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Infrared Spectroscopy Marianne L. McKelvy,*,† Thomas R. Britt,† Bradley L. Davis,† J. Kevin Gillie,*,‡ Felicia B. Graves,† and L. Alice Lentz†
Analytical Sciences Laboratory, The Dow Chemical Company, U.S.A., Midland, Michigan 48667, and Applied Extrusion Technologies, 15 Reads Way, Newcastle, Delaware 19720 Review Contents Overview of Analytical Infrared Spectroscopy Books and Reviews Databases, Software, and Algorithms Infrared Accessories and Sampling Techniques Quantitative Analysis Spectra-Structure Correlation Hypenated Techniques Time-Resolved Infrared Spectroscopy Reflectance Techniques Single-Crystal and Bulk Analysis Applications Thin-Film Applications Interfacial Applications Adsorption and Surface Reaction Applications Attenuated Total Reflectance Diffuse Reflectance Emission Process and in Situ Analysis Environmental Analysis Carbon and Carbon Complexes Chemical Reactions/Organic Chemistry Hydrogen-Bonding Studies Catalysis Studies Solvent/Matrix Effects Organic Reactions/Characterization Food and Agriculture Biochemistry Literature Cited
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This review covers the published literature for the period November 1995 to October 1997 on aspects of infrared spectroscopy that are relevant to chemical analysis. Our review is directed to papers written in English or in certain aspects of IR spectroscopy that are of particular interest to one or more of the coauthors. Where some overlap may occur in a particular area, a few selected references to Raman or FT-Raman spectroscopy are included. OVERVIEW OF ANALYTICAL INFRARED SPECTROSCOPY Infrared radiation is commonly defined as electromagnetic radiation with frequencies between 14 300 and 20 cm-1 (0.7 and 500 µm). When a normal molecular motion such as a vibration, rotation, rotation/vibration, or lattice mode or a combination, difference, or overtone of these normal vibrations results in a change in the molecule’s dipole moment, a molecule absorbs infrared radiation in this region of the electromagnetic spectrum. The corresponding frequencies and intensities of these infrared † ‡
The Dow Chemical Co. Applied Extrusion Technologies.
S0003-2700(98)00006-7 CCC: $15.00 Published on Web 04/24/1998
© 1998 American Chemical Society
bands, the infrared spectrum, may be used to characterize the material. Infrared spectral information may be used to identify the presence and amount of a particular compound in a mixture. Different classes of chemical compounds contain structural units that absorb infrared radiation at essential similar frequencies and intensities within that class of compound. These bands are called “group frequencies”. The infrared spectroscopist uses knowledge of these group frequencies to predict the structures of unknown molecules when standard infrared spectra are not available. Sample collection and presentation accessories exist which allow the analyst to collect spectra as solids, liquids, and vapors and in solution, at various temperatures, and while undergoing mechanical deformation. Experiments conducted under such conditions assist the spectroscopist in the determination of the structures of molecules in different phases as well as structure-property relationships of materials. Modern instrumentation allows the collection of infrared spectra of materials at low-picogram levels. The ability of infrared spectroscopy to examine and identify materials under such a wide variety of conditions has earned this technique the premier position as the “work horse” of analytical science. BOOKS AND REVIEWS A compilation of IR and Raman spectra of inorganic compounds was published (A1). A book regarding infrared spectroscopy of biomolecules provided a comprehensive review of this area (A2). This work contains references to studies of protein structures, nucleic acids, ultrafast spectroscopy, lipids, enzymes, and cell surface polysaccharides. A textbook prepared as an instructional aid in the study of vibrational spectroscopy was presented (A3). A book detailing applications of infrared spectroscopy in electrochemistry was published (A4). Computerized applications of infrared spectroscopy, such as data manipulation, databases, multivariate techniques, and spectrometer networking, were detailed (A5). Internet sites that deal with infrared spectroscopy and instructional issues were listed (A6). Group frequency assignments for the major bands in 20 common polymers were compiled (A7). Methods for obtaining characteristic group frequencies were reviewed (A8). Resources and references for interpretation of spectra were discussed (A9, A10). Several general reviews of vibrational spectroscopy were presented (A11-A13). The application of far-IR spectroscopy was reviewed (A14). The infrared spectroscopy of radicals was reviewed (A15). The role of step-scanning interferometers was reviewed by several authors for the study of polymeric systems (A16, A17) and for transition metal complexes (A18). Progress Analytical Chemistry, Vol. 70, No. 12, June 15, 1998 119R
