Untersuchungen zur Trennung von N-Alkylbenzylamin-Gemischen durch multiplikative Verteilung

Zusammenfassung Die Entwicklung von Lösungsmittelsystemen für die Trennung von Amingemischen durch multiplikative Verteilung wird beschrieben und ihre Eignung durch Aufteilen der 8 homologen Basen, Benzylamin bis N-Heptylbenzylamin, bewiesen.

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Studies on the separation of N-alkylbenzylamine mixtures by multiplicative distributionOn the separation of organic bases by Craig distribution. VIII

The development of solvent systems for the separation of amine mixtures by Craig counter current distribution is described and its aptitude proved by the partition of 8 homologous bases, benzylamine to N-heptylbenzylamine.

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VII. Mitteilung: Schönenberger, H., K. D. Fuchsberger u. R. Brinkmann: Arch. Pharm. Ber. Deut. Pharm. Ges. 300, 126 (1967).

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Wir danken der Deutschen Forschungsgemeinschaft und dem Fonds der Chemischen Industrie für die Förderung unserer Untersuchungen.     

The determination of the efficiency of energy dispersive X-ray spectrometers by a new reference material.

A calibration procedure for the detection efficiency of energy dispersive X-ray spectrometers (EDS) used in combination with scanning electron microscopy (SEM) for standardless electron probe microanalysis (EPMA) is presented. The procedure is based on the comparison of X-ray spectra from a reference material (RM) measured with the EDS to be calibrated and a reference EDS. The RM is certified by the line intensities in the X-ray spectrum recorded with a reference EDS and by its composition. The calibration of the reference EDS is performed using synchrotron radiation at the radiometry laboratory of the Physikalisch-Technische Bundesanstalt. Measurement of RM spectra and comparison of the specified line intensities enables a rapid efficiency calibration on most SEMs. The article reports on studies to prepare such a RM and on EDS calibration and proposes a methodology that could be implemented in current spectrometer software to enable the calibration with a minimum of operator assistance.     

Fluorodaturatin und Homofluorodaturatin—zwei neue β-Carbolinderivate in Samen von

In the transverse section of the seeds ofDatura stramonium L. var.stramonium a conspicuous sea-green fluorescence under UV-light (365 nm) can be observed. Thinlayer chromatography of a methanolic extract shows many blue and sea-green fluorescing substances, the main component being a polar, sea-green fluorescing compound. This substance is characteristic for all of the four varieties ofDatura stramonium L., and therefore of taxonomic interest. Isolation was tried by means of different chromatographic techniques. Combination of column chromatography and preparative thinlayer chromatography allowed the isolation of the main product, which was shown to consist of two substances (GF andGFa). Application of chemical and spectroscopic methods established the structure ofGF, named Fluorodaturatin, as 2,3,5,6-Tetrahydro-9-hydroxy-1H-pyrido-[1,2,3-l, m]--carboline-3-one. The second substanceGFa, called Homofluorodaturatin, was identified as analogue ofGF and the structure could be determined as 1,2,3,4,6,7-Hexahydro-10-hydroxyazepino-[1,2,3-l, m]--carboline-4-one.

Teil der DissertationI. Maier, Universität Wien, 1981; Auszugsweise vorgetragen bei der 2. Wissenschaftlichen Tagung der Österreichischen Pharmazeutischen Gesellschaft, 17. bis 19. Mai 1981, Graz.     

