Retention of85Sr and147Pm on insoluble hydroxides and phosphates prepared by the sol-gel procedure

Retention of strontium and promethium on hydroxides (hydrated oxides) and phosphates of iron and chromium prepared by the sol-gel method was studied. The sorption was determined under static conditions depending on the pH of the solution. The sorption isotherms and retention were investigated under dynamic conditions.     

Intramolecular "Aryl-metal chelate ring" pi,pi-interactions as structural evidence for metalloaromaticity in (aromatic alpha,alpha'-diimine)-copper(II) chelates: molecular and crystal structure of aqua(1,10-phenanthroline)(2-benzylmalonato)copper(II) three-hydrate

By reaction of Cu(2)CO(3)(OH)(2), 2-benzylmalonic acid (H(2)Bzmal), and 1,10-phenanthroline (phen), [Cu(Bzmal)(phen)(H(2)O)] x 3H(2)O (compound 1) has been obtained and characterized by thermal, spectral, magnetic, and X-ray diffraction methods. The molecular structure of 1 is remarkably similar to that of [Cu(Bzmal)(bipy)(H(2)O)] x 2H(2)O (compound 2, bipy = 2,2'-bipyridine). In both complexes, the aryl(Bzmal) ring produces an unexpected pi,pi-stacking interaction with the Cu(II)-(aromatic alpha,alpha'-diimine) chelate ring, at an average distance d(pi)(-)(pi) of 3.40 A, involving roughly parallel and smoothly slipped rings. This insight is discussed as new structural evidence for metalloaromaticity of Cu(II)-(aromatic alpha,alpha'-diimine) chelate rings. Interestingly, 1 recognizes itself by a weak intermolecular pi,pi-stacking interaction between aryl(Bzmal) ligands to give pairs of complex molecules. In contrast, there is an intermolecular pyridyl-pyridyl pi,pi-stacking interaction also forming pairs of complex molecules in 2.     

Automation of the gas analysis of14C-labelled compounds utilizing a piston-type counter tube

In this paper an automatic apparatus designed for the radioactivity measurement of¹⁴C-labelled organic compounds in the gaseous phase is described. The labelled organic compounds are combusted in a mixture of argon and oxygen. After combustion the oxygen content of the gas is eliminated by passing it through a copper packing. The water and heteroelements present are also removed and the radioactive carbon dioxide gas is swept by argon carrier gas into a piston-type counter tube. In the counter tube the piston forming a dividing wall moves forward in accordance with the rate of combustion and sweeping, and thus sucks the gases leaving the combustion tube into the effective tube volume. The anode wire is carried by a reel located in the piston and a spring device ensures its stretched state. At the end of the sweeping period methane is fed into the counter tube and the activity of the argon—methane—carbon dioxide mixture is measured in the limited proportional region. Manual and automatic operation is possible. The piston-type counter tube provides possibility for strandardization by means of extrapolation and for measurement of absolute activities.     

Some investigations on the photostabilization of polypropylene

The effect of substituted hydroxybenzophenone, benzotriazole and organic metal complexes on the photooxidation of PP films has been studied. It has been established that NiDBTC added in 1.0 wt. % is the most effective photostabilizer.While in the case of other stabilizers there is a slight increase in the Co content even during the induction period, with the application of NiDBTC practically no oxidation can be observed before the stabilizer completely disappears. This means that NiDBTC inhibits the photooxidation of the polymer even in low concentration.

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, - . , Ni, 1,0 . %. . , Ni , . , Ni .

     

Spektrophotometrische Bestimmung von L-Askorbinsäure mit 2,2',5,5'-Tetra-(4-nitrophenyl)-3,3'-(3,3'-dimethoxy-4, 4'-biphenyl)-ditetrazoliumchlorid (TNBT)

Zusammenfassung Die Optimalbedingungen für die spektrophotometrische Bestimmung der L-Askorbinsäure mit TNBT wurden ermittelt. Die L-As-korbinsäure wurde in Anwesenheit eines 100fachen Überschusses folgender Stoffe bestimmt: Glukose, Fruktose, Saccharose, Wein-, Zitronen-, Oxal-, Äpfel- und Bernsteinsäure. 0,5g/ml ist die minimale Askorbinsäurekonzentration, die sich bestimmen läßt. Die rel. Standardabweichung beträgt 2,1%, der rel. Fehler 0,875%.

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Spectrophotometric assay of L. ascorbic acid with 2,2,5,5-tetra-(4-nitro-phenyl)-3, 3-(3,3-dimethoxy-4,4-biphenyl)-ditetrazolium chloride (TNBT)

Summary The optimal conditions for spectrophotometric assay of L-ascorbic acid with TNBT were determined. L-ascorbic acid was assayed in the presence of a 100 fold excess of the following substances: glucose, fructose, sucrose, tartaric acid, citric acid, oxalic acid, malic acid and succinic acid. 0.5g/ml is the minimum concentration of ascorbic acid which can be assayed. The relative standard deviation is 2.1%, the relative error 0.875%.

