Identification of Different Crystalline Forms of Diatrizoic Acid

1978 ◽  
Vol 61 (1) ◽  
pp. 72-75
Author(s):  
Victor A Folen ◽  
George Schwartzman ◽  
Millard Maienthal ◽  
Wilson L Brannon

Abstract Standard reference samples of diatrizoic acid gave 2 different infrared (IR) spectra, x-ray diffraction patterns, and differential thermal and thermal gravimetric curves. One form, the anhydrous acid, shows no weight loss when heated to 170°C. The other form, the dihydrate, loses 5.36% of its weight when heated from 86 to 144°C. The anhydrous diatrizoic acid is the preferred reference standard, because it has an IR spectrum and x-ray diffraction pattern suitable for identification purposes.

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch

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.


1999 ◽  
Vol 14 (6) ◽  
pp. 2644-2654 ◽  
Author(s):  
F. Rajabalee ◽  
V. Métivaud ◽  
D. Mondieig ◽  
Y. Haget ◽  
M. A. Cuevas-Diarte

X-ray diffraction analyses of the pure components n-tricosane and n-pentacosane and of their binary mixed samples have enabled us to characterize the crystalline phases observed at “low temperature.” Contrary to what was announced in literature on the structural behavior of mixed samples in odd-odd binary systems with Δn = 2, the three domains are not all orthorhombic. This work has enabled us to show that two of the domains are, in fact, monoclinic (Aa, Z = 4), and the other one is orthorhombic (Pca21, Z = 4). The conclusions drawn in this work can easily be transposed to other binary systems of n-alkanes.


Detailed interpretations of the X -ray diffraction patterns of fibres and sheets of 66 and 6.10 polyamides (polyhexam ethylene adipamide and sebacamide respectively) are proposed. The crystal structures of the two substances are completely analogous. Fibres of these two polyam ides usually contain two different crystalline forms, α and β, which are different packings of geometrically similar molecules; most fibres consist chiefly of the α form. In the case of the 66 polymer, fibres have been obtained in which there is no detectable proportion of the β form. Unit cell dimensions and the indices of reflexions for the α form were determined by trial, using normal fibre photographs, and were checked by using doubly oriented sheets set at different angles to the X -ray beam. The unit cell of the a form is triclinic, with a — 4·9 A, b = 5·4 A, c (fibre axis) = 17·2A, α = 48 1/2º, β = 77º, γ = 63 1/2º for the 66 polymer; a = 4·95A, b = 5·4A, c (fibre axes) = 22·4A, α = 49º, β = 76 1/2º, γ = 63 1/2º for the 6.10 polymer. One chain molecule passes through the cell in both cases. Atomic coordinates in occrystals were determined by interpretation of the relative intensities of the reflexions. The chains are planar or very nearly so; the oxygen atoms appear to lie a little off the plane of the chain. The molecules are linked by hydrogen bonds between C = 0 and NH groups, to form sheets. A simple packing of these sheets of molecules gives the α arrangement.


1987 ◽  
Vol 2 (3) ◽  
pp. 176-179 ◽  
Author(s):  
G. Wilson ◽  
F. P. Glasser

AbstractA systematic survey of phase formation in the Na2O-ZrO2-SiO2 system has revealed inconsistencies in the number and identity of ternary phases, and of their X-ray powder data. The phases Na2ZrSiO5, Na4Zr2Si3O12, Na2ZrSi2O7 and Na2ZrSi4O11 were prepared by solid-state reaction and their experimental X-ray diffraction patterns measured. Calculated X-ray diffraction patterns were generated by computer, using published crystallographic data, and critically compared with the experimentally observed values. The unit-cell constants were redefined to a greater accuracy than the presently accepted values published in the Powder Diffraction File. Only Na4Zr2Si3O12 produced an X-ray diffraction pattern which agreed with that previously published; those from the other phases were significantly different in both the intensities and positions of the reflections. Data for synthetic Na2ZrSi4O11 identical to the mineral vlasovite are reported.


2014 ◽  
Vol 955-959 ◽  
pp. 2824-2830 ◽  
Author(s):  
Yong Feng Xiao ◽  
Bao Dong Wang ◽  
Xiao Ting Liu ◽  
Xiao Huan Wang ◽  
Li Jun Zhao ◽  
...  

In this paper, the de-silicated fly ash (DSFA) was sintered with soda and calcium oxide. Detailed analysis and characterization was carried out by using thermal gravimetric analysis (TGA) and X-ray diffraction (XRD). Two dominant reactions take place in the sintering process. The kinetics was studied by using Jander mode, and the sintering activation energies were determined based on the weight loss of CO2.


