Thin-layer chromatography of steroisomeric 2,4-dinitrophenylhydrazones of aliphatic aldehydes.
Abstract The stereoisomeric forms of 2,4-dinitrophenylhydrazones (2,4-DNP) of some aliphatic aldehydes and unsymmetrical detones were separated by several reverse phase thin-layer chromatographic procedures. Evidence indicated that the reaction to produce the 2,4-DNP produces both the syn and anti form, but that repeated recrystallization in ethanol yielded the pure syn crystalline form. Racemizaton of the crystalline syn form could be stimulated by dissolving it in chloroform or by the addition of a small amount of hydrochloric acid to an acetone or methanol solution. Certain thin-layer chromatographic systems separated the homologous series to the greatest extent and the isomers the least (undecane/75% methanol-25% water). Another system separated the isomers to a considerable extent but was not too effective in separating the homologous series (dimethylformamide/heptane). Combinations of these systems should be of value in resolving mixtures of syn and anti forms of mixtures of aliphatic aldehyde 2.4-DNP.
Dünnschicht-chromatographische Trennung der 2,4-Dinitrophenylhydrazone von Formaldehyd, Acetaldehyd, Acrolein, Crotonaldehyd und Furfurol
The derivatives are applied on rapid plates silica gel F 254 from pyridine, tetrahydrofuran or dioxan solution and separated during 6 h by ascending overrun development using carbon tetrachloride/pyridine (90∶10) as a solvent. The distances travelled from the starting point are in the ratio 1∶1.3∶1.7∶2.1∶2.3.ZusammenfassungEs wird ein dünnschicht-chromatographisches Verfahren zur Trennung von Formaldehyd, Acetaldehyd, Furfurol, Acrolein und Crotonaldehyd in Form der 2,4-Dinitrophenylhydrazone beschrieben. Die Derivate werden aus Pyridin, Tetrahydrofuran oder Dioxan aufgetragen und innerhalb von 6 h nach der Durchlauftechnik an Kieselgel F 254-Rapidplatten mit Tetrachlorkohlenstoff/Pyridin (90∶10) aufsteigend entwickelt. Die Laufstrecken verhalten sich wie 1∶1,3∶1,7∶2,1∶2,3.
Refinement of crystal structure parameters using convergent‐beam electron diffraction: the low‐temperature phase of SrTiO3
The method to refine crystal structure parameters (atom positions and Debye–Waller factors) using convergent-beam electron diffraction (CBED), which is applicable to crystal structure analysis of a small specimen area down to a few nm in diameter, is studied. The line profiles of higher-order Laue-zone reflections are recorded using imaging plates. Theoretical intensities are calculated based on the dynamical theory of electron diffraction with the aid of the generalized Bethe approximation to shorten calculation time. The structural parameters are determined by fitting the experimental profiles with the theoretical ones using a nonlinear least-squares method. The present method has been applied to the low-temperature phase of SrTiO3. The structural parameter or the rotation angle of the oxygen octahedron has been determined to be \varphi = 1.12 (4)°, which shows good agreement with that obtained from electron spin resonance experiments.