Mg/Zn/Al类水滑石的热分解和水化性能研究

采用共沉淀法制备了Mg2Al1、Zn2Al1和Mg1Zn1Al1LDHs,利用XRD和SEM表征手段,对它们的热分解及焙烧物在Na2CO3溶液中恢复层状结构的能力进行了对比研究。结果表明,在400～700℃温度范围内,Zn2Al1LDH和Mg2Al1LDH的焙烧物中均出现氧化物相(ZnO和MgO)和尖晶石相(ZnAl2O4和MgAl2O4相);而Mg1Zn1Al1LDH的焙烧物中始终以ZnO相为主,仅在700℃时出现微弱的MgAl2O4相。三种焙烧物恢复层状结构的能力为:Mg1Zn1Al1LDO>Mg2Al1LDO>Zn2Al1LDO,其与焙烧物组成有关。原始LDHs和水化LDHs均呈片状。     

煤焦在燃烧过程中孔隙结构变化的模拟

煤焦在燃烧过程中的物理特性，如比表面积和孔径分布会发生连续变化，直接测量煤焦在燃烧过程中的孔隙结构变化很困难，但可以通过合适的数学模型来观察，二维的圆柱孔模型已大量用来对煤焦气化与燃烧过程中表面积和孔隙结构的变化进行模拟，这个模型把孔隙分成两大部分－－大孔与小孔，因为小孔构成比表面的绝大部分，所以在反应过程中比表面积的变化可以由单一小孔模型来拟合，本文采用了用Ｔｓｅｎｇ和Ｅｄｇａｒ提出的孔模型对几     

一种受阻胺封端的聚芴蓝光材料的合成及其稳定性研究

以五甲基哌啶醇、对溴苯酰氯为原料合成了一种受阻胺抗氧稳定剂,通过Suzuki反应将其封端到聚(9,9-二辛基)芴上.通过核磁共振谱、凝胶渗透色谱对合成材料的分子结构进行了表征;并利用荧光发射光谱和退火方法,对其光谱热稳定性进行了细致研究.实验结果表明,当在聚芴分子链上引入受阻胺五甲基哌啶醇后,其荧光发射光谱的稳定性显著提高,绿光区发射现象明显减弱.     

氨·二甲胺·羧酸根合铂(Ⅱ)类配合物的合成、抗肿瘤活性和与DNA的键合水平

本工作设计合成了6种新型混胺羧酸根合铂(Ⅱ)类配合物[Pt((?)NH)(NH₃)X₂](a～f){其中，X=CH₃COO^-(乙酸根)，CH₃Cl COO^-(氯乙酸根)，CHCl₂COO^-(二氯乙酸根)，C₆H₅-COO^-(苯甲酸根)，p-CH₃-C₆H₄-COO^-(对甲基苯甲酸根)，p-CH₃O-C₆H₄-COO^-(对甲氧基苯甲酸根)}。通过元素分析、摩尔电导、差热分析、红外光谱、紫外光谱和 ¹H核磁共振谱对配合物进行了表征。通过MTT法研究了配合物的体外抗肿瘤活性，通过等离子体质谱研究了配合物与细胞DNA的键合量；体外抗肿瘤活性测试表明，配合物(a～f)对所测试的肿瘤细胞MCF-7、HCT-8和BGC-823没有表现出活性，但对EJ和HL-60两种肿瘤细胞表现出好的活性，而且配合物(d～f)对HL-60细胞的活性与顺铂相当。配合物(a～f)与HL-60细胞的DNA键合量与其作用浓度表现出一定的依赖性，从小到大的顺序为：cisplatin < c < b < a < f < e < d。     

Synthesis of a Novel Type of Phosphates of Puerarin

A novel type of phosphated puerarin derivatives were synthesized through a simplified Atheron‐Todd reaction for the first time. The structure of these compounds were elucidated by IR, ESI‐MS and NMR. Moreover, the reason the dialkylphophite reagent had different chemselectivities toward different hydroxys on the puerarin was discussed.     

