LLDPE/LLDPE-g-AA共混物的接触角及红外光谱表征

利用熔融共混的方法制备了线性低密度聚乙烯/线性低密度聚乙烯接枝丙烯酸(LLDPE/LLDPE-g-AA)共混物。用傅里叶红外光谱(FT-IR)和测定接触角的方法对不同LLDPE-g-AA含量的LLDPE/LLDPE-g-AA共混物膜的表面进行了表征。结果表明,随着共混物中LLDPE-g- AA含量的增加,水和甘油等极性液体与共混物表面的接触角下降。依据共混物的FT-IR计算了其羧基峰强度。发现极性液体与LLDPE/LLDPE-g- AA共混物膜表面的接触角越小,羧基峰强度越大。

Synthesis and properties of three tris(1,10-phenanthroline) ruthenium (II) derivatives

Three new asymmetrical ruthenium (II) complexes: [Ru(phen)(2){phen-NHCO(CH2)(4)Br}](PF6)(2), [Ru(phen)(2){phen-NHCO(CH2)(5)Br}](PF6)(2) and [Ru(phen)(2){phen-NHCO(CH2)(10)Br}](PF6)(2) were synthesized, which were confirmed by the technique of FT-IR, H-1 NMR and ESI-MS. The electrochemical and fluorescent properties of three Ru (II) complexes were investigated with cyclic voltammetry and fluorometry.

Synthesis, electrochemistry and fluorescence of four new Ru(phen)(3)(2+) derivatives

Four typical LB monolayer film materials, Ru(phen)(3)(2+) complexes with one ligand attached to different long chain alkyl amides, were designed and synthesized. Their chemical structures were identified by the techniques of FT-IR, H-1 NMR and ESI-MS. Also, UV-Vis, electrochemistry and fluorescence of these complexes are reported.

Sol-gel thin-film immobilized soybean peroxidase biosensor for the amperometric determination of hydrogen peroxide in acid medium

An acid-stable soybean-peroxidase biosensor was devel oped by immobilizing the enzyme in a sol-gel thin film. Methylene blue was used as a mediator because of its high electron-transfer efficiency. The sol-gel thin film and enzyme membrane were characterized by FT-IR, and the effects of pH, operating potential, and temperature were explored for optimum analytical performance by using the amperometric method. The H2O2 sensor exhibited a fast response (5 s), high sensitivity (27.5 mu A/mM), as well as good thermostability and long-term stability. In addition, the performance of the biosensor was investigated using flow-injection analysis (FIA).

Observations on photochemical fluorescence enhancement of the terbium(III) sparfloxacin system

Fluorescence of terbium(III) was sensitized when excited in the presence of sparfloxacin (SPFX) in the aqueous solution because a Tb(III)-SPFX complex was formed. The sensitized fluorescence was further enhanced when this system was exposed to 365 nm ultraviolet light. By the spectral properties and contrast experiments, it is proved that irradiation makes this system undergo photochemical reactions and a new terbium complex which is more favorable to the intramolecular energy transfer is formed. The mechanism of photochemical fluorescence enhancement of the Tb(III)-SPFX system is discussed and a new sensitive and selective photochemical fluorimetry for the determination of SPFX is established. Under the optimum conditions, the linear range is 1.0-50 x 10(-7) M for SPFX, the detection limit is 3.0 x 10(-9) M and the R.S.D. for 5.0 x 10(-7) M SPFX is 1.3% (n = 9). Without any pretreatment the recovery of SPFX in human urine was determined with satisfaction. (C) 1999 Elsevier Science B.V. All rights reserved.

Synthesis and characterization of a water-soluble endohedral metallofullerol

A water-soluble endohedral metallofullerol, Pr@C82Om(OH)(n)(m approximate to 10 and n approximate to 10), was successfully synthesized through the reaction of a pure endohedral metallofullerene, Pr@C-82, with a concentrated nitric acid and a subsequent hydrolysis process. The formation of endohedral metallofullerols Pr@C82Om(OH)(n) is thought to involve a NO2 radical formation step, in much the same way as the reaction of empty fullerenes. FT-IR, XPS, and LD-TOF MS techniques were employed to characterize the structure of the endohedral metallofullerol from the above reaction.