in the use of mid-IR optical fibers was presented (A19). Developments in infrared microspectroscopy were discussed (A20). Emission spectroscopy was reviewed (A21). Reflection-absorption spectroscopy and its applications were discussed (A22). Other infrared techniques for the analysis of surfaces were also explored (A23). The applications of microcolumn LC/FT-IR were discussed (A24). A comprehensive review of infrared and Raman spectroscopies of polymeric systems was published (A25). This publication covers the entire field of analytical chemistry of polymer systems; no other attempt will be made within the format of the current review to expand on this treatment of polymer systems. Several reviews with summaries of the application of mid-IR spectroscopy to particular industries or product areas were presented for the following: dyes (A26), wood products (A27, A28), textiles (A29), petrochemicals (A30), pharmaceuticals (A31-A33), medicine (A34), materialography (A35), and ionomers (A36). A tutorial on the use of quantitative analysis via spectroscopic data, with emphasis on sensitivity and selectivity measurements, was published (A37). Chemometric procedures for quantitative analysis via infrared spectroscopy were reviewed (A38-A40). Quantitative analysis of glass structure and properties was summarized (A41). General applications of near-IR spectroscopy were reviewed (A42-A45). Applications of this technique to analysis of agricultural products (A46) and the food industry were presented (A47-A50). Biological and medical applications were also reviewed (A51). A comparison of near-IR and mid-IR procedures for process analysis along with a discussion of the fundamentals of these techniques was offered (A52). The use of multivariate techniques as an aid to spectral interpretation was extensively reviewed (A53). Interpretation of near-IR spectra was discussed (A54). Calibration models and standardization of near-IR instruments were reviewed (A55). A review of the use of thermo-IR spectroscopy to study the interaction between organic pollutants and clay minerals was presented (A56). Open-path IR to monitor volcanic plumes was discussed (A57). Ab initio calculations of unstable organic molecules and reactive intermediates were discussed (A58). The use of spectroscopic methods in the study of carbohydrate chemistry was reviewed (A59). The role of infrared spectroscopy in the characterization of surface colloids at solid-liquid interfaces was presented (A60). The literature pertaining to the use of IR spectroscopy to study ion solvation and ion association was reviewed (A61). Protein structure analysis was discussed (A62-A64). Isotopeedited infrared spectroscopy for the study of biomolecules was discussed (A65, A66). An extensive review of the IR spectra of lipids was presented (A67). The use of IR to study liposomes and biomembranes was presented (A68). Biomedical applications, such as diagnosis of disease states and tissue analysis, were reviewed (A69). Infrared measurement techniques for the analysis of biofluids were compared (A70). Analysis of steroids with spectroscopic methods was reviewed (A71). Reviews of the application of IR to the study of photosynthetic reaction centers were presented (A72). Studies of the spectroscopic determination of bacterial cell structure were discussed (A73). 120R
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A review of spectroscopic techniques for characterization of catalysts was presented, with discussion as to technological improvements in this area (A74). Catalyst intermediate studies were reviewed (A75). Reviews of infrared spectra of inorganic nitrides were presented (A76, A77). Characterization of zeolites by spectroscopic techniques was summarized (A78-A80). The application of spectroscopic techniques in the study of metal complexes was discussed (A81-A85). Metal oxide catalysts were the basis of several reviews (A86, A87). The spectroscopy of materials adsorbed on metal surfaces was reviewed (A88, A89). Infrared spectroscopic techniques used to characterize metalelectrolyte interfaces were presented (A90). Characterization of Grignard reagents was summarized (A91). The role of infrared and Raman spectroscopy in the study of semiconductor alloys was reviewed (A92). Identification of defects in semiconductor