A thermal decomposition study of some nickel(II)thioureachloride complexes

TG/DTA and Thermal Degradation Mass spectrometry (TDMS) data are presented for a series of nickel(II)thiourea chloride complexes: NiL₄Cl₂:L=thiourea or methyl-, dimethyl-, tetramethyl-, di-n-butyl, naphthyl-, ethylene- or allylthiourea. Two different thermal decomposition mechanisms are proposed for these complexes, and it is apparent that the thermal decomposition mechanism adopted by a particular complex depends on the structure of the relevant thiourea ligand and not on the nature of the halide ligand or on the existence of geometrical isomerism for these complexes.

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Zusammenfassung Durch TG, DTA und thermodegradative Massenspektrometrie (TDMS) von Nickel(II)-thioharnstoff-chlorid-Komplexen, NiL₄Cl₂ (L=Thioharnstoff oder Methyl-, Dimethyl-, Tetramethyl-, Di-n-butyl-, Naphthyl-, Vinyl- oder Allylharnstoff), erhaltene Daten werden angegeben. Zwei verschiedene Mechanismen werden für die thermische Zersetzung vorgeschlagen. Es ist offensichtlich, daß der Mechanismus, nach der die thermische Zersetzung eines gegebenen Komplexes verläuft, von der Struktur des relevanten Thioharnstoffliganden und nicht von der Natur des Halidliganden oder vom Vorliegen einer geometrischen Isomerie abhängt.

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/ - NiL₄Cl₂, L= , -, -, -, ---, -, - . . , .

     

Multifunctional Reagents for Quantitative Proteome‐Wide Analysis of Protein Modification in Human Cells and Dynamic Profiling of Protein Lipidation During Vertebrate Development

Novel multifunctional reagents were applied in combination with a lipid probe for affinity enrichment of myristoylated proteins and direct detection of lipid‐modified tryptic peptides by mass spectrometry. This method enables high‐confidence identification of the myristoylated proteome on an unprecedented scale in cell culture, and allowed the first quantitative analysis of dynamic changes in protein lipidation during vertebrate embryonic development.     

STEM (scanning transmission electron microscopy) analysis of femtosecond laser pulse induced damage to bulk silicon

This work reports on the structural changes that take place in wafer grade silicon when it is micro-machined with ultra-short laser pulses of 150 fs duration. A Chirped Pulse Amplification (CPA) Ti:Sapphire laser was used, with an operating wavelength centered on 775 nm and a maximum repetition rate of 1 KHz. The laser induced damage was characterized over the fluence range 0.43–14 Jcm^-2, and for each fluence a progressively increasing number of pulses was used. The analytical tools used to characterize the samples were all based upon electron microscopy. A 30 KeV scanning transmission electron microscope (STEM) imaging technique was developed to observe defects in the crystal lattice and the thermal-mechanical damage in the area surrounding the laser machined region. Mechanical cross sectioning (in conjunction with Scanning Electron Microscope (SEM) surface imaging) was also used to reveal the internal structure, composition, and dimensions of the laser machined structures. Based on this analysis, it will be shown that laser machining of silicon with femtosecond pulses can produce features with minimal thermal damage, although lattice damage created by mechanical stresses and the deposition of ablated material both limit the extent to which this can be achieved, particularly with high aspect ratios. A key feature of the work presented here is the high-resolution STEM images of the laser-machined structures. PACS  42.65.Re; 42.62.Cf; 61.80.Ba; 61.82.Fk; 68.37.Hk; 68.37.Lp     

The effect of dissolved water on the viscosities of hydrophobic room-temperature ionic liquids

Data for viscosity vs. water content for three hydrophobic room-temperature ionic liquids show that their viscosities are strongly dependent on the amount of dissolved water.     

Analysis of gases and vapours by spectroscop1c techniques—I Emission spectroscopy

Theoretical and experimental aspects of the analysis of gases and vapours by emission spectroscopy are discussed and the current literature on molecular emission spectroscopy is reviewed.     

Infrared spectra for the identification of some inorganic anions using nitron as precipitant

Summary Using infrared absorption spectroscopy a method has been developed which permits the identification, either singly or in admixture, of the following anions: ferrocyanide, ferricyanide, cobalticyanide, chlorate, bromate, perchlorate, periodate, nitrate, nitrite, tungstate, molybdate and chromate. The anions are precipitated by nitron, and using the KBr-disc technique characteristic bands are obtained in the near infrared.

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Zusammenfassung Durch Infrarotabsorptionsspektroskopie lassen sich entweder allein oder in Gemischen folgende Anionen identifizieren: Cyanoferrat(II), Cyanoferrat(III), Cyanokobaltat, Chlorat, Bromat, Perchlorat, Perjodat, Nitrat, Nitrit, Wolframat, Molybdat und Chromat. Die Anionen werden mit Nitron gefällt und geben bei Verwendung einer Kaliumbromid-Linse charakteristische Banden im nahen Infrarot.

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Résumé On a développé une méthode permettant l'identification par spectrographie d'absorption infrarouge des anions suivants, séparément ou en mélanges: ferrocyanure, ferricyanure, cobalticyanure, chlorate, bromate, perchlorate, periodate, nitrate, nitrite, tungstate, molybdate et chromate. On précipite les anions par le nitron et l'on met en évidence les bandes caractéristiques dans l'infrarouge proche, par la technique à la pastille de KBr.

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Dedicated to ProfessorA. A. Benedetti-Pichler on the occasion of his 70th birthday.

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One of us (S. A. E. S.) acknowledges gratefully the award of a scholarship from the U. A. R. Government, which has enabled him to take part in this work.     

The post-hydrogenation of low-pressure chemical vapor deposited amorphous silicon

Amorphous silicon films prepared by low pressure chemical vapor deposition were exposed to atomic hydrogen in an rf plasma. Concentrated hydrogen and 20% hydrogen in argon was used for the plasma. The hydrogen concentration as a function of depth was measured for various process parameters with secondary ion mass spectrometry (SIMS). Hydrogenation temperatures of 250 to 400°C and exposure times from 30–120 min were used. The hydrogen surface concentration varied between 4 and 10 at%, whereby the higher values were obtained with plasma treatments in concentrated hydrogen.The fit of an error function diffusion profile to the experimentally measured SIMS concentration results in a diffusion coefficient at 400°C of D = 6 × 10^?14 cm² s^?1.     

Determination of human immunodeficiency virus-1 protease inhibitors in patient serum using free solution capillary zone electrophoresis.

The goal of this study was to develop a fast, inexpensive and quantitative method for serum determination of the human immunodeficiency virus protease inhibitors Crixivan (C), Viracept (V), Invirase (I) or Fortovase (F), and Norvir (N), using common conditions for isolation and analysis. The best separation procedure developed thus far involves uncoated silica capillary and a buffer containing formic acid and acetonitrile. This procedure allows us to analyze three drugs (C, V and I or F) in 15 min. Norvir requires different analytical conditions. These four drugs are isolated from patient sera with a mixture of ethyl acetate and hexane. Sensitivity of the capillary zone electrophoresis protocols is sufficient for the detection of these pharmacological agents at the lowest clinically relevant concentrations (0.1 microgram/ml).