A computer system for measuring fast-scan lowresolution mass spectra

A microprocessor-based satellite computer system (MASDAT) controls a low-resolution, fast-scan mass spectrometer for the measurement of series of spectra. Special digitization hardware (logarithmic A/D converter) and software algorithms are necessary to achieve a dynamic range (ratio of highest to lowest intensity) of about 10⁵ in peak heights. Up to three MASDAT satellites can be connected to a host computer. Synchronized parallel programs in the host system communicate with the operator, calibrate the mass scale, print an interscan report, and store final spectra and, optionally, unreduced data on mass storage devices. Host software is described for a RSX11M and for a VAX/VMS operating system.     

Beiträge zur Chemie des Siliciums und Germaniums. XVII. Über die Aufbewahrung von Silanen in Behältern aus Stahl

For the storage of raw silane and silane isomeres isolated by distillation or gaschromatographic separation, 40 Mn 4-steel vessels are proposed. A metallographic analysis of a steel vessel containing silanes over a period of six years shows only a small partiel decarbonization of the material up to a depth of 200–250 μm. Decomposition of the silane was not observed.     

Colachrom,a command language for chromatographic data processing

A command language for the interactive computer processing of chromatograms is described. Report data files, resulting from a peak evaluation program, are processed with single-line commands. Reference peaks for quantitative evaluation or for retention index calculations can be specified, compound names or response factors be assigned, etc. Customer-specific reports can be generated. Several commands operate on the unreduced digitized chromatograms, e.g., repeat peak evaluation with modified peak search parameters or with a user-corrected baseline. Commands can be combined into procedures for semi-automatic processing of series of chromatograms. Various forms of interactive graphical presentations supplement the command language.     

Spektroskopische und physikalische Daten von Jodsilanen

Zusammenfassung Von den Jodderivaten der Silane SiH₄, Si₂H₆ und Si₃H₈ werden Dichte, Dampfdruck und Molrefraktion sowie die entsprechenden Atom- und Bindungsinkremente mitgeteilt. Die Ramanspektren von SiH₃J, Si₂H₅J und Si₃H₇J werden aufgenommen und zugeordnet.

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Spectroscopic and other physical investigations of silanyl iodides

Density, vapour pressure and molecular refraction as well as the corresponding atom increments and bond increments of the iodine derivatives of the silanes SiH₄, Si₂H₆ and Si₃H₈ are communicated. The Raman spectra of SiH₃J, Si₂H₅J and Si₃H₇J are recorded and assigned.

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XX. Mitt.:F. Fehér, B. Mostert, A. G. Wronka undG. Betzen, Mh. Chem.103, 959 (1972).

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A. G. Wronka, Dissertation Univ. Köln 1961.

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B. Mostert, Dissertation Univ. Köln 1961.     

Präparative Darstellung von Disilanyl- und Trisilanyljodiden

Zusammenfassung Die Darstellung von Si₂H₅J sowie von Si₂H₄J₂ (SiH₃–SiHJ₂+SiH₂J–SiH₂J), Si₃H₇J (SiH₃–SiH₂–SiH₂J+SiH₃–SiHJ–SiH₃) und Si₃H₆J₂ (Isomerengemisch) durch Umsetzung der entsprechenden Silane mit elementarem Jod (ohne Verwendung eines Lösungsmittels) wird mitgeteilt. Durch katalytische Mengen Alkohol wird die Reaktion von Jod mit Silanen beschleunigt, gleichzeitig jedoch die Spaltung der Si–Si-Bindung gefördert.

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Preparation of disilanyl iodide and trisilanyl iodide

The preparation of Si₂H₅J as well as Si₂H₄J₂ (SiH₃–SiHJ₂+SiH₂J–SiH₂J), Si₃H₇J (SiH₃–SiH₂–SiH₂J+SiH₃–SiHJ–SiH₃) and Si₃H₆J₂ (isomeric mixture) by reaction of the corresponding silanes with elementary iodine without using a solvent is communicated. The reaction of iodine with silanes is accelerated by catalysings amounts of alcohol. At the same time, however, the cleavage of the Si–Si-bond is stimulated.

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Mit 3 Abbildungen

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19. Mitt.:F. Fehér, D. Schinkitz undH. Strack, Z. anorg. allgem. Chem.385, 202 (1971).

