2,2-亚戊基-1,3-二氧六环-4,6-二酮与原甲酸三乙酯和芳香胺的反应

剂,在有机合成中已有一定应用。开展Meldrum's 酸系列化合物的研究,旨在:1.寻找有结构特点的新试剂,2.合成一系列新化合物,3.研究新化合物的应用。本文通过控制反应温度(28～29℃)催化剂用量(比文献用量多近一倍),提高了2,2-亚戊基-1,3-二氧六环-4,6-二酮(PDDO,3)的制备得率(由15%     

碱基在十二胺-N,N-二亚甲基膦酸改性氧化锆固定相上色谱行为的研究

研究了碱基在十二胺-N,N-二亚甲基膦酸(DDPA)改性氧化锆固定相（DPZ）上的色谱保留行为,考察了流动相中甲醇含量、流动相pH值、缓冲溶液中离子类型和离子强度对碱基保留的影响,对DDPA在氧化锆表面的吸附方式进行了研究。研究结果表明,DDPA仅以一个膦酸基与氧化锆结合,因而DPZ固定相表面上除了有长链的疏水烷基外,还有酸性的膦酸基和碱性的氨基。碱基分子中也存在氨基和酰胺基等极性基团,因此碱基在DPZ固定相上除了有疏水作用外,还具有电荷排斥作用、离子交换作用等多种保留机理。由于多种保留机理的存在,使得碱基在DPZ固定相上具有较好的分离选择性,在酸性条件下对碱基混合样品的分离取得了满意的结果。     

Mechanical characterisation of a viscoplastic material sensitive to hydrostatic pressure

The present paper deals with the characterisation of the static mechanical behaviour of an energetic material all along its lifespan. The material behaviour is viscoplastic, damageable and sensitive to hydrostatic pressure. For such materials, existing models have generally been developed in the framework of transient dynamic behaviour. These models are not suitable for a static study. Therefore a specific experimental protocol and an associated model are developed. Characterisation is derived from both uniaxial compressive, tensile tests and triaxial tests. Plastic behaviour is described by means of a parabolic yield criterion and a new hardening law. Non-associated plastic flow rule and isotropic damage complete the model. The performance of the model is illustrated through the simulation of various loading paths.     

甘氨酸衍生化β-环糊精键合硅胶液相色谱固定相的合成与评价

 β-环糊精键合硅胶经对甲苯磺酰化后,与甘氨酸反应得到甘氨酸衍生化β-环糊精键合硅胶固定相(GCDS)。考察了GCDS对位置异构体、丹磺酰化氨基酸异构体、苯丙酸类药物等的分离性能,研究了流动相中甲醇浓度、pH以及柱温对色谱保留行为的影响。     

利用浅海声场干涉条纹反演海底参数方法研究

浅海频散特性导致声场在距离-频率平面形成干涉条纹,该干涉条纹蕴含着声源以及海底信息。本文通过降噪、滤波等方法,提取船舶辐射噪声干涉条纹中距离域干涉准周期、波导不变量以及去扩展衰减系数(不考虑扩展损失后接收到噪声级随距离的衰减程度)三种特征量的观测值,基于无限均匀沉积层海底模型,采用简正波计算程序理论计算上述三种特征量作为拷贝,提出一种以模拟退火法作为搜索寻优策略的新的匹配反演海底参数的方法。海试数据处理结果表明,该方法反演估计所得海底密度、声速、衰减系数三参数用于浅海负跃层条件下的声场预报效果比较良好。     

有机杂化硫代碲酸盐化合物(H_2en)TeS_3和[Ni(en)_3]TeS_3的溶剂热合成与表征

用低温溶剂热法合成了2种分立结构的有机杂化硫代碲(Ⅳ)酸盐化合物(H2en)TeS3(1)和[Ni(en)3]TeS3(2)(en=乙二胺),通过X-射线单晶衍射,红外光谱,元素分析等手段对它们的结构进行了表征。晶体结构解析结果表明:2个化合物均属单斜晶系,空间群分别为P21和P21/c。化合物1和2具有孤立三角锥[TeS3]2-阴离子,化合物1的平衡阳离子为双质子化乙二胺[H2en]2+,阴离子基团[TeS3]2-和阳离子基团[H2en]2+之间通过N-H…S氢键连接。化合物2的阳离子基团为过渡金属Ni与乙二胺的配合物[Ni(en)3]2+。另外,对该2种晶体进行了紫外-可见漫反射光谱测试和热重分析。     

SECOND-ORDER CONVERGENCE PROPERTIES OF TRUST-REGION METHODS USING INCOMPLETE CURVATURE INFORMATION, WITH AN APPLICATION TO MULTIGRID OPTIMIZATION

Convergence properties of trust-region methods for unconstrained nonconvex optimiza-tion is considered in the case where information on the objective function's local curvatureis incomplete,in the sense that it may be restricted to a fixed set of "test directions"and may not be available at every iteration.It is shown that convergence to local "weak"minimizers can still be obtained under some additional but algorithmically realistic condi-tions.These theoretical results are then applied to recursive multigrid trust-region meth-ods,which suggests a new class of algorithms with guaranteed second-order convergenceproperties.     

Icems and dcems study of Fe layers evaporated onto Al and Si

Thin layers of⁵⁷Fe (2.5 nm, 10 nm and 70 nm thickness), vacuum evaporated onto Al and Si plates, have been investigated by conversion electron Mössbauer spectroscopy (CEMS). The measurements were performed employing both a proportional counter and a channeltron for conventional and ultrahigh-vacuum integral CEMS (UHV-ICEMS) studies, respectively, and a channeltron for depth-selective CEMS (DCEMS). The phase analysis of the layers on base of experimental results has indicated the presence of metallic iron and one or two iron compounds, ascribed to iron reaction products formed with the residual gas during evaporation. These products are most likely rather stable iron nitrides, are more or less clustered and are distributed throughout the whole layer.