Study of diffusion creep accompanying superplastic deformation of the alloy ZhS6KP

The development of diffusion creep (DC) accompanying superplastic deformation (SPD) of the highly doped nickel alloy ZhS6KP is studied based on an investigation of the redistribution of dispersed intragrain deposits of the phase of Ni₃(Al, Ti). Deposit-free zones (DFZ) are formed in the alloy, held at the temperature of SPD and accompanying deformation at the grain boundaries. The contribution of DC to the deformation was determined from a comparative analysis of the width of the DFZ in the deformed and undeformed parts of the samples for different grain sizes and rates of DC taking into account diffusion accommodation. It was established that for the optimum rate of SPD the upper limit of the contribution of DC to deformation for 2-m grains does not exceed 11%. It is concluded, based on the distribution of DFZ, that the effect of DC accompanying SPD is determined by diffusion fluxes, associated with the local concentration of stress accompanying the development of grain-boundary slipping.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 6, pp. 40–45, June, 1986.In conclusion, we thank Yu. M. Mishin for a useful discussion of the results.     

Optical frequency doubling of a single-mode dye laser in an external ring resonator

Optical frequency doubling of a single-mode cw Rhodamin 6G ring dye laser is performed with a thin angle-tuned LiIO₃ Brewster cut crystal in a stabilized passive ring resonator. A conversion efficiency of =5 mW uv/320 mW fundamental input power was achieved at =603 nm.     

R?ntgenspektrometrische Elementbestimmung in Abwasser: Probenvorbereitung und Matrixkorrekturverfahren

Zusammenfassung Für Elementbestimmungen in Abwasser wird ein Röntgenfluorescenzverfahren beschrieben. Zur Probenvorbereitung werden die Elemente durch Gefriertrocknung auf einem inerten Träger angereichert. Diese Anreicherung ist nicht selektiv und erfaßt praktisch alle in Abwasser gelösten und suspendierten Verunreinigungen. Für die Berechnung der Elementkonzentrationen aus den gemessenen Fluorescenzintensitäten wird ein Matrixkorrekturverfahren angegeben, welches dem unterschiedlichen Absorptionsverhalten der Probenmatrix Rechnung trägt. Die Massenabsorptionskoeffizienten werden durch Messung der diffus gestreuten Bremsstrahlung bzw. der Comptonstreustrahlung ermittelt. Die Selbstabsorption des zu bestimmenden Elementes wird rechnerisch berücksichtigt. Das Korrekturverfahren kann auf alle mit Röntgenfluorescenzanalyse bestimmbaren Elemente angewendet werden.

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Determination of elements in waste water by x-ray fluorescence analysis: Sample preparation and matrix correction method

Summary For sample preparation the elements are enriched upon an inert carrier by freeze-drying. This enriching procedure is not selective and collects all dissolved and suspended contaminations from the waste water. In order to calculate the element concentrations from the measured fluorescence intensities a matrix correction method is given which considers the different absorption behaviour of the matrix. The mass absorption coefficients are obtained by measuring the scattered X-ray tube spectrum or a Compton scattered X-ray tube line, respectively. The self-absorption of the element to be determined is taken into account. The correction method is applicable to all elements detectable by X-ray fluorescence.

Herrn Dr. H. Wagner danken wir für das stete Interesse, die zahlreichen konstruktiven Diskussionen und die Hilfe beim Abfassen des Manuskripts.     

Einkristalle von CoNbO4 mit AlNbO4-Struktur

Single Crystals of CoNbO₄ with AlNbO₄ Structure The hitherto unknown single crystals of CoNbO₄ were prepared. CoNbO₄ has AlNbO₄ structure with monoclinic symmetry (space group C?C2/m; a = 1212.9; b = 374.9; c = 651.2 pm; β = 107.6°). X-ray investigations shows on ordered arrangement of Co³⁺ and Nb⁵⁺ with well defined differences in respect to oxocobaltates with Columbite type (CoNb₂O₆ = Co_0.33Nb_O.66O₂) and Rutil type (CoNbO₄ = Co_0.5-xNb_0.5+xO₂; 0 ? × ? 0.166) structure.     

