SYNTHESIS AND THERMAL PROPERTIES OF POLYBENZOXAZOLE FROM SOLUBLE PRECURSOR WITH HYDROXY-SUBSTITUTED POLYENAMINONITRILE

Aromatic polybenzoxazole (PBO) precursor, hydroxy-substituted polyenaminonitrile, was prepared by direct polycondensation of 1,4-bis(l-chloro-2,2-dicyanovinyl)benzene (CCB) and 4,6-diaminoresorcinol dihydrochloride (DAR) using pyridine and N,N-dimethylacetamide as condensing agent and solvent. The precursor has good solubility in polar aprotic solvent which is due to the strong dipolar nature of the main chain. The soluble precursor was subjected to thermal cyclization in an inert atmosphere to convert it into the corresponding PBO, which has its 5% weight loss temperature at 540℃ The fully cyclized PBO were characterized by FT-IR and TGA. The introduction of 10% mol 1,3,5-benzenetricarboxylic chloride (BTC) into the main chain not only has little effect on the solubility of PBO precursor but also raises its 5% weight loss temperature to 552℃ and char yield at 700℃ for the cyclized PBO with BTC.     

氟环唑外消旋体在纤维素-三(3,5-二甲基苯基氨基甲酸酯)手性固定相上的高效液相色谱法拆分

在纤维素-三(3,5-二甲基苯基氨基甲酸酯)（CDMPC）手性固定相上,分别采用正相、反相及极性有机相色谱模式对氟环唑外消旋体进行了拆分,并考察了流动相组成在手性识别中对手性分离的影响。氟环唑在Chiralcel OD-H手性色谱柱（填充CDMPC手性固定相）上采用反相色谱模式,以甲醇-水(体积比为80∶20)为流动相,获得了最佳的拆分,其两对对映异构体的分离度Rs分别为1.64和6.50。     

三酰甘油氧化聚合物的制备型快速柱层析-体积排阻色谱测定法

建立了一种简便、灵敏、无需内标的检测油脂中三酰甘油氧化聚合物(TGP)的分析方法。以制备型快速层析柱(PFC)(flash硅胶柱,20 g,40～60μm,6 nm)分离1 g油脂样品中极性组分(PC),经高效体积排阻色谱(HPSEC)(GPC柱,Ф7.8 mm×300 mm,粒径5μm,孔径10 nm)将PC细分为氧化三酰甘油寡聚物(TGO)、氧化三酰甘油二聚物(TGD)、氧化三酰甘油单体(ox-TGM)、二酰甘油(DG)、游离脂肪酸(FFA)。结合重量法测定油脂中PC、面积归一法测定PC中TGP,可准确定量油脂中的TGP含量。结果表明,TGO、TGD分别在28～1 800、11～2 800 mg/L范围内线性关系良好,相关系数(r2)分别为0.998 2、0.998 7,TGO及TGD的检出限(LOD)分别为28、11 mg/L,定量下限(LOQ)分别为113、44 mg/L;相当于油脂中TGP的LOD为0.01%。PFC-HPSEC法检测油脂TGP的相对标准偏差(RSD)均小于10%。PFC对3个PC加标水平(2.27%、8.47%、30.94%)的平均回收率为95%～98%,相对标准偏差(RSD)均低于4%。PFC-HPSEC方法与经典的硅胶柱-HPSEC方法定量油脂TGP的结果吻合度高,相对误差为0～8.9%。该方法能够在2 h内实现各种油脂中TGP含量的定量检测,包括使用过的废弃油脂与未使用的食用油脂,尤其适用于低含量TGP的初榨油和精炼油脂。     

岩石抽提物中极性化合物超高分辨质谱识别

采用具有超高分辨率的负离子电喷雾-傅立叶变换离子回旋共振质谱（ESI FT-ICR MS）分析了储层岩石抽提物中的石油酸及中性氮化物的分子组成,得到了抽提物中杂原子化合物类型分布、等效双键数（Double bonds equivalent,DBE）及碳数分布特征。研究结果表明,储层抽提物中含有多达16种不同杂原子类型的化合物,包括N1、N1O1、N1O2、N1O3、N1S1、N1S2、N2、N2S1、O1、O1S1、O2、O2S1、O1S2、O2S2、O3和O4,其中N1、N1S1、O2及O2S1类具有较高的相对丰度。抽提物中的N1类化合物以咔唑和苯并咔唑类化合物为主;N1S1类化合物以C2~C8烷基取代的咔唑并苯并噻吩类化合物为主;O2类化合物主要为1~2环环烷酸,其次还在抽提物中鉴别出具有较高相对丰度的DBE为5和6的O2类化合物;而O2S1类化合物中以DBE为7和8的O2S1具有最高的相对丰度。     