materials as monitored by IR microspectroscopy was discussed (A93). Gap states in superconductors were studied by infrared spectroscopy (A94). DATABASES, SOFTWARE, AND ALGORITHMS A review of databases associated with UV-visible, NMR, IR, Raman, and mass spectral databases has been reported (B1). Also included was a brief discussion of Moessbauer, NQR, XPS, and CD databases. A strategy for knowledge acquisition in the collection of IR spectra involving automated generation of correlation tables has been reported. These tables are converted into rules that can be used to infer the existence of molecular substructures from the IR spectrum of an analyzed compound (B2). Two computer programs have been designed for aiding the library handing and microbial identification from IR spectra. The programs run on IBM-PC compatibles (B3). Other reviews on IR characterization included obtaining group frequency characterization (B4) preprocessing methods and data transformations (B5) and automatic spectrum interpretation techniques (B6). The main features of GEISA-PC, an IBM-PC software package designed for the use and management of large scaled databases of the atmosphere physics and spectroscopy interests, were presented (B7). The performance of an IR library search system has been examined using four different similarity measures for spectral search (B8). A combinatorial library of catalyst candidates, each consisting of a different metal element supported on alumina, has been screened for hydrogen oxidation catalytic activity. This method offers some promise for screening and optimizing catalyst formulations more efficiently than current methods (B9). A novel method for searching spectral libraries with spectra of mixtures, using a mix-match search algorithm, was tested extensively with good results (B10). Several articles have been published in relationship to the development of IR spectral databases or to enhancement of the effectiveness of these databases to the spectroscopist. A knowledge base has been proposed that adopts a set of rules that express the laws of spectra interpretation and the experience of special field experts in order to imitate the reasoning process of the human brain in relation to the group frequency correlation of organophosphorus compounds (B11). A strategy for the automatic generation of correlation tables for IR spectral interpretation has been proposed (B12). A combination of the IDIOTS algorithm
with the algorithm by Blaffert has been used to improve computerized structure elucidation (B13). Hierarchical organization of a knowledge base with IR spectral bands has been used to improve expert system spectral interpretation (B14). Computerized IR band assignment programs have been developed. One program employs information from 700 functional groups to develop its knowledge database (B15). A basis for simulating IR- and Ramanactive spectra of large-molecule systems has been developed using the internal coordinate correlation based on molecular dynamics algorithms and an autocorrelation function (B16). The development of a computerized IR spectral library from scanned and digitized IR spectra has been discussed (B17). A review covering two strategies used in discriminate high-dimensional spectral data analysis has been written. One method involves a preprocessing method followed by a low-dimensional classifier. The other method involves a high-dimensional classifier capable of handling large numbers of variables (B18). Nonparametric piecewise linear discriminant analysis (PLDA) has been employed to develop an automated detection scheme for FT-IR remote sensing interferogram data (B19). A method has been developed for the simple and effective approximation of the optical constants of neat liquids (B20). The issues of crossvalidation and missing data have been investigated relative to the partial least-squares (PLS) algorithm. Both a full EM algorithm and a reduced EM algorithm are discussed (B21). A comparison of PLS and artificial neural networks in the prediction of concentrations of compounds involved in the fermentation process of ethanol has been reported (B22). The use of calculations of absorption bands and absorption intensities in conjunction with present day theoretical methods have been used in the quantitative IR analysis of compounds (B23). An algorithm for passive FT-IR has been developed for implementation in air-monitoring systems, with specific emphasis on military gases as measured from a helicopter or tank (B24). An adaptation on an algorithm for plume signature data analysis has been examined for open-path FT-IR data reduction (B25). A new information content-based look-up table technique for