食品中维生素D与25-羟基维生素D检测技术及含量分布研究进展

维生素D是一种对于维持人体健康具有重要作用的脂溶性维生素,25-羟基维生素D是其在人体内循环和存储的主要形式。食品中维生素D和25-羟基维生素D前处理的通常采用碱皂化、有机溶剂提取、固相萃取或者半制备色谱净化;其测定方法多为放射免疫法和液相色谱法。液相色谱串联质谱凭借高灵敏度和高准确度,目前在食品中维生素D和25-羟基维生素D测定中发挥重要作用。近年来二维液相色谱和超高效超临界流体色谱由于其强大的分离能力,在食品中维生素D和25-羟基维生素D的分析中表现出强大的潜力。该文综述了近年来食品中维生素D和25-羟基维生素D的检测方法及二者在动物食品和植物食品中的含量分布研究,以期为建立适合不同食物样品的测定方法,指导居民合理膳食,进行膳食摄入量评估等研究工作提供参考。     

Application of a contactless conductometric detector for the simultaneous determination of small anions and cations by capillary electrophoresis with dual-opposite end injection

A contactless conductometric detection (CCD) system for capillary electrophoresis (CE) with a flexible detection cell was applied for the simultaneous determination of small anions and/or cations in rain, surface and drainage water samples. The applied frequency, the amplitude of the input signal, the electrolyte conductivity and electrode distance were found to be the most significant factors affecting the detection sensitivity. 2-(N-Morpholino)ethanesulfonic acid/histidine-based (MES/His) electrolytes were used for direct conductivity detection of anions and cations, while ammonium acetate was selected for indirect conductivity determination of alkylammonium salts. For the simultaneous separation procedure, involving dual-opposite end injection, an electrolyte consisting of 20 mM MES/His, 1.5 mM 18-crown-6 and 20 microM cetyltrimethylammonium bromide provided baseline separation of 13 anions and cations in less than 6 min. The detection limits achieved were 7-30 micrograms/l for direct conductometric detection of various common inorganic cations and anions, excluding F- (62 micrograms/l) and H2PO4- (250 micrograms/l), and 35-178 micrograms/l for indirect conductometric detection of alkyl ammonium cations. The developed electrophoretic method with conductometric detection was compared to ion chromatography.     

Three-dimensional quantum dynamics study of vibrational predissociation of HeI_2 van der Waals molecule for low vibrational excitation using the time-dependent wave packet method

Three-dimensional quantum mechanical calculations for vibrational predissociation of HeI2(B) van der Waals molecules are presented using the time-dependent wave packet technique within the golden rule approxima tion.The total and partial decay widths,lifetimes,rates and their dependence on initial vibrational states were obtained for HeI2 at low initial vibrational excited levels.Our calculations show that the calculated tota decay widths,lifetimes and rates agree well with those extrapolated from experimental data available The predicted total decay widths as a function of initial vibrational states exhibit highly nonlinear behavior.The very short propagation time (less.than 1 ps) required in the golden rule wave packet calculation is determined by the duration time of the final state inter-action between the fragments on the vibrationally deexcited adiabatic potential surface.The final state interaction between the fragments is shown to play an important role in determining the final rotational distri     

聚醚桥连二异羟肟酸单核和双核过渡金属配合物催化PNPP水解

Two polyether bridged dihydroxamic acids and their mono-and binuclear manganese(Ⅱ), zinc(Ⅱ) complexes have been synthesized and employed as models to mimic hydrolase in catalytic hydrolysis of p-nitrophenyl picolinate (PNPP). The reaction kinetics and the mechanism of hydrolysis of PNPP have been investigated. The kinetic mathematical model for PNPP cleaved by the complexes has been proposed. The effects of the different central metal ion, mono-and binuclear metal, the pseudo-macrocyclic polyether constructed by polyethoxy group of the complexes, and reactive temperature on the rate for catalytic hydrolysis of PNPP have been examined. The results showed that the transition metal dthydroxamates exhibited high catalytic activity to the hydrolysis of PNPP, the catalytic activity of binuclear complexes was higher than that of mononuclear ones, and the pseudo-macrocyclic polyether might synergetically activate H20 coordinated to metal ion with central metal ion together and promote the catalytic hydrolysis of PNPP.     

芥子气纯度测定不确定度分析与评定

采用酸碱滴定法测定芥子气纯度,对测量结果的不确定度进行评定。分析了测定过程中不确定度来源,包括滴定剂的标定、消耗滴定剂体积、样品称量等引入的不确定度及其计算方法,最后合成得到标准不确定度。当芥子气纯度测定结果为94.78%时,扩展不确定度为0.34%(k=2)。实验结果表明,样品称量引入的不确定度对测量结果的影响最大。