scholarly journals Rietveld Method Applied for Triacylglycerol Polymorphism Analysis

2014 ◽  
Vol 70 (a1) ◽  
pp. C1764-C1764
Author(s):  
Guilherme Calligaris ◽  
Ana Paula Ribeiro ◽  
Adenilson dos Santos ◽  
Lisandro Cardoso
Keyword(s):  
Rietveld Method ◽  
Rietveld Analysis ◽  
Polymorphic Form ◽  
Polymorphism Analysis ◽  
X Ray Diffraction ◽  
Full Characterization ◽  
Β Phase ◽  
Lack Of Information ◽  
Refinement Method

The characterization of the fat components becomes very useful in the formulation of shortening, margarines and fatty products due to their unique properties of plasticity, texture, solubility and aeration. The qualitative analysis obtained by X-ray diffraction (XRD) can be further improved in order to fulfill the lack of information on the triacylglycerol (TAG) in the hardfat systems aiming a complete polymorph characterization. In this work, as an attempt to quantify the distinct β and β' TAG polymorphs, XRD was combined with Rietveld refinement method and applied to two types of samples: mixtures (M) and blended hardfats (B) samples involving fully hydrogenated of soybean (FHSO) and palm (FHPO) oils. M-samples were prepared with linear concentrations of FHSO (β) and FHPO (β') and their Rietveld analysis have provided the expected content trend through the involved polymorphic phases with a very good agreement (~5%). This result validates the Rietveld method applicability on this kind of materials. The Rietveld method applied for B-samples has shown that β' polymorphic form prevails over the β-form, even for samples originally prepared with FHSO (β)/FHPO (β') = 60/40 ratio (see figure). This result indicates the influence of the seeding process (earlier crystallization of β' phase). This first quantitative approach for blended samples represents a very useful contribution towards the full characterization of fats.

scholarly journals A Versatile Approach to Access Trimetallic Complexes Based on Trisphosphinite Ligands

Molecules ◽  
2020 ◽  
Vol 25 (3) ◽  
pp. 593
Author(s):  
Juan Miranda-Pizarro ◽  
Macarena G. Alférez ◽  
M. Dolores Fernández-Martínez ◽  
Eleuterio Álvarez ◽  
Celia Maya ◽  
...  
Keyword(s):  
Coordination Chemistry ◽  
Late Transition Metal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Full Characterization ◽  
Metal Precursors ◽  
Straightforward Method ◽  
One Step ◽  
Late Transition

A straightforward method for the preparation of trisphosphinite ligands in one step, using only commercially available reagents (1,1,1-tris(4-hydroxyphenyl)ethane and chlorophosphines) is described. We have made use of this approach to prepare a small family of four trisphosphinite ligands of formula [CH3C{(C6H4OR2)3], where R stands for Ph (1a), Xyl (1b, Xyl = 2,6-Me2-C6H3), iPr (1c), and Cy (1d). These polyfunctional phosphinites allowed us to investigate their coordination chemistry towards a range of late transition metal precursors. As such, we report here the isolation and full characterization of a number of Au(I), Ag(I), Cu(I), Ir(III), Rh(III) and Ru(II) homotrimetallic complexes, including the structural characterization by X-ray diffraction studies of six of these compounds. We have observed that the flexibility of these trisphosphinites enables a variety of conformations for the different trimetallic species.

Quantitative Characterization of Hydration of Cement Pastes by Rietveld Phase Analysis and Thermoanalysis

2013 ◽  
Vol 539 ◽  
pp. 19-24 ◽  
Author(s):  
Yong Qi Wei ◽  
Wu Yao
Keyword(s):  
Phase Analysis ◽  
Cement Paste ◽  
Rietveld Method ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Quantitative Characterization ◽  
Cement Pastes ◽  
Hydration Mechanism ◽  
Spot Check

The quantitative characterization of hydration of cement pastes has always been one of focuses of researchers’ attention. Rietveld phase analysis (RPA), a combination of quantitative X-ray diffraction (QXRD) and the Rietveld method, supplies a tool of an enormous potential for that. Although a few of related researches were conducted by RPA, the reported attention was not paid to the neat cement paste with a low w/c ratio. Therefore, this work aimed at the quantitative study on hydration of such a cement paste chiefly by this method, meanwhile, cooperated with the hyphenated technique of thermogravimetry with differential scanning calorimetry (TG-DSC), as a spot check. Results indicated that RPA was a reliable method in quantitatively characterizing hydration of cement pastes, and gave a clear decription of evolution of all main crystal phases in cement pastes; and that the evolution of monosulphate(Afm_12) was also able to be tracked quantitatively. This will help to understand better the hydration mechanism of cement pastes, as well as to investigate quantitatively effects of mineral and chemical admixtures on hydration of composite cementitious systems.

scholarly journals Characterization of hydrochlorothiazide in solid formulations

2015 ◽  
Vol 30 (S1) ◽  
pp. S127-S130
Author(s):  
Simone T. B. de Salvi ◽  
Diego Luiz Tita ◽  
Carlos de O. Paiva-Santos ◽  
Selma G. Antonio
Keyword(s):  
Rietveld Method ◽  
Package Insert ◽  
Polymorphic Form ◽  
Crystalline Form ◽  
Active Principle ◽  
Lauryl Sulfate ◽  
X Ray ◽  
Lactose Monohydrate ◽  
Solid State Characterization

