Thermodynamic Study of the Three Isomers of Bromobenzoic Acid

The enthalpies of sublimation and fusion and triple-point temperatures of 2-bromo-. 3-bro-mo- and 4-bromobenzoic acids have been determined precisely by sublimation calorimetry, drop calorimetry and differential thermal analysis. The measurements of sublimation enthalpy of the three acids were made at 333, 348 and 363 K, respectively, using a Tian-Calvet microcalorimeter equipped with Knudsen effusion cells. The derived standard molar enthalpies of sublimation at 298.15 K are (95. 94±0. 41), (99. 20± 0.18), and (103. 08±0. 59) kJ · mol-1for the 2-bromo-, 3-bromo- and 4-bromobenzoic acids, respectively. In addition, the saturated vapour pressure of these compounds was also calculated on the basis of the sublimation experiments. The enthalpy of fusion, the triple-point temperatures and the mole fraction purities of the samples of the investigated substances were measured using the mean temperature version DTA apparatus developed by the CTM of the CNRS in Marseille. The triple-point temperature and the     

Mg0.9-xTi0.1PdxNi(x=O.04～0.1)贮氢合金电极腐蚀行为研究

研究了Pd部分替代Mg对Mg0.9-xTi0.1PdxNi(x=0.04～0.1)贮氢合金腐蚀性能的影响.利用机械合金化方法制备了Mg0.9-xTi0.1PdxNi(x=0.04～0.1)贮氢合金.XRD和TEM分析表明经120 h球磨后该合金完全非晶化.循环充放电测试结果表明,Pd的替代有效地延长了Mg0.9-xTi0.1PdxNi(x=0.04～0.1)合金的循环寿命.采用开路电位测量,阳极极化,电化学阻抗和X射线光电子能谱研究了该合金的腐蚀行为.结果表明,随着Pd含量增加,合金腐蚀电位正移,初始腐蚀电流下降,腐蚀电流增加的速度变缓.采用本文提出的等效电路模型较好地拟合了合金的电化学阻抗谱.分析表明,随着Pd含量的增加,合金表面钝化膜厚度和电阻逐渐增大.X射线光电子能谱分析表明,Pd的加入减弱了合金在充放电过程中的氧化程度.当Pd含量达到0.1时,Mg0.9-xTi0.1PdxNi(x=0.04～0.1)合金的耐腐蚀性能最好,其放电容量保持率最高.     

流动注射在线共沉淀HG-AFS测定痕量铅

建立了流动注射在线共沉淀HG-AFS测定痕量铅的分析方法。方法基于铅在碱性介质中与氢氧化镁共沉淀，沉淀收集在锥形沉淀腔中，用HCl溶洗沉淀和NaBH4反应，产生的氢化物被载气引入原子化器中进行测定。测定铅的RSD为3％(5ng/mL，n=10)，检出限为0．01ng。检出限较直接进样降低了11倍。对国家标准物质中铅的测定结果与标准值相符。     

Synthesis and Bioactivity of Novel Fluorinated Heteroaromatic Ureas

In order to find new urea cytokinins, a series of novel fluorinated heteroaromatic ureas have been designed and synthesized. The crystal structure of 3g was further determined by single crystal X-ray diffraction to obtain the structural feature of this class of urea compounds. The preliminary bioassay showed that some title compounds have good cytokinin activity.     

高效液相色谱和热重分析在树形聚酰胺胺合成中的应用

优化了聚酰胺胺树形分子合成工艺条件，采用HPLC和热重分析（TG）相结合的方法对所合成的树形聚酰胺胺进行分析与表征；HPLC的分析表明，在各不同代的目标化合物中，均有反应物单体存在，在高代产物中除了含有少量反应物外，还有少量的低代数分子；TG分析表明，产物中小分子反应物占的比例很少，一般为2％－3％左右，如果将减压蒸馏后的产物重新进行真空干燥，对半代树形大分子，能进一步有效除去小分子反应物，而对于整数代树形大分子，则效果并不理想。     

