Specific features of separate and joint mastication of natural and 1,4-cis-butadiene rubbers in the presence of dibenzoylaminodiphenyl disulfide

Variation of the molecular structure characteristics and properties of natural and 1,4-cis-polybutadiene rubbers (gel content, molecular weight, degree of branching of macromolecules, viscosity) in the course of their separate and joint mastication in the presence of dibenzoylaminodiphenyl sulfide as mastication accelerator or without it was studied.     

Methods in carbon K-edge NEXAFS: Experiment and analysis

Near-edge X-ray absorption spectroscopy (NEXAFS) is widely used to probe the chemistry and structure of surface layers. Moreover, using ultra-high brilliance polarised synchrotron light sources, it is possible to determine the molecular alignment of ultra-thin surface films. However, the quantitative analysis of NEXAFS data is complicated by many experimental factors and, historically, the essential methods of calibration, normalisation and artefact removal are presented in the literature in a somewhat fragmented manner, thus hindering their integrated implementation as well as their further development. This paper outlines a unified, systematic approach to the collection and quantitative analysis of NEXAFS data with a particular focus upon carbon K-edge spectra. As a consequence, we show that current methods neglect several important aspects of the data analysis process, which we address with a combination of novel and adapted techniques. We discuss multiple approaches in solving the issues commonly encountered in the analysis of NEXAFS data, revealing the inherent assumptions of each approach and providing guidelines for assessing their appropriateness in a broad range of experimental situations.     

Deep trench etching in macroporous silicon

We present a method to create at the same time trenches and ordered macropore arrays during photo-electrochemical etching of n-type silicon. This novel method allows in situ separation of single devices with a submicrometer precision. It also enables new device structures in macroporous silicon in the areas of photonics, sensing and electronics. The limits of this new process are simulated using electrostatic models and are verified experimentally. PACS 82.45.Yz; 81.16.-c     

Differentiation of chiral phosphorus enantiomers by P and H NMR spectroscopy using amino acid derivatives as chemical solvating agents

The ability of commercially available amino acid derivatives, especially Fmoc-Trp(Boc)-OH, to differentiate enantiomers of chiral phosphonates, phosphinates, phosphates, phosphine oxides, and phosphonamidates is demonstrated with (31)P, (13)C, and (1)H NMR spectroscopy. The chiral differentiation provided a rapid and convenient method for measuring the enantiomeric purity of these phosphorus compounds.     

Self-inhibition or the lack of it in the pyrolyses of neopentane and n-hexane

Published data show that in its early stages (up to 3% decomposition), the pyrolysis of n-hexane in the ranges 723–823 K and 10–100 Torr is not inhibited by the olefin products, in contrast with neopentane pyrolysis which is very strongly inhibited in similar conditions. Detailed consideration of the chain mechanisms for the two pyrolyses shows that the reactivity of the chain terminating radical towards hydrogen abstraction from an allylic C? H bond in product olefin is the factor which determines whether or not observable self-inhibition occurs. Thus, n-hexane pyrolysis, whose chain decomposition is terminated by recombination and disproportionation of ethyl, is not significantly self-inhibited, whereas that of neopentane which is terminated by recombination of methyl is very strongly inhibited because methyl is 14× more reactive than ethyl. The implications for other alkanes are briefly discussed.     

HPLC studies of isomeric chromium-N-benzoylphenylhydroxylaminates

Summary N-Benzoylphenylhydroxylarnine complexes of some metals have been investigated by HPLC. The green chromium complex formed by this reagent shows conclusive evidence of the presence of geometrical isomers. It is photosensitive and changes to a brown modification when irradiated with ultra violet or visible light. Elution behaviour of the complexes has been studied with different solvent mixtures. Attempts have been made to characterize the complexes from different measurements.

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Untersuchung von isomeren Chrom-N-benzoylphenylhydroxylaminaten durch HPLC

     

High reliability atomic absorption spectrometry of major and minor elements in biological materials

Summary Reliable analytical information is of fundamental importance for decisions of far-reaching impact in many regulatory, medical and scientific areas and disciplines. It is however at times elusive. Although the technique of atomic absorption spectrometry (AAS) as become widely established in analytical laboratories throughout the world for the determination of inorganic elements, only few AAS-based methods have reached official status and even fewer have attained reference method status. Research is underway to delineate impacts of a number of parameters on method performance to lead to protocols for standard and reference flame AAS (FAAS) methods for the reliable measurement of major and minor levels of elements of nutritional and toxicological pertinence in clinical and biological materials. Factors investigated include preparation of standards, calibration techniques, sampling and sample decomposition, solution preparation, instrumental parameters, and measurement protocols. Examples of some pronounced effects of sample decomposition and calibration techniques are presented as well as indications of the excellent performance of well-applied AAS procedures determined by use of standard reference materials and comparison with other techniques of analysis. Reference will be made to the determination of the major and minor nutrient elements Na, K, Mg, Ca, Mn, Fe, Cu and Zn in plant biological reference materials.Formerly at Plant Research Centre, Agriculture Canada, Ottawa, Ontario K1A OC6, CanadaContribution No. 1030 from Plant Research Centre