1960 ◽  
Vol 4 ◽  
pp. 175-193 ◽  
Author(s):  
Norman F. H. Bright

AbstractX-ray diffraction studies have revealed that a titanium oxide with an NaCl-type structure is stable over a wide range of nonstoichiometric compositions, both above and below the 1:1 Ti/O atomic ratio. Attempts to prepare a strictly stoichiometric TiO as a single phase have revealed a marked tendency for such a composition to disproportionate into two nonstoichiometric “TiO”-type structures of variable composition, whereas nonstoichiometric compositions can be readily prepared under similar conditions as single, well-crystallized phases.The oxide Ti3O5, which forms a constituent of the titanium-bearing slags produced in ilmenite smelting, has been prepared as a pure compound in two different crystalline forms, both monoclinic in structure, but one being very close to the orthorhombic pseudobrookite, Fe2O3 · TiO2, or ferrous dititanate, FeO · 2TiO2 structure. This “dititanate” form inverts to the other monoclinic form at high temperatures. Single crystals of the latter monoclinic form are readily made. The studies of the “dititanate” form have been restricted to powder diffraction work, since it inverts to the other form after melting. The two forms show different oxidation behaviors,


1931 ◽  
Vol 4 (3) ◽  
pp. 445-449
Author(s):  
Charles W. Stillwell ◽  
George L. Clark

Abstract New x-ray diffraction data for gutta-percha and balata are given and considered in the light of von Susich's recent conclusion that these substances are identical and exist in two crystalline forms. The data also support the assumption that gutta-percha is a mixture of balata and another crystalline constituent, an assumption that is in some respects preferable to that of von Susich. Although the relation between gutta-percha and balata has been established and there may be no ultimate difference between them, it is pointed out that the majority of specimens examined of material classified commercially as balata produce a diffraction pattern different from that of gutta-percha, a fact of practical significance. THERE has been considerable disagreement as to the significance of x-ray diffraction data for gutta-percha and balata as reported by different investigators. The main point at issue has been the fundamental difference between gutta-percha and balata. Clark (1) and Hauser (2) have obtained different diffraction patterns for the two when unstretched, while Hauser has found them to be the same when stretched. Von Susich (3) has recently done much to clarify the problem. He reaches the conclusion, as a result of x-ray diffraction data, that gutta-percha and balata are identical, and that the substance exists in two different crystalline modifications, the alpha form being stable below about 60° C. and changing to the beta form when heated above this temperature. Of course, this at once explains Hauser's results, since the specimens were doubtless heated above 60° C. when stretched and would then show the beta pattern.


Clay Minerals ◽  
1981 ◽  
Vol 16 (4) ◽  
pp. 383-393 ◽  
Author(s):  
S. J. Van Der Gaast ◽  
A. J. Vaars

AbstractA method is described for calculating, and then subtracting, the background from X-ray diffraction patterns of oriented clay mineral samples. Ti-Kα radiation is used and, to minimize the absorption of this radiation by air, a vacuum and helium-flushed device has been developed. This device can be used with other X-ray sources, offering a considerable increase of intensity—e.g. Co-Kα radiation is increased by 125%. With the background-eliminated patterns a better semi-quantitative estimate of the composition of clay mineral mixtures is possible. Small differences in composition of two samples can be identified by subtracting one of the background-eliminated patterns from the other. Using this method, peak maxima of smectite-group minerals can also be accurately determined.


1975 ◽  
Vol 55 (3) ◽  
pp. 363-379 ◽  
Author(s):  
B. MUTWEWINGABO ◽  
C. R. DE KIMPE ◽  
G. A. BOURBEAU ◽  
R. W. BARIL ◽  
P. LAJOIE

Five profiles were sampled in the till deposits of the Laurentides Hills. Two were obtained at Duchesnay, near Quebec City and three north of Montreal, including two profiles of the Gatineau and one of the Sainte-Agathe series of soils. Results of the particle-size distribution, morphological and mineralogical analyses suggested that the parent material was similar in all profiles. A high bulk density, about 2.00 g/cm3, was observed in the fragic horizon. Maximum weathering was found in the A horizons resulting in the formation of montmorillonite and kaolinite. The X-ray diffraction patterns obtained for the samples from Duchesnay were better defined than those obtained from the other profiles. In addition to illite, chlorite and vermiculite, two types of interstratified minerals were observed: illite–montmorillonite in the Podzolic-B and illite–vermiculite in the fragic horizons. High values, up to about 700 meq/100 g were obtained for the Al interlayers in the clay fraction. These profiles were classified as fragic ferro-humic Podzols (Sainte-Agathe and the profiles from Duchesnay) and fragic humo-ferric Podzols (Gatineau). The concept of fragic horizon in the soils from the Laurentides is discussed.


1929 ◽  
Vol 1 (3) ◽  
pp. 201-213 ◽  
Author(s):  
T. Thorvaldson ◽  
N. S. Grace ◽  
V. A. Vigfusson

Further studies on the isometric form of hydrated tricalcium aluminate are reported. These include methods of preparation, crystalline forms, X-ray diffraction pattern, and determinations of solubility and density. The products formed when the hexagonal form of hydrated tricalcium aluminate is dehydrated at definite vapor pressures of Water at 21 °C., were studied. The density, refractive indices, heats of solution in HCl.200 H2O, and the X-ray diffraction patterns of several probable hydrates were determined. The experimental evidence given indicates that hydrates of 3CaO.Al2O3 having 6, 8, 91/2, 101/2, and 12 moles of water are formed, but that the water in excess of 8 moles is very loosely held and that its removal does not materially affect the crystal structure. The exact composition of some of the higher hydrates requires confirmation.


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