Endocyclic P-P bond cleavage in carbaborane-substituted 1,2-diphosphetane: a new route to secondary phosphinocarbaboranes

Carbaborane-substituted 1,2-diphosphetane reacts with elemental lithium and hydrogen chloride to give exclusively secondary mono- and bis(phosphino)carbaboranes. The latter reacts with two equivalents of formaldehyde and one equivalent of aniline to give a carbaborane-substituted 1-aza-3,6-diphosphepane.     

Allocation of the particle concentration for the SPH-method

In this paper a method is presented to optimize the number of particles in three-dimensional computations using the SPH method, based on the nearest neighbour. The process is presented for the breaking dam problem. (© 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim)     

High-performance liquid chromatography profiling of the major carotenoids in Arabidopsis thaliana leaf tissue

Carotenoids are extremely sensitive to a variety of physico-chemical attacks which may have a profound effect on their characteristic properties, thereby influencing the accurate identification and quantification of individual compounds. In this light, a comprehensive summary of the pitfalls encountered and precautions to be administered during handling and storage of authentic standards and samples was found to be incomplete. Furthermore, acceptable baseline separation of trans-lutein from trans-zeaxanthin and between the cis- and trans-forms of neoxanthin and violaxanthin has not been satisfactorily demonstrated. Hence the most optimal sample preparation and analytical steps were determined and a sensitive and reproducible method for the quantitative HPLC profiling of the principal carotenoids found in plant leaf tissue was developed. A reverse-phase C(30) column with a binary mobile solvent system was used for the baseline separation of eight of the major carotenoids and the two chlorophylls (a and b) within 18min. These compounds were identified via the use of authentic standards, their spectral characteristics and HPLC-atmospheric pressure chemical ionization (APCI)-mass spectrometry (MS) confirmation. This method has been successfully applied for the quantification of plant pigments in Arabidopsis thaliana wild-type (WT) leaf tissue and in two A. thaliana non-photochemical mutants, namely npq1 and npq2. These mutants have previously been well-characterised and provided valuable reference data as well as acting as internal controls for the assessment of our new method.     

Preparation of Magnesium,Cobalt and Nickel Ferrite Nanoparticles from Metal Oxides using Deep Eutectic Solvents

Natural deep eutectic solvents (DESs) dissolve simple metal oxides and are used as a reaction medium to synthesize spinel‐type ferrite nanoparticles MFe₂O₄ (M=Mg, Zn, Co, Ni). The best results for phase‐pure spinel ferrites are obtained with the DES consisting of choline chloride (ChCl) and maleic acid. By employing DESs, the reactions proceed at much lower temperatures than usual for the respective solid‐phase reactions of the metal oxides and at the same temperatures as synthesis with comparable calcination processes using metal salts. The method therefore reduces the overall required energy for the nanoparticle synthesis. Thermogravimetric analysis shows that the thermolysis process of the eutectic melts in air occurs in one major step. The phase‐pure spinel‐type ferrite particles are thoroughly characterized by X‐ray diffraction, diffuse‐reflectance UV/Vis spectroscopy, and scanning electron microscopy. The properties of the obtained nanoparticles are shown to be comparable to those obtained by other methods, illustrating the potential of natural DESs for processing metal oxides.     

Establishment of a novel in vitro test setup exposing adherent cells to wear particles made of polyethylene

Wear debris from endoprostheses leads to osteolysis and causes aseptic loosening. Cellular interactions with ultra-high-molecular-weight polyethylene (UHMW-PE) particles are rarely described because of the difficulty of incubation of adherent cells with floating polyethylene particles in vitro.The aim of this study was to develop a technique for analysing interactions of adherent cells with UHMW-PE particles in vitro. Therefore, different volumes of a wear particle suspension, generated in a standard hip wear simulator, were digested and filtered through polycarbonate filters. The filters were applied to cell culture inserts cultivated with human osteoblasts. Particle analysis resulted in a significant reduction of particle numbers in different suspension volumes.Exposure to the highest particle density resulted in a significant decrease of collagen 1 synthesis as well as a tendency for increasing matrix metalloproteinase-1 (MMP-1) production. Therefore, involvement of osteoblasts in matrix degradation due to wear debris can be assumed.     

Standardization of fluorescence excitation-emission-matrices in aquatic milieu

Fluorescence excitation-emission-matrices (EEM) are a useful tool for water quality monitoring. Recent publications show the potential of the method for real time drinking water control. However, in fluorescence measurements there is still a need for standardization to make data interpretation comparable. In this work a standardization procedure based on excitation and emission correction as well as normalization and optional inner filter effect correction is presented. By measurements of humic acid and tryptophan standards with two different spectrometers (LS 50 and LS 55 by PerkinElmer) the procedure application leads to comparable fluorescence intensities with relative standard deviations (median) of 6.6-8.4% and 10.6-12.0%, respectively. These small differences are not avoidable even if all possible correction methods are implemented and constant measurement conditions are given. The used BAM kit for emission correction induced good agreement in peak shape not only for single wavelengths but also for the whole EEM. As a consequence it is necessary to use identical equipment and identical experimental conditions in order to apply this method in fields of water quality control if small changes of fluorescence intensities are relevant for data assessment.     

Molecular beam-controlled nucleation and growth of vertically aligned single-wall carbon nanotube arrays

The main obstacle to widespread application of single-wall carbon nanotubes is the lack of reproducible synthesis methods of pure material. We describe a new growth method for single-wall carbon nanotubes that uses molecular beams of precursor gases that impinge on a heated substrate coated with a catalyst thin film. In this growth environment the gas and the substrate temperature are decoupled and carbon nanotube growth occurs by surface reactions without contribution from homogeneous gas-phase reactions. This controlled reaction environment revealed that SWCNT growth is a complex multicomponent reaction in which not just C, but also H, and O play a critical role. These experiments identified acetylene as a prolific direct building block for carbon network formation that is an order of magnitude more efficient than other small-molecule precursors. The molecular jet experiments show that with optimal catalyst particle size the incidence rate of acetylene molecules plays a critical role in the formation of single-wall carbon nanotubes and dense vertically aligned arrays in which they are the dominant component. The threshold for vertically aligned growth, the growth rate, the diameter, and the number of walls of the carbon nanotubes are systematically correlated with the acetylene incidence rate and the substrate temperature.