Internal standard method utilized for 14 MeV neutron induced characteristic X-ray emission analysis

1989 ◽  
Vol 130 (1) ◽  
pp. 209-219 ◽  
Author(s):  
A. M. Barouni ◽  
L. Bakos ◽  
É. Zemplén-Papp
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.


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.


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.


2010 ◽  
Vol 177 ◽  
pp. 1-4
Author(s):  
Jian Peng Wu ◽  
Chun Yan Yao ◽  
Li Yun Cao ◽  
Jian Feng Huang ◽  
Hai Yan He ◽  
...  

In order to make quantitative analysis by internal standard method, 24 standard curves of inorganic compounds including quartz, corundum, TiO2, BaTiO3, etc. were obtained and the corresponding quantitative analyses were accomplished based on the quantitative analysis software attached in Rigaku D/Max-2200 X-Ray diffractometer. Results show that the coefficient of association R of the as-prepared curves are at the range of 0.928-0.980. By validating the samples with due content, it reveals that the analytical results are consistent with the actual values well, which indicate that the prepared standard curves are suitable for high-precision XRD phase quantitative analysis. Uniformity of samples is an important factor in the quantitative analysis by internal standard method.


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