红外光谱法测定酚醛树脂的羟甲基指数

介绍用红外光谱法测定酚醛树脂羟甲基指数的原理和实验条件。红外光谱积分强度法和基线法测定酚醛树脂羟甲基指数的不确定度分别为6.2%和3.2%。以红外光谱积分强度法为例，测定了ZnO催化型酚醛树脂在45℃和25℃时，其羟甲基指数随时间的变化规律。试验结果表明，该方法可以于酚醛树脂的质量控制。     

铁表面硅烷试剂膜的反射吸收红外光谱

以大角度反射吸收红外光谱（RA－IR）研究了铁金属表面涂覆乙烯基硅烷，环氧丙氧丙基硅烷成膜后膜的结构及膜和金属表面之间的结合状态，比较和探讨了不同条件下处理溶液在金属上成膜后膜的特性，并以此来指导工艺预处理过程的处理条件。     

掠角反射吸收红外光谱在有序分子超薄膜结构研究中的应用

综述了掠角反射吸收红外光谱在超薄膜结构研究中的应用,对掠角反射吸收光谱的测试原理及其与透射光谱相结合在超薄膜分子取向的研究中特色和所取得的结果进行了总结．     

化学简讯

普通透射光谱研究天然及合成纤维,有机物针状晶体的红外二色性是困难的,南京大学在研究光波反射时的叠加效应及红外吸收选择定则的基础上,用效率较高的漫反射装置的椭球形光学镜子来收集合轴向样品的外反射光谱,得到了与反射吸收光谱类似的效果。并研究了纤维、针状晶体的表面结构和红外二色性。     

浙江青田石的红外光谱特异性

分别采用傅里叶变换红外光谱的反射模式与透射模式就矿物主体组成分别为叶腊石、地开石、伊利石及绢云母四大类型的浙江青田石进行对比研究。在反射模式下,绢云母型与伊利石型的红外光谱基本类同,但伊利石在其谱图的1 118cm~(-1)附近存在较弱的吸收峰;而叶腊石型与地开石型青田石红外光谱差异显著。在透射模式下,红外光谱的高频区的OH振动峰位与1 200cm~(-1)以下的特征吸收皆可作为鉴别四类青田石的指标性依据。     

CO在载钯分子筛薄膜电极上的增强红外吸收

以NaY分子筛超笼为微型反应器,通过“瓶中造船”技术合成钯原子簇(Pd₁₃).并首次把粗糙的分子筛薄膜电极引入到电化学原位红外反射光谱研究,发现了一类新的增强红外吸收现象.与金属钯电极相比,CO红外吸收带的谱峰强度显著增加,半峰宽加宽.研究结果表明,这种增强红外吸收取决于钯原子簇的纳米尺度及分子筛超笼的特殊环境.     

酸性溶液中过渡金属及合金纳米薄膜电极的异常红外效应研究

以循环伏安方法在玻碳载体上制备纳米级厚度的过渡金属 (Pt,Pd ,Rh ,Ru)和合金 (PtPd ,PtRu)薄膜电极 ,并运用原位FTIR反射光谱研究了CO的吸附过程 .发现所制备的纳米薄膜电极均具有异常红外效应 ,即与本体金属电极相比较 ,吸附在纳米薄膜电极上的CO分子的红外吸收被显著增强 ,并且红外谱峰方向倒反 .本文的结果进一步证明异常红外效应是一种新的、普遍的现象 ,主要取决于过渡金属或合金膜的结构和厚度 .对异常红外效应的深入认识 ,不仅将推动红外反射光谱及界面电化学理论的发展 ,而且将在表面和界面分析中得到广泛应用 .     

团聚铂纳米粒子电极在甲醇氧化中的电催化特性

用H2还原法并以Nafion作为稳定剂合成团聚的Pt纳米粒子，附载于玻碳表面制备电催化剂.透射电子显微镜（TEM）和扫描电子显微镜（SEM）表征结果指出,团聚Pt纳米粒子的平均尺寸约为400 nm.运用电化学循环伏安法(CV)和原位傅立叶变换红外反射光谱（in situ FTIRS）研究甲醇的氧化过程，发现团聚Pt纳米粒子电极具有较高的电催化活性.原位FTIRS研究结果检测到甲醇在所制备的电催化剂上氧化的中间体为线型吸附态CO物种，其红外吸收给出异常红外效应的光谱特征.     