     

Determination of the pH of binary mobile phases for reversed-phase liquid chromatography

The measurement of pH in chromatographic mobile phases has been a constant subject of discussion during many years. The pH of the mobile phase is an important parameter that determines the chromatographic retention of many analytes with acid-base properties. In many instances a proper pH measurement is needed to assure the accuracy of retention-pH relationships or the reproducibility of chromatographic procedures. Three different methods are common in pH measurement of mobile phases: measurement of pH in the aqueous buffer before addition of the organic modifier, measurement of pH in the mobile phase prepared by mixing aqueous buffer and organic modifier after pH calibration with standard solutions prepared in the same mobile phase solvent, and measurement of pH in the mobile phase prepared by mixing aqueous buffer and organic modifier after pH calibration with aqueous standard solutions. This review discusses the different pH measurement and calibration procedures in terms of the theoretical and operational definitions of the different pH scales that can be applied to water-organic solvent mixtures. The advantages and disadvantages of each procedure are also presented through chromatographic examples. Finally, practical recommendations to select the most appropriate pH measurement procedure for particular chromatographic problems are given.     

Thermal reactivities of potassium and cadmium hydrogenhexavanadates

The thermal reactivities of KHV₆O₁₆·3H₂O and Cd(HV₆O₁₆)₂·12H₂O were investigated. By means of IR spectroscopy and X-ray phase analysis it was found that, after dehydration, both compounds decompose to vanadium pentoxide and the corresponding metavanadate. Potassium metavanadate and vanadium pentoxide react together to form bronzes of different compositions. In contrast, vanadium pentoxide and cadmium metavanadate are the predominant components of the reaction products obtained within the temperature range from 300° to 800°C.     

Anwendung mikroanalytischer Methoden zur Lösung kunst- und kulturgeschichtlicher Probleme

Zusammenfassung Mit bekannten mikroanalytischen Arbeitsmethoden — Oberflächenreaktionen, Abstrichuntersuchungen mit dem Korundstäbchen, Schutzschichtreaktionen sowie dem Abdruckverfahren — lassen sich archaeometrische Probleme einer Lösung näherbringen. Die Art der Korrosion kupferhaltiger Oberflächen wurde diskutiert.

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Application of microanalytical methods to the solution of artistic- and cultural historical problems

Summary Archeometrical problems are brought closer to a solution by means of known microanalytical procedures-surface reactions, surface scraping studies with the corundum rod, protective layer reactions as well as the imprint method. A discussion of the corrosion of copper-bearing surfaces is included.

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Vortrag anläßlich der Tagung Chemische Analysen — Kunst- und Kulturwissenschaften im Reiß-Museum in Mannheim, 19.–21. September 1974.     

The surface activity of the lower homologues of n-alkylammonium chlorides in aqueous solutions. Effect of hydrophobic hydration

Summary The surface tensions of aqueous solutions ofn-alkylammonium chlorides (methyl to hexyl) have been measured at 25 °C. With methylammonium chloride the surface tension increased with concentration, whereas with ethylammonium chloride and higher homologues, the surface tension decreased with concentration. The results suggest that this transition is attributed to the effect of hydrophobic hydration. For propylammonium chloride and higher homologues, the relation between the surface tension lowering da and the concentrationC in the range of 0–10 dyne/cm, can be expressed by the equation; = AC + BC, whereA andB are constants. The surface tension coefficientB has been found to increase approximately twofold for each additional CH₂ group of alkyl chain.

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Zusammenfassung Es wurden die Oberflächenspannungen wäßriger Lösungen vonn-Alkylammoniumchloriden (Methyl- bis Hexylammoniumchloride) bei 25 °C gemessen. Für Methylammoniumchlorid nimmt die Oberflächenspannung mit der Konzentration zu, aber bei allen höheren Homologen mit der Konzentration ab. Die Ergebnisse deuten darauf hin, daß dieser Übergang durch die hydrophobe Hydration bedingt wird. Für Propylammonium-chlorid und die höheren Homologen wird die Beziehung zwischen der Erniedrigung der Oberflächenspannung und der KonzentrationC in dem Bereich von 1 bis 10 dyn/cm durch die folgende Gleichung ausgedrückt: = AC + BC (A undB sind Konstanten). Es wurde gefunden, daß B für jede zusätzliche CH₂-Gruppe etwa um den Faktor 2 größer wird.

     

Thermal investigations on the crystallization of sorbitol

The melting and crystallization of sorbitol were investigated with the DSC method and thermal microscopy. Sorbitol was found to have two crystalline modifications (confirmed by X-ray diffraction) with different melting points, while rapid cooling of molten sorbitol resulted in an amorphous form. The effect of inoculation on the crystallization of the melt was studied too. Powders of both crystalline modifications were used for this purpose. A new technological process for rapid crystallization of molten sorbitol has been worked out on the basis of the thermal analysis results.