Synthesis and characterization of dinuclear p-, m- and o-xylyl bridged complexes of molybdenum and tungsten. The crystal structures of μ-p-xylyl- bis(η-pentamethyl-cyclopentadienyltri- carbonylmolybdenum) and μ-m-xylyl-bis(η- pentamethylcyclopentadienyltricarbonyltungsten)

The reactions of (M = Mo, W) with α,α′-p-, m- and o-dichloro-xylenes yielded p-, m- and o-xylyl bridged dinuclear complexes of in high yields. All of such new complexes are stable to air and water, even stable in dilute acids and bases.     

Preparations of Tris(Triphenylphospnine)copper and Tris(triphenylphosphine)silver Complexes of Phenalenone,Diphenylcyclopropenone and Tropone

The tris(triphenylphosphine)copper and tris(triphenylphosphine)silver complexes of phenalenone 4 , diphenylcyclopropenone 5 and tropone 6 were prepared by treating tris(triphenylphosphine)copper tetrafloroborate 2 and tris(triphenylphosphine)silver tetrafluoroborate 3 with basic ketones 4, 5 and 6 in high yields. All these complexes are stable in either air or moisture, and soluble in common organic solvents such as dichloromethane and chloroform.     

Recent advances in enhancing the sensitivity of electrophoresis and electrochromatography in capillaries and microchips (2016–2018)

One of the most cited limitations of capillary and microchip electrophoresis is the poor sensitivity. This review continues to update this series of biannual reviews, first published in Electrophoresis in 2007, on developments in the field of online/in‐line concentration methods in capillaries and microchips, covering the period July 2016–June 2018. It includes developments in the field of stacking, covering all methods from field‐amplified sample stacking and large‐volume sample stacking, through to isotachophoresis, dynamic pH junction, and sweeping. Attention is also given to online or in‐line extraction methods that have been used for electrophoresis.     

Concentration dependence of the linear viscoelastic properties of particle suspensions

The response under small amplitude oscillatory deformations of a suspension of non-Brownian spheres dispersed in a viscoelastic fluid is investigated. The correspondence principle of linear viscoelasticity is used to derive a simple constitutive model from a model for a suspension in a Newtonian liquid. The theory predicts that for a specific particulate system the concentration dependence of the viscoelastic properties should collapse to a single master curve when the values are normalized with those of the carrier fluid alone. Measurements with the micro-Fourier rheometer using oscillatory squeeze flow are carried out on two suspensions of 60 and 80 μm sized particles dispersed in polymeric fluid and in silicon oil, and the master curve is verified. Received: 27 April 1999/Accepted: 15 October 1999     

DNA sensing by field-effect transistors based on networks of carbon nanotubes

We report on the sensing mechanism of electrical detection of deoxyribonucleic acid (DNA) hybridization for Au- and Cr-contacted field effect transistors based on single-walled carbon nanotube (SWCNT) networks. Barrier height extraction via low-temperature electrical measurement provides direct evidence for the notion that the energy level alignment between electrode and SWCNTs can be affected by DNA immobilization and hybridization. The study of location-selective capping using photoresist provides comprehensive evidence that the sensing of DNA is dominated by the change in metal-SWCNT junctions rather than the channel conductance.     

Tunable nonadiabatic excitation in a single-electron quantum dot

We report the observation of nonadiabatic excitations of single electrons in a quantum dot. Using a tunable-barrier single-electron pump, we have developed a way of reading out the excitation spectrum and level population of the dot by using the pump current as a probe. When the potential well is deformed at subnanosecond time scales, electrons are excited to higher levels. In the presence of a perpendicular magnetic field, the excited states follow a Fock-Darwin spectrum. Our experiments provide a simple model system to study nonadiabatic processes of quantum particles.     

Study on the effects of electrolytes and solvents in the determination of quaternary ammonium ions by nonaqueous capillary electrophoresis with contactless conductivity detection

A study on the separation of lipophilic quaternary ammonium cations in NACE coupled with contactless conductivity detection (NACE‐C⁴D) is presented. The suitability of different salts dissolved in various organic solvents as running electrolytes in NACE‐C⁴D was investigated. A solvent mixture of methanol/acetonitrile at a ratio of 90%:10% v/v showed the best results. Deoxycholic acid sodium salt as BGE was found to provide exceptional high stability with low baseline noise that leads to highest S/N ratios for the target analytes among all BGEs tested. Under the optimum conditions, capillaries with different internal diameters were examined and an id of 50 μm was found to give best detection sensitivity. The proposed method was validated and showed good linearity in the range from 2.5 to 200 μM, low limits of detection (0.1–0.7 μM) and acceptable reproducibility of peak area (intraday RSD 0.1–0.7%, n = 3; interday RSD 5.9–9.4%, n = 3).     

Economical Access to Diverse Enantiopure Tetrahydropyridines and Piperidines Enabled by Catalytic Borrowing Hydrogen

We disclose herein a catalytic borrowing hydrogen method that enables an unprecedented, economical one-pot access to enantiopure tetrahydropyridines with minimal reagent use or waste formation. This method couples a few classes of readily available substrates with commercially available 1,3-amino alcohols, and delivers the valuable tetrahydropyridines of different substitution patterns free of N-protection. Such transformations are highly challenging to achieve, as multiple redox steps need to be realized in a cascade and numerous side reactions including a facile aromatization have to be overcome. Highly diastereoselective functionalizations of tetrahydropyridines also result in a general access to enantiopure di- and tri-substituted piperidines, which ranks the topmost frequent N-heterocycle in commercial drugs.