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Identification of organic compounds by microscopy and X-ray diffractometry

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Summary

Primary and secondary crystallographic constants can be utilized conveniently for identifications of crystalline organic and inorganic materials by microscopy and X-ray diffractometry. Several specific properties can be measured under the petrographical microscope, including optic axial angle, character, dispersion, and in addition, refractive index directions can be established. The “d” spacings and their intensities as determined with the X-ray diffractometer serve to identify crystalline materials. The two instruments should be considered as supplementary tools for identifying crystals.

Both instruments supply a means for identification and semiquantitative analysis of mixed crystal systems. Data are presented for the systems: acetic-propionic p-bromoanilides and acet-propion-2.4-dinitro-phenylhydrazones.

Zusammenfassung

Primäre und sekundäre kristallographische Konstanten können zur Identifizierung kristallisierter organischer und anorganischer Stoffe auf mikroskopischem Wege und durch Röntgendiffraktometrie gut herangezogen werden. Einzelne spezifische Eigenschaften können unter dem petrographischen Mikroskop gemessen werden, so der optische Achsenwinkel, der Charakter, die Dispersion. Außerdem kann man Angaben über den Brechungsindex erhalten. Die mit dem Röntgendiffraktometer bestimmten Netzebenenabstände „d“ und deren Intensitäten dienen zur Identifizierung kristallisierter Stoffe. Die beiden Instrumente sind als Hilfsmittel zur Erkennung von Kristallen anzusehen.

Sie bieten die Möglichkeit zur Identifizierung und halbquantitativen Analyse von Mischkristallsystemen. Daten für die Systeme Essigsäure-Propionsäure-p-Bromanilid und Acetaldehyd-Propionaldehyd-2,4-Dinitrophenylhydrazon werden mitgeteilt.

Résumé

Les constantes cristallographiques primaires et secondaires sont utilisables pour l'identification de composés cristallins organiques et minéraux par microscopie et diffractométrie de rayons X. Il est possible de mesurer diverses propriétés spécifiques sous le microscope pétrographique, savoir: l'angle des axes optiques, le caractère et la dispersion optiques. Il est en outre possible de déterminer les directions des indices de réfraction primaires. Les espacements «d» et leurs intensités déterminés par le diffractomètre à rayons X permettent d'identifier les substances cristallines. Les deux instruments doivent être considérés comme complémentaires pour l'identification de cristaux. Chacun d'entre eux fournit un moyen d'identification et d'analyse semi quantitative des systèmes de cristaux mixtes. On rend compte de résultats obtenus pour les systèmes: p-bromoanilides acétique et propionique ainsi que 2, 4-dinitro phénylhydrazones de l'acétaldéhyde et du propionaldéhyde.

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Authors and Affiliations

  1. Polychemicals Department, Contribution from E. I. du Pont de Nemours & Company, Inc., Wilmington, Delaware, USA

    John Mitchell Jr & Ada L. Ryland

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  1. John Mitchell Jr
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  2. Ada L. Ryland
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Mitchell, J., Ryland, A.L. Identification of organic compounds by microscopy and X-ray diffractometry. Mikrochim Acta 44, 422–436 (1956). https://doi.org/10.1007/BF01216628

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