A rapid method for quantifying single mineral phases in heterogeneous natural dusts using X-ray diffraction

2009 ◽  
Vol 24 (1) ◽  
pp. 17-23 ◽  
Author(s):  
Jennifer S. Le Blond ◽  
Gordon Cressey ◽  
Claire J. Horwell ◽  
Ben J. Williamson

Quantification of potentially toxic single mineral phases in natural dusts of heterogeneous composition is critical for health hazard assessment. For example, crystalline silica, a human carcinogen, can be present as respirable particles in volcanic ash such as quartz, cristobalite, or tridymite. A method to rapidly identify the proportions of crystalline silica within mixed dust samples, such as volcanic ash, is therefore required for hazard managers to assess the potential risk of crystalline silica exposure to local populations. Here we present a rapid method for quantifying the proportions of single phases in the mineral assemblage of mixed dusts using X-ray diffraction (XRD) with a fixed curved position-sensitive detector. The method is a modified version of the whole-pattern peak-stripping (PS) method (devised by Cressey and Schofield [Powder Diffr.11, 35–39 (1996)]) using an internal attenuation standard (IAS) but, unlike the PS method, it requires no knowledge of other phases present in the sample. Ten synthetic sample mixtures were prepared from known combinations of four pure phases (cristobalite, hematite, labradorite, and obsidian), chosen to represent problematic constituents of volcanic ash, and analyzed by XRD. Results of the IAS method were directly compared with those of the PS method. The proportions of cristobalite estimated using the methods were comparable and accurate to within 3 wt %. The new IAS method involved less sample preparation and processing and, therefore, was faster than the original PS method. It therefore offers a highly accurate rapid technique for determination of the proportions of individual phases in mixed dusts.

1990 ◽  
Vol 5 (3) ◽  
pp. 121-124 ◽  
Author(s):  
David J. Devlin ◽  
Kamal E. Amin

AbstractThe relative intensities ratios for the determination of the relative amounts of alpha and beta phases in silicon nitride and the relative amounts of delta yttrium disilicate (Y2Si2O7) and nitrogen apatite [Y5(SiO4)3N] are reported. These constants were determined using an iterative method applicable when the pure phases are not easily prepared. In addition, a calibration curve was obtained for the quantitative measurement of free silicon in silicon nitride over the range 0 to 0.3% by weight of Si.


Clay Minerals ◽  
1973 ◽  
Vol 10 (1) ◽  
pp. 51-55 ◽  
Author(s):  
M. E. Cosgrove ◽  
A. M. A. Sulaiman

AbstractAn X-ray diffraction method for the estimation of quartz is described using rock powder pellets originally prepared for X-ray spectrometry, correcting the X-ray intensities for mass absorption. A coefficient of variation of 3·8% is claimed; 95% of all estimates fall within ± 5·5%.


1989 ◽  
Vol 33 ◽  
pp. 493-497 ◽  
Author(s):  
R. D. Hamilton ◽  
N. G. Peletis

AbstractIARC's designation of crystalline silica as a “probable carcinogen” triggered the requirement to label products containing greater than 0.1 % crystalline silica. For perlite and other materials which may contain crystalline silica in levels close to 0.1% an accurate determination is critical from both legal and marketing considerations.Existing analytical techniques for the determination of crystalline silica at levels of less than 1.0% were found to be inadequate to meet the new requirements. An improved technique based on x-ray diffraction has been developed specifically to analyze perlite for crystalline silica, which occurs largely in the form of quartz, at the 0.1%. level. The technique employs long counting times and improved sample preparation and mounting to increase both precision and accuracy, and to lower the detection limit to less than 0.1%.The technique was tested on a large number of samples from a variety of sources and proven to give excellent results for all types of expanded perlites and perlite ores. The procedures developed are applicable to a wide variety of materials in addition to perlite.


1992 ◽  
Vol 47 (1-2) ◽  
pp. 141-146
Author(s):  
Valentin P. Feshin

AbstractThe 35Cl and 79Br NQR spectra of halogen-containing organic compounds of Si, Ge, Sn and Te, in which these atoms may be tetra- or pentacoordinated, have been compared to the results of their X-ray diffraction analysis. The NQR technique was also used to study a large number of such compounds for which X-ray investigations were found to be impossible. It has been shown that the NQR technique may be considered as a rapid method for the determination of the electronic and spatial structure of these compounds. The conditions for pentacoordination of atoms of IVA group elements have been also formulated.


MRS Advances ◽  
2019 ◽  
Vol 4 (57-58) ◽  
pp. 3163-3169
Author(s):  
J. López-Cuevas ◽  
J.C. Rendón-Angeles ◽  
J.L. Rodríguez-Galicia ◽  
C.A. Gutiérrez-Chavarría

ABSTRACTAn alternative method for the standardless quantitative x-ray diffraction analysis of mixtures of inorganic crystalline phases proposed in the literature several years ago is presented. Our method requires only previously calculated μ*i values from tabulated data for all phases present in the mixtures. It does not require either the determination of calibration constants or the use of external standards, but it does require that the number of analyzed mixtures is larger than or equal to the number of phases present in them, and that the chemical composition of the mixtures are significantly different from each other. The integrated intensities of the chemically pure phases are estimated by a least-squares procedure from XRD data obtained from the mixtures. The method was tested against data published in the literature, with good results. Finally, a general expression for the “Normalized Height Law” proposed on an empirical basis by other researchers, has been theoretically derived.


2009 ◽  
Vol 24 (2) ◽  
pp. 145-145
Author(s):  
Jennifer S. Le Blond ◽  
Gordon Cressey ◽  
Claire J. Horwell ◽  
Ben J. Williamson

Author(s):  
R. J. Narconis ◽  
G. L. Johnson

Analysis of the constituents of renal and biliary calculi may be of help in the management of patients with calculous disease. Several methods of analysis are available for identifying these constituents. Most common are chemical methods, optical crystallography, x-ray diffraction, and infrared spectroscopy. The application of a SEM with x-ray analysis capabilities should be considered as an additional alternative.A scanning electron microscope equipped with an x-ray “mapping” attachment offers an additional dimension in its ability to locate elemental constituents geographically, and thus, provide a clue in determination of possible metabolic etiology in calculus formation. The ability of this method to give an undisturbed view of adjacent layers of elements in their natural state is of advantage in determining the sequence of formation of subsequent layers of chemical constituents.


Author(s):  
M. D. Vaudin ◽  
J. P. Cline

The study of preferred crystallographic orientation (texture) in ceramics is assuming greater importance as their anisotropic crystal properties are being used to advantage in an increasing number of applications. The quantification of texture by a reliable and rapid method is required. Analysis of backscattered electron Kikuchi patterns (BEKPs) can be used to provide the crystallographic orientation of as many grains as time and resources allow. The technique is relatively slow, particularly for noncubic materials, but the data are more accurate than any comparable technique when a sufficient number of grains are analyzed. Thus, BEKP is well-suited as a verification method for data obtained in faster ways, such as x-ray or neutron diffraction. We have compared texture data obtained using BEKP, x-ray diffraction and neutron diffraction. Alumina specimens displaying differing levels of axisymmetric (0001) texture normal to the specimen surface were investigated.BEKP patterns were obtained from about a hundred grains selected at random in each specimen.


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