Quantitative Analysis Of X-Ray Images From Geological Materials

Author(s):  
J. M. Paque ◽  
R. Browning ◽  
P. L. King ◽  
P. Pianetta

Geological samples typically contain many minerals (phases) with multiple element compositions. A complete analytical description should give the number of phases present, the volume occupied by each phase in the bulk sample, the average and range of composition of each phase, and the bulk composition of the sample. A practical approach to providing such a complete description is from quantitative analysis of multi-elemental x-ray images.With the advances in recent years in the speed and storage capabilities of laboratory computers, large quantities of data can be efficiently manipulated. Commercial software and hardware presently available allow simultaneous collection of multiple x-ray images from a sample (up to 16 for the Kevex Delta system). Thus, high resolution x-ray images of the majority of the detectable elements in a sample can be collected. The use of statistical techniques, including principal component analysis (PCA), can provide insight into mineral phase composition and the distribution of minerals within a sample.

Author(s):  
V. V. Damiano ◽  
R. P. Daniele ◽  
H. T. Tucker ◽  
J. H. Dauber

An important example of intracellular particles is encountered in silicosis where alveolar macrophages ingest inspired silica particles. The quantitation of the silica uptake by these cells may be a potentially useful method for monitoring silica exposure. Accurate quantitative analysis of ingested silica by phagocytic cells is difficult because the particles are frequently small, irregularly shaped and cannot be visualized within the cells. Semiquantitative methods which make use of particles of known size, shape and composition as calibration standards may be the most direct and simplest approach to undertake. The present paper describes an empirical method in which glass microspheres were used as a model to show how the ratio of the silicon Kα peak X-ray intensity from the microspheres to that of a bulk sample of the same composition correlated to the mass of the microsphere contained within the cell. Irregular shaped silica particles were also analyzed and a calibration curve was generated from these data.


2016 ◽  
Vol 113 (26) ◽  
pp. 7071-7076 ◽  
Author(s):  
Richard V. Morris ◽  
David T. Vaniman ◽  
David F. Blake ◽  
Ralf Gellert ◽  
Steve J. Chipera ◽  
...  

Tridymite, a low-pressure, high-temperature (>870 °C) SiO2 polymorph, was detected in a drill sample of laminated mudstone (Buckskin) at Marias Pass in Gale crater, Mars, by the Chemistry and Mineralogy X-ray diffraction instrument onboard the Mars Science Laboratory rover Curiosity. The tridymitic mudstone has ∼40 wt.% crystalline and ∼60 wt.% X-ray amorphous material and a bulk composition with ∼74 wt.% SiO2 (Alpha Particle X-Ray Spectrometer analysis). Plagioclase (∼17 wt.% of bulk sample), tridymite (∼14 wt.%), sanidine (∼3 wt.%), cation-deficient magnetite (∼3 wt.%), cristobalite (∼2 wt.%), and anhydrite (∼1 wt.%) are the mudstone crystalline minerals. Amorphous material is silica-rich (∼39 wt.% opal-A and/or high-SiO2 glass and opal-CT), volatile-bearing (16 wt.% mixed cation sulfates, phosphates, and chlorides−perchlorates−chlorates), and has minor TiO2 and Fe2O3T oxides (∼5 wt.%). Rietveld refinement yielded a monoclinic structural model for a well-crystalline tridymite, consistent with high formation temperatures. Terrestrial tridymite is commonly associated with silicic volcanism, and detritus from such volcanism in a “Lake Gale” catchment environment can account for Buckskin’s tridymite, cristobalite, feldspar, and any residual high-SiO2 glass. These cogenetic detrital phases are possibly sourced from the Gale crater wall/rim/central peak. Opaline silica could form during diagenesis from high-SiO2 glass, as amorphous precipitated silica, or as a residue of acidic leaching in the sediment source region or at Marias Pass. The amorphous mixed-cation salts and oxides and possibly the crystalline magnetite (otherwise detrital) are primary precipitates and/or their diagenesis products derived from multiple infiltrations of aqueous solutions having variable compositions, temperatures, and acidities. Anhydrite is post lithification fracture/vein fill.


2020 ◽  
Vol 13 (7) ◽  
pp. 147
Author(s):  
Yuta Otsuka ◽  
Yuiko Utsunomiya ◽  
Daiki Umeda ◽  
Etsuo Yonemochi ◽  
Yayoi Kawano ◽  
...  

This study aimed to investigate the effect of polymers and storage relative humidity on amorphous rebamipide (RB) and its solid dispersion phase transformation using chemometrics based on multiple datasets. The amorphous RB was prepared using particle mixture and grinding methods with hydroxypropyl cellulose, polyvinylpyrrolidone, and sodium dodecyl sulfate. Prepared amorphous RB and solid dispersion samples were stored under a relative humidity of 30% and 75% for four weeks. Infrared spectra of the dispersion samples suggested that the hydrogen bond network was constructed among quinolinone, carbonyl acid, and amide of RB and other polymers. The dataset combining near-infrared (NIR) spectra and powder X-ray diffractograms were applied to principal component analysis (PCA). The relationship between diffractograms and NIR spectra was evaluated using loadings and the PCA score. The multiple spectra analysis is useful for evaluating model amorphous active pharmaceutical ingredients without a standard sample.


