Beam deflection for temporal encoding in time-of-flight mass spectrometry

The pulsed ion sources used in conventional time-of-flight mass spectrometry (TOFMS) generally do not provide adequate resolving power across the mass range required for applications such as gas chromatography combined with mass spectrometry (GC/MS). Theoretical and experimental aspects of beam deflection techniques, which provide time encoding for TOFMS with continuous ions sources, are explored here. In this approach, ion source conditions do not affect resolving power, allowing for a greater variety of ionization modes to be used. Theoretical predictions for the resolving power attainable with beam deflection, which are satisfactory for GC/MS applications, agree well with experimentally determined values. The combination of GC-beam deflection-TOFMS with time-array detection is evaluated, and the capabilities of this system are compared to those of scanning mass spectrometers.     

Aza-analogues of cage compounds: Potential precursors to azacubanes and 1-azahomocubanes

Exploration of the reactions of the 9-azahomocubane system led to derivatives of two small-ring systems containing aza-bridging atoms, 5-azatetracyclo[4.2.0.0^3,8.0^4,7]octane and 9-azatetracyclo[4.3.0.0^2,5.0^4,7]nonane. The structures were characterized by X-ray diffraction analyses. There are no prior X-ray structural reports on these systems.     

Etude de la séparation du thorium d'avec les terres cériques

Résumé Nous avons étudié les complexes que forment les acides éthylèneglycolbis-(-aminoéthyléther)] Sr,N-tétracétique et ,-diaminodiéthylétherN,N-tétracétique, soit avec le thorium, soit avec les terres cériques et, à la suite de cette étude, nous avons pu établir une méthode d'analyse et une séparation du thorium d'avec les terres cériques qui nous a donné satisfaction.

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Summary A study has been conducted of the complexes formed by the ethyleneglycol-bis (-amino-ethylether)-N,N-tetraacetic acid and,-diaminodiethylether-N,N-tetraacetic acid with either thorium or the ceric earths. As a result of this investigation, it was possible to set up a method of analysis and a separation of thorium from the cerium earths. These procedures have proved satisfactory.

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Zusammenfassung Die von Äthylenglykol-bis-(-aminoäthyläther)-N,N-tetraessigsäure bzw.von ,-Diaminodiäthyläther-N,N-tetraessigsäure mit Thorium bzw. mit den Cer-Erden gebildeten Komplexe wurden untersucht. Auf Grund der Ergebnisse konnte ein Analysenverfahren und eine Trennungsmethode für Thorium und Cer-Erden entwickelt werden.

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Une communication de ce travail a été faite à Graz, lors de la commémoration du centenaire de la naissance deF. Emich.     

Efforts to expand the genetic alphabet: identification of a replicable unnatural DNA self-pair

Six unnatural nucleotides featuring fluorine-substituted phenyl nucleobase analogues have been synthesized, incorporated into DNA, and characterized in terms of the structure and replication properties of the self-pairs they form. Each unnatural self-pair is accommodated in B-form DNA without detectable structural perturbation, and all are thermally stable and selective to roughly the same degree. Furthermore, the efficiency of polymerase-mediated mispair synthesis is similar for each unnatural nucleotide in the template. In contrast, the efficiency of polymerase-mediated self-pair extension is highly dependent on the specific fluorine substitution pattern. The most promising unnatural base pair candidate of this series is the 3-fluorobenzene self-pair, which is replicated with reasonable efficiency and selectivity.     

The use of inverse gas chromatography to study surface thermal oxidation of polypropylene

Thermo-oxidative effects on the surface energy of polypropylene were measured by inverse gas chromatography as a function of exposure time and temperature. Unaltered polypropylene had a surface energy of 33 mJ/m². Oxidized polypropylene, after exposure to air at temperatures of 100 °C and 110 °C, had a range of maximum surface energies from 38 to 41 mJ/m². Comparisons between FTIR carbonyl peak growth and the surface energy showed that both methods detect oxidation, though the increase in surface energy is detected before the carbonyl peak growth is noticeable. The work of adhesion predicted by the surface free energies obtained in this work between a coated calcium carbonate and polypropylene changes by 10% due to the oxidation of the polymer at 110 °C.     

Redetermination of the lanthanum iron sulfide La52Fe12S90

A redetermination of the structure of `La_32.66Fe₁₁S₆₀' in the trigonal space group Rm led to the new formula La₅₂Fe₁₂S₉₀ and to a redefinition of the structure type. In the structure, the Fe²⁺ cations occur in Fe₂S₉ dimers of face‐sharing octa­hedra (with 3m symmetry). The dimers are linked by face‐ and vertex‐sharing bi‐ and tricapped LaS₆ trigonal prisms (with m symmetry) to form a three‐dimensional network containing two types of cubocta­hedral cavities. The larger cavities remain empty, while the smaller ones accommodate alternative sites for disordered La³⁺ cations.     

Synthesis of an unsymmetrically doubly bridged calix[4]arene in the 1,3-alternate conformation

We report the synthesis of the first calix[4]arene constrained to a 1,3-alternate conformation by one crown ether and one di-aza-benzo crown ether bridgings. Preliminary binding properties are also given.