the fast computation of near-monochromatic atmospheric transmittance in the IR that is well suited for satellite and airplane observations has been developed (B26). A selfmodeling mixture analysis has been demonstrated using the Simplisma and Tsimplisma approaches (B27). Computer simulation of the IR spectra of substituted bicyclic and tricyclic amidines, hexahydroimidazo[1,2-a]pyrazine-3,6-diones, and hexahydroimidazo[1,2-a]imidazo[1,2-d]pyrazine-3,8-diones has been verified using GC/FT-IR/MS (B28). Using a second derivative with PLS techniques, NIR diffuse reflectance spectroscopy (NIRS) was used to determine the active compounds in a pharmaceutical preparation (B29). A software-based digital signal processing method has been used to demodulate the photoacoustic responses of stepscan FT-IR photoacoustic measurements without any additional hardware (B30). The interpretation of multivariate calibration and rule induction classification models can be significantly improved by adopting a new representation of data profiles containing identifiable peaks using nonlinear curve fitting (B31). A methodology has been developed for the in situ IR monitoring and analysis of solid-phase organic reactions (B32). A simple PCbased scientific spreadsheet has been used to construct a math software package which provides a compliant solution to a design
problem for thermal imager performance (B33). A method for the measurement of concentrations of an analyte present in a biological fluid has been developed using NIR and an outlier detection method (B34). An algorithm for the NIR-based portable tissue oximeter has been developed and tested (B35). An improved simulation of vibrational spectra for larger molecules that removes artifacts has been developed by a direct transfer of Cartesian molecular force fields and electrical property tensors instead of internal coordinates (B36). Passive FT-IR remote sensing techniques have been used in the automated detection of trichloroethylene vapor in the presence of a variety of IR background signatures. Using piecewise linear discrimination developed in this study, successful detection of trichloroethylene was achieved in 96% of the cases studied (B37). An automated method for calculating the IO spectrum of openpath FT-IR spectra has been developed and implemented to correct for totally absorbing atmospheric species and instrument drifts (B38). A rationing algorithm has been developed for the quantitative analysis of the passive FT-IR spectrum of chemical plumes. The algorithm removes the background, eliminates the spectrometer internal signature, and enables quantitative examination of the spectral transmission (B39). A special algorithm for the analysis of a cross structure of the temperature and concentration of emitting components for nonuniformly heated gas flows using radiometric measurements in the IR band of a spectrum has been proposed (B40). Testing of the MOPITT algorithm test radiometer (MATR) has been done to provide support for the prelaunch testing of the data retrieval algorithms for the MOPITT satellite instrument (B41). Improvements have been made in the Nimbus 7 limb IR monitor algorithms to improve the predictions of ozone levels in the lower altitudes (B42). Stratospheric atlases of high-resolution IR absorption spectra have been prepared from balloon-borne spectrometer systems by the University of Denver. These atlases contain spectra at 0.02- and 0.002-cm-1 resolutions (B43). Observations of solid-state absorption features due to H2O ice, CO ice, and silicate dust have been reported in the study of the Herbig-Haro nebula in the R Coronae Australis dark cloud (B44). A computer program for the interpretation of IR spectra of organic compounds has been developed (B45). Solvent-induced frequency shifts have been modeled using a continuum defined by its static and high-frequency dielectric constants and application to formaldehyde has been demonstrated (B46). A computer program has been developed for automatic assignment of an IR spectrum to create a knowledge database containing the information of 700 functional groups (B47). The integrated spectrum of interstellar metal-rich globular clusters has been synthesized using the HR diagram and a stellar library (B48). A method for accurate film thickness measurement has been developed that separates the effects of interference and absorption effectively (B49). FT-IR has been used as a continuous emission monitor for on-line measurements of most volatile organics and some inorganic compounds. This instrumentation can be used for the monitoring of stack emissions and thermal treatment processes (B50). A review of structural and spectroscopic properties of transition metal compounds covering a variety of modeling topics has been written (B51). The problem with discontinuities in piecewise direct standardization (PDS) has been identified and a procedure for its eliminaAnalytical Chemistry, Vol. 70, No. 12, June 15, 1998
