Characterization infrared spectroscopy

While the broad mission of the National Bureau of Standards was concerned with standard reference materials, Dr. Isbell centered the work of his laboratory on his long interest in the carbohydrates and on the use of physical methods in their characterization. Infrared spectroscopy had shown promise in providing structural and conformational information on carbohydrates and their derivatives, and Isbell invited Tipson to conduct detailed infrared studies on the extensive collection of carbohydrate samples maintained by Isbell. The series of publications that rapidly resulted furnished a basis for assigning conformations to pyranoid sugars and their derivatives. Although this work was later to be overshadowed by application of the much more powerful technique of nuclear magnetic resonance spectroscopy, the Isbell— Tipson work helped to define the molecular shapes involved and the terminology required for their description. 

Ori ally ai lied jH edominantly as an analytical tool in the field of polymer characterization infrared spectroscopy has bem increasingly utilized in the last decades for the ducidation of the diysical structure of polymers. However, with the advent of rapid-scanning FTIR instruments and the development of the iheo-optical FTIR technique infrared spectro py has been launched into a completely new ex of polymer ph ical applications. 

Fourier transform infrared (FTIR) analysis (characterization) Infrared spectroscopy using the adsorption of IR radiation by the molecular bonds to identify the bond types that can absorb energy by vibrating and rotating. In Fourier transform infrared spectrometry (FTIR), the need for a mechanical slit is eliminated by frequency modulating one beam and using interferometry to choose the IR band. 

Porter M D, Bright T B, Allara D L and Chidsey C E D 1987 Spontaneously organized molecular assemblies. 4. Structural characterization of normal-alkyl thiol monolayers on gold by optical ellipsometry, infrared-spectroscopy, and electrochemistry J. Am. Chem. Soc. 109 3559-68... 

Most hydrocarbon resins are composed of a mixture of monomers and are rather difficult to hiUy characterize on a molecular level. The characteristics of resins are typically defined by physical properties such as softening point, color, molecular weight, melt viscosity, and solubiHty parameter. These properties predict performance characteristics and are essential in designing resins for specific appHcations. Actual characterization techniques used to define the broad molecular properties of hydrocarbon resins are Fourier transform infrared spectroscopy (ftir), nuclear magnetic resonance spectroscopy (nmr), and differential scanning calorimetry (dsc). 

Characterization. In many cases, ftir is a timely and cost-effective method to identify and quantify certain functionaHties in a resin molecule. Based on developed correlations, ftir is routinely used as an efficient method for the analysis of resin aromaticity, olefinic content, and other key functional properties. Near infrared spectroscopy is also quickly becoming a useful tool for on-line process and property control. 

The ease of sample handling makes Raman spectroscopy increasingly preferred. Like infrared spectroscopy, Raman scattering can be used to identify functional groups commonly found in polymers, including aromaticity, double bonds, and C bond H stretches. More commonly, the Raman spectmm is used to characterize the degree of crystallinity or the orientation of the polymer chains in such stmctures as tubes, fibers (qv), sheets, powders, and films... 

Amides can be titrated direcdy by perchloric acid ia a nonaqueous solvent (60,61) and by potentiometric titration (62), which gives the sum of amide and amine salts. Infrared spectroscopy has been used to characterize fatty acid amides (63). Mass spectroscopy has been able to iadicate the position of the unsaturation ia unsaturated fatty amides (64). Typical specifications of some primary fatty acid amides and properties of bisamides are shown ia Tables 5 and 6. 

There are a variety of analytical methods commonly used for the characterization of neat soap and bar soaps. Many of these methods have been pubUshed as official methods by the American Oil Chemists Society (29). Additionally, many analysts choose United States Pharmacopoeia (USP), British Pharmacopoeia (BP), or Pood Chemical Codex (FCC) methods. These methods tend to be colorimetric, potentiometric, or titrametric procedures. However, a variety of instmmental techniques are also frequendy utilized, eg, gas chromatography, high performance Hquid chromatography, nuclear magnetic resonance spectroscopy, infrared spectroscopy, and mass spectrometry. 

Infrared Spectroscopy (ir). Infrared curves are used to identify the chemical functionality of waxes. Petroleum waxes with only hydrocarbon functionality show slight differences based on crystallinity, while vegetable and insect waxes contain hydrocarbons, carboxyflc acids, alcohols, and esters. The ir curves are typically used in combination with other analytical methods such as dsc or gc/gpc to characterize waxes. 

An unusual method for the preparation of syndiotactic polybutadiene was reported by The Goodyear Tire Rubber Co. (43) a preformed cobalt-type catalyst prepared under anhydrous conditions was found to polymerize 1,3-butadiene in an emulsion-type recipe to give syndiotactic polybutadienes of various melting points (120—190°C). These polymers were characterized by infrared spectroscopy and nuclear magnetic resonance (44—46). Both the Ube Industries catalyst mentioned previously and the Goodyear catalyst were further modified to control the molecular weight and melting point of syndio-polybutadiene by the addition of various modifiers such as alcohols, nitriles, aldehydes, ketones, ethers, and cyano compounds. 

Infrared spectroscopy, including Fourier-transform infrared (FTIR) spectroscopy, is one of the oldest techniques used for surface analysis. ATR has been used for many years to probe the surface composition of polymers that have been surface-modified by an etching process or by deposition of a film. RAIR has been widely used to characterize thin films on the surfaces of specular reflecting substrates. FTIR has numerous characteristics that make it an appropriate technique for... 