小波变换用于光声光谱的数据分析

７０年代以来，光声光谱研究日渐广泛和深入。光声光谱研究的是物质吸收光受到激发后，通过无辐射跃迁返回初始状态的过程，因此对已被吸收、湮没或发生相互作用的光子也能进行检测和分析。特别是对不透明、高反射、高散射的粉末样品能直接测定，无需进行复杂的前处理，可...     

生物电极的原位FTIR反射光谱研究

利用原位FTIR反射光谱对介体型酶电极、酶免疫电极进行了研究 .通过不同电极电位下的电位差谱和同一电位不同状态下的单光束光谱之差 ,确定并解析了葡萄糖氧化酶 (GOD)和葡萄糖的特征谱峰 ,同时 ,还初步研究了酶免疫电极的红外吸收特征     

Routine determination of the absorption and dispersion spectra of solids with a Fourier-transform infrared spectrometer

A method is given for the routine determination of the absorption and refractive index spectra of solids from their Fourier-transform infrared (F.t.i.r.) specular reflection spectra. The innovation responsible for making these determinations routine and rapid is the application of the fast Fourier-transform software of the F.t.i.r. spectrometer in the calculation of the optical constants. For strongly absorbing materials, accurate values of the resonance absorption frequencies and corresponding absorptivities cannot be obtained from either the reflectance or transmittance spectra. The absorption and refractive index spectra of fused silica are determined here by this method. Starting with a reflection spectrum, the entire procedure requires only 20 min at a resolution of 2 cm^?1. These calculations are impossible with the existing software of most small F.t.i.r. spectrometers; minor software modifications reduce the time required to a few minutes.     

Orientation distribution of liquid-crystalline polyester sheets studied by polarized infrared spectroscopy

Polarized infrared spectroscopy was applied to evaluate the orientation distribution in extrusion-molded sheets of a liquid-crystalline copolyester consisting of 73 mol % of 4-hydroxy benzoic acid units and 27 mol % of 2-hydroxy-6-naphthoic acid units. The surface orientation function was evaluated from the polarized attenuated total reflection/Fourier transform infrared spectra and the polarized specular reflection spectra. In the case of the specular reflection method, the absorption and refractive indices were obtained from the specular reflectance using the Kramers–Kronig relation and the Fresnel equation. On the other hand, the microscopic orientation functions inside the sheets were evaluated by Fourier-transform infrared microspectroscopy. The polarized FTIR microspectra of microtomed section of sheets were measured in a microscopic domain as small as 40 μ at various positions from the center of the sheet. The surface orientation function was shown to be higher than the interior orientation function. Orientation functions obtained by the spectroscopic techniques are lower than crystal orientation functions determined by wide-angle x-ray diffraction, implying that the crystal orientation function is higher than the orientation function of noncrystalline molecular chains. The orientation distribution in the sheet is discussed in relation to the morphological structures studied by scanning electron microscopy. © John Wiley & Sons, Inc.     

十八烷基胺在铁上成膜结构和耐腐蚀性研究

十八烷基胺(ODA)应用于热力设备停用保护技术在国外开发较早[1－3],国内电厂这二年来应用该技术也日益增多,但由于基础研究做得较少,使用效果受到影响.1996年以来我们对ODA的成膜条件和机理进行了一些研究[4－6],本文利用交流阻抗、俄歇电子能谱、红外镜反射光谱、光电化学等方法对ODA的成膜结构和耐蚀性进行探讨,同时介绍ODA在电厂的应用情况.1实验实验材料为DT-4型纯铁.样品制备及交流阻抗测试见文献[4－6].　　俄歇能谱(AES)Perkin-ElmerPHI550ESCA/SAM.实验在机械工业部上海材料研究所进行.　　红外镜反射(SR)Bio-R…     

Complex refractive indexes for polymers over the infrared spectral region: Specular reflection IR spectra of polymers

A dispersion analysis is used to determine the complex refractive indexes over the infrared for the following polymeric systems: isotactic poly(methyl methacrylate), syndiotactic poly(methyl methacrylate), poly(2-methyl-1-pentene)sulfone, poly(perfluoropropylene oxide), poly(pyromellitimide), poly(styrene), and poly(vinyl alcohol). These were combined with solutions of Maxwell's equations for electromagnetic radiation at interfaces in a FORTRAN computer code to model specular relection infrared spectra. Calculations and experimental data are compared to demonstrate the complicated nature of specular reflection and the ability of the modelling to simulate the observed spectra.     