Traceability in laboratory medicine

In laboratory medicine meaningful measurements are essential for diagnosis, risk assessment, treatment and monitoring of patients. Thus methods applied in diagnostic measurements must be accurate, precise, specific and comparable among laboratories. Inadequate or incorrect analytical performance has consequences for the patients, the clinicians, and the health care system. One key element of metrology is the traceability of a measurement result to the SI system ensuring comparable results. This principle is described in the ISO/TC 212/WG2 N65 prEN 17511 Standard. In addition to the principles of metrology, the clinical usefulness, the diagnostic needs, and the biological and disease associated variations in patients' specimens have to be considered when the analytical biases for diagnostic purposes are defined. It must be the general goal of diagnostic laboratories to produce results that are true and comparable worldwide. The recent European in vitro diagnostic (IVD) Directive 98/79 EC follows the above mentioned standard of the International Organization for Standardization (ISO) and the European Committee for Standardization (CEN) requesting its application for all IVD reagents used within the European Union. This new European legislation will have a worldwide impact on manufacturers and clinical laboratories and will be implemented in 2003. It states that "traceability of values assigned to calibrators and/or control materials must be assured through available reference measurement procedures and/or available reference materials of a higher order". Thus a worldwide reference system needs to be established by collaboration and mutual recognition between the United States National Institute of Standards and Technology (NIST), European Metrology Institutes (EUROMET), regulatory bodies (e.g. United States Food and Drug Administration, FDA) the IVD industry and professional organizations (e.g. International Federation of Clinical Chemistry and Laboratory Medicine, IFCC). In June 2002, in Paris, representatives of international and regional organizations and institutions decided to form the "Joint Committee on Traceability for Laboratory Medicine" (JCTLM), which will support industry in registration and licensing of the "CE" label to test systems conforming to the IVD Directive.Presented at the International ILAC/IAF Conference on Accreditation in Global Trade, 23–25 September 2002, Berlin, Germany     

In situ formation of new crosslinking agents from acrylate derivatives and bisepoxides

The synthesis of several newly available diacrylate crosslinking agents derived from hydroxy functional acrylates and bisepoxides is described. These crosslinking agents are synthesized via the acid catalyzed addition of hydroxyl-containing acrylate monomers to bisepoxides derived from bisphenol-A and its hexafluoropropyl analog. These materials are generated in an excess of the acrylate monomer and the reaction mixtures are then converted directly to highly crosslinked materials. The alcohol functional monomers include hydroxyethyl methacrylate (HEMA) and the butyl and ethyl esters of (α-hydroxymethyl)acrylic acid. The latter are especially interesting for several reasons. First, they are readily available through the addition of the corresponding acrylate to formaldehyde. Second, these monomers react with the bisepoxides to give all-ether-linked connecting groups, in conrast to HEMA which yields a molecule with both ether and ester linkages between the two acrylate units. Third, the monomers are very different in solubility from HEMA and the polymers display very different chemical and physical properties. For example, while the crosslinked HEMA polymers are swellable in water, those of the (α-hydroxymethyl)acrylates are insoluble in water but swellable in organic solvents such as chloroform. All monomers, crosslinking agents, and crosslinked polymers were characterized by FT-IR, solution or solid state ¹³C-NMR spectroscopy, and thermal analysis.     

A novel system for purge-and-trap with thermal desorption: Optimization using tomato juice volatile compounds

A system for purge-and -trap with thermal desorption was developed and optimized to moniotor aroma compounds at ambient temperatures. Canned tomato juice volatiles were used as a model system to develop and evaluate the method. Volatile components were first adsorbed on insert-traps packed with Tenax-TA polymer, then thermally desorbed directly inside a gas chromatograph injector. Volatile matgerials occuring in Very low amounts could be entrained and subsequently chrfomatographed, with sensitivity limited by the purity of the sweep gas. Quantitative measurement of tomato juice volatiles was linear with sample size upn to 100 gram samples. The amount of trapped volatiles was proportional to trapping time; howver, low-and intermediate-boilers broke through the trap after one hour while high-boilers continued to be retained. Apurge gas flow rate of 20ml/min gave optimum results mediate-biolers. Optimum recovery of volatile compounds was obtained with a desorption temperature of 200°c for 5 min. Coefficients of variation from triplicate runs were relatively small. The method showed promise for a simple, sensitive, and reproducibel flavor volatiles collection system for the accurate analysis of tomato compounds.     

Solvation states of HCl in mixed ether:acid crystals: a computational study

Acid solvation states are investigated in the recently discovered mixed ether:acid crystalline solids. The solids are simulated using on-the-fly molecular dynamics as implemented in the density functional code QUICKSTEP employing Gaussian basis sets. The solids are shown to display a remarkably broad range of acid solvation states, depending on the ether:acid ratio, including proton sharing in the 1:1 case, proton transfer to the ether in 1:2, and perturbed molecular acid in 1:6. The observed variation of the infrared spectra with the composition is accounted for qualitatively with the help of the calculations.