In order to characterize the surface regions of a sample that has been modified in some way, as is usually the case in adhesion-related investigations, some sort of a reflection experiment is required. Two types of experiments, attenuated total reflection (ATR) and reflection-absorption infrared spectroscopy (RAIR),... 

As indicated above, the penetration depth is on the order of a micrometer. That means that in ATR, absorption of infrared radiation mostly occurs within a distance 8 of the surface and ATR is not as surface sensitive as some other surface analysis techniques. However, ATR, like all forms of infrared spectroscopy, is very sensitive to functional groups and is a powerful technique for characterizing the surface regions of polymers. 

The value of infrared spectra for identifying substances, for verifying purity, and for quantitative analysis rivals their usefulness in learning molecular structure. The infrared spectrum is as important as the melting point for characterizing a pure substance. Thus infrared spectroscopy has become an important addition to the many techniques used by the chemist. 

His researches and those of his pupils led to his formulation in the twenties of the concept of active catalytic centers and the heterogeneity of catalytic and adsorptive surfaces. His catalytic studies were supplemented by researches carried out simultaneously on kinetics of homogeneous gas reactions and photochemistry. The thirties saw Hugh Taylor utilizing more and more of the techniques developed by physicists. Thermal conductivity for ortho-para hydrogen analysis resulted in his use of these species for surface characterization. The discovery of deuterium prompted him to set up production of this isotope by electrolysis on a large scale of several cubic centimeters. This gave him and others a supply of this valuable tracer for catalytic studies. For analysis he invoked not only thermal conductivity, but infrared spectroscopy and mass spectrometry. To ex-... 

Useful information such as the functionality and crystallinity of the polymers can be obtained by using infrared spectroscopy. Elemental analysis is also considered as one of die tools for die characterization of die polymers. Due to die endgroups and incomplete combustion of the carbon, it is common to observe die low-value carbon content than die theoretical one. 

Complexes. The structure of an n a charge-transfer complex between quinoxaline and two iodine atoms has been obtained by X-ray analysis and its thermal stability compared with those of related complexes. The hydrogen bond complex between quinoxaline and phenol has been studied by infrared spectroscopy and compared with many similar complexes. Adducts of quinoxaline with uranium salts and with a variety of copper(II) alkano-ates have been prepared, characterized, and studied with respect to IR spectra or magnetic properties, respectively. 

If gaseous S2O-SO2 mixtures are dissolved in dry solvents such as CS2, CCI4, CHCI3, CH2CI2, and liquid SO2 at temperatures between -75 and -1-25 °C, intense yellow solutions of polysulfuroxides are obtained which have been characterized only very poorly [19]. In contrast to the opinion of some authors [20], S2O cannot be detected in such solutions, e.g., by infrared spectroscopy. Most probably, mixtures of cyclic polysulfuroxides are present besides SO2 (see below, in particular the preparation of S5O), e.g. ... 

This is a nonpolar rubber with very little unsamration. Nanoclays as well as nanotubes have been used to prepare nanocomposites of ethylene-propylene-diene monomer (EPDM) rubber. The work mostly covers the preparation and characterization of these nanocomposites. Different processing conditions, morphology, and mechanical properties have been smdied [61-64]. Acharya et al. [61] have prepared and characterized the EPDM-based organo-nanoclay composites by X-ray diffracto-gram (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy... 

Adsorption phenomena from solutions onto sohd surfaces have been one of the important subjects in colloid and surface chemistry. Sophisticated application of adsorption has been demonstrated recently in the formation of self-assembhng monolayers and multilayers on various substrates [4,7], However, only a limited number of researchers have been devoted to the study of adsorption in binary hquid systems. The adsorption isotherm and colloidal stabihty measmement have been the main tools for these studies. The molecular level of characterization is needed to elucidate the phenomenon. We have employed the combination of smface forces measmement and Fomier transform infrared spectroscopy in attenuated total reflection (FTIR-ATR) to study the preferential (selective) adsorption of alcohol (methanol, ethanol, and propanol) onto glass surfaces from their binary mixtures with cyclohexane. Om studies have demonstrated the cluster formation of alcohol adsorbed on the surfaces and the long-range attraction associated with such adsorption. We may call these clusters macroclusters, because the thickness of the adsorbed alcohol layer is about 15 mn, which is quite large compared to the size of the alcohol. The following describes the results for the ethanol-cycohexane mixtures [10],... 

Owing largely to research over the last twenty years, the sulfided C0-M0/AI2O3 system is one of the best-characterized industrial catalysts [H. Topsoe, B.S. Clausen and F.E. Massoth, Hydrotreating Catalysis (1996), Springer-Verlag, Berlin]. A combination of methods, such as Mbssbauer spectroscopy, EXAFS, XPS, and infrared spectroscopy, has led to a picture in which the active site of such a catalyst is known in almost atomic detail. 

In the present study, we synthesized in zeolite cavities Co-Mo binary sulfide clusters by using Co and Mo carbonyls and characterized the clusters by extended X-ray absorption fine structure (EXAFS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and high resolution electron microscopy (HREM). The mechanism of catalytic synergy generation in HDS is discussed. 

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