镀锡板镀层测试

以８０９８单片机作智能部件研制开发的对镀锡板度测试装置，采用ＳＴＤ标准总线结构，汉字菜单提示，人－机对话方式操作，采用电解剥离法检测电位跃变曲线，根据电流和起始时间计算出镀层厚度，可直接显示，打印测试曲线和分析结果。     

Chronocoulometric study of the electrochemistry of Prussian blue

During the electrochemical oxidation of Prussian blue (PB) to Prussian yellow (PY), an electrocatalytic oxygen production proceeds at the electrode when aqueous electrolyte solutions are used. The formed oxygen is scavenged by the PY, probably by absorption, and it is consumed during the electrochemical reduction of PY to PB by a heterogeneous chemical reaction of PB with oxygen to PY and hydrogen peroxide. Because of this catalytic regeneration of PY, it is impossible to determine the amount of low-spin iron by chronocoulometry using a potential program in which PB is first oxidized to PY and then the charge is measured to reduce PY to PB. The latter charge is biased by the electrocatalytic PY regeneration.     

Mechanism of action of a fire retardant chloroparaffin

The mechanism by which a typical fire retardant chloroparaffin imparts fire retardant characteristics to high density polyethylene, polypropylene and polystyrene is studied by comparing the oxygen indices of these mixtures measured before and after dehydrochlorination. It is shown that flame poisoning by HCl evolved from the chloroparaffin is negligible in polystyrene and high density polyethylene, whereas it is noticeable in polypropylene. The results obtained are related to previous data on the thermal degradation of these mixtures. It is concluded that the chloroparaffin acts mainly by modifying the mechanism of pyrolysis of these polymers in the burning process. Only in the case of polypropylene is there an appreciable contribution by flame poisoning.     

几种建筑材料的氡射气系数研究

通过天然γ能谱测量方法测定建材样品中的镭含量,计算理论上衰变产生的氡密度,以及用硫化锌闪烁法测定由样品释放到空气中的氡密度的方法来计算氡的射气系数。通过改变样品的颗粒度大小,以及改变样品的灼烧温度等条件,来研究氡射气系数的变化规律。结果表明,土坯砖射气系数在8.5%~29.4%,红砖射气系数在0.031%~3.5%之间,瓷砖射气系数在0.74%~4.5%之间;建筑材料的氡射气系数随着其自身颗粒度的增大而减小,随加工(灼烧)温度升高而减小。     

Advances in the field of the synthesis of amino derivatives of terpenoids

Information on the synthesis of amino derivatives of monoterpenes by the reduction of oximes by the Leuckart reaction, and by the reductive amination of ketones by amines and nitriles is generalized. The stereochemistry of the amines formed as the result of the above-mentioned reactions is discussed.     

Sorption and desorption of water vapor by grains of native starch of some crops

The sorption-desorption of water vapor by grains of potato, corn, and wheat native starch is studied. It is shown that water vapor is mainly sorbed inside starch grains. A model is proposed for water vapor sorption by starch grains. Constructed sorption isotherm is shown to adequately describe the process in a wide humidity range. The kinetics of the sorption and desorption of water vapor by starch grains is shown to have an abnormal character.     

Emulation of racemase activity by employing a pair of stereocomplementary biocatalysts

Racemization is the key step to turn a kinetic resolution process into dynamic resolution. A general strategy for racemization under mild reaction conditions by employing stereoselective biocatalysts is presented, in which racemization is achieved by employing a pair of stereocomplementary biocatalysts that reversibly interconvert an sp3 to a sp2 center. The formal interconversion of the enantiomers proceeds via a prochiral sp2 intermediate the formation of which is catalyzed either by two stereocomplementary enzymes or by a single enzyme with low stereoselectivity. By choosing appropriate reaction conditions, the amount of the prochiral intermediate is kept to a minimum. This general strategy, which is applicable to redox enzymes (e.g., by acting on R2CHOH and R2CHNHR groups) and lyase-catalyzed addition-elimination reactions, was proven for the racemization of secondary alcohols by employing alcohol dehydrogenases. Thus, enantiopure chiral alcohols were used as model substrates and were racemized either with highly stereoselective biocatalysts or by using (rarely found) non-selective enzymes.     