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tion has been proposed (B52). A genetic algorithm has been applied to optimization of PLDA with specific application to remote sensing data (B53). A joint neural network has been developed by combining gas-phase IR spectra with mass spectral data to predict 26 different molecular substructures from multispectral information. The combined database gives better prediction of functional groups than either the IR or MS databases alone (B54). A comparison of direct-deposition FT-IR and supercritical fluid FTIR spectra of quinones and barbiturates showed significant enough variations of these spectra with KBr disk IR spectral libraries to produce occasional incorrect identifications (B55). An IR spectral library was prepared for the characterization of 55 nerve agent homologues using GC/FT-IR spectroscopy (B56). Resolution enhancement of the IR linear dichroic (IR-LD) spectra of partially oriented molecules in a liquid crystal has been studied using reference Fourier self-deconvolution (RFSD) (B57). Application of an analog-digital converter to measurements made with a charge-coupled device (CCD) has enabled a resolution enhancement in the spectral features without limiting the measuring range of the CCD (B58). NIR and NIT for use in the agriculture and food industries have been developed by which the instruments can be calibrated at the factory and can be used the day the instrument is received (B59). Genetic algorithms have been implemented in automated wavelength selection procedures to build multivariate calibration models based on partial least-squares methods for NIR (B60). A modification of the standardization method of Shenk and Westerhaus for calibration model transfers between NIR instruments has shown an improvement by use of locally weighted regression (B61). Standardization of near-IR spectrometric instruments using the piecewise direct standardization method has been improved by modification of the algorithms (B62). NIR pattern recognition has been improved using the wavelet packet transform (B63). A recommendation has been made that offers some improvement on the discrepancies observed on NIR analysis of living tissues (B64). A pattern recognition algorithm has been combined with near-IR reflectance spectroscopy to function as a nondestructive analytical technique for identifying dyes present in textiles (B65). Application of a forward selection in the subsets selected by a genetic algorithm for linear regression of near-IR spectroscopic data has been shown to overcome some the selection of irrelevant variables (B66). A detailed study of 13 conflicting patterns of change in cytochrome c oxidase redox status from near-IR spectroscopy have identified possible sources of error that could cause the discrepancies (B67). A multivariate calibration procedure based on the use of a genetic algorithm to guide the coupling of band-pass digital filtering and PLS regression has been applied to near-IR spectroscopy for the analysis of glucose in biological matrixes, resulting in better correlation of results (B68). The vibrational spectra of (FeSi2 has been calculated by molecular dynamics simulations with a tight binding potential and verified by IR measurements on small monocrystals (B69). NIR and NIT instruments for use in the agriculture and food industry have been shown to be useble on the same day as delivery by using a precalibration procedure. Recommendations for enhancing the accuracy of the instrument were also presented (B70). The spatial resolution of IR systems used in IR thermography has been enhanced by use of a digital image restoration technique based on the accurate determination 122R
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of the optical transfer function (B71). A recommendation of the use of a weighted optimization for numerical correction of spectrometric data has been proposed for resolution improvement techniques (B72). A process to use multivariate signal responses to analyze a sample has been proposed (B73). Principle component analysis (PCA) has been applied to discriminate rapidly between extractable compounds that are indigenous to papers and nonindigenous compounds using SFE/SFC/FT-IR techniques (B74). Infrasoft International (ISI) has developed NIR spectroscopy programs that have been used in the determination of water, oil, and protein content in food and agricultural