新型亚微米亲水作用色谱的制备及其在加压毛细管电色谱中的应用

采用改良Stöber法合成580 nm亚微米单分散的二氧化硅微球，并以此为基质，通过"巯基-烯"点击化学反应将半胱氨酸成功键合到修饰有乙烯基团的二氧化硅微球表面，合成了一种新型亚微米亲水作用固定相（Cys-VTMS-SiO₂）。采用高压匀浆法制备了新型亚微米亲水色谱填充柱，通过不同乙腈比例、缓冲盐浓度和pH条件下对甲苯、丙烯酰胺和硫脲的分离分析揭示其亲水机理。依托加压毛细管电色谱平台，成功实现了对核苷、酚类、胺类及多肽等亲水性物质的快速有效分离，其有望应用于其他强极性和亲水性化合物的分离分析。     

多工况多约束下离散变量桁架结构的拓扑优化设计

提出了一个多工况下受应力、位移约束的离散变量桁架结构的拓扑优化方法，给出了结构拓扑形式变更时的约束处理方法及杆件删除策略，使基结构设计空间的维数不断降低，达到最优拓扑，避免了奇异解的出现，在算例中指出了截面离散集和位移约束对最优拓扑的影响；算例给出了满意的拓扑优化解。     

Lukasiewicz 命题逻辑系统一种新的理论的相容度

根据演绎定理和完备性定理,应用公式真度理论在Lukasiewicz命题模糊逻辑系统中讨论理论Γ的相容性,根据矛盾式■是Γ-结论的真度的大小,提出了一种新的极指标和相容度的概念.给出了理论Γ相容、不相容及其它相关结论的充分必要条件,并且获得了相容度与发散度之间联系的重要关系式.     

双螺旋叠栅条纹检测光束准直性的两种方法

介绍双螺旋叠栅条纹检测光束准直性的基本原理,进一步就双螺旋叠栅条纹的特征参量与被测光束发散角(即光束准直精度)的关系进行分析和推导。在分析双螺旋叠栅条纹进行时,首先采用频域低通滤波提取纯叠栅条纹,然后提取纯叠栅条纹的特征参量。提出两种特征参量的提取方法,一种依次进行傅里叶变换计算相位信息的傅里叶变换方法,另一种是受传统时间相移算法启发而提出的空间相移算法,讨论了在两种方法中极坐标的重采样问题和相应的计算公式,并进行了计算机模拟。结果表明,傅里叶变换方法和空间相移算法实质都是获取叠栅条纹全场趋势的平均值,使最终光束发散角的检测具有很高的精度,对自成像条纹周期的检测误差在±2.8‰以内。     

Loop Groups and Twin Buildings

In these notes we describe some buildings related to complex Kac–Moody groups. First we describe the spherical building of SL_n() (i.e. the projective geometry PG(ⁿ)) and its Veronese representation. Next we recall the construction of the affine building associated to a discrete valuation on the rational function field (z). Then we describe the same building in terms of complex Laurent polynomials, and introduce the Veronese representation, which is an equivariant embedding of the building into an affine Kac–Moody algebra. Next, we introduce topological twin buildings. These buildings can be used for a proof which is a variant of the proof by Quillen and Mitchell, of Bott periodicity which uses only topological geometry. At the end we indicate very briefly that the whole process works also for affine real almost split Kac–Moody groups.Supported by a Heisenberg fellowship by the Deutsche Forschungsgemeinschaft.     

Atmospheric,hydrological and oceanic comprehensive contributions to seasonal polar wobble of Earth Rotation

The geophysical quantitative excitation on seasonal polar wobble of Earth Rotation has not been well achieved so far. The atmospheric, hydrologic and oceanic angular momentum variations are investigated from monthly values simulated by a coupled ocean-atmosphere general circulation model. The simulated equatorial AAM functions agree well with that from the JMA operational analysis in 90°:E direction, but disagree along Greenwich meridian. As for the annual cycle, not only the hydrologic and oceanic excitations partly match the residuals between geodetic functions of polar wobble and JMA AAM functions, but also the combinations with NCEP and JMA analysis AAM functions are better than those estimated from NCAR-CSM1 climate model.