Crystal structure of 1-[N-2-aminoethyl)-aminopropyl]silatrane

The crystal structure of 1-[N-(2-aminoethyl)aminopropyl]silatrane has been determined by x-ray diffraction at room temperature. The Si←N bond distance (2.165(2) Å) is in the range observed for other 1-X-propylsilatranes (X = CN, OH, SH, Cl and SCN). The structure is partially disordered: the silatrane moiety displays a disorder that is typical for silatranes and the aminoethyl group terminating the planar chain linked to silicon is rotationally disordered.     

Thermal properties of tetrahydroperparine derivatives

The thermal behaviour of tetrahydroperparine (THP) and its derivatives with various acids has been investigated. The acid is liberated from the formate derivative basically in two steps, while the other aliphatic acids are released quantitatively before the thermal decomposition of the THP molecule. The thermoanalytical curves, electrical conductivity data measured in the molten phase, and infrared spectra prove that while part of the formic acid is hydrogen-bonded the other part is bound ionically in the molecule. It may be assumed that the marked biological activity of the compound can be explained by this difference in the nature of the bonds.     

Rapid determination of aliphatic amines in water samples by pressure-assisted monolithic octadecylsilica capillary electrochromatography-mass spectrometry

A pressure-assisted capillary chromatography-mass spectrometry method based on the use of a monolithic octadecylsilica (ODS) capillary is proposed for the determination of aliphatic amines. A 25 mM citric acid buffer containing 10% methanol is used as running electrolyte. Separation is achieved by simultaneously applying a capillary electrophoresis (CE) voltage of 13 kV and an overimposed pressure of 8 bar. The use of pressure is required to ensure stable electrospray conditions. Analysis times are reduced by using a capillary column consisting of a 30 cm long monolithic silica capillary column bound with ODS and a fused-silica capillary column also 30 cm long. The proposed method was successfully applied to the determination of low-molecular-weight aliphatic amines in tap and river water. The analysis of real samples requires cleanup and preconcentration, which can be performed automatically by inserting a minicolumn in the replenishment system of the commercial instrument.     

Infrared laser ablation study of pressed soil pellets with inductively coupled plasma atomic emission spectrometry

Potential of infrared laser ablation (LA) coupled with ICP-AES as a technique suitable for the determination of trace elements (Zn, Cu, Ni, Cr, and V) in agricultural soils was studied. Operating parameters such as laser beam energy, laser beam focusing with respect to the sample surface, and velocity of the sample translation in the plane perpendicular to the laser beam were optimized. Soil samples were mixed with powdered Ag as a binder, and an internal standard (GeO(2)), and pressed into pellets. Calibration samples were prepared by adding known amounts of oxides of elements of interest into soils of known elemental composition and then processed in the same way as the analyzed samples. Calibration curves were found to be linear at least up to several hundreds of mg kg(-1) for the elements of interest. The elemental contents obtained by using LA-ICP-AES were compared with those obtained by analysis using wet chemistry followed by ICP-AES with pneumatic nebulization (PN). The results were in good agreement. Accuracy was also tested using certified reference soils with a bias not exceeding 10% relative.     

Zwei neue pentacyclische dimere des cycloheptatriens

Titanium - catalyzed dimerization of cycloheptatriene affords pentacyclo[7.5.0.0^2,8.0^5,14.0^7,11]tetradeca-3,12-diene, $\text{3}$, and pentacyclo[8.4.0.0^3,7.0^4,14.0^6,11]tetradeca-8,12-diene, $\text{4}$. By heating, $\text{3}$ is converted quantitatively into $\text{4}$.     

Ion-pair extraction of pentacaine from biological materials

Simple and rapid extraction method for quantitative and selective isolation of the new local anesthetic pentacaine from biological materials is proposed. The technique of ion-pair formation was found to be more effective than usual access using the extraction of the nonionized species. The extraction yield of the unchanged molecule³H-pentacaine after double extraction and single scrubbing was found to be more than 90%. The radiochemical purity was over 90%. The method appears suitable for pharmacokinetic studies in the animal body.     

Novel electroanalytical techniques for pollution analysis

Summary Two new analytical techniques are described. The so-called injection technique operates on evaluating a dynamic concentration signal as a result of following the concentration change in a certain part of a flow-through channel after injecting a sample or reagent at a small volume into the current of an appropriate solution flowing at a constant rate.The second technique, the programmed coulometric titration technique, also uses the flow-through channel principle; that means this novel technique allows the more precise titrimetric way of analysis in flowing solutions. In the case of both techniques potentiometric and voltammetric detectors were involved. Several examples proved the multifold advantages of these techniques for environmental analysis.

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Neue elektroanalytische Verfahren für die Umweltanalyse

Zusammenfassung Zwei neue Methoden werden beschrieben. Die sog. Injektionstechnik wertet ein dynamisches Konzentrationssignal aus, das sich aus der Änderung in einem Durchflußkanal ergibt, wenn Probe oder Reagens in kleinen Volumina in einen konstant fließenden Flüssigstrom injiziert werden. Das zweite Verfahren, die programmierte coulometrische Titration, erlaubt die Anwendung der genaueren titrimetrischen Technik auf fließende Lösungen. Bei beiden Methoden werden potentiometrische und voltammetrische Detektoren verwendet. Mehrere Beispiele zeigen die vielfachen Vorteile dieser Verfahren bei der Anwendung auf die Analyse von Umweltmaterial.

Presented at the 6th Annual Symposium on Recent Advances in the Analytical Chemistry of Pollutants, April 21–23, 1976; Vienna, Austria     

The extraction of HCl by TDPO in benzene

The results of the extraction of HCl by TDPO in benzene and the co-extraction of water are discussed. From the infrared spectra of normal (HCl-H₂O) and deuterated (DCl-D₂O) systems it may be concluded that TDPO·HCl·H₂O is formed in the organic phase on extraction from aqueous solutions with c_HCl≤5M, and TDPO·HCl with c_HCl>5M. Compounds such as TDPO·2HCl are found in the organic phase if there is an excess of HCl in the organic phase. From cryoscopic and viscosity measurements of the organic phase, conclusions can be made about the presence of polymeric compounds in this phase.     

On-line sorbent extraction, preconcentration and determination of lead by atomic absorption spectrometry

A method for the quantitative preconcentration of lead based on an existing batch process was developed for implementation in a flow system including a flame AAS detector. Lead can be quantitatively preconcentrated as pyrrolidinedithiocarbamate or dithizonate on an activated carbon minicolumn. The chelates are eluted in methyl isobutyl ketone and introduced directly into the nebuliser-burner. An enrichment factor of 50 is typically obtained for a preconcentration time of 2 min (lead can be determined at concentrations between 15 and 400 ng/ml), which results in a throughput of ca. 25 samples per hr. The sensitivity achieved with the two reagents is similar, but the selectivity provided by APDC exceeds that of dithizone. Based on the results obtained in the determination of lead in reference materials (minerals and skim milk), the proposed APDC method is applicable to real samples.     

Solubility product relations in the rare earth hydrous hydroxides

The solubility products for some rare earth hydroxides and their temperature dependence have been shown. Greater solubility is shown for larger atomic radii and for lower temperature.