多重衰减全反射-红外光谱法在复合材料表面分析中的应用

应用衰减全反射-傅立叶变换红外光谱技术(FTIR-ATR)分析三种不同类型复合材料成分,并运用扫描电镜和光电子能谱方法对结果进行了确证,确定了:1.复合材料密封膜HNP由聚丙烯、(乙烯-乙酸乙烯酯)共聚物和聚酰胺三层材料组成;2.纤维复合膜中间层的粘结材料为聚四氟乙烯;3.金属复合包装膜中聚合物材料为(偏二氯乙烯-丙烯酸酯)共聚物。实验表明FTIR-ATR技术在复合材料表层和夹层中高分子材料成分的分析应用中有明显的优势,简化了繁杂的分离纯化样品工作,方法简单、易于操作。文中对使用FTIR-ATR技术进行定性分析中的若干问题提出探讨。     

Investigation of the hydrothermal stability of cross-linked liquid silicone rubber (LSR)

We investigate the hydrothermal stability of cross-linked liquid silicone rubber (LSR) in water at 100 °C up to period of two years. Optical microscopy of cross-sections of the exposed samples reveal that only the outer 100 μm of the surface layer is affected after two years. However, the surface chemistry of the material after prolonged exposure becomes significantly modified, as monitored by X-ray photoelectron spectroscopy (XPS) and attenuated total reflectance Fourier transform infrared (ATR-FTIR), which probes depths of 10 nm and 1 μm, respectively. In addition, changes to the bulk physical properties of the rubber samples, prior to and after the exposure, were investigated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Micro-hardness analysis showed that surface roughness of the two year exposed sample increased from 60 (IRHD) to 75 (IRHD). Furthermore, the volume change (%) measurement showed a significant decrease in the course of exposure at prolonged time. The results provide the experimental basis for development of LSR materials suitable for numerous technical applications.     

Influence of Sodium Periodate and Tyrosinase on Binding of Alginate to Adlayers of Mytilus edulis Foot Protein 1

Mytilus edulis foot protein 1 (Mefp-1) is the most well-characterized component of this sea mussel's adhesive plaque. The plaque is a condensed, heterogeneous mixture consisting of a large proportion of cross-linked biopolymers that bonds the mussel to a chosen mooring. Mefp-1 is densely populated with lysine and -3,4-dihyroxyphenylalanine ( -dopa) residues incorporated into a repeating amino acid sequence motif. It has been proposed that one plaque cross-linking reaction is the nucleophilic addition of the ε-amino groups of the lysine residues into the oxidized catechol (o-diphenol) functionality (quinone) of the -dopa residues. In order to determine if this reaction occurs in adlayers of Mefp-1, a previously developed assay for ε-amino groups was applied. Adlayers of Mefp-1 were exposed to an oxidant, either the enzyme, mushroom tyrosinase, or sodium periodate. Binding of alginate to adlayers was used to probe for accessibility of ε-amino groups. It was found that lysine residues lose the ability to bind alginate after exposure to sodium periodate, but that this loss is not clearly due to a reaction with -dopa residues. There is a slight decrease of binding of alginate to adlayers of Mefp-1 exposed to either active or thermally deactivated mushroom tyrosinase, probably due to the obstruction of binding sites by bound enzyme. Adsorption kinetics of mushroom tyrosinase onto adlayers of Mefp-1 for active and thermally inactivated enzyme were nearly identical. Attenuated total reflection Fourier transform infrared spectroscopy was used to characterize these interactions at a germanium (Ge) interface.     

Spectroscopic study of conformation changes of bovine serum albumin in aqueous environment

The secondary structural changes of protein aqueous solutions with and without calcium cations were investigated by attenuated total reflection-Fourier transform infrared (ATR-FTIR) technology.     