超分子化合物[M(4,4''''-bipy)2(H2O)4]·(4,4''''-bipy)2·(3,5-diaba)2·8H2O](M=Co,Ni,Cd)的合成及晶体结构

合成了3个超分子化合物[M(4,4'-bipy)2(H2O)4]·(4,4'-bipy)2·(3,5-diaba)2·8H2O(M=Co(1),Ni(2),Cd(3);4,4'-bipy=4,4'-联吡啶;3,5-diaba=3,5-二氨基苯甲酸阴离子),用红外光谱、元素分析及X-射线单晶衍射进行了表征。3个化合物的晶体都属于单斜晶系,空间群为P2/c。晶体学参数:化合物1:a=0.9389(2)nm,b=0.7751(1)nm,c=3.9284(6)nm,β=90.14(2)°,V=2.85880(69)nm3,Z=4,Dc=1.397g·cm-3,F(000)=1266,μ=0.380mm-1,R1=0.0349,wR2=0.0829;化合物2:a=0.9383(2)nm,b=0.7753(1)nm,c=3.9218(6)nm,β=90.09(1)°,V=2.85280(68)nm3,Z=2,Dc=1.399g·cm-3,F(000)=1268,μ=0.420mm-1,R1=0.0366,wR2=0.0805;化合物3:a=0.94091(13)nm,b=0.77885(11)nm,c=3.9712(5)nm,β=90.10°,V=2.9102(7)nm3,Z=2,Dc=1.433g·cm-3,F(000)=1308,μ=0.454mm-1,R1=0.0468,wR2=0.0964。3,5-diaba未参与配位,在配位阳离子[M(4,4'-bipy)2(H2O)4]2 中,金属离子M髤与来自2个4,4'-bipy的2个氮原子和4个水分子的氧原子配位,呈八面体的几何构型。分子中还存在未配位的4,4'-bipy。通过配位阳离子、游离4,4'-bipy及未配位的3,5-diaba间的丰富氢键,构建成具有三维结构的超分子化合物。     

富勒醇清除OH自由基的ESR研究

富勒醇清除·ＯＨ自由基的ＥＳＲ研究祝严师，孙大勇，刘桂珍，刘子阳，詹瑞云，刘淑莹（中国科学院长春应用化学研究所应用谱学开放实验室，长春，１３００２２）关键词Ｃ_（６０），富勒醇，ＯＨ自由基，自旋捕捉，ＥＳＲ生物体内的许多现象均涉及到自由基反应，现已发?..     

碳化树脂全孔结构分析

本文阐述了改良的MP法,对含中孔和微孔的碳化树脂,用改良的MP法计算其微孔分布;用模型法计算其中孔分布,两种方法分析的和表示其全部孔结构分析。     

线粒体和亚线粒体体外代谢及漆酶影响的微量热研究

首次将微量热用于亚细胞层次的研究，测定了鲤鱼肝脏线粒体和亚线粒体代谢的热谱及其漆树漆酶的影响，并用ＭＴＤ方程和演化计算技术对它们的代谢热动力学参数进行了全局优化。     

Calorimetric Study of Thermal Denaturation of Superoxide Dismutase

The thermal denaturation of superoxide dismutase (SOD) from bovine erythrocytes was studied at various pH values of different buffers and at various concentrations of solutions of two neutral salts by differential scanning calorimetry. The experiments performed indicate that the PIPES is a buffer non-coordinating with the SOD, and that the binding of the anions studied influences more or less the thermal denaturation of SOD, but the effect on the oxidation form of SOD is more apparent. A new conformer of SOD with lower thermostability was discovered by the experiments performed in different buffers at certain pH values higher than the isoelectric point of SOD, or at higher concentrations of neutral salt solutions. The new conformer may be converted irreversibly into the usual conformer with high thermostability during heating. Based on the thermodynamic parameters obtained in distilled water and by thermodynamic analysis using the Ooi's model, it is revealed that the large enthalpy △Hdc contributed by