Fabrication and characterization of heteropolyanion Langmuir-Blodgett films

The possibility of the formation of Langmuir-Blodgett (LB) films with dimethyldioctadecylammonium (DODA) after the addition of cobalt(II)-substituted Dawson-type tungstodiphosphate anion (briefed as (H2O)(CoP2W17O618-)-P-11) in the subphase has been explored. Marked modifications of the compression isotherms are observed when this anion is dissolved in the subphase, which demonstrates that the polyanions interact with the monolayers. LB films have been readily obtained from this system. The adsorption Fourier transform IR (FT IR) spectroscopy, atomic force microscopy (AFM), X-ray diffraction (XRD) and cyclic voltammetry (CV) have been used to investigate the morphological and molecular structure of the deposited film. The FT IR results showed the presence of the polyanion within the LB films, and the shift for its characteristic bands may be related to the presence of positively charged DODA. AFM measurement reveals that the LB films of DODA/(H2O)(CoP2W17O618)-P-II are regularly and uniformly deposited on the substrate. XRD experiments prove that the lamellar structure of the LB films of DODA/(H2O)(CoP2W17O618-)-P-II is well-defined. The LB films of DODA/(H2O)(CoP2W17O618-)-P-II immobilized onto an indium-oxide (ITO) glass, in aqueous solutions of pH 2.0-5.0, show quite facile redox reactions even for multilayers. All the experiments carried out in the present study suggest that the new materials of heteropolyanions can be formed by LB techniques and beneficial physicochemical properties of heteropolyanions can be maintained/enhanced through molecular-level design. (C) 1999 Elsevier Science S.A. All rights reserved.

TiO_2纳米粉的热处理过程研究

用溶胶凝胶法制备出纳米凝胶粉，于不同温度下热处理形成纳米晶，研究热处理温度对粒子大小、形貌、品相转变及吸附能力的关系．XRD、FT-IR、Raman光谱研究表明200～600℃热处理1h的TiO2纳米晶为锐钛矿相，在700℃热处理的纳米晶为锐钛矿相与金红石相共存，800℃热处理的纳米晶完全为金红石相;TEM、TG、XPS的结果证明热处理温度越高，纳米粒子的粒径越大，吸附能力也越弱.

推进剂组分对聚醚聚氨酯粘合剂热氧降解的影响 (Ⅱ)固体填料和助剂的影响

采用FT-IR和多种NMR技术研究了推进剂中常用的几种填料和助剂对聚醚聚氨酯粘合剂热氧降解的影响。高氯酸铵、奥克托金、铝粉、硝化纤维素、键合剂、碳黑等均不改变聚氨酯粘合剂的降解机理，但表现出不同程序的稳定作用。过氯酸铵的吸附作用使样品始终保持固体形态，而含其它组分的样品在降解过程中逐渐变为液态。在ＮＥＰＥ推进剂的热氧降解过程中，硝酸酯和中定剂逐渐挥发分解，粘合剂发生降解，导致推进剂强度降低。

环氧乙烷/四氢呋喃共聚醚聚氨酯的热氧降解

采用FT-IR和13CNMR、1HNMR技术研究羟基环氧乙烷/四氢 呋喃共聚醚(EO/THF)聚氨酯在90℃空气中降解产物的结构．结果表明，聚醚聚氨酯的热氧降解既有软段的氧化降解，又有硬段的解缩聚过程，同时还存在重聚合反应；并且软、硬段互有影响，硬段中的交联结构和氢键增加了软段的热氧稳定性，而软段降解产生的醇的含量和结构影响硬段的解缩聚和重聚合过程．90℃下聚氨酯 的热氧降解并不发生硬段的氧化反应，也不存在碳化二亚胺和假脲醚结构.

