On the underestimated influence of synthetic conditions in solid ionic conductors

The development of high-performance inorganic solid electrolytes is central to achieving high-energy- density solid-state batteries. Whereas these solid-state materials are often prepared via classic solid-state syntheses, recent efforts in the community have shown that mechanochemical reactions, solution syntheses, microwave syntheses, and various post-synthetic heat treatment routines can drastically affect the structure and microstructure, and with it, the transport properties of the materials. On the one hand, these are important considerations for the upscaling of a materials processing route for industrial applications and industrial production. On the other hand, it shows that the influence of the different syntheses on the materials'' properties is neither well understood fundamentally nor broadly internalized well. Here we aim to review the recent efforts on understanding the influence of the synthetic procedure on the synthesis – (micro)structure – transport correlations in superionic conductors. Our aim is to provide the field of solid-state research a direction for future efforts to better understand current materials properties based on synthetic routes, rather than having an overly simplistic idea of any given composition having an intrinsic conductivity. We hope this review will shed light on the underestimated influence of synthesis on the transport properties of solid electrolytes toward the design of syntheses of future solid electrolytes and help guide industrial efforts of known materials.

Influence of synthesis and processing on the nature of ultimate product and the ionic transport properties of superionic conductors.     

Reaction of γ-picoline N-oxide with ketenimines in the presence of organic acids: Preparation of α-acyloxyamides

A synthesis of a-acyloxyamides is described which utilizes the reaction of 7-picoline N-oxide and various organic acids with diphenylketene N-p-tolylimine.     

The synthesis of phenanthrodibenzothiophenes

The synthesis of phenanthro[1,2-c]dibenzothiophene (6) , phenanthro[4,3-c]dibenzothiophene (10) , phenanthro[2,1-a]dibenzothiophene (14) , phenanthro[3,4-a]dibenzothiophene (16) , phenanthro[1,2-a]dibenzothiophene (19) , phenanthro[2,1-b]dibenzothiophene (20) , 8-methylphenanthro[3,2-a]dibenzothiophene (24) , 7-methylphenanthro[1,2-a]dibenzothiophene (25) , phenanthro[3,4-a]dibenzothiophene (27) , phenanthro[4,3-a]-dibenzothiophene (28) , 6-methylphenanthro[2,3-a]dibenzothiophene (31) , and 5-methylphenanthro[4,3-a]dibenzothiophene (32) is described.     

Heptane-soluble homogeneous zirconocene catalyst: Synthesis of a single diastereomer,polymerization catalysis,and effect of silica supports

Bis(1-indenyl)-di[1′S, 2′R, 5′S)-methoxy]silane ( 1 ) was converted into a mixture of corresponding ansa-diastereomeric zirconocenes. Further purification afforded a single dia-stereomer, di[(1′S, 2′R, 5′S)-methoxy] silylene-bis[η⁵-1(R, R)-(+)-indenyl] dichlorozirconium ( 2 ), which is optically active and hydrocarbon soluble. Extremely rapid ethylene, propylene, and ethylene-hexene polymerizations were observed both in toluene and n-heptane solutions; for instance, at 50°C, activity for ethylene polymerization reaches ～ 1.5×10¹⁰ (g of PE/((mol of Zr) · [C₂H₄] · h). The “bare” zirconocenium ion generated from 2/TIBA/Ph₃CB(C₆F₅)₄ exhibits unusual polymerization behaviors; the polymerization activity increases monotonically with temperature of polymerization (T_p) up to a conventional polymerization condition (50–70°C), and the ¹³C NMR study shows that the isotactic poly-propylene obtained has fairly high [mmmm] methyl pentad distributions at high T_p (?25°C with [mmmm] ～ 0.93–0.75) and a perfect stereoregularity at low T_p (?0°C with [mmmm] > 0.99). The catalyst precursors 2 and Et(Ind)₂ZrCl₂ ( 3 ) supported on silica by different approaches produced poly(olefins) of different molecular weights and stereoregularities, and a methylaluminokane and Ph₃CB(C₆F₅)₄ free silica-supported zirconocene system was found to be activated by triisobutylaluminum. © 1995 John Wiley & Sons, Inc.     