Thermal properties of some complexes of quinolinic acid with divalent metal ions

Studies of the complexes of pyridinecarboxylic acids with divalent metal ions as a function of the position of the carboxyl groups were extended. The thermal properties of the complexes of quinoline acid (pyridine-2,3-dicarboxylic acid) with several divalent metal ions were determined by thermogravimetry (TG) and differential thermal analysis (DTA). A correlation between these compounds and others obtained by reaction between the studied metal ions with similar acids (lutidinic acid (pyridine-2,4-dicarboxylic acid) and isocinchomeronic acid (pyridine-2,5-di-carboxylic acid) is discussed in terms of the position of the carboxyl group far from the aza group. The thermal stability of the metal complexes is in the order Mn(II) > Fe(II) > Zn(II) ? Co(II) > Ni(II) > Cu(II).     

Reaction of β-amino-α,β-unsaturated esters and amides with aryl diazonium salts : Synthesis of cinnoline derivatives

Conjugated esters and amides react with aryldiazonium salts at room temperature (MeCN) to form the corresponding iminium hydrazone derivatives, which can be thermally cyclized to cinnoline-3-esters and cinnoline-3-amides. In general the intermediate iminium salts derived from the enamine amides cyclize faster than those from the enamine esters. Furthermore, the ease of cyclization depends upon the structure of the base-component of the enamine ester or the amide and the substituent in the aryl moiety of the diazonium salt. The configurational structure of the iminium hydrazones, studied by NMR spectroscopy, has been shown to involve H-bonding of the hydrazonyl N-H with the ester or the amide CO group.     

Vernetzung und Abbau von Polyäthylenterephthalat durch Elektronenbestrahlung

Zusammenfassung PÄT-Folien wurden in Luft, Stickstoff und Vakuum bei 20 °C mit 1 MeV-Elektronen bestrahlt. Untersucht wurden Löslichkeit und Viskosität von Proben, die unmittelbar nach der Bestrahlung gelöst wurden.In allen untersuchten Fällen trat bei hohen Bestrahlungsdosen ein unlöslicher, d. h. vernetzter Anteil auf, dessen Ausbildung jedoch durch in den Proben enthaltene Feuchtigkeit verzögert werden kann. Bei niedrigen Bestrahlungsdosen bewirkt Feuchtigkeit einen Abbau des Polymeren, wie durch Viskositätsmessungen gezeigt wird.Aus den Gel-Messungen wurde derp ₀/q ₀-Wert für Bestrahlung in Luft, Stickstoff und Vakuum zu 1,05 bestimmt.Die Änderung des Gel-Anteils bei Lagerung der Proben zwischen Bestrahlung und Lösung wird diskutiert.

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Summary Polyethyleneterephthalate samples were irradiated in air, nitrogen and vacuum at 20 °C with 1 MeV electrons. The solubility of the samples and the viscosity of the solutions were studied immediately after irradiation. At high doses an insoluble crosslinked part was always observed. Crosslinking was delayed by moisture in the samples. At low irradiation doses moisture causes chain scission as shown by viscosity measurements. The ratiop ₀/q ₀ of degradation to crosslinking in the case of irradiation in air, nitrogen and vacuum was found by gel measurements to be 1.05. The insoluble gel-part changes with increasing storage time of the samples between irradiation and solution.

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Herrn Diplom-PhysikerH. Fischer sei an dieser Stelle für wertvolle Anregungen und Diskussionen besonders gedankt.     

Hydroformylation and hydrocarbethoxylation of 1,2-dicarbethoxy-1,2,3,6-tetrahydropyridazine and 1,2-dicarbethoxy-1,2,3,4-tetrahydropyridazine

The unsaturated compounds 1,2-dicarbethoxy-1,2,3,6-tetrahydropyridazine 1 and 1,2-dicarbethoxy-1,2,3,4-tetrahydropyridazine 2 have been hydroformylated and hydrocarbethoxylated in the presence of some well known cobalt, rhodium, palladium and platinum catalysts. The hydroformylation reaction can be tuned by a suitable choice of the catalyst precursor and reaction conditions, thus allowing the synthesis with high selectivity of one of the two possible isomeric aldehydes. The carbonylation reaction is less synthetically useful, since it shows low activity and unsatisfactory chemo- and regio-selectivity. However, the ester 1,2,4-tricarbethoxyhexahydropyridazine 10 can be prepared in good yield from olefin 1 by using the complex [PdCl₂(PPh₃)₂] as the catalyst precursor.