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Calibrating for X-Ray Diffraction Analysis of Trace Quartz

Published online by Cambridge University Press:  06 March 2019

Jacques Renault
Affiliation:
New Mexico Bureau of Mines and Mineral Resources Division New Mexico Institute of Mining and Technology Campus Station, Socorro, NM 87801, USA
Chris McKee
Affiliation:
New Mexico Bureau of Mines and Mineral Resources Division New Mexico Institute of Mining and Technology Campus Station, Socorro, NM 87801, USA
James Barker
Affiliation:
New Mexico Bureau of Mines and Mineral Resources Division New Mexico Institute of Mining and Technology Campus Station, Socorro, NM 87801, USA
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Abstract

Trace analysis of quartz at the <0.1 wt% level can be routinely accomplished by x-ray diffraction using rotating pressed-powder briquettes and a peak deconvolution strategy due to Wiedemann, et al. (1937a, b) which permits reproducible determination of background and enhances peak resolution without changing the integrated intensity.

Four calibration methods were tested: (1) calibration with perlites microscopically analyzed by Hamilton and Peletls (1988), (2) with artificial mixtures of quartz and glass, (3) with chemical analysis and massbalance calculation of quartz in glass mixtures, and (4) with a new method of additions for XRD.

Methods (2) and (4) gave the best results. Method (2) has a precision of 16.9 pet at the 0.1 wt% level and a LLD of 0.05 wt% at 3σ. Method (4) is particularly attractive because large spikes can be used which minimize homogenization errors and permit preparation of standards which have properties very similar to run-of-the-mill samples; the problem of non-zero intercepts is avoided.

Type
VI. XRD Instrumentation, Techniques and Reference Materials
Copyright
Copyright © International Centre for Diffraction Data 1991

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