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B. Mostert, Dissertation Univ. Köln 1961.

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A. G. Wronka, Dissertation Univ. Köln 1961.

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G. Betzen, Dissertation Univ. Köln 1967,G. Betzen, Diplomarbeit Univ. Köln 1963.     

Structural,thermal, and electrical properties of carbonaceous films containing palladium nanocrystals

Carbonaceous films containing Pd nanocrystals can be applied as active layers in gas sensor applications. In this article we show results of studies of C-Pd films, obtained with two different methods: (1) physical and (2) physical + chemical deposition. First type of film prepared by physical vapor deposition (PVD) process was composed of fullerenes, amorphous carbon, and palladium nanograins. In the second method PVD film was modified in chemical vapor deposition (CVD) process forming a foam-like structure. Both types of films were studied by SEM, TEM, TGA, and electrical characterization (measurement of resistivity versus composition of gaseous hydrocarbons mixture).     

Chromatographic Study of Novel Heteronuclear Complexes with Schiff Base as Main Ligand

The properties of 12 new heterodi- and heterotrinuclear complexes having general formulae [Cu₂Ln(L)₂(NO₃)(H₂O)₂](NO₃)₂·3H₂O [where Ln = Pr (1), Nd (2), Sm (3) and Eu (4)], and [CuLn(L)(NO₃)₂(H₂O)₃MeOH]NO₃·MeOH [where Ln = Gd (5), Tb (6), Dy (7), Ho (8), Ef (9), Tm (10), Yb (11) and Lu (12)], and their main ligand [L = C₁₉H₁₈N₂O₄Br₂ = N,N’-bis(5-bromo-3-methoxysalicylidene)propylene-1,3-diamine] have been characterized by chromatographic analyses. The parameter of relative lipophilicity (R _M0) of the tested compounds was determined experimentally by reversed-phase high-performance thin layer chromatography method with mixtures of methanol and water as a mobile phase. We also described interactions between chromatographed substances and various surfaces (silica—SiO₂ and modified by hydrocarbon chains—RP-2, RP-8, RP-18 phases). This study also investigates the effect of pH of the mobile phase on the retention on the polar stationary phase. Thin layer chromatography combined with magnetic and electric field has been proposed as a complementary method for the determination of physicochemical properties of the investigated compounds. The chromatograms in the field and outside of it were developed simultaneously in three identical chromatographic chambers. One of them was placed in external magnetic field of 0.4 T inductivity, and the second in external electrical field. In magnetic and electric fields, retention of some complexes changed, which indicated that the presence of these fields influenced physicochemical properties of the compounds and their interactions with the stationary phase.     

Reduction processes in the fast atom bombardment mass spectrometry of sulfonyl esters of diazonaphthalenones

Orthoquinone diazides, which are widely used in microlithography, have attracted considerable attention, especially in terms of their application in the production of high-contrast resists. Previous electron impact mass spectrometric results have confirmed that the primary fragmentation process of these compounds is the elimination of N₂ to form an indenoketene ion. This is analogous to the photodecomposition pathway which makes them effective in the lithographic process. Those results also revealed the occurrence of an alternative process, which involves a two-hydrogen reduction of the intermediate species formed prior to conversion to the ketene. The present study investigates the behaviour of the orthoquinone diazides when there is an abundance of protons available to form the reduction product. Several different types of diazonaphthalenone sulfonyl esters, ranging in complexity from the monosubstituted phenol esters to disubstituted dihydroxybenzophenones, were examined using fast atom bombardment mass spectrometry. Although reduction was the primary process in the hydrogen-rich matrices, the extent of reduction was characteristic of the particular isomer as well as the matrix used.     

Influence of high vacuum annealing treatment on some properties of carbon nanotubes

Carbon nanotubes (CNTs) were synthesized using a chemical vapour deposition (CVD) method. The properties of CNTs before and after vacuum annealing treatment were studied using scanning electron microscopy (SEM), scanning tunneling microscopy/spectroscopy (STM/STS) and thermogravimetric analysis (TG). Field emission characteristics of the raw and vacuum heated (up to 650°C) carbon nanotube films (CNTFs) were measured in a diode system. Emissive properties of the CNTFs depend on an annealing process during which structural changes in the nanotube walls take place. The structural changes, related to saturation of dangling bonds, influence a rate of oxidation process and also improve the emissive field properties.