Quantitative X-ray diffraction analysis of urinary calculi by use of the internal-standard method and reference intensity ratios.

1988 ◽  
Vol 34 (2) ◽  
pp. 289-293 ◽  
Author(s):  
M A Wandt ◽  
A L Rodgers
Keyword(s):  
Standard Method ◽  
Urinary Calculi ◽  
Internal Standard ◽  
Xrd Analysis ◽  
Internal Standard Method ◽  
X Ray Diffraction ◽  
Stone Composition ◽  
X Ray ◽  
Intensity Ratios

Abstract The internal-standard method and the powder diffractometer have been applied here to the quantitative determination of urinary stone constituents by x-ray diffraction (XRD). Reference intensity ratios determined for six stone substances were used in the reduction of intensity data. Constituent concentrations calculated for 21 stones were compared with values obtained from an element-sensitive technique. We conclude that XRD analysis alone cannot be regarded as a routine technique for the quantitative characterization of uroliths, but that semiquantitative XRD analysis supplemented by accurate quantitative elemental data is more suitable for the precise determination of true stone composition.

X-Ray Fluorescence Spectrometric Determination of Rare Earths in Plutonium

1968 ◽  
Vol 22 (5) ◽  
pp. 434-437 ◽  
Author(s):  
E. A. Hakkila ◽  
R. G. Hurley ◽  
G. R. Waterbury
Keyword(s):  
Rare Earths ◽  
Internal Standard ◽  
Internal Standard Method ◽  
X Rays ◽  
Measured Intensity ◽  
X Ray ◽  
Low Concentrations ◽  
Relative Standard ◽  
Intensity Ratios

Two methods were evaluated for determining rare earths in plutonium: (1) For the lighter rare earths ( Z≦66), or low concentrations of the heavier rare earths, an adjacent rare earth was added as a carrier and also as an internal standard, the rare earths were separated from plutonium by fluoride precipitation, and the measured intensity ratios for the sample and for solutions having known concentrations were compared. The Lβ1 x-rays were measured for the lighter rare earths and the Lα1 x rays for the remaining lanthanides. (2) For the heavier rare earths ( Z>66), the Lα1 x-ray intensities were measured from a nitric acid solution of the sample and compared to intensities obtained for solutions having known concentrations. The minimum concentrations that could be measured with a relative standard deviation no greater than 4% by the separation internal standard method varied from approximately 0.5% for lanthanum to 0.01% for lutetium. The direct measurement of x-ray intensity was much less sensitive. Applicability of the methods was shown by successful analyses of plutonium alloys containing dysprosium, thulium, or lutetium.

Quantitative X-Ray Diffraction Analysis of Anhydrous and Hydrated Portland Cement - Part 2: Computer-Based Methods

2015 ◽  
Vol 1087 ◽  
pp. 498-503 ◽  
Author(s):  
Duong D. Nguyen ◽  
Liam Devlin ◽  
Pramod Koshy ◽  
Charles C. Sorrell
Keyword(s):  
Portland Cement ◽  
Rietveld Method ◽  
Internal Standard ◽  
Xrd Analysis ◽  
Internal Standard Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
External Standard ◽  
Computer Based ◽  
General Aspects

The present work reviews current practices in quantitative XRD analysis of anhydrous and hydrated Portland cement. While Part 1 of this two-part work reviews the conventional internal standard method and the reference intensity ratio (RIR) method, Part 2 reviews the more commonly used computer-based methods, which include the Rietveld method (with or without internal standard) and the G-factor method (with external standard). Further, some critical general aspects of the experimental procedures that affect the accuracy of the analysis are discussed.

X-ray methods for quantitative determination of inorganic fillers in paper

1985 ◽  
Vol 63 (1) ◽  
pp. 243-248 ◽  
Author(s):  
Terry L. Bluhm ◽  
Arthur Y. Jones ◽  
Yves Deslandes
Keyword(s):  
Standard Method ◽  
Empirical Evaluation ◽  
Internal Standard ◽  
Diffraction Method ◽  
Internal Standard Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intensity Measurements ◽  
Commercial Paper ◽  
Ray Methods

X-ray diffraction methods have been investigated as means of quantifying filler contents of paper. Both an "internal standard method" and an "absorption–diffraction method" were applied. Because of preferential orientation of the filler particles in commercial paper samples, the "internal standard method" was modified to include an empirical evaluation of the proportionality constant, K. Values of K specific for each filler material investigated (clay, calcite, talc, and titanium dioxide) were obtained by X-ray diffraction intensity measurements on standard papers containing different amounts of each filler. These values of K were then used to calculate the filler content of various commercial papers. The filler contents of these same commercial papers were also determined using the X-ray "absorption–diffraction method" and ash determination. Comparisons made among results from all these methods indicated that both X-ray methods give acceptable agreement with ash determination, but that the "absorption–diffraction method" is preferred due to its ease of application. In addition, the X-ray methods are more rapid and versatile than ash determination.