Review on grazing incidence X-ray spectrometry and reflectometry

Grazing incidence X-ray techniques are now widely used for surface and thin film analysis. The present article overviews the recent advancement since 1993 of the grazing incidence X-ray spectrometry and reflectometry in both theoretical and experimental aspects. Every current topic related to the total reflection X-ray fluorescence spectrometry (TXRF) is described in detail through the introduction of numerous published works on the application in the various fields of the science and industrial technologies. Recent rapid growth in diffuse scattering at grazing incidence as well as in specular reflection is another important scope. The combined measurements of different grazing incidence X-ray techniques might be a future trend for realizing further advanced analysis of the surface and interfaces of materials.     

Surface enhanced infrared absorption spectroscopy (SEIRA) using external reflection on low-cost substrates

A novel approach for spectroscopic trace analysis is introduced by combining surface enhanced infrared absorption (SEIRA) spectroscopy with external reflection techniques on disposable inexpensive substrates. SEIRA-active surfaces produced by electrochemical deposition of silver on smooth metal surfaces and glass improve the sensitivity of IR reflection measurements significantly since the infrared absorption of organic substances such as p-nitrobenzoic acid is considerably increased in the vicinity of rough noble metal surfaces. The enhancement properties of thus prepared substrates are characterized and compared using IR-spectroscopy. These low-cost substrates used in single- and multiple external reflection arrangements, respectively, yield a significant increase of the detection level compared to conventional reflection absorption infrared spectroscopy (RAIRS) up to one order of magnitude. Hence, a notable step towards a wide-spread application of SEIRA in routine IR reflection analysis is presented.     

Detection of Casting Material on Historical Violins by Infrared Spectroscopy and Total Reflection X-Ray Fluorescence Spectrometry

Abstract

Infrared spectroscopy and total reflection X-ray fluorescence spectrometry are used for the analysis of historical varnishes. Total reflection X-ray fluorescence spectrometry is used in the analysis of the elemental composition; infrared spectroscopy is used to determine the inorganic and organic molecules of the binding media, pigments and additives. On historical violins made by A. Guarneri and L. Widhalm silicon and tin were found by total reflection X-ray fluorescence spectrometry. Silicon was proved to be present in the form of silicon rubber by infrared spectroscopy. A further experiment confirmed that the treatment of a violin with silicon rubber casting material is detectable.     

Surface enhanced infrared absorption spectroscopy (SEIRA) using external reflection on low-cost substrates

A novel approach for spectroscopic trace analysis is introduced by combining surface enhanced infrared absorption (SEIRA) spectroscopy with external reflection techniques on disposable inexpensive substrates. SEIRA-active surfaces produced by electrochemical deposition of silver on smooth metal surfaces and glass improve the sensitivity of IR reflection measurements significantly since the infrared absorption of organic substances such as p-nitrobenzoic acid is considerably increased in the vicinity of rough noble metal surfaces. The enhancement properties of thus prepared substrates are characterized and compared using IR-spectroscopy. These low-cost substrates used in single- and multiple external reflection arrangements, respectively, yield a significant increase of the detection level compared to conventional reflection absorption infrared spectroscopy (RAIRS) up to one order of magnitude. Hence, a notable step towards a wide-spread application of SEIRA in routine IR reflection analysis is presented. Received: 20 January 1998 / Revised: 3 June 1998 / Accepted: 5 June 1998     

Surface orientation of a liquid-crystalline polymer studied by polarized reflection spectroscopy

The polarized reflection spectrum was used to evaluate the surface orientation of extruded sheets of liquid-crystalline copolyester consisting of 73 mol % 4-hydroxybenzoic acid units and 27 mol % 2-hydroxy-6-naphthoic acid units. The anisotropy of absorption index was evaluated from the specular reflectance using the Fresnel equation and the Kramers-Kronig relation. An intense absorption and observed in the ultraviolet region was assigned to the π^* ←π transitions of the constituent monomeric units. The observed spectra of the liquidcrystalline polymer were successfully interpreted by use of the spectroscopic data on the monomers. The transition moment directions of the monomeric units were calculated by molecular orbital calculations within the framework of the CNDO/S-Cl approximation. The Surface orientation functions obtained from polarized reflection spectra were compared with the crystal orientation functions in the bulk, which were obtained from the azimuthal intensity distribution of wide-angle x-ray diffraction. The orientation behaviour at the surface of the liquid-crystalline polymer was shown to be equivalent to the orientation behaviour in the bulk at higher draw-down ratio.