The effect of dissolved oxygen on the rate of pulsed electrodeposition of copper and bismuth nanowires under the conditions of template synthesis

The effect of dissolved oxygen on the electrodeposition under the conditions of template synthesis (the fabrication of arrays of meso- and nanowires by the electrochemical deposition into the aluminum oxide membranes with pore diameter of 20 to 200 nm, which were coated with a conducting metal on one side) is studied. It is shown that, when the deposition rate is controlled by mass transfer, it can be raised by using the pulsed electrolysis due to additional delivery of electroactive substance during a pause. However, the method is limited by the material corrosion during the pause (this is shown by the examples of copper deposition from the pyrophosphate solution and bismuth deposition from the nitrate solution). By the example of copper deposition from the pyrophosphate electrolyte, it is shown that corrosion proceeds with oxygen depolarization. The electrodeposition in the inert gas atmosphere gives the possibility to raise the deposition rate by several times, and the rate becomes close to the Faradaic one.     

Kinetics and mechanisms of the oxidation by permanganate of L-Phenylalanine

The oxidation of L-Phenylalanine by permanganate ion in aqueous phosphate buffers is autocatalized by the inorganic reaction product, which is stabilized in solution by adsorption of phosphate ions on its surface. This product is a soluble form of colloidal manganese dioxide. The rate of the noncatalytic reaction pathway is first-order in both the oxidizing and reducing agent. It is not affected by potassium chloride addition to the solution, but by phosphate addition. The rate increases with the pH of the medium. The autocatalytic pathway is first-order in both permanganate ion and colloidal manganese dioxide, (the permanganate ion according to the Langmuir isotherm). The autocatalytic rate increases with reductant concentration (follows the Langmuir adsorption isotherm). It is not affected by potassium chloride addition to the solution, whereas an increase in the phosphate concentration results in an increase in the rate with the same pH of the medium. Mechanisms consistent with the experimental data are proposed.     

Features of the sorption of phenylalanine by profiled ion-exchange membranes

Features of the equilibrium sorption of phenylalanine from neutral media by profiled ion-exchange membranes in a wide range of concentrations is studied under static conditions. The mechanism of phenylalanine sorption by ion-exchange membranes with profiled and smooth surfaces is discussed. It is shown that phenylalanine sorption is accompanied by the formation of spatial associative structures of the aminoacid in an external equilibrium solution, and in a solution of the membrane’s pore spaces or on its surface. The increased sorption capacity of the profiled membranes is explained by features of the microstructure of their surface and volume.     

The Role of Viscoelastic Adhesive Contact in the Sintering of Polymeric Particles

The sintering of polymeric particles is analyzed by considering the growth of contact between viscoelastic spheres driven by adhesive intersurface forces. This process is dominant during the initial phase of sintering and is succeeded by a viscous sintering step that is driven by surface tension and accommodated by viscous flow. The intersurface forces in this work are described by a cohesive zone model. A new formulation of adhesive contact that does not require the cohesive zone to be smaller than the contact radius, together with finite element simulations is used to study the growth of contact. The results of this paper establish conditions that determine the dominant mechanism of contact growth during sintering. These conditions are described using a "deformation map". For a Maxwell material, if particle radius R(max),相似文献   

Synthesis of the glivocarcin-M aglycone

The synthesis of the agylcone of the antibiotic Gilvocardin-M by a sequential Meerwein Diels-Alder route is reported. The D-ring of the agylcone is attached by a halogen atom directed Meerwein arylation reaction and the A-ring is attached by a halogen atom directed Diels-Alder reaction. In the key step the directing chlorine atom is removed by a new thiophenylation reduction sequence.     

用废电池锌片制备硫酸锌的实验改进

用废电池锌片制备硫酸锌的学生实验,因锌的酸溶解过程所需时间太长而影响实验教学质量。本文采取加热、加入稀CuSO4溶液"催化"并实施锌的"部分溶解"等措施较好地解决了这一问题。     

Analysis of heavy organic pollutants of confined atmospheres

Summary An improved procedure for the determination of the less volatile air pollutants of recycled closed atmospheres by activated carbon-Soxhlet extraction is proposed. After total treatment of desorbate, PAH determination is then accomplished by RP-HPLC using both adsorptiometric and fluorimetric UV detection; phenolic compounds are determined by GC-MS.This technique is suitable for very low levels of PAH and phenolic compounds.     