添加型聚丙烯大分子表面改性剂PP-g-PEG的制备及其应用

以马来酸酐为桥联剂,通过其与单端羟基聚乙二醇的反应,合成了大分子表面改性剂聚丙烯-聚乙二醇接枝共聚物,探索了反应条件对接枝反应的影响,用IR、NMR、TGA、DSC对接枝物的结构及性能进行研究,并通过共混研究了接枝物对聚丙烯的表面改性效果.结果表明,提高马来酸酐接枝聚丙烯或聚乙二醇的分子量,会阻碍接枝反应的进行,接枝率明显下降;接枝聚乙二醇降低了接枝物的结晶能力;聚丙烯-聚乙二醇接枝共聚物的热稳定性随着聚乙二醇的含量增加及侧链聚乙二醇长度的增加略有下降;聚丙烯-聚乙二醇接枝共聚物组分在共混物中具有明显的向外择优迁移特性,可以作为聚丙烯的添加型表面改性剂使用.     

羟基磷灰石与牛血清白蛋白相互作用的原位红外光谱研究

应用原位(in situ)全反射红外光谱研究牛血清白蛋白在电化学法制备的羟基磷灰石表面的吸附和成键行为, 探索电化学法制备的HA生物材料/生物环境界面过程和生物相容性的微观本质.     

Effect of nitrogen additives on flame retardant action of tributyl phosphate: Phosphorus-nitrogen synergism

The effects of three nitrogen additives (urea, guanidine carbonate, and melamine formaldehyde) on the flame retardant action of cotton cellulose treated with tributyl phosphate (TBP) were investigated in this research. The limiting oxygen index (LOI) of treated cotton cellulose clearly revealed the synergistic interactions of TBP and nitrogen compounds. The Kissinger method was used to evaluate the kinetics of thermal decomposition on treated cellulose. The results show that adding nitrogen additives increases the activation energy at a higher degree of degradation, thus indicating better thermal stability at higher temperatures. Scanning electron microscope pictures of chars formed after a LOI test show the formation of protective polymeric coatings on char surfaces. Evaluating char surfaces using attenuated total reflectance-Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy suggests that these coatings are composed of species containing phosphorus-nitrogen-oxygen. Possible chemical interactions of phosphorus and nitrogen compounds during the burning process and the formation of a protective coating could be the reason for the observed synergism. Potential reaction pathways contributing to the formation of this protective polymeric coating have also been proposed.     

ATR-FTIR光谱法同时测定香精的相对密度和折光指数

傅里叶变换衰减全反射红外光谱 (ATR- FTIR)分析技术与偏最小二乘法 (PL S)相结合 ,建立了香精相对密度、折光指数的校正模型。模型的预测结果与标准方法测定结果在 5 %显著性水平下无显著性差异。该法用于香精物理指标的检测 ,操作简单、快速、准确。     

乐果和氧化乐果水解过程的衰减全反射-傅立叶变换红外光谱(ATR-FTIR)研究

运用ATR-FTIR深入探讨了乐果和氧化乐果分子结构的特征振动及其酸、碱条件下水解历程对其特征结构振动的变化规律. 由实验结果, ATR-FTIR能够显著地区分乐果和氧化乐果两分子的结构振动. 氧化乐果在3302 cm^－1 ν_as (NH), 3089 cm^－1ν_as (CH₂), 1739 cm^－1 ν (C-O), 1554 cm^－1 ν (O＝C-N) II等峰位明显区别于乐果分子对应结构的振动峰位及其峰位强度. 碱性水解条件下, 乐果的ATR-FTIR特征表现在2108 cm^－1平宽峰增强, 氧化乐果则表现为ν (P＝O)红移和ν_as (P-O-C)蓝移|酸性水解条件下, 乐果ATR-FTIR中高波段的NH, CH₃振动较强, 氧化乐果则因其分子链被破坏, 表现出无特征振动. 以上ATR-FTIR获得的结果从另一角度, 互补性地揭示了乐果和氧化乐果两分子内部的结构振动差别和酸、碱水解历程对其振动结构的影响变化. 为便捷、高效地区分物质分子结构的差异, 尤其是分子结构极为相似的细微结构的差异提供了较为完整的信息, 同时也为研究物质结构及其形态变化提供了十分有益的参考.