Synthesis and characterization of Mn-, La-Mn- and La-Ca-Mn-citrates as precursors for LaMnO<Subscript>3</Subscript> and La<Subscript>1−x</Subscript>Ca<Subscript>x</Subscript>MnO<Subscript>3</Subscript>

Mn-, LaMn- and LaCaMn-citrates were synthesized at 60–120°C in ethylene glycol medium using chlorides or nitrates as metal sources. Their composition, IR spectra and thermal decomposition were studied. Equimolar La/Mn ratio has been established in the complex, prepared from chloride solution with the same initial composition of the metals. In the isolated three-metallic complex the molar ratio of the metals deviates from the composition in the initial solution. The final products of the heating of Mn- and mixed-metal LaMn-citrates at 1000°C are phase-homogeneous Mn₃O₄ (hausmannite) and LaMnO₃ respectively. Parasitic phase(s) are observed in La_xCa_1−xMn_yO₃, produced from LaCaMn-citrate.     

A new dimension in thermal analysis

Summary An enormous development has taken place within the last five years in synchronous teaching over the Internet, i.e. both the teacher and the students are simultaneously in direct communication with each other as in a normal class-room or auditorium. With this concept it is possible to communicate orally, to exchange Power Point Presentations, documents, programmes and live web-camera pictures. It is even possible to use an electronic black board on which both the teacher and the students can work simultaneously. The great advantage with this type of teaching is that it is not restricted to a single class-room/auditorium with limited access, but in a virtual room accessible to everybody in principle all over the world, and which certainly open up new possibilities in teaching. The purpose of this paper is to present and to discuss the concept of virtual class-room teaching, how the system operates in practice, its advantages and, finally, how its inherent limitations can be overcome.     

Cyanide attack at low-spin iron(II)–diimine complexes: the structure of a cyanide-containing derivative of a leaving ligand

The isolation and structural characterisation of the product of addition of HCN to the Schiff base derived from phenyl 2-pyridyl ketone and 3,4-dimethylaniline (Me2bsb) provides evidence in favour of a mechanism involving nucleophilic attack at the coordinated ligand for reaction of the complex [Fe(Me₂bsb)₃]²⁺ with cyanide.     

Addition of amines to the triple bond in alpha,alpha,alpha-trichloromethylpropargyl mesylate: synthesis of alpha,alpha-dichloromethylenaminones and preparation of 2-phenyl-4-dichloromethylquinolines

[reaction: see text] Addition of amines to the triple bond in alpha,alpha,alpha-trichloromethylpropargyl mesylate to give alpha,alpha-dichloromethylenaminones and its use in the preparation of 2-phenyl-4-dichloromethylquinolines in good yields are reported.     

Efficient synthesis of complex glycopeptides based on unprotected oligosaccharides

N-Glycopeptides containing 1 to 4 trisaccharide chains, with the carbohydrates vicinal to each other in the multivalent glycopeptides, were efficiently synthesized by using the glycosylated Fmoc-asparagine as a key building block. While the couplings of amino acids with glycopeptides could be achieved in the homogeneous solutions in N-methylpyrrolidinone (NMP) to give excellent yields, all products were conveniently isolated from the reaction mixtures through a precipitation method by using the free carbohydrate chains as phase tags. Commercially available pentafluorophenyl (Pfp) esters of amino acids were employed for the glycopeptide elongation. Longer glycopeptides were constructed by means of a highly convergent synthetic design that is based on the coupling of glycopeptide/peptide fragments. Hydrogen bond interactions between free oligosaccharides were proposed to explain the exceptionally high efficiency of the couplings between two glycosylated building blocks.     

Determination of medecamycin by adsorptive stripping voltammetry with an activated electrode

The adsorptive and electrochemical behaviors of medecamycin were investigated on a glassy carbon electrode (GCE) pretreated by anodic oxidation at +1.8 V for 5 min in 0.025 mol l^–1 NH₃-NH₄Cl (pH 8.6) solution. An adsorptive stripping voltammetric method for the determination of medecamycin at the pretreated glassy carbon electrode has been developed. Medecamycin was accumulated in NH₃-NH₄Cl buffer (pH 9.0) at a potential of –0.7 V (vs. saturated calomel electrode (SCE)) for a certain time, and then determined by second-order differential anodic stripping voltammetry. The second-order differential anodic stripping peak current at +0.72 V was proportional to the concentration of medecamycin in the range 2.0 g ml^–1 to 50.0 g ml^–1. The detection limit (three times the signal-to-noise) was 1.0 g ml^–1 and the relative standard deviation of the results was 3.28% for eight successive determinations of 10.0 g ml^–1 medecamycin. This method has been applied to the direct determination of medecamycin in commercial tablets and spiked urine samples with satisfactory results.     

Rank-1 approximation to the van der Waals interaction

We present and discuss a variational single-product approximation to the van der Waals dispersion interaction leading to a simple formula for C ₆ that seems capable to give more than 99% of the ‘exact’ value. The formula is derived from Hylleraas’ variational principle in the tensor product space of the interacting molecules and therefore enjoys bounding properties. The formula has been tested by computing the C ₆ dispersion constants of H–H, and, at Full CI level, of the following systems: He–He, He–Li, Li–Li, LiH–LiH, HF–HF. Connections with the London formula are discussed. Contribution to the Fernando Bernardi Memorial Issue.     

Synthesis,characterization, X-ray structural analysis and study of oxidative properties of propyltriphenylphosphonium bromochromate

The complex of propyltriphenylphosphonium bromochromate(VI), PrPh₃P[CrO₃Br] is easily synthesized in nearly quantitative yield using a direct reaction of chromium(VI) oxide and propyltriphenylphosphonium bromide. This compound is a versatile reagent for the efficient and selective oxidation of organic substrates, in particular for alcohols to their corresponding aldehydes or ketones, under mild conditions. This compound was characterized by IR, UV/Visible, ¹³C-n.m.r. and ¹H-n.m.r. techniques. It crystallized in the monoclinic form and its crystal and molecular structure have been determined by X-ray crystallography.     

Microwave synthesis,characterization and catalytic properties of titanium-incorporated ZSM-5 zeolite

Titanium-incorporated ZSM-5 zeolites (Si/Al = 50–200 and Si/Ti = 70) were successfully synthesized in a one-step sol-gel process under microwave irradiation. The characteristics of Ti-ZSM-5 zeolites were investigated using X-ray power diffraction, UV/Vis-DRS, FT-IR spectroscopy and solid-state ²⁷Al-NMR to monitor the physico-chemical properties. Simultaneously, the acidic properties were characterized by the NH₃-TPD profile. The characterization results revealed that the Ti⁴⁺ and Al³⁺ ions were well incorporated into the framework of Ti-ZSM-5 zeolite. The prepared zeolite was moderately active but selective in the dehydration of methanol to dimethyl ether.     

实验室废液的回收及效果评价——以“铬废液回收及评价”为例

This paper introduces an experiment about waste liquid recovery and effect evaluation in laboratory. Through this experiment, the basic operations of crystal preparation, chemical analysis and instrumental analysis are further consolidated. At the same time, it allows students to experience a series of possible problems of condition selection and control in the process of waste liquid treatment. We hope to improve the students' ability to analyze and solve problems, enhance their interest in learning, and strengthen their humanistic education.