Mass‐Spectrometric Observation of Counter Anion Production in SU‐8 Exposed to UV Light and its Use for Dill C Parameter Determination

Photopolymerization is a phenomenon that is the basis of much of today's microfabrication technology and intense research is conducted to improve its control and the characteristics of end products for a variety of applications. The design of microscopic structures often relies on the accurate knowledge and modeling of photopolymer's behavior upon exposure, i.e. the Dill parameters, for each radiation species of interest and therefore the development of flexible characterization techniques is of great importance. SU‐8 is a popular compound that is representative of a whole class that relies on cationic polymerization, where an acid is obtained via photolysis of an onium salt during exposure. Here we report on the observation of SbF₆^? via laser desorption mass spectrometry on SU‐8 exposed to UV light at the wavelength of 365 nm and demonstrate that the yield of this counter‐anion as a function of exposure is consistent with the Dill C parameter value available in the literature. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2019 , 57, 967–972     

Brodie's or Hummers’ Method: Oxidation Conditions Determine the Structure of Graphene Oxide

Synthesis and studies of graphite oxide started more than 150 years ago and turned into a boom by the measurements of the outstanding physical properties of graphene. A series of preparation protocols emanated trying to optimize the synthesis of graphene oxide in order to obtain a less defective material, as source for graphene. However, over-oxidation of the carbon framework hampered establishing structure-property relationships. Here, the fact that two different synthetic methods for graphene oxide preparation lead to very similar types of graphene oxide with a preserved graphene lattice is demonstrated. Either sodium chlorate in nitric acid (similar to Brodie's method) or potassium permanganate in sulfuric acid (similar to Hummers’ method) treatment are possible; however, reaction conditions must be controlled. With a preserved carbon lattice analytical differences between the samples relate to the altered on-plane functionality. Consequently, terming preparation protocols “according to Brodie's/Hummers’ method” is not sufficient.     

Tuning the Product Spectrum of a Glycoside Hydrolase Enzyme by a Combination of Site-Directed Mutagenesis and Tyrosine-Specific Chemical Modification

Selective chemical modification of proteins plays a pivotal role for the rational design of enzymes with novel and specific functionalities. In this study, a strategic combination of genetic and chemical engineering paves the way for systematic construction of biocatalysts by tuning the product spectrum of a levansucrase from Bacillus megaterium (Bm-LS), which typically produces small levan-like oligosaccharides. The implementation of site-directed mutagenesis followed by a tyrosine-specific modification enabled control of the product synthesis: depending on the position, the modification provoked either enrichment of short oligosaccharides (up to 800 % in some cases) or triggered the formation of high molecular weight polymer. The chemical modification can recover polymerization ability in variants with defective oligosaccharide binding motifs. Molecular dynamic (MD) simulations provided insights into the effect of modifying non-native tyrosine residues on product specificity.     

An LC–MS/MS method for quantification of HR011303, a novel highly selective urate transporter 1 inhibitor in beagle dogs and the application to a pharmacokinetic study

HR011303 is a novel and highly selective urate transporter 1 (URAT1) inhibitor. In this study, a sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for quantification of HR011303 in beagle dog plasma. Plasma samples were pretreated with protein‐precipitation extraction by acetonitrile and added with a trifluoromethyl substituted analog of HR011303 as internal standard. The chromatographic separation was performed on a Shiseido C₁₈ column (100 × 4.6 mm, i.d., 5 μm) by mobile phases consisting of 5 mm ammonium–formic acid (100:0.1) and acetonitrile–formic acid (100:0.1) solutions in gradient elution. The MS detection was conducted in electrospray positive ionization with multiple reactions monitoring at m/z 338 → 240 for HR011303 and m/z 328 → 230 for the internal standard using 25 eV argon gas collision induced dissociation. The established LC–MS/MS method showed good selectivity, sensitivity, precision and accuracy. The plasma pharmacokinetics of HR011303 in beagle dogs following both oral and intravenous administration were then successfully evaluated using this LC–MS/MS method.     

Structural and phase characteristics of the diamond/matrix interfacial zone in high-resistant diamond composites

The structural-phase state of the contact zone and the factors that influence on the strength of diamond retention in the diamond carbide composites were determined. Composites were obtained by the new hybrid technology that eliminates the reheating of the metalized coating. The elaborated technology combines the thermal diffusion metallization of a diamond and the sintering by the scheme of self-dosed impregnation in a one-stage technological cycle. By the methods of electron microscopy, X-ray diffraction analysis, and Raman spectroscopy the structural and phase characteristics of the interphase boundary were investigated. The improvement of chemical and mechanical adhesion between the diamond and carbide matrix was obtained. It was shown that the specific productivity of the samples with a metalized diamond component is 39% higher than those without metallization.     

Sobolev spaces on Lie groups: Embedding theorems and algebra properties

Let G be a noncompact connected Lie group, denote with ρ a right Haar measure and choose a family of linearly independent left-invariant vector fields X on G satisfying Hörmander's condition. Let χ be a positive character of G and consider the measure ${\mu }_{\chi }$ whose density with respect to ρ is χ. In this paper, we introduce Sobolev spaces $L_{\alpha }^p({\mu }_{\chi })$ adapted to X and ${\mu }_{\chi }$ ($1<p<\infty$, $\alpha \ge 0$) and study embedding theorems and algebra properties of these spaces. As an application, we prove local well-posedness and regularity results of solutions of some nonlinear heat and Schrödinger equations on the group.     

Electrical Impedance Spectroscopic Study of CNT/Ethylene-alt-CO/Propylene-alt-CO Polyketones Nanocomposite

Impedance spectroscopy was utilized to investigate the dielectric properties, ac conductivity and charge transport mechanisms in propylene-alt-CO/ethylene-alt-CO (EPEC) random terpolymer filled with multi-walled carbon nanotubes (MWCNT) as a function of nanofiller content, frequency, and temperature. Equivalent resistor-capacitor (RC) circuit models were proposed to describe the impedance characteristics of the unfilled terpolymer and the nanocomposite at different temperatures. For the nanocomposites, the ac conductivity tended to be frequency independent at low frequencies. At high frequencies, the ac conductivity increased with frequency. The dc conductivity (i.e., plateau of the ac conductivity at low frequencies) at room temperature increased from 10^?9 (Ω·m)^?1 for the unfilled polymer to l0^?3 (Ω·m)^?1 for the 6 wt% MWCNT/EPEC nanocomposite. At low temperatures, the equivalent RC model for EPEC-0 and EPEC-2 was found to consist of a parallel RC circuit. However, for 6 wt% MWCNT/EPEC nanocomposite, an RC model consisting of an R/constant phase element (CPE) circuit and a resistor in series was required to describe the impedance behavior of the nanocomposite.