Improved Synthesis and Structure of 3-Carboxy-2-pyrazinecarbohydroxamic Acid

3-Carboxy-2-pyrazinehydroxamic acid was prepared by a one pot reaction starting from pyrazine-2,3-dicarboxylic anhydride with a high yield, and characterized by IR, Mass spectrum, 1H NMR and 13C NMR spectra and single-crystal X-ray diffraction. It crystallizes in triclinic, space group Pī with a=4.8659(10), b=7.4233(15), c=11.602(2), α=96.904(2), β=92.422(3), γ=107.454(2)°, V=395.51(14)3 , Z=2, Dc=1.689g/cm3 , F(000)=208, μ(MoKα)=0.149 mm-1 , the final R=0.0473 and wR=0.1306 for 2853 observed reflections (I>2σ (I)). A three-dimensional framework was assembled through intermolecular hydrogen bonding between water and 3-carboxy-2-pyrazine-carbohydroxamic acid molecules.     

Rejoinder for Gaining effciency via weighted estimators for multivariate failure time data

We thank all the discussants for their interesting and stimulating contributions. They have touched various aspects that have not been considered by the original articles.     

中药炮制机理研究的思路与方法——以咖啡豆的烘焙原理研究为例

中药炮制是中药学的特色和优势,也是最具我国自主知识产权的学科之一.中药炮制研究的核心是阐明中药炮制机理,这也是制约中药现代化的关键节点.目前大部分中药的炮制机理尚不明确,有待进行系统深入的研究.咖啡豆需要烘培后才可以制成饮料,这个高温烘培过程类似于中药的炮制过程.近年来,国内外专家对咖啡豆高温烘培过程化学成分变化及其机理进行了深入研究,各种新方法和新技术得到广泛应用,取得了系列研究成果,这些研究成果为中药炮制机理研究提供了多种新思路和新方法,也为中药炮制机理的研究和阐明提供了重要示范.     

Highly Selective Synthesis of Methyl 1-Phenyl-1-(9-hydro-)fullerenylacetate

Isomerically pure methyl 1-phenyl-1-(9-hydro-)fullerenylacetat is synthesized in 75% yield by the reaction of C₆₀ with the carbanions of methyl phenylacetate in C₆H₆/THF mixed solvent under a purified N₂ atmosphere at 20°C.     

A STUDY OF LOW CYCLE FATIGUE PROPERTIES OF MATERIALS BASED ON THE FUNNEL-SHEET SPECIMENS1)

根据能量等效方法,针对漏斗薄片试样,提出了关联Ramberg-Osgood 幂律参数、试样几何参数的载荷-位移半解析统一模型。采用有限元数值模拟,正、反向验证了该模型的有效性。在此基础上,提出了通过漏斗薄片试样低循环试验实现材料低周疲劳性能的预测方法。基于薄片试样低循环试验数据,完成了SS316L, N18及SAPH440 三种材料的低周疲劳性能预测,预测结果与标准试样试验结果具有良好的一致性。并利用该方法完成了N18与SAPH在不同温度条件下的低周疲劳性能预测。     

NATIONAL STANDARD OF HEAT CAPACITY MEASUREMENT OF SOLIDS IN THE RANGE OF 4.2—90K——AN AUTOMATED ADIABATIC CALORIMETER FROM 25 TO 90K AND MOLAR HEAT CAPACITIES OF α-ALUMINA

The construction of an automated adiabatic calorimeter for heat capacity measurement ofsolids in the temperature range of 25- 90K is described in detail. The sample vessel of thecalorimeter has thin radial vanes which make no contact with its inner wall and are distrib-uted evenly, thus greatly improving the internal thermal equilibration of the vessel. Theprecision of temperature control for the adiabatic shields and electrical leads of the calori-metric system are heightened to a great extent by using the high precision ACD- 79 modeladiabatic controller specially developed by us for this purpose. Measurements of the heatcapacities of high purity α-Al_2O_3, one of the internationally-accepted standard referencematerials, agree with those of the National Bureau of Standards (NBS), USA within ±0.3%,demonstrating the reliability of this apparatus.     

高效液相色谱法测定胶粘剂中的游离甲醛

建立了胶粘剂中游离甲醛的高效液相色谱检测方法,对提取方法、衍生化条件及色谱条件进行了研究。结果表明,采用超声波萃取法代替经典的水蒸气蒸馏法能更快速、高效地提取目标物。液相色谱法对甲醛的检出限为0．024μg／mL,在0．1～12μg／mL范围内,线性相关系数R^2=0．9995,在1、2、8μg／mL三个添加水平下,回收率在98．73％～101．68％之间。五个实验室间的相对标准偏差为2．6％。对某白乳胶样品的测定结果表明,本法在定性检测、抗干扰能力及稳定性上都高于常用的乙酰丙酮比色法。     

邻苯二酚在活化玻碳电极上的电化学行为

邻苯二酚( QH2,儿茶酚)等有机化合物是人体内的电活性物质,直接参与人体内的各种生理过程.     

山地输电线动刚度计算及模态分析

为了揭示地形变化对连续档输电线动态特性的影响，本文提出了基于任意高差角的动刚度理论．首先将单档导线视为连续档导线的子结构，构建了两悬挂点不等高的单档导线振动方程，并在该理论方程中引入了二次项，能够考虑重力沿弦向分量的影响，推导出绝缘子串绕其悬挂点转动的动刚度计算方法，通过动刚度理论研究连续档导线横向振动模态和频率，并应用有限元软件ABAQUS 验证理论模态和频率公式的准确性．所得结果表明，动刚度的计算方法具有较高的精度，理论模态与有限元输出结果吻合较好，同时获得的频率和模态可为山地高压输电线路防舞技术的研究提供依据．     

锆钛酸钡钙压电陶瓷的晶粒尺寸效应研究进展

锆钛酸钡钙无铅压电陶瓷具有可与锆钛酸铅媲美的压电性能,受到国内外广泛关注.晶粒尺寸是影响锆钛酸钡钙陶瓷电性能的重要因素,其晶粒尺寸效应已成为研究的热点.为此,综述了粉体制备方法、烧结方法、烧结温度和保温时间对锆钛酸钡钙陶瓷的晶粒尺寸及其电性能的影响,并提出了研究中亟待解决的问题.