氧化条件下NOx催化的甲烷均相部分氧化

考察了没有固体催化剂时NOx对甲烷气相氧化的促进作用.实验结果表明，即使在强氧化条件下（O2/CH4=5），NOx对甲烷部分氧化制一氧化碳仍然有明显的催化活性.在CH4-O2体系中加入0.005％～0.2％的NO后，反应温度可降低200-300 ℃.在反应产物中还可观察到甲醛和乙烯，通过改变反应条件可以控制它们的相对浓度.     

A new type of Zeeman-effect atomic-absorption spectrophotometer

A new type of Zeeman-effect atomic-absorption spectrophotometer has been developed. It uses fast heating of a special atomizer made from a pyro-coated graphite tube lined with tungsten-tantalum alloy, for easier determination of refractory and rare-earth elements. A boxcar integrator is used, and the atomic absorption, background absorption and atomization temperature can be recorded. By means of the Zeeman effect, the instrument can correct for background absorbance up to 2.0.     

Determination of aniline in silica gel sorbent by one-step in situ microwave-assisted desorption coupled to headspace solid-phase microextraction and GC-FID

Microwave-assisted desorption (MAD) coupled to in situ headspace solid-phase microextraction (HS-SPME) was first proposed as a possible alternative pretreatment of samples in absorbent collected from workplace monitoring. Aniline collected on silica gel was investigated. Under microwave irradiation, the aniline was desorbed from silica gel and directly absorbed onto the SPME fiber in the headspace. Having been sampled on the SPME fiber, and desorbed in the GC injection port, aniline was analyzed using a GC-FID system. Parameters that affect the proposed extraction efficiency, including the extraction media and its pH, the microwave irradiation power and the irradiation time as well as desorption parameters of the GC injector, were investigated. Experimental results revealed that the extraction of a 150-mg silica gel sample using a 0.8-ml aqueous solution (pH 12) and a PDMS/DVB fiber under medium-high-powered irradiation (345 W) for 3 min maximized the efficiency of extraction. Desorption of aniline from the SPME fiber was optimal at 230 °C held for 3 min. The detection limit was 0.09 ng. The proposed method provided a simple, fast, and organic solvent-free procedure to analyze aniline from a silica gel matrix.     

A new cucurbitane triterpenoid from Momordica charantia

One new cucurbitane-type triterpenoid saponin, 5b,19-epoxycucurbita-6,23-diene-3b,19,25-triol-3-O-b-D-allopyranoside (1), named momordicoside P was isolated from the fresh fruits of Momordica charantia. The structure of the saponin was elucidated byspectral methods, including 2D-NMR spectra.     

Ion size dominated 1D and 2D Salen lanthanide coordination complexes and their luminescence

Lewis acid/base addition between Ln(NO₃)₃ · 6H₂O (Ln = Pr, Nd, Sm, Eu, Tb and Lu) and H₂salen [H₂salen = N,N′-ethylenebis(salicylideneimine)] gives rise to an array of coordination polymeric structures. Crystal structural analysis reveals that Salen effectively functions as a bridging ligand in these compounds. The size of the lanthanide ions controls the structures of these Salen lanthanide complexes. Two representative structures with one dimensional and two dimensional topologies, viz. [Pr(H₂salen)(NO₃)₃(CH₃OH)₂]_n (1) and [Ln(H₂salen)_1.5(NO₃)₃]_n [Ln = Pr (2), Nd (3), Sm (4), Eu (5), Tb (6) and Lu (7)] are reported. Luminescent spectra of complexes 4 and 5 exhibit characteristic metal-centered emission lines. However, the characteristic luminescence of the terbium(III) ion is not observed either in solution or in the solid state of complex 6.     