New combining rules for rare gas van der waals parameters

New combining rules are proposed for the well depth, ?, and interaction distance, σ, describing nonbonded interatomic forces for rare gas pair interactions. Concepts underlying current combining rules applied in simulations of macromolecular and polymer systems are shown to be incompatible with experimental data on the rare gases. The current combining rules are compared with the new results using the experimental data. Mathematical properties of combining rules are considered, and it is shown how to reduce combining rule formulas from a two-parameter to a single-parameter problem. It is also shown how to graphically analyze combining rules against experimental data. We demonstrate using this analysis technique that the rare gas potentials do not obey a single combining rule for the ? parameter but do follow a single combining rule for the σ parameter. Finally, we demonstrate that a combining rule using both ? and ω can be used to predict the ? parameters for the mixed rare gas pairs. © John Wiley & Sons, Inc.     

Characterization of lactosylated proteins of infant formula powders using two-dimensional gel electrophoresis and nanoelectrospray mass spectrometry

Infant formula powders were analyzed by liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) to assess the whey proteins quality, which may be altered by the heat treatment used during the processing conditions. Lactosylation was found to be the major chemical modification occurring in whey proteins. In parallel, a two-dimensional (2-D) gel electrophoresis was performed on the milk sample and the entire protein patterns were analyzed by nano-ESI-MS after cutting the different gel spots and in-gel trypsin digestion. A highly selective and specific tandem MS technique has been developed to characterize and localize up to ten lactosylation sites in beta-lactoglobulin (beta-Lg) and alpha(S2)-casein. alpha-Lactalbumin (alpha-La), with five lactosylated peptides, was found to be an interesting protein marker in the milk powder sample to detect chemical modification induced by the processing/storage conditions.     

Relativistic calculation of Stokes' parameters for intermediate energy electron impact excitation of cesium atoms

The integrated and differential Stokes' parameters of the light emitted in the decay 6p ² P _1/2,3/2→6s ² S _1/2 fore-Cs scattering in the intermediate energy range are presented. These have been calculated using scattering amplitudes obtained by a relativistic distorted-wave method.     

Identifizierung von Aminen

Zusammenfassung 2,4-Dinitrophenylderivate von Aminen (DNP-Amine) werden dünnschicht-chromatographisch und massenspektrometrisch untersucht. Die Fragmentierung der Verbindungen bei Elektronenbeschuß wird diskutiert.Die Untersuchungen zeigen, daß Amine als DNP-Derivate bis auf einige kritische Paare dünnschicht-chromatographisch getrennt werden können. Aus den Massenspektren der DNP-Amine kann die Struktur eines Amins so weit ermittelt werden, daß durch Vergleich mit authentischem Material und IR-Spektroskopie eine rasche und sichere Identifizierung möglich ist.

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Identification of aminesI. Thin-layer chromatography and mass spectrometry of 2,4-Dinitrophenyl derivatives (DNP-amines)

2,4-Dinitrophenyl derivatives of amines (DNP-amines) were investigated by thin-layer chromatography and mass spectrometry. The fragmentation of the compounds upon electron impact is discussed.The investigations show that amines in their form as DNP-derivatives can be separated by TLC except for some critical pairs. From the mass spectra of the DNP-amines the structure of an amine can be elucidated so far that a quick and reliable identification is possible by comparison with authentic material and IR spectroscopy.

     

On Dirichlet series satisfying Riemann's functional equation

Summary According to convention, Hamburger's theorem (1921) says-roughly-that Riemann's (s) is uniquely determined by its functional equation. In 1944 Hecke pointed out that there are two distinct versions of Hamburger's theorem. Hecke's remark has led me, in examining just how rough the convention is, to prove that, with a weakening of certain auxiliary conditions, there are infinitely many linearly independent solutions of Riemann's functional equation (Theorem 1). In Theorem 1, as in Hamburger's theorem, the weight parameter is 1/2. In Theorem 2 we obtain stronger results when this parameter is 2: a Mittag-Leffler theorem for Dirichlet series with functional equations.Oblatum 23-XII-1992 & 9-IX-1993Research supported in part by NSA/MSP Grant MDA 90-H-4025 To the memory of Martin Eichler     

The equation of state of hard hyperspheres in four and five dimensions

The equation of state of hard hyperspheres in four and five dimensions is calculated from the value of the pair correlation function at contact, as determined by Monte Carlo simulations. These results are compared to equations of state obtained by molecular dynamics and theoretical approaches. In all cases the agreement is excellent.