Influence of higher harmonics of the undulator in X‐ray polarimetry and crystal monochromator design

The spectrum of the undulator radiation of beamline P01 at Petra III has been measured after passing a multiple reflection channel‐cut polarimeter. Odd and even harmonics up to the 15th order, as well as Compton peaks which were produced by the high harmonics in the spectrum, could been measured. These additional contributions can have a tremendous influence on the performance of the polarimeter and have to be taken into account for further polarimeter designs.     

First passage percolation and escape strategies

Consider first passage percolation on with passage times given by i.i.d. random variables with common distribution F. Let be the time from u to v for a path π and the minimal time among all paths from u to v. We ask whether or not there exist points and a semi‐infinite path such that for all n. Necessary and sufficient conditions on F are given for this to occur. When the support of F is unbounded, we also obtain results on the number of edges with large passage time used by geodesics. © 2014 Wiley Periodicals, Inc. Random Struct. Alg., 47, 414–423, 2015     

Direct detection of carrier traps in Si solar cells after light‐induced degradation

In solar cells fabricated from boron‐doped Cz‐Si wafers minority and majority carrier traps were detected by deep level transient spectroscopy (DLTS) after so‐called “light‐induced degradation” (LID). The DLTS signals were detected from mesa‐diodes with the full structure of the solar cells preserved. Preliminary results indicate metastable traps with energy levels positioned at E_V + 0.37 eV and E_C – 0.41 eV and apparent carrier capture cross‐sections in the 10^–17–10^–18 cm² range. The concentration of the traps was in the range of 10¹²–10¹³ cm^–3. The traps were eliminated by annealing of the mesa‐diodes at 200 °C. No traps were detected in Ga‐doped solar cells after the LID procedure or below the light protected bus bar locations in B‐doped cells. (© 2015 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)     

Platinum Carbonyl Clusters Chemistry: Four Decades of Challenging Nanoscience

The state of art of the chemical, spectroscopic and structural characterization of platinum carbonyl clusters is reviewed. We begin by enlightening the fundamental contribution given to this chemistry of two great scientists: Paolo Chini and Larry Dahl, two without equal maestros of science and life. We then focus the main body of this review on the challenge represented by studying molecular ions already belonging to the nano regime by size almost 50 years ago, and the challenges their chemistry continues to present also nowadays. In detail, the possible reasons which enable the [Pt_3n (CO)_6n ]^2? oligomers to grow up to n = 10, and why the oligomers with n > 5 may self-assemble in infinite molecular conductor wires are suggested. The interplay between the CO/Pt_surface ratios and electronic effects in driving the platinum cluster from pseudo one- to tri-dimensional globular structures, often representing chunks of the fcc metal lattice or interpenetrated pentagonal prisms and icosahedra, is examined by means of two significant examples. The nanocapacitor behavior of most high-nuclearity carbonyl clusters is briefly recalled and is confirmed by most recent results. The size-induced transition of their metal kernels from insulator to semiconductor and the expected consequences of their eventual transition to a metallic state are also discussed. Finally, we conclude by commenting the present lack of Pt cluster interstitially lodging a main group element and not yet quantitatively-assessed aggregation phenomena in solution, perhaps peculiar of ionic salts of carbonyl clusters, which could make undetectable the NMR signal of any spin-active nuclei beyond a cluster nuclearity of ca. 20–25.     

Surface Roughness Characterization of Poly(methylmethacrylate) Films with Immobilized Eu(III) β-Diketonates by Fractal Analysis

The structural complexity of the 3-D surface of poly(methylmethacrylate) films with immobilized europium β-diketonates was studied by atomic force microscopy and fractal analysis. Fractal analysis of surface roughness revealed that the 3-D surface has fractal geometry at the nanometer scale. Poly(methylmethacrylate) (PMMA) as immobilization matrix is dense and uniform, and a tendency for formation of chain structures was observed. Fractal analysis can quantify key elements of 3-D surface roughness such as the fractal dimensions D _f determined by the morphological envelopes method of the Eu(DBM)₃ and Eu(DBM)₃ · dpp nanostructures, which are not taken into account by traditional surface statistical parameters.     