Preparation and properties of poly(vinyl alcohol)/silica nanocomposites derived from copolymerization of vinyl silica nanoparticles and vinyl acetate

Nanocomposites of poly(vinyl alcohol)/silica nanoparticles (PVA-SNs) were prepared by in-situ radical copolymerization of vinyl silica nanoparticles functionalized by vinyltriethoxysilane (VTEOS) and vinyl acetate with benzoyl peroxide (BPO, i.e., initiator), subsequently saponified via direct hydrolysis with NaOH solution. The resulting vinyl silica nanoparticles, PVA-SNs were characterized by means of fourier transformation spectroscopy (FTIR), transmission electron microscopy (TEM) and the elemental analysis method. Effects of silica nanoparticles on viscosity and alcoholysis of PVA-SNs were studied by a ubbelohode capillary viscometer and the back titration method. The morphological structure of PVA-SN films was investigated by scanning electron microscopy (SEM). Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and tensile test were used to determine the thermal and mechanical properties of PVA-SN films. The results indicated that the content of vinyl groups on the surface of the vinyl silica nanoparticles was up to 3.02 mmol/g and vinyl silica nanoparticles had been successfully copolymerized with vinyl acetate. Furthermore, compared to pure PVA, silica nanoparticles bonded with polymer matrix in a low concentration affected the viscosity and alcoholysis of the PVA-SNs materials. At the same time, it resulted in the improvement of the thermal and mechanical properties of the PVA-SN materials due to a strong interaction between silica nanoparticles and the polymer matrix via a covalent bond. It could be found that the optical clarity of the membrane was changed through UV-Vis absorption spectrum due to the introduction of silica nanoparticles.     

Two Novel Oxamidato-bridged Tetranuclear Complexes M[Cu(PMoxd)]3(ClO4)2 (M=Mn, Ni, Cu(PMoxd)=N,N′-bis(pyridyl-methyl)-oxamidatocopper(II)): Syntheses, Spectra, Magnetic and Electrochemical Properties

Two novel oxamidato-bridged Mn[Cu(PMoxd)]₃(ClO₄)₂ (1) Ni[Cu(PMoxd)]₃(ClO₄)₂ (2) tetranuclear complexes were prepared and characterized by i.r., e.p.r., electronic spectra, cyclic voltammograms, and magnetic properties. The magnetic analysis was carried out by means of the theoretical expression of the magnetic susceptibility deduced from the spin Hamiltonian H=−2JS_M(S_Cu1+ S_Cu2 + S_Cu3) (M=Mn, Ni), leading to J=−20.4 cm⁻¹; −121.1 cm⁻¹ for complexes (1) and (2) respectively. Magnetic measurements indicate that the overall magnetic behavior of the tetranuclear species are antiferromagnetic.     

Crystal Structure of Complex Tris（4,4,4—trifluoro—1—pheny1—1,3—butanedione）（1,10—phenanthroline）Europium（Ⅲ）

The complex Eu(btfa)₃ (phen) (btfa=4,4,4‐trifluoro‐1‐phenyl‐1, 3‐butanedione, phen = 1,10‐phenanthroline) has been prepared and characterized by elemental analysis, IR and UV spectroscopies. The crystal and molecular structures of the complex have been determined by X‐ray diffraction analysis. It belongs to the monoclinic crystal system, space group P2₁/c with a = 0.9700(2) nm, b = 3.7450(5) nm, c = 1.0917(3) nm, β = 92.51(2)°, V = 3.962(1) nm⁵, Z = 4, D_c = 1.639 g/cm³, μ = 1.676 mm^?1, F(000) = 1936, R₁, = 0.0388, wR₂ = 0.0775. Structure analysis shows that the europium(III) ion is coordinated to six oxygen atoms of β‐diketonate anions and two nitrogen atoms of phenanthroline molecule. The coordination polyhedron is an approximate square antiprism.     

Electrocatalytic Oxidation of Dopamine by Ferrocene in Lipid Film Cast on a Glassy Carbon Electrode

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Three New Triterpenoids from Lycopodium japonicum Thunb

Three new triterpenoids, (3β,8β,14α,21α)‐26,27‐dinoronocerane‐3,8,14,21‐tetrol ( 1 ), (3β,8β,14α,21β)‐26,27‐dinoronocerane‐3,8,14,21‐tetrol ( 2 ), and lycopodiin A ( 3 ), together with four known compounds, lycoclavanol ( 4 ), lycoclaninol ( 5 ), α‐onocerin ( 6 ), and 3‐epilycoclavanol ( 7 ), were isolated from Lycopodium japonicum Thunb (Lycopodiaceae). Their structures were established by means of spectroscopic analyses. Compounds 3 and 7 showed moderate antitumor activity. Compounds 4 and 6 exhibited acetylcholinesterase inhibition activity.