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

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.

1988 ◽  
Vol 34 (2) ◽  
pp. 289-293 ◽  
Author(s):  
M A Wandt ◽  
A L Rodgers

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.


Nafta-Gaz ◽  
2021 ◽  
Vol 77 (5) ◽  
pp. 293-298
Author(s):  
Urszula Zagórska ◽  
◽  
Sylwia Kowalska ◽  

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.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1096-C1096
Author(s):  
Ana Cuesta ◽  
Gema Alvarez Pinazo ◽  
Angeles De la Torre ◽  
Susana Sanfélix ◽  
Inmaculada Peral ◽  
...  

XRPD is a powerful tool for material characterization in general, and for in-situ studies of chemical processes in particular. The use of an intense X-ray source, .i.e. synchrotron X-rays, coupled with fast X-ray detection permits time-resolved diffraction experiments allowing in-situ quantitative phase analysis during the early ages of cement hydration. Calcium sulfoaluminate, CSA, cements may have variable compositions, but all of them contain high amounts of ye'elimite, Ca4Al6O12SO4. Commercial CSA cements have special applications such as high strength developments at early-ages. Ye'elimite is very reactive and most of its hydration heat is released during the first eight hours of hydration . The aim of this work is to better understand the early age hydration of stoichiometric (orthorhombic) and doped (pseudo-cubic) ye'elimite samples. The parameters studied by SXRPD, LXRPD and calorimetry have been: polymorphism; water/ye'elimite ratio; and sulfate (gypsum and anhydrite) contents. This work has allowed establishing mechanisms and kinetics for hydration of ye'elimite samples by in-situ SXRPD with internal standard methodology. Moreover, pastes were also studied by ex-situ LXRPD with the external standard method, G-factor, at 2 and 7 days. Both strategies were able to quantify the amorphous contents, including free water. It is important to highlight that the results obtained at early ages, by the internal standard method, are in agreement with those obtained at later ages, G-method, showing the consistence and complementarity of both methodologies. The hydration of stoichiometric ye'elimite in the presence of gypsum is strongly hastened, when compared to the hydration process without gypsum. However, the presence of gypsum has a little effect in the hydration of doped ye'elimite. Moreover, anhydrite has also accelerated the hydration of stoichiometric ye'elimite, although its lower solubility has provoked the formation of an intermediate phase in the first hours.


1985 ◽  
Vol 49 (353) ◽  
pp. 531-538 ◽  
Author(s):  
Covadonga Brime

AbstractAn X-ray diffraction method has been successfully applied to the quantitative determination of mineral mixtures. The absorptive properties of the samples and the number of components determine the analytical procedure to be used. The methods described (external standard plus empirical determination of the mass attenuation coefficient) provides an accurate and rapid alternative to the direct measurement of the mass attenuation, Compton diffusion or internal standard methods. The relative accuracy obtained is of the order of 10% at the 0.1% level, independent of the sample composition.


1992 ◽  
Vol 7 (4) ◽  
pp. 186-193 ◽  
Author(s):  
Robert L. Snyder

AbstractEach of the RIR based methods for carrying out quantitative X-ray powder diffraction analysis are described and a consistent set of notation is developed. The so called “standardless” analysis procedures are shown to be a special case of the internal-standard method of analysis where the normalizing assumption is used. All analytical methods, other than the Rietveld whole pattern matching procedure, require the use of explicitly measured standards, typically in the form of RIR values. However, if only semi-quantitative results can be tolerated, the standards may be obtained by using published RIR and relative intensity values. The exciting new techniques of whole pattern fitting and Rietveld constrained quantitative analysis are also described in RIR notation and shown also to be forms of the internal-standard method with the normalization assumption. The quantitative results obtained from Rietveld quantitative analysis are derived from computed standards in the form of computed, normalized, RIRN values. The normalization assumption in Rietveld analysis allows the exclusive use of computed standards and comes as close to a “standardless” analysis as one can achieve: relying on the absence of amorphous material and on the validity of the structural models. Relationships are given for obtaining quantitative analysis from these RIRN values obtainable from the least-squares scale factors.


2015 ◽  
Vol 1087 ◽  
pp. 498-503 ◽  
Author(s):  
Duong D. Nguyen ◽  
Liam Devlin ◽  
Pramod Koshy ◽  
Charles C. Sorrell

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.


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