Selectivity of catalytic methods of determination

By means of catalytic analytical methods, extremely low levels can be determined at low cost and with a high sensitivity that is equal to that of physical methods of trace analysis. The selectivity of the catalytic determinations, is, however, usually rather lower than that of other methods of trace analysis. The selectivity can sometimes be improved by modification of the indicator reaction through variation of the reagents and their concentrations, or by use of masking reagents or activators, or by combination with a separation method. Modification of the indicator reaction can be exemplified by the selective determination of osmium and ruthenium by their catalysis of the nitrate oxidation of 1-naphthylamine. By variation of the nitrate concentration and the use of 1,10-phenanthroline and 8-hydroxyquinoline as complexing agents it is possible to determine these two elements simultaneously. An especially significant increase in the selectivity is made possible by use of a preliminary separation step. If the ion to be determined is separated by solvent extraction and then catalytically determined directly in the extract, a very specific determination is possible; this technique has been called "extractive catalytic determination". This method has been used for determination of molybdenum (0.5 ng/ml) in sea-water, iron (5 ng/ml) in heavy metal salts, and copper (3 ng/ml) in the presence of numerous elements.     

Structure elucidation of thermal degradation products of amlodipine

Thermal degradation of amlodipine base causes intramolecular reactions affording three cyclic products, referred to as AMLDEG-I, AMLDEG-II, and AMLDEG-III, respectively. AMLDEG-I is a cyclized product formed by intramolecular elimination of ammonia from amlodipine. AMLDEG-II is a positional isomer of AMLDEG-I. AMLDEG-III is also intramolecular cyclisation product. The three degradation products were isolated by column chromatography and characterized by FT-IR and 1H and 13C NMR spectroscopy data. The AMLDEG-III was crystallized and its structure was solved by single crystal X-ray diffraction (SXRD).     

Synthesis and kinetics of non-isothermal degradation of acetylene terminated silazane

Novel acetylene terminated silazane compounds,with three types of substituent,were synthesized by the aminolysis of dichlorosilane with 3-aminophenylacetylene(3-APA).Thermal property of the compounds is studied by thermogravimetry analysis (TGA).It shows that the acetylene terminated silazane has high temperature resistance.The char yield at 1000℃is 77.6,81.9 and 68.7 wt%for methyl,vinyl,and phenyl substituted silazane,respectively.The pyrolysis kinetics of the silazane is investigated by non-isothermal thermogravimetric measurement.The pyrolysis undergoes three stages,which is resolved by PEAKFTT.The kinetic parameters are calculated by the Kissinger method.The role of functionalities on the thermal resistance is discussed.The vinyl-silazane exhibits higher thermal stability because of higher cross-linking density.     

Effect of the addition of polyelectrolytes on monolayers of carboxybetaines

We have studied the effect of the addition of sodium poly(styrene sulfonate) polymers on the properties of monolayers formed by the adsorption of two carboxybetaines with different number of separation methylenes between their charged groups. Fluorescence and surface tension measurements indicate that above the critical aggregation concentration a surfactant-polymer complex of electrostatic origin is formed in bulk. The complexes have a negative charge that is repelled by the negative charge of the surfactant adsorbed at the interface; consequently, the monolayer seems to be exclusively formed by surfactant carboxybetaines. The high-frequency surface viscoelasticity of the monolayers was studied by surface dynamic light-scattering measurements. The behavior of the dilational elasticity and viscosity is explained by relaxation involving molecular reorientation within the adsorbed layer.     

Application of competitive reaction systems to catalytic kinetic analysis-determination of phosphate

A technique is described for the determination of catalytically active substances, in which a slow catalysed reaction is coupled to a fast competitive reaction. One reactant, which at the same time serves as the indicator substance, is removed by the slow reaction as well as by the competitor added to the system from outside. Under suitable conditions the time for the complete removal of the indicator substance is dependent only on the rate of the catalysed reaction and consequently on the catalyst concentration. The technique is illustrated by means of the phosphate-catalysed reduction of Mo(VI) by ascorbic acid.     

Assessment of a new method for the differential pulse polarographic determination of silicon in steel

A procedure is described by which silicon in steel may be determined by differential pulse polarography after removal of iron. Silicomolybdic acid is formed within 20 min by reaction of the silicon with molybdate in the presence of methyl ethyl ketone: subsequent addition of citrate buffer prevents interference from phosphate and excess of molybdate. At the levels present in high-purity iron ( approximately 0.002%) the precision for silicon is better than that usually quoted for the molybdenum blue method. The steel is dissolved by standard procedures but iron must be removed before the silicon is determined. The lower limit imposed by the polarography is about 10(-5)% silicon, but the practical lower limit is probably set by the difficulty of removing the last traces of iron.