Hydrochlorothiazide (HCTZ) is a diuretic used for the treatment of blood pressure (hypertension). HCTZ has two anhydrous polymorphs denoted as Forms I and II. Aiming at solid-state characterization, X-ray powder diffraction (XRPD) is known to be a powerful technique which has been successfully applied in investigating polymorphism in medicines. In this work, three tablets of HCTZ (a reference and two generic) were analyzed. The data were collected using Rigaku RINT2000 diffractometer copper rotate anode. The Rietveld method (RM) was applied for the characterization of HCTZ polymorphic form. For the crystalline excipients where the crystal structure is known, their phases were identified by the RM either. The results showed that all the tablets exhibit Form I of HCTZ, while the excipient lactose monohydrate is found to exhibit the crystalline form. One of the generics is also found to exhibit the excipient sodium lauryl sulfate (SLS) in the crystalline form. Therefore, the RM and XRPD are an efficient methodology for characterization of the crystalline Form I of the active principle of HCTZ and crystalline excipients lactose monohydrate and SLS in solid formulations. It is also interesting to observe excipients not described in the package insert of the medicament.

CONTROLLED SYNTHESIS AND CHARACTERIZATION OF TiO2 NANOPARTICLES VIA A SOL–GEL METHOD

2004 ◽  
Vol 03 (06) ◽  
pp. 749-755 ◽  
Author(s):  
YING LI ◽  
SUO HON LIM ◽  
TIM WHITE
Keyword(s):  
Sol Gel ◽  
Critical Role ◽  
Rietveld Analysis ◽  
Nanocrystalline Powders ◽  
X Ray Diffraction ◽  
Gelation Temperature ◽  
Gel Method ◽  
Sol Gel Method ◽  
Transmission Electron

The properties influencing the photocatalytic activity of TiO 2 particles have been suggested to include the surface area, crystallinity, crystallite size and crystal structure. Therefore, manipulation of the microstructure of titania, especially of nanocrystalline powders, is very important in the preparative process. In this study, nanocrystalline TiO 2 powders with controlled particle size and phase composition were synthesized at low temperature (<80°C) by a modified sol–gel method. The effects of gelation temperature were systematically investigated. It was found that this parameter played a critical role in determining the crystallinity of single phase anatase. With increasing gelation temperature, the crystallinity of anatase improved initially and then decreased if the temperature was raised to 80°C. These nanomaterials were characterized comprehensively by powder X-ray diffraction (including Rietveld analysis), high-resolution transmission electron microscopy, DSC/TGA thermal analysis and UV–Vis spectrometry.

The Synthesis of Ce-Filled CoSb3 and Characterization of its Magnetic and Structural Properties

2003 ◽  
Vol 793 ◽  
Author(s):  
Arwyn L. E. Smalley ◽  
Brandon Howe ◽  
David C. Johnson
Keyword(s):  
Low Temperatures ◽  
Magnetic Measurements ◽  
Rietveld Analysis ◽  
X Ray Diffraction ◽  
Electrical Measurements ◽  
X Ray ◽  
Ferromagnetic Component ◽  
Phase Pure ◽  
Powder Samples

ABSTRACTA series of cerium-containing CoSb3 samples were synthesized, with cerium quantities varying from 0 to 2 stoichiometric equivalents. These samples were annealed at low temperatures to crystallize the kinetically stable phases CexCo4Sb12 (x = 0–0.5). X-ray diffraction showed that these samples were phase pure, and Rietveld analysis on x-ray diffraction data from powder samples indicated that these samples were 25–88% crystalline. Electrical measurements showed that these samples are n-type, which was previously unknown in CexCo4Sb12. Magnetic measurements showed that the samples were paramagnetic due to the cerium being incorporated into the diamagnetic CoSb3 compound. In addition, they contained a ferromagnetic component that was attributed to the amorphous, cerium-containing phase.

Structure Characterization of Sulfate and Oxysulfate Phases Formed During Sulfuric Acid Digestion of Ilmenites

1996 ◽  
Vol 49 (7) ◽  
pp. 801 ◽  
Author(s):  
IE Grey ◽  
MR Lanyon ◽  
R Stranger
Keyword(s):  
Sulfuric Acid ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Structure Characterization ◽  
Acid Digestion ◽  
X Ray Diffraction ◽  
Titanium Sulfate ◽  
Structural Relationships ◽  
Concentrated Sulfuric Acid

Laboratory digestion of natural and upgraded ilmenites with concentrated sulfuric acid has been carried out under conditions simulating the sulfate-route pigment process. X-Ray diffraction studies on the solid digestion cakes led to the characterization of a number of different iron titanium sulfate and oxysulfate compounds, whose formation was dependent on the ilmenite composition and digestion conditions. Two different sulfate phases were identified, with structures related to those for Fe2(SO4)3 and H2O[ Zr (HPO4)2]. Four different iron titanium oxysulfates , ( Fe,Ti )(O,OH)SO4, were identified as major digestion products, three having structures related to those for β-NbOPO4, GeOHPO4 and lazulite , Mg[AlOHPO4], and the fourth being a new struture type. The structures of the oxysulfate phases were refined by the Rietveld method. Both the sulfates and the oxysulfates have three-dimensional framework structures formed by corner linking of ( Ti,Fe )O6 octahedra and SO4 tetrahedra, and containing channels or interlayer regions that can be occupied by cations such as H3O+ and Fe2+. The different structures have many features in common. Their structural relationships are discussed and mechanisms are proposed for the phase transformations encountered in the digestion studies.