HPLC‐MS/MS method for quantitative determination of the novel dual inhibitor of FGF and VEGF receptors E‐3810 in tumor tissues from xenograft mice and human biopsies

We developed and validated a high‐performance liquid chromatography–tandem mass spectrometry analytical method to measure E‐3810, a novel dual inhibitor of fibroblast growth factor receptor 1 and vascular endothelial growth factor receptor 1–3 in tissues and determined the drug concentration in a biopsy of human breast cancer for the first time. The method is a modification of our previous one in plasma to study the clinical pharmacokinetics of the drug during the phase I/II trial. In view of the changes in matrix, we applied a partial validation protocol to determine recovery, sensitivity, range of linearity, precision, accuracy and stability of the method over three runs in a mouse tumor tissue and liver. The recovery of E‐3810 from liver or tumor homogenate was >69%, and the lower limit of quantification was 5 ng/ml. The method was linear in the concentration range 5.0–500.0 ng/ml, as demonstrated by a determination coefficient R² ≥ 0.9955. The range of the calibration curve was appropriate for the analysis, as demonstrated by the accuracy, which was between 91.4% and 106.7%. Interday precision and accuracy on quality control samples at 9, 30 and 300 ng/ml were 3.1‐11.2% and 98.3–111.4%, respectively. The assay was applied successfully to determine the intratumor concentration of E‐3810 in different mouse xenograft tumor models and in a biopsy of a patient with breast cancer included in the phase I/II trial of the drug. In mouse tumors, the concentrations of E‐3810 were higher than necessary to exert antitumor activity in vitro (1 µM). Even more of interest was the result obtained in a human biopsy of few milligrams, where E‐3810 reached 4.9 µg/g (11 µM). Copyright © 2014 John Wiley & Sons, Ltd.     

Thermal and structural investigation of random ethylene/1-hexene copolymers with high 1-hexene content

Random ethylene/1-hexene copolymers with the 1-hexene content in the range from 2 to 28 mol% were produced with a novel post-metallocene catalyst and analyzed by three techniques, FTIR, ¹³C NMR, and DSC. The 1-hexene content and the sequence distribution in the copolymers were determined by means of FTIR-M and ¹³C NMR. The crystallization behavior of the copolymers was studied by DSC under dynamic and isothermal conditions; the Avrami model was used to analyze the crystallization kinetics. It was found that both the 1-hexene content and the crystallization temperature affect the relative crystallinity. The bulk crystallization rate decreases with the 1-hexene content and reduces exponentially with an increase of T _c. The melting behavior of isothermally crystallized samples was also investigated and it was found that the melting temperatures of the copolymers under equilibrium conditions were related to the composition.     

Studies on thermal,spectral, magnetic and biological properties of new Ni(II), Cu(II) and Zn(II) complexes with a bismacrocyclic ligand bearing an aromatic linker

Novel complexes of M₂LCl₄·nH₂O type (M:Ni, n = 4; M:Cu, n = 3 and M:Zn, n = 0; L: ligand resulted from 1,4-phenylenediamine, 3,6-diazaoctane-1,8-diamine and formaldehyde one-pot condensation) were synthesized and characterised by microanalytical, ESI–MS, IR, UV–Vis, ¹H NMR and EPR spectra, magnetic data at room temperature and molar conductivities as well. The electrochemical behaviour of complexes was investigated by cyclic voltammetry. Simultaneous TG/DTA measurements were performed in order to evidence the thermal behaviour of the obtained complexes. Processes such as water elimination, fragmentation and oxidative degradation of the organic ligand as well as chloride elimination occurred during thermal decomposition. The antimicrobial assays demonstrate that the compounds exhibited good antibacterial activity, especially against S. aureus and E. coli strains, the most active being the copper(II) complex, which also exhibited the most prominent anti-biofilm effect, suggesting its potential use for the development of new antimicrobial agents. The biological activity was correlated with log P _ow values. All complexes disrupt the membrane integrity of HCT 8 tumour cells.     

Characterization of Pentaclethra macroloba oil

The Pracaxi oil—(Pentaclethra macroloba) contains high concentrations of fatty acids with emollient action that contribute to skin hydration. The use of this oil is supported by the utilization of natural resources thus enabling regional development and social contribution. The objective of this study was to characterize the P. macroloba oil by thermogravimetry (TG, DTG, and DTA), gas chromatography, Fourier transform infrared spectroscopy (FT-IR), and oxidation stability—Rancimat, aiming at the quality control of plant raw material. Three samples of crude oil sold by Amazon Oil Industry (Ananindeua, Pará, Brazil) were studied. The analysis of these oil samples showed different fatty acids, especially the behenic, oleic, linoleic, and lignoceric acids totalizing approximately 96 % of the grease composition and in smaller percentage arachidic, lauric, myristic, palmitic, and linolenic acids were found. The major acids have wide medicinal use. According to the TG/DTG curve, thermal stability was observed up to 220 °C, indicating a greater mass loss related to the dehydration and elimination of volatile substances. The thermal decomposition process occurred in the range of 430–450° C according to the DTG curve. The absorption spectrum in the infrared region (FT-IR) showed well-defined bands confirming the presence of functional groups present in the oil. Tests in a Rancimat have shown an induction period between 8 and 10 h demonstrating that the samples are in agreement with the standards required by ANP No. 14/2012 which requires at least 6 h of testing.