Determination of the Relative Amounts of α-carbamazepine and β-carbamazepine in a Mixture by Powder X-Ray Diffractometry

1990 ◽  
Vol 5 (3) ◽  
pp. 155-159 ◽  
Author(s):  
Raj Suryanarayanan
Keyword(s):  
Weight Fraction ◽  
Preparation Technique ◽  
X Ray Diffraction ◽  
Experimental Conditions ◽  
X Ray ◽  
Sample Preparation Technique ◽  
Integrated Intensity ◽  
Diffraction Patterns ◽  
Good Agreement

AbstractA powder X-ray diffraction technique has been developed to quantify the relative amounts of α-carbamazepine (A) and β-carbamazepine (B) when they occur as a mixture. The theoretical basis of this technique was developed in 1948 by Alexander and Klug (Anal. Chem., 20:886-889). The powder X-ray diffraction patterns of A and B revealed that the line with d-spacing of 10.1 Å was unique to A. The ratio of the integrated intensity of the 10.1 Å line in a mixture of A and B, to the intensity of the 10.1 Å line in a sample consisting of only A, was calculated as a function of weight fraction of A in the mixture. These ratios were also experimentally determined, and there was a good agreement between the theoretical and experimental intensity ratios. The particle size of the samples, the sample preparation technique and the experimental conditions were controlled so as to eliminate the major sources of error in powder X-ray diffractometry. In order to minimize preferred orientation of the particles, a sample holder was specially fabricated.

Assessment of the X-ray diffraction–absorption method for quantitative analysis of largely amorphous pharmaceutical composites

2003 ◽  
Vol 36 (1) ◽  
pp. 74-79 ◽  
Author(s):  
P. Bergese ◽  
I. Colombo ◽  
D. Gervasoni ◽  
Laura E. Depero
Keyword(s):  
Weight Fraction ◽  
Toxic Waste ◽  
X Ray Diffraction ◽  
Amorphous Halo ◽  
Scanning Calorimetry ◽  
X Ray ◽  
The Matrix ◽  
Diffraction Patterns ◽  
Challenging Question

Determination of the residual weight fraction of a crystalline drug in a largely amorphous pharmaceutical composite is still a challenging question. None of the quantitative X-ray diffraction (QXRD) methods found in the literature is suitable for these inclusion systems. The composite's diffraction patterns present a structured amorphous halo (arising from the amorphous matrix and drug molecular clusters) in which the crystalline drug peaks rise up. Moreover, the matrix traps a non-negligible quantity of water (which cannot be directly detected by X-ray diffraction) and the crystal structure of the drug may be unknown. In this work, a development of the QXRD analysis based on the diffraction–absorption technique is presented. The method is standardless, avoids the interpretation of the amorphous halo and the knowledge of the crystal structures of the phases, and takes into account the absorbed water. Results are in excellent agreement with those obtained by differential scanning calorimetry (DSC). The general features of the technique open its application to other classes of largely amorphous composite materials, like glass systems generated in the stabilization/solidification of toxic waste.

Automatic determination of diffuse-peak positions and the centre of a diffraction pattern

1999 ◽  
Vol 32 (2) ◽  
pp. 332-335 ◽  
Author(s):  
S. J. Wilkinson ◽  
D. W. L. Hukins
Keyword(s):  
Annulus Fibrosus ◽  
Gaussian Function ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oriented Molecules ◽  
Beam Stop ◽  
Diffraction Patterns ◽  
Good Agreement

Correlation with a two-dimensional Gaussian function was used to locate the positions of diffuse peaks in X-ray diffraction patterns. The centre of a pattern was defined as the centroid of the image of the undeflected beam, found by convolution with a two-dimensional Gaussian function. These methods were implemented using the IDL programing language. They were tested on diffraction patterns from systems containing oriented molecules of the protein collagen: collagen tape, elastoidin spicules and annulus fibrosus of intervertebral disc. Specimens were dusted with quartz to calibrate the diffraction patterns. These patterns were recorded on film, using a semi-transparent beam stop to obtain an image of the undeflected beam, and digitized at a resolution of 105 µm. Intermolecular spacings, calculated from the distance between a peak and the centre of a pattern, were in good agreement with those determined previously.

scholarly journals Born out of Fire and Ice: Polymorph Studies of the Antiviral Famciclovir

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Variable Temperature ◽  
Chemical Properties ◽  
Crystal Form ◽  
X Ray Diffraction ◽  
Crystal Forms ◽  
X Ray ◽  
Physical Chemical ◽  
Diffraction Patterns ◽  
Crystalline Forms

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.

Evaluation of Reference X-ray Diffraction Patterns in the ICDD Powder Diffraction File

1990 ◽  
Vol 34 ◽  
pp. 369-376
Author(s):  
G. J. McCarthy ◽  
J. M. Holzer ◽  
W. M. Syvinski ◽  
K. J. Martin ◽  
R. G. Garvey
Keyword(s):  
Powder Diffraction ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
Cd Rom ◽  
X Ray ◽  
Binary Oxides ◽  
Diffraction Patterns ◽  
Input Format ◽  
Good Agreement

AbstractProcedures and tools for evaluation of reference x-ray powder patterns in the JCPDSICDD Powder Diffraction File are illustrated by a review of air-stable binary oxides. The reference patterns are evaluated using an available microcomputer version of the NBS*A1DS83 editorial program and PDF patterns retrieved directly from the CD-ROM in the program's input format. The patterns are compared to calculated and experimental diffractograms. The majority of the oxide patterns have been found to be in good agreement with the calculated and observed diffractograms, but are often missing some weak reflections routinely observed with a modern diffractometer. These weak reflections are added to the PDF pattern. For the remainder of the phases, patterns are redetermined.

scholarly journals Synthesis of the Modifications of Ca2SiO4 and the Determination of their Powder X-ray Diffraction Patterns

1963 ◽  
Vol 71 (806) ◽  
pp. 63-68 ◽  
Author(s):  
Goro YAMAGUCHI ◽  
Yoshio ONO ◽  
Shigeo KAWAMURA ◽  
Yoshiaki SODA
Keyword(s):  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Patterns
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