添加剂对EO/THF共聚醚聚氨酯热氧降解的影响

采用FT-IR及NMR技术研究固化催化剂、增塑剂、抗氧剂及聚醚二元醇结构对聚醚聚氨酯热氧降解过程的影响． 增塑剂邻苯二甲酸二丁酯(DBP)在聚醚聚氨酯热氧降解过程中起阻降作用． 而固化催化剂二月桂酸二丁基锡(DBTDL)和三苯基铋(TPB)对聚醚聚氨酯的热氧降解有着截然不同的影响． 以聚乙二醇(PEG)为聚醚二元醇的聚醚聚氨酯与环氧乙烷/四氢呋喃(EO/THF)共聚醚聚氨酯具有相似的降解机理；DBP增塑时PEG聚醚聚氨酯比共聚醚聚氨酯具有较低的热氧稳定性，而硝酸酯增塑时PEG体系比共聚醚体系表现出较高的热氧稳定性.

Studies on uniaxially drawn poly(vinylidene fluoride) films

Poly(vinylidene fluoride) (PVDF), under certain conditions, shows a crystal transition between the alpha (TGT (G) over bar) and beta (TTT) forms, where T, G, and (G) over bar, respectively, denote trans, gauche, and minus gauche. We investigated the mechanism of this crystal transition by FT-TR and X-ray diffraction, which yielded consistent results. We also carried out differential scanning calorimeter experiments.

Miscibility and specific interactions in poly(beta-hydroxybutyrate-co-beta-hydroxyvalerate) and poly(P-vinylphenol) blends

The blends of poly(beta-hydroxybutyrate-co-beta-hydroxyvalerate) (P(HB-co-HV)/poly(p-vinylphenol)(PVPh) were investigated by differential scanning calorimetry (DSC), Fourier transform IR (FT-IR) spectroscopy and high-resolution solid-state C-13 NMR techniques. Single glass transition temperatures existing in the whole composition range indicates that these blends are miscible. The presence of hydrogen bonding between the hydroxyl of PVPh and carbonyl of P(HB-co-HV), shown by FT-IR spectra, is the origin of the miscibility. Furthermore, results obtained by high-resolution solid-state C-13 NMR give more information about the structure of the blends. (C) 1998 Elsevier Science Ltd. All rights reserved.

Macrocyclic oligomeric arylene ether ketones: Synthesis and polymerization

Some novel macrocylic(arylene ether ketone)oligomers were synthesized in high yields by a nucleophilic aromatic substitution reaction of 4,4'-dinitrobenzophenone with bisphenols in the presence of anhydrous potassium carbonate under pseudo-high-dilution conditions. Detailed structural characterization of these oligomers by matrix-assisted laser desorption/ionization-time of flight-mass spectrometry (MALDI-TOF-MS), H-1 NMR and FT-IR confirmed their cyclic nature and the compositions of the oligomeric mixtures was indicated by GPC analysis. Ring-opening polymerization of cyclic oligomers 3a to a high molecular weight polymer with M-w of 52.3 and M-n of 17.2 k was achieved by heating at 280 degrees C for 40 min in the presence of a nucleophilic initiator.

Synthesis and characterization of soluble polyimides from 1,1-bis(4-aminophenyl)cyclohexane derivatives

A series of novel aromatic diamines (1-3) containing kinked cyclohexylidene moieties was synthesized by a reaction of excess aniline and corresponding methyl-substituted cyclohexanone derivatives. The structures of (1-3) were identifield by H-1 NMR, C-13 NMR, and FT-IR. The polymers were synthesized from the obtained diamines and various aromatic dianhydrides by the conventional polycondensation reaction followed by chemical imidization as well as high-temperature one-step polymerization. The inherent viscosities and weight-average molecular weights of the resulting polyimides were in the ranges of 0.55-1.58 dL/g and (7.4-15.2) x 10(4) g/mol, respectively. The prepared polyimides showed excellent thermal stabilities and good solubility. All polymers were readily soluble in common organic solvents such as tetrahydrofuran, chloroform, tetrachloroethane, etc., and the glass transition temperatures were observed at 290-372 degrees C.