Author(s):  
R. T. Owen ◽  
M. M. Madden ◽  
S. R. Bates

Using an SEM for quantitative analysis often requires intensity profiles along a single scan line. These profiles are usually obtained by either: 1) selecting a scan line from the CRT display, switching to Y-modulation and photographing the displayed intensity profile, or 2) scanning the negative of a photograph of the entire CRT display along a line using a microdensitometer. The first method requires additional measurements of the CRT beam deflection to get quantitative information, and thus has limited accuracy. The second method places another interface between the measurement and the detector signal.For SEMs or STEMs equipped for energy dispersive x-ray analysis with a multichannel analyzer (MCA) and minicomputer, modifications can be made to the circuitry to allow digital recording of line scan intensity data directly with the MCA.


Clay Minerals ◽  
2000 ◽  
Vol 35 (1) ◽  
pp. 291-302 ◽  
Author(s):  
S. Hillier

AbstractX-ray diffraction is used widely for quantitative analysis of geological samples but studies which document the accuracy of the methods employed are not numerous. Synthetic sandstones of known composition are used to compare a ‘routine application’ of a Rietveld and a reference intensity ratio (RIR) method of quantitative phase analysis. Both methods give similar results accurate to within ~±3 wt.% at the 95% confidence level. The high degree of accuracy obtained is believed to depend to a large extent on the spray-drying method of sample preparation used to eliminate preferred orientation.


MRS Advances ◽  
2018 ◽  
Vol 3 (34-35) ◽  
pp. 1969-1983 ◽  
Author(s):  
S.N. Panya panya ◽  
A.H. Galmed ◽  
M. Maaza ◽  
B.M. Mothudi ◽  
M. A. Harith ◽  
...  

AbstractLIBS is a developing analytical technique, which is used to perform qualitative and semi-quantitative elemental analysis of materials (solid, liquid and gas). Recently LIBS became an attractive technique to be used for geological samples, due to its advantages such as fast data collection and the lack of sample preparation. This study is done to improve analytical methods for geochemical analysis of samples during different exploration phases (Mining, filed analysis, etc.), to be used in the future as a real-time analysis method to save money and time spent in labs. In this work, LIBS has been used to differentiate between some geological samples gathered from different areas: South Africa and Namibia. Using principal component analysis (PCA), it was found that LIBS was able to differentiate between the samples even those of the same area. The results from the LIBS technique were correlated with subsequent analysis of the same samples by Particle-Induced X-ray emission (PIXE).


Author(s):  
H.J. Dudek

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S


Author(s):  
Brian Cross

A relatively new entry, in the field of microscopy, is the Scanning X-Ray Fluorescence Microscope (SXRFM). Using this type of instrument (e.g. Kevex Omicron X-ray Microprobe), one can obtain multiple elemental x-ray images, from the analysis of materials which show heterogeneity. The SXRFM obtains images by collimating an x-ray beam (e.g. 100 μm diameter), and then scanning the sample with a high-speed x-y stage. To speed up the image acquisition, data is acquired "on-the-fly" by slew-scanning the stage along the x-axis, like a TV or SEM scan. To reduce the overhead from "fly-back," the images can be acquired by bi-directional scanning of the x-axis. This results in very little overhead with the re-positioning of the sample stage. The image acquisition rate is dominated by the x-ray acquisition rate. Therefore, the total x-ray image acquisition rate, using the SXRFM, is very comparable to an SEM. Although the x-ray spatial resolution of the SXRFM is worse than an SEM (say 100 vs. 2 μm), there are several other advantages.


Author(s):  
John T. Armstrong

One of the most cited papers in the geological sciences has been that of Albee and Bence on the use of empirical " α -factors" to correct quantitative electron microprobe data. During the past 25 years this method has remained the most commonly used correction for geological samples, despite the facts that few investigators have actually determined empirical α-factors, but instead employ tables of calculated α-factors using one of the conventional "ZAF" correction programs; a number of investigators have shown that the assumption that an α-factor is constant in binary systems where there are large matrix corrections is incorrect (e.g, 2-3); and the procedure’s desirability in terms of program size and computational speed is much less important today because of developments in computing capabilities. The question thus exists whether it is time to honorably retire the Bence-Albee procedure and turn to more modern, robust correction methods. This paper proposes that, although it is perhaps time to retire the original Bence-Albee procedure, it should be replaced by a similar method based on compositiondependent polynomial α-factor expressions.


Sign in / Sign up

Export Citation Format

Share Document