动,静态硫化（NR＋SBR）／PE共混体系的结构与性能

用TEM研究了(NR SBR)/PE共混体系经动、静态硫化后的形态结构及其与力学性能的关系。未硫化和静态硫化体系的形态结构与其组成有关,均以含量大的组份为连续相;对动态硫化体系,当(NR=SBR)/PE<70/30时,均以PE为连续相,其性能主要依赖于构成连续相组份的性质。 动态硫化体系的T_g值低于静态体系,随PE组份含量的增加变化不大,而静态硫化体系的T_g值则随PE含量增加向高温方向迁移。用DSC测得动态硫化体系的结晶度比静态体系的大。前者的应力-应变性能也低于后者。     

Thermal decomposition of the composite hydrotalcites of iowaite and woodallite

The thermal stability and thermal decomposition pathways for synthesized composite iowaite/woodallite have been determined using thermogravimetry analysis in conjunction with evolved gas mass spectrometry. Dehydration of the hydrotalcites occurred over a range of 56–70°C. The first dehydroxylation step occurred at around 255°C and, with the substitution of more iron(III) for chromium(III) this temperature increased to an upper limit of 312°C. This trend was observed throughout all decomposition steps. The release of carbonate ions as carbon dioxide gas initialised at just above 300°C and was always accompanied by loss of hydroxyl units as water molecules. The initial loss of the anion in this case the chloride ion was consistently observed to occur at about 450°C with final traces evolved at 535 to 780°C depending of the Fe:Cr ratio and was detected as HCl (m/z=36). Thus for this to occur, hydroxyl units must have been retained in the structure at temperatures upwards of 750°C. Experimentally it was found difficult to keep CO₂ from reacting with the compounds and in this way the synthesized iowaite-woodallite series somewhat resembled the natural minerals.     

新试剂3,5—二溴—4—偶氮8—羟基喹啉苯基荧光酮光度法测定微量铝

在溴化十六烷基三甲胺（ＣＴＭＡＢ）存在下，ＰＨ６，０的ＨＡｃ－ＮａＡｃ缓冲介质中，铝与新试剂３，５－二溴－４－偶氮８－羟基喹啉苯基荧光酮形成红色三元胶束配合物，最大吸收波长位于５６４ｎｍ，表观摩尔吸光系数ε为１．３５×１０＾５．ｍｏｌ＾－１．ｃｍ＾－１，铝浓度在０～５μｇ／２５ｍＬ范围内符合比耳定律，拟定的方法用于铝铁黄铜中微量铝的测定，结果满意。     

Mesoporous micelle templated silica with incorporated C<Subscript>8</Subscript> and C<Subscript>18</Subscript> phase

Mesoporous silica material of MCM-41 type was synthesized by co-condensation of highly concentrated octyltriethoxysilane (OTEOS), octadecyltriethoxysilane (ODTEOS) and tetraethoxysilane (TEOS). The obtained hybrid materials were characterized using XRD, TG-DSC and low temperature adsorption/desorption of nitrogen. It was shown that the applied method of synthesis allows to obtain silica of MCM-41 type with a high degree of hydrocarbon saturation.     

Preparation of HPMC–EA–DMAEMA nanosized latex

Nanosized copolymer latex of hydroxypropylmethylcellulose (HPMC) grafted with ethyl acrylate (EA) and dimethylaminoethyl methacrylate (DMAEMA) has been prepared by acidifying submicron-sized latex particles synthesized by soap-free emulsion graft copolymerization using potassium persulfate (KPS) as initiator. The effects on the diameter of the latex particles of different conditions, for example concentration of DMAEMA, amount of HPMC, and ratio of HCl to DMAEMA for acidification, were investigated. It was found that increasing the mole ratio of HCl to DMAEMA to 1.0 and increasing the DMAEMA content both resulted in a decrease in particle diameter, whereas increasing the amount of HPMC resulted in larger particle sizes. Measurement by dynamic light scattering (DLS) revealed the diameter of the latex particles was >200 nm before acidification and <100 nm after acidification. Evidence of grafting was obtained by use of Fourier transform infrared (FTIR) spectroscopy. Transmission electron microscopy (TEM) was used to characterize the morphology of the copolymer particles before and after acidification.     

Influence of thermal and thermo-mechanical treatment

Two lipids with similar melting ranges but of different composition were analyzed using differential scanning calorimetry and X-ray diffraction. The lipids were processed via extrusion or were tempered at different temperatures; they were analyzed directly after extrusion and after storage at 40°C. Precirol ATO 5® showed high sensitivity to storage time and varied temperature exposure. Extrusion showed only marginal influences on the solid state. Melting peaks were narrower and shifted to higher temperatures in comparison to the untreated powder. Dynasan 114® was more robust, changes in the solid state could only be shown for samples treated above the melting range. Thus, Dynasan 114® is more appropriate for solid lipid extrusion of pharmaceutical products.     

Calorimetric approach to tetronic/water interactions

Tetronic^®comprises X-shaped copolymers formed by four poly(propylene oxide) (PPO) andpoly(ethylene oxide) (PEO) block chains bonded to an ethylene diamine centralgroup. Micellization behaviour of three representative Tetronics (T304, T904and T1307) was characterized to gain an insight into the interactions betweenthe copolymer unimers and the state of water in their solutions. The enthalpyof demicellization, recorded at 37°C in an isoperibol microcalorimeter,indicated that the process was in all cases exothermic and the enthalpy rankedin the order T1307≥T904>>T304. Micellization is entropy-driven owing tohydrophobic interactions between the PPO chains.DSC analysisshowed that the crystallization and melting peaks of the free water remainingin T304 and T904 solutions were progressively shifted toward lower temperaturesas the surfactant proportion increased, owing to a colligative effect. Boundwater corresponded to 3 water molecules per EO repeating unit. In the caseof T1307, which has longer PEO chains, a splitting of the melting peak wasobserved, one peak appearing around 0°C due to free water and anotherat –15°C due to interfacial water. As T1307 proportion raised, theenthalpy of the former decreased, whilst the enthalpy of the latter increased.In 40% T1307 solutions, interfacial water overcame the proportion of freewater; there being 1 interfacial and 3 bound water molecules per EO repeatingunit. Gaussian deconvolution of FTIR spectra also enabled to characterizethe evolution of free water as a function of Tetronic proportion. The dependenceof micellization and water interaction behaviour on Tetronics structure shouldbe taken into account to use these copolymers as drug solubilizers and micellarcarriers.     

希土烯丙基化合物的研究——Ⅷ.镝、钬、铒、镱和镥的2-甲基烯丙基化合物的合成

用无水希土氯化物与2-甲基烯丙基氯化镁及四甲基乙二胺,0℃下,在四氢呋喃中反应,加乙醚后可得到五个含2-甲基烯丙基的重希土元素的化合物。经元素分析、红外光谱和质谱分析的鉴定,确定该化合物的组成为Ln(C₄H₇)₂Cl₅Mg₂(tmed)₂。