Template synthesis in the nickel(II)–thiocarbohydrazide–propanone triple system

The complexing process proceeding in the Ni^II–thiocarbohydrazide (H₂N–H–NC(=S)–NH–NH₂)–propanone triple system in EtOH solution and nickel(II)hexacyanoferrate(II) gelatin-immobilized matrix has been studied. It has been found that in the first case, template synthesis leading, as a minimum, to formation of three coordination compounds of Ni^II with (N,N,S,S)-donor tetradentate ligands having NiL¹, NiL² and NiL³compositions where L¹ is 4,6,6-trimethyl-2,3,7,8-tetraazanonen-3-di(thiohydrazide)-1,9, L² is 4,6,6,12-tetrametyl-1,9-dithio-2,3,7,8,10,11-hexaazatridekadien-3,11-hydrazide-1 and L³ is 2,8,10,10,16-pentamethyl-5,13-dithio-3,4,6,7,11,12,14,15-octaazaheptadekatrien-2,7,15 is observed, whereas in the gelatin-immobilized matrix, a complexing process in the system considered does not occur.     

缓慢炭化部分氧化对制备煤质活性炭的影响

研究了炭化升温速度、炭化低温区引入空气部分氧化对活性炭制备过程中炭化阶段、炭化物结构、活性炭性能等的影响。结果表明，炭化时低温部分氧化可提高炭化物得率，使炭化物微晶的ｄ００２值升高和Ｌｃ值减小；而较慢的炭化升温速度有利于制备优质活性炭。缓慢炭化、部分氧化可以在一定程度上控制炭化路径，使炭化向生成取向性差、难石墨化、各向同性、呒定形炭多的炭化物的方向进行；并讨论了它们控制炭化的作用机理。以此为指导，     

Hydrothermal Synthesis and Crystal Structure of a Cadmium（Ⅱ） Polymer with One-dimensional Chain Structure： [Cd（MDPPz）（BDC）（H2O）]n

A metal-organic coordination compound formulated as [Cd(MDPPz)(BDC)(H2O)]n 1 (MDPPz=11-methyldipyrido[3,2-a:2',3'-c]phenazine,BDC=1,4-benzenedicarboxylate) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system,space group C2/c,with a=30.673(8),b=9.623(3),c=20.784(6) ,β=98.646(3)o,V=6065(3)3,C27H17CdN4O5,Mr=589.85,Dc=1.292 g/cm3,μ(MoKα)=0.757 mm-1,F(000)=2360,Z=8,the final R=0.0381 and wR=0.0855 for 4191 observed reflections (I>2σ(I)). 1 exhibits blue fluorescence property at room temperature.     

溶剂化金属原子浸渍法制备的Ni-Ag/γ-Al2O3催化剂的结构表征

应用溶剂化金属原子浸渍法和普通浸渍法制备了三种不同摩尔比的γ－Ａｌ２Ｏ３负载Ｎｉ－Ａｇ双金属催化剂。ＸＲＤ和磁测定结果表明ＳＭＡＩ催化剂中Ｎｉ和Ａｇ的粒度均小于金属相同的ＣＩ催化剂。ＳＭＡＩ催化剂中Ｎｉ和Ａｇ未形成合金，而ＣＩ催化剂中Ｎｉ和Ａｇ形成了合金。     

Direct electrochemistry and enzymatic activity of hemoglobin in positively charged colloid Au nanoparticles and hemoglobin layer-by-layer self-assembly films

Alternate adsorption of positively charged colloid-Au nanoparticles (nano-Au⊕) and negatively charged hemoglobin (Hb) on L-cysteine (L-cys) modified gold electrode resulted in the assembly of {Hb/nano-Au⊕}n layer-by-layer films/L-cys modified gold electrode. The nano-Au⊕ was characterized by transmission electron micrograph (TEM) and microelectrophoresis. The modified electrode interface morphology was characterized by electrochemical impedance spectroscopy (EIS), atomic force mi- croscopy (AFM), cyclic voltammograms (CV) and chronoamperometry. Direct electron transfer between hemoglobin and gold electrodes was studied, and the apparent Michaelis-Menten constant ( km app) of the modified electrode was evaluated to be 0.10 mmol·L?1. Moreover, the higher activity of proteins in the nano-Au⊕ films could be retained compared with the electropolymerization membrane, since the pro- teins in nano-Au⊕ films retained their near-native structure. Direct electron transfer between hemoglo- bin and electrode and electrochemically catalyzed reduction of hydrogen peroxide on a modified elec- trode was studied, and the linear range was from 2.1×10-8 to 1.2 ×10?3 mol·L-1 (r = 0.994) with a detection limit of 1.1×10-8 mol·L-1 H2O2.     

