Functional group characterizations

Vibrational spectroscopy is the method of choice for the characterizing functional groups in complex organic molecules. Infrared transmission spectroscopy has been used on dried humics pressed into KBr pellets to determine the relative carboxylate content of humic materials (14-16). However, interferences arise from the presence of water bands and possible alterations of the samples under the high pressures used to form the pellets. Diffuse-reflectance techniques can avoid some of the difficulties associated with the KBr pressed-pellet method (9,17-18). To obtain a spectrum analogous to an absorption spectrum, the data are transformed from reflectance units to Kebulka-Munk (K-M) units. However, K-M units are related to... 

Little use has been made of the IR spectra of phospholes. A few reports exist on such spectral measurements, but primarily they have been made for the purpose of characterizing functional groups on the ring. From the spectrum reported for methyl l-methylphosphole-3-carboxylate (vch3110, 1535, 1250 and 1186, unassigned at 1075, 1062, 888, 793, 740, 700 cm ... 

The main experimental parameter in IR is the frequencies (e.g. v for stretching, 5 for in-plane bending and y for out-plane bending) of the absorption bands characterizing functional groups, in particular Vc=o and Vn-h for biomolecules. The vibrational frequency Vyib of a bond can be approximately described by the formula... 

Fourier transfer IR (FTIR) spectroscopy has been widely nsed to characterize functional groups in polymers and organic componnds. Manbrane chemical degradation, which usually introduces new functional gronps, can be readily monitored... 

In addition to characterizing functional groups, in situ micro-Raman experiments were used to monitor the water content inside the membrane. It is found that the anode side membrane has lower water content when a current is applied (Matic et al. 2005). Overall water content is lower under load, which may be due to higher temperature. 

Fourier transform infrared (FTIR) spectroscopy was used to identify the presence of sulfonic acid groups in polymer samples. It was also used to observe the interactions between SPEEK polymer and solvent in the SPEEK membrane. Also, FTIR spectroscopy has been widely used to characterize functional groups in polymers and organic compounds. Membrane based on SPEK, which usually introduces new functional groups, can be readily monitored by FTIR. FTIR spectra were recorded by using either powder samples inside a diamond cell or KBr pellets composed of 50 mg of IR spectroscopic grade KBr and 1 mg polymer sample. ... 

Section 4 1 Functional groups are the structural units responsible for the character istic reactions of a molecule The hydrocarbon chain to which a func tional group is attached can often be considered as simply a supporting framework The most common functional groups characterize the fami lies of organic compounds listed on the inside front cover of the text... 

The proportionality between the concentration of chromophores and the measured absorbance [Eqs. (6.8) and (6.9)] requires calibration. With copolymers this is accomplished by chemical analysis for an element or functional group that characterizes the chromophore, or, better yet, by the use of isotopically labeled monomers. 

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... 

The two most useful supplementary techniques for the light microscope are EDS and FTIR microscopy. Energy dispersed x-ray systems (EDS) and Eourier-transform infrared absorption (ETIR) are used by chemical microscopists for elemental analyses (EDS) of inorganic compounds and for organic function group analyses (ETIR) of organic compounds. Insofar as they are able to characterize a tiny sample microscopically by PLM, EDS and ETIR ensure rapid and dependable identification when appHed by a trained chemical microscopist. 

Collectors ndFrothers. Collectors play a critical role ia flotation (41). These are heteropolar organic molecules characterized by a polar functional group that has a high affinity for the desired mineral, and a hydrocarbon group, usually a simple 2—18 carbon atom hydrocarbon chain, that imparts hydrophobicity to the minerals surface after the molecule has adsorbed. Most collectors are weak acids or bases or their salts, and are either ionic or neutral. The mode of iateraction between the functional group and the mineral surface may iavolve a chemical reaction, for example, chemisorption, or a physical iateraction such as electrostatic attraction. 

The functional group ia collectors for nonsulfide minerals is characterized by the presence of either a N (amines) or an O (carboxyUc acids, sulfonates, etc) as the donor atoms. In addition to these, straight hydrocarbons, such as fuel oil, diesel, kerosene, etc, are also used extensively either as auxiUary or secondary collectors, or as primary collectors for coal and molybdenite flotation. The chain length of the hydrocarbon group is generally short (2—8 C) for the sulfide collectors, and long (10—20 C) for nonsulfide collectors, because sulfides are generally more hydrophobic than most nonsulfide minerals (10). 

Hydrogels are water-containing polymers, hydrophilic in nature, yet insoluble. In water, these polymers swell to an equiUbrium volume and maintain thek shape. The hydrophilicity of hydrogel is a result of the presence of functional groups such as —NH2, —OH, —COOH, —CONH2, —CONH—, —SO H, etc. The insolubihty and stabiUty of hydrogels are caused by the presence of a three-dimensional network. The scope, preparation, and characterization of hydrogels has been reviewed (107). 

The molecular stmcture of the copolymers is also important. Molecular-weight measurements (osmometry, gpc) and functional group analysis are useful. Block copolymers require supermolecular (morphological) stmctural information as well. A listing of typical copolymer characterization tools and methods is shown in Table 6. 

Types of Solids Geldart [Fowder TechnoL, 7, 285-292 (1973)] has characterized four groups of solids that exhibit different properties when fluidized with a gas. Figure 17-j shows the division oi the classes as a function of mean particle size, d,, Im, and densitv difference, (p, — P/ ), g/cm, where p, = particle density and p = fluid density... 

In general, air quality data are classified as a function of time, location, and magnitude. Several statistical parameters may be used to characterize a group of air pollution concentrations, including the arithmetic mean, the median, and the geometric mean. These parameters may be determined over averaging times of up to 1 year. In addition to these three parameters, a measure of the variability of a data set, such as the standard deviation... 

All the well-characterized proteinases belong to one or other of four families serine, cysteine, aspartic, or metallo proteinases. This classification is based on a functional criterion, namely, the nature of the most prominent functional group in the active site. Members of the same functional family are usually evolutionarily related, but there are exceptions to this rule. We... 

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. 

Microchemical reactions These can be carried out either with universal reagents [11] or with such substances which react with particular functional groups (group-characterizing reagents). If the separation process ensures that only one component occurs at a particular spot on the chromatogram, then this can be detected sub-stance-specifically . But specificity in an unequivocal sense can only be produced by a combination of the separation and the detection process. (The same is true of other forms of detection.)... 

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