Quantitative X-Ray Diffraction Analysis of Anhydrous and Hydrated Portland Cement – Part 1: Manual Methods

2015 ◽  
Vol 1087 ◽  
pp. 493-497 ◽  
Author(s):  
Duong D. Nguyen ◽  
Liam Devlin ◽  
Pramod Koshy ◽  
Charles C. Sorrell
Keyword(s):  
Portland Cement ◽  
Building Materials ◽  
Internal Standard ◽  
Mineralogical Composition ◽  
Xrd Analysis ◽  
Internal Standard Method ◽  
X Ray Diffraction ◽  
Accurate Analysis ◽  
Cement Pastes ◽  
X Ray

Portland cement is one of most important construction and building materials and its properties depend strongly on the mineralogical composition. Consequently, accurate analysis of the mineralogical composition of anhydrous Portland cement is crucial for both product quality control and optimisation of performance following initial hydration. In the latter sense, analysis of the mineralogical composition of hydrated Portland cement paste is critical to understand (1) the mechanism and kinetics of hydration of unmodified pastes and those modified with additives and (2) the resultant properties of cement pastes, mortars, and concretes. Such analyses typically are undertaken by quantitative X-ray diffraction (XRD).The present work reviews current practices in quantitative XRD analysis of anhydrous and hydrated Portland cement. To this end, Part 1 of this two-part work briefly mentions the point-counting method and the Bogue calculation method. The more commonly applied internal standard method and reference intensity ratio (RIR) method are discussed in more detail.

Determination of alcohols in mixtures by 19F NMR spectroscopy using hexefluoroacetone reagent

1982 ◽  
Vol 47 (7) ◽  
pp. 1973-1978 ◽  
Author(s):  
Jiří Karhan ◽  
Zbyněk Ksandr ◽  
Jiřina Vlková ◽  
Věra Špatná
Keyword(s):  
Standard Deviation ◽  
Nmr Spectroscopy ◽  
Standard Method ◽  
Internal Standard ◽  
Internal Standard Method ◽  
Concentration Region ◽  
Experimental Conditions ◽  
Curve Method ◽  
Sample Preparation Procedure

The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.

scholarly journals An Insight into Chemistry and Structure of Colloidal 2D-WS2 Nanoflakes: Combined XPS and XRD Study

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Xrd Analysis ◽  
Crystal Habit ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
X Ray ◽  
Morphological Evaluation ◽  
Rational Understanding ◽  
Structural Inspection

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.

Crystallization of simonkolleite (Zn5Cl2(OH)8 ∙ H2O) in powder samples prepared for mineral composition analysis by quantitative X-ray diffraction (QXRD)

Nafta-Gaz ◽  
2021 ◽  
Vol 77 (5) ◽  
pp. 293-298
Author(s):  
Urszula Zagórska ◽  
◽  
Sylwia Kowalska ◽  
Keyword(s):  
Quantitative Analysis ◽  
Internal Standard ◽  
Mineralogical Composition ◽  
Hydrocarbon Exploration ◽  
Composition Analysis ◽  
Internal Standard Method ◽  
X Ray Diffraction ◽  
Method Error ◽  
X Ray ◽  
Significant Difference

The analysis of mineralogical composition by quantitative X-ray diffraction (QXRD) is one of the standard research methods used in hydrocarbon exploration. In order to improve it and to obtain better results, the methodology of quantitative analysis used at Well Logging Department is being periodically (more or less) modified. After the introduction of the improvements, comparative analyses were performed on archival samples. Reflections from an unidentified phase which did not occur in the tested Rotliegend sandstone samples were noticed on X-ray diffractograms of archival samples. Reflections of a mineral called simonkolleite were identified in the X-ray diffraction database. Chemically it is a hydrated zinc chloride of the formula: Zn5Cl2(OH)8 × H2O. Analysis of the composition of samples in which simonkolleite crystallised, indicated that the mineral is being formed in the result of the slow reaction of zinc oxide with halite (NaCl) and water vapour. An attempt was made to determine the influence of the presence of this mineral on the results of the quantitative analysis of mineralogical composition. The above methodology was applied on a group of ten samples. The results of the quantitative analysis conducted for archival samples stored with added zincite standard containing simonkolleite and for new, freshly grinded (without artifact) samples were compared. The comparison of the obtained results showed a slight influence of this mineral on the quantitative composition of the remaining components. The difference between the results usually did not exceed the method error. At the same time a significant difference in the calculated content of the internal standard was noted – on average 1% less in archival than in new samples. This shows that the reaction occurring in the archival samples will affect the evaluation of the quality of the obtained quantitative analysis, at the same time excluding the possibility of determining the rock’s amorphous substance content with the internal standard method.

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