journal is the primary place where crystallographic computer program information is published.
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