Structure of Carbonated Hydroxyapatite Based on Rietveld Method

2008 ◽  
Vol 368-372 ◽  
pp. 1187-1189
Author(s):  
Xu Ran ◽  
Jun Guo Ran ◽  
Li Gou ◽  
Ji Yong Chen ◽  
Jiao Min Luo
Keyword(s):  
Crystal Structure ◽  
Sintering Temperature ◽  
Rietveld Method ◽  
Rietveld Analysis ◽  
Structure Parameters ◽  
X Ray Diffraction ◽  
Carbonated Hydroxyapatite ◽  
X Ray ◽  
Quantitative Results ◽  
Distortion Index

The crystalline structures of B-type carbonated hydroxyapatite (CHA) powders sintered at 700, 900 and 1100°C, respectively, were studied by Rietveld analysis of powder X-ray diffraction (XRD) data. A series of structure parameters, including lattice parameters (a and c), bond length and the distortion index of PO4 tetrahedron (Dind) were calculated by Rietveld method to characterize the fine structure of CHA. The broadening effect of XRD reflections was separated to calculate the micro-strain and crystalline size. The results showed that CHA become more stable with the increase of sintering temperature, but the CO3 2- is almost lost at temperature of 1100°C. The quantitative results about crystal structure of CHA based on crystalline structure simulated by Rietveld method are obtained.

scholarly journals Study of selection and purification of Brazilian bentonite clay by elutriation: a XRF, SEM and Rietveld analysis

Cerâmica ◽  
2016 ◽  
Vol 62 (361) ◽  
pp. 1-8 ◽  
Author(s):  
J. L. Alves ◽  
A. E. Zanini ◽  
M. E. de Souza ◽  
M. L. F. Nascimento
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Rietveld Method ◽  
Bentonite Clay ◽  
Rietveld Analysis ◽  
Industrial Applications ◽  
X Ray Diffraction ◽  
X Ray ◽  
Almost All ◽  
Scanning Electron

Abstract Clays obtained from nature have a lot of impurities. Therefore, for best using of these materials, it is necessary its selection and purification. Thus, the aim of this work is to separate and to purify the smectite fractions using water as a solvent at a low flux mixed with a bentonite clay extracted from a mine in Vitória da Conquista - Bahia / Brazil. For this a separation method of fractions of expandable clays based on the Stokes' Law was applied - this process is called elutriation, in order to ensure and to expand possible industrial applications of this material. The samples were characterized by analysis of X-ray diffraction, X-ray fluorescence and scanning electron microscopy. The Rietveld method enabled the quantification of main phase minerals: montmorillonite, kaolinite, nontronite and quartz, reaching 85% in mass of montmorillonite phase at the end of the process. Results showed that the method used was efficient to remove almost all quartz, carbonates and organic matter from the sample. It was also observed a monomodal grain size distribution of elutriated materials with thinner grains, around (18.1 ± 1.8) μm at the end of the process. It has been concluded that the method developed and applied showed promising characters to be applied to elutriate kilograms of clays and could be used in industrial scale.

A semi-empirical asymmetry function for X-ray diffraction peak profiles

1995 ◽  
Vol 10 (3) ◽  
pp. 204-206 ◽  
Author(s):  
P. Riello ◽  
P. Canton ◽  
G. Fagherazzi
Keyword(s):  
Goodness Of Fit ◽  
Rietveld Method ◽  
Rietveld Analysis ◽  
Opening Angle ◽  
X Ray Diffraction ◽  
X Ray ◽  
Asymmetry Function ◽  
The Asymmetry ◽  
Fit Index ◽  
Semi Empirical

A new semi-empirical approximation for the asymmetry function to be used in the X-ray Rietveld analysis has resulted in lower values of the so-called goodness-of-fit index, defined as S = Rwp/Rexp, where Rwp is the R-weighted pattern and Rexp is the R-expected [R. A. Young, The Rietveld Method (Oxford U.P., Oxford, 1993)], with respect to the corresponding values obtained with the classical approximation used by Rietveld in his fundamental paper. A comparing test of the two asymmetry functions was carried out for the cubic Y2O3 and for αAl2O3 using either pseudo-Voigt or Pearson VII symmetrical functions and two diffractometers. As in the case of the Rietveld approximation, the present one, which employs an exponential function, is optimized using only one fitting parameter. Experimentally, the asymmetry can be considerably diminished by using Soller slits with a small opening angle (≤2°).

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