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.     

丙烯腈中微量有机杂质的测定

本文采用ＸＥ－６０交联弹性石英性细管柱及４０７有机体埴充柱气色谱法可分分析丙烯腈中有机杂质。通过对柱长、担体粒度、液膜厚度、柱温和载气流量的选择。确定出最佳色 谱条件。     

Acidity and alkali metal adsorption on the SiO2-aqueous solution interface

The intrinsic deprotonation constant (pK(a(2))(int)) and the intrinsic ion exchange constants (pK(Me(+))(int)) of Li(+), Na(+), and K(+) on SiO(2) were uniquely determined at 30 degrees C by using the potentiometric titration data, the Gouy-Chapman-Stern-Grahame (GSCG) model for the structure of the electrical double-layer (edl) and the double-extrapolation method. The values of these constants were pK(a(2))(int) = 6.57, pK(Li(+))(int) = pK(Na(+))(int) = pK(K(+))(int) = 5.61. The chemical meaning of intrinsic equilibrium constants and the equality in the values of pK(Li(+))(int), pK(Na(+))(int) and pK(K(+))(int) were discussed.     

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.     

Binding of brucine to human serum albumin

The feature of brucine binding to human serum albumin (HSA) was investigated via fluorescence and UV/vis absorption spectroscopy. The results revealed that brucine caused the fluorescence quenching of HSA by the formation of brucine–HSA complex. The hydrophobic interaction plays a major role in stabilizing the complex; the binding site number n and apparent binding constant K_A, corresponding thermodynamic parameters the free energy change (ΔG), enthalpy change (ΔH) and entropy change (ΔS) at different temperatures were calculated. The distance r between donor (HSA) and acceptor (brucine) was obtained according to fluorescence resonance energy transfer. The effect of brucine on the conformation of HSA was analyzed using synchronous fluorescence spectroscopy and UV/vis absorption spectroscopy.     

Temperature-programmed desorption and adsorption of hydrogen on Mo2N

Hydrogen adsorption-desorption over Mo₂N has been studied using a temperature-programmed technique. It is revealed that hydrogen on Mo₂N exhibits very high mobility leading to migration of the surface hydrogen into the sublayer and bulk of the sample or the reverse. The surface hydrogen species are preferentially formed when adsorption is carried out below 573 K. On increasing the adsorption temperature to above 573 K, the quantity of hydrogen species located in the sublayer or/and bulk of the Mo₂N sample increases significantly.     

漆树漆酶的催化氧化作用——Ⅳ.二茂铁及其衍生物的酶促氧化

In phosphate buffer-diethylene glycol monobutyl ether(DGBE), the oxidations of ferrocene and 15 derivatives were investigated in the presence of Rhus vernicifera laccase. The results showed that ferrocene and 11 derivatives can be oxidized. The mechanism of Laccase catalyzed oxidation of ferrocene was put forward.     

合成多肽的电喷雾质谱研究

利用电喷雾多极串联质谱对3种合成多肽进行了系统的鉴定和分析研究。首先通过全扫描模式测定了其分子量，然后选择[M H]^ 或[M 2H]^2 离子通过串联质谱(MS／MS)得到碎片离子，采用y离子和b离子互补的方法测定了多肽序列。利用文献数据对这种方法进行了验证，实验结果表明，该方法简便、快速、实用。     

Sorption and desorption of radiostrontium on calcareous soil and its solid components

The effect of different solid components of calcareous soil on the retention of Sr was investigated by using batch technique and selective extraction method. The sorption and desorption isotherms of Sr on the untreated calcareous soil and the three treated soils were determined at 20°C, pH 7.8±0.2 and in the presence of 0.001 M CaCl₂. It was found that all isotherms are linear and that the sorption of Sr on the calcareous soil can be described by a reversible sorption process and the sorption mechanism is mainly ion exchange.     

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