Ba-K-Bi-O超导体熔盐阳极电结晶研究

用ＸＰＳ和ＸＲＤ表征了Ｂａ－Ｋ－Ｂｉ－Ｏ超导体熔盐电结晶的阳极和阴 极产物，用ＳＥＭ分析了Ｂａ－Ｋ－Ｂｉ－Ｏ单生长形态。结果表明，阳极产物是Ｂａ－Ｋ－Ｂｉ－Ｏ超导体单晶，以台阶式方式生长。－Ｋ－Ｂ－     

Strategies for multi-site GLP studies

 A GLP study can be performed at more than one site. This is called a multi-site study. Although, the study is performed at different sites, it is still one study and must completely comply with the GLP principles. The fact that different activities are conducted at different sites implies that the planning, the organization and the communication are crucial for the success of the study. This means that all the staff involved should know their responsibilities and should have the knowledge and skills to realize all the phases of the study according to the GLP principles. To achieve a well managed multi-site study, several strategies for setting up such a study can be followed. This paper focuses on the responsibilities, communication, and collaboration of the personnel, which are involved in a multi-site study. Several case studies are highlighted, and we concluded that the basic communication triangle in a single-site GLP study between test facility management, study director, and the quality assurance unit should be extended to the communication among test facility and test site management, study director, principle investigator(s), and the quality assurance units at the test sites. Introduction Received: 14 August 2002 Accepted: 26 November 2002     

New Host Molecules with Imidazoliums as Functional Arms:Syntheses and Anion Recognition

The bridged tri-imidazoliums 3.3X^--5.3X^-(X^-=PF6^-,Br^-,I^-)and bis-imidazoliums 6.2PF6^- were synthesized by N-quaternization of imidazole derivative 1 in acetonitrile under reflux.UV spectroscopic titration experiments showed that the halide salts and hexafluorophosphate salts of these imidazoliums exhibited good recognition toward anions in water and in acetonitrile,respectively.     

Synthesis of Lanthanide Coordination Polymers with Benzophenone-4,4′-dicarboxylate： Effect of Lanthanide Contraction on Structures

Four lanthanide coordination polymers with benzophenone‐4,4′‐dicarboxylic acid (H₂bpndc) and 1,10‐phenanthroline (phen), [Ln₂(bpndc)₃(phen)] (Ln=La (1), Pr (2) and Tb (3)), [Yb(bpndc)₁₅(phen)].05H₂O (4) were obtained through solvothermal synthesis. The crystallographic data show that 1, 2, and 3 are isostructural, the Ln(III) ions in 1, 2 and 3 are all eight‐ and ten‐coordinated, respectively, and thus the Ln(III) ions are connected by bpndc ligands, resulting in an interpenetrating 3D structure. While in 4, the Yb(III) ions are eight‐coordinated and connected by bpndc ligands into a 3D structure with 1D rhombic channels, which result from the effect of lanthanide contraction from La(III) to Yb(III) ions, and the bpndc ligands in 1, 2, 3, and 4 display three types of coordination modes.     

Electrocatalytic activity of binary Palladium Ruthenium anode catalyst on Ni-support for ethanol alkaline fuel cells

In search for a cheaper anode catalyst for the oxidation of ethanol for development of direct alcohol fuel cells, Pd has been considered here as an interesting substitute for Pt in Pt Ru binary electrodeposite. The binary catalyst when co-deposited on nickel support has been found to increase the current density and decrease the anodic overvoltage significantly with respect to pure Pt, Pd and Ni. Its electrocatalytic capability is also comparable with that of the Pt-Ru binary electrocatalyst on Ni-support, when studied in 1 M EtOH containing 1 M NaOH solution. The effect of loading of Pd Ru electrocatalyst on Ni support has also been tested. The electrocatalytic activity of the electrodes for oxidation of ethanol has been explained by studies of cyclic voltammetry, chronopotentiometry, steady-state polarization, and conjugated scanning electron microscopy–energy dispersion X-ray spectroscopy. It has been found that electrode containing the higher amount of deposit are less affected by carbonaceous poisons.