products (B75). A software-based method has been developed to remove spikes in NIR spectra measured with Ge detectors (B76). NIR has been used in refractive index modeling with PLS for hydrotreated gas oils (B77). A review has been published on the use of chemometrics in NIR calibrations with emphasis on criteria and procedures for the transfer of methods between instruments (B78). INFRARED ACCESSORIES AND SAMPLING TECHNIQUES Articles were published on the use of Teflon tape (C1) and disposable cards (C2, C3) as sample supports for IR spectroscopy. A universal sampling tool for analysis of liquids and solids by IR was described (C4). The use of rotational casting for preparation of thin polymer films for IR analysis was discussed (C5). New cells reviewed in the literature include a micro-FT-IR cell (C6), a high-pressure IR cell for studying the interactions of polymers and supercritical fluids (C7), modified NIR powder reflectance cells (C8), a fiber-optic transmission cell for on-line SFE/FT-IR (C9), and a channel flow cell for attenuated total reflectance (ATR)/FT-IR measurements of species at an electrode (C10). A scanning near-field IR microscope (C11) and a design enhancement to increase the spatial resolution of FT-IR microscopes (C12) were reported. A review described four sample devices for NIR (C13). The devices included a fiber-optic system, a robotic system, the use of HPLC vials for scanning liquids in a sealed container, and a moving blend cell. The use of an adapted FT-IR microscope to follow a photoinitiated polymerization reaction was discussed (C14). A ceramic sample heater for variable-temperature diffuse reflectance FT-IR analysis of solids was described (C15). The mechanochemical reactions that take place during preparation of alkali halide disks were discussed in a review (C16). A new FTIR imaging technique has been developed by combining a focal plane array detector with a step-scan Fourier transform interferometer (C17). The use of a movable two-dimensional Hadamard mask and an FT-IR spectrometer for chemical mapping was described (C18). Portable IR analyzers used for repetitive analysis were reviewed (C19). QUANTITATIVE ANALYSIS A review has been written related to FT-IR emission spectroscopy of solids. Also included in this review were a correction equation for the single-beam emission spectra, proper data manipulation procedures, and the use of a linear emission intensity scale for quantitative work. Also included was a discussion on multilayer samples (D1). A review of the application of quantitative FT-IR spectroscopy to aqueous solutions has been written
(D2). This review was targeted at the evaluation of the ATR technology. A variety of instrumentation and parameters were used in the analysis. Results of these variations on the end results are discussed. The examination of glasses with IR spectroscopy has been reviewed with emphasis on obtaining information on static dielectric constants and the calculation of semiempirical calculations of vitreous solids’ IR spectra (D3). A review has also been written on the use of multivariate quantitative infrared analysis (D4). This review is focused at providing a tool to assess quantitative methods and evaluate their conformity to ASTM practices. A review of several methods for quantitative analysis of gas-phase samples using FT-IR has focused on particular advantages and disadvantages (D5). A review of the trends in chemometrics as applied to NIR spectroscopy has been reported with discussion of building databases of calibration samples, regression models, and calibration transfer (D6). A method has been developed for the utilization of synthetic calibration spectra in calibration of instrumentation to provide quantitative analysis of gas-phase IR spectra (D7). This method uses the multiple atmospheric layer transmission (MALT) program to create synthetic spectra that closely approximate real measured spectra. This technique has proven useful in lung openpath and solar FT-IR spectroscopy. A nonlinear multivariate infrared analysis method has been used to research octane number (RON) and other physical properties (D8). FT-IR with curve fitting has been used in conjunction with NMR for the quantitation of various components in rolling oils without their separation (D9). FT-IR was used for quantitation of mineral oil deposition on plant leaves (D10). FT-IR has been used in conjunction with solid-state NMR (13C-SP/MAS) to determine structural parameters of low-rank Czech coals (D11). An FT-IR method has been developed to rapidly screen soil samples for hazardous waste site (D12). The method was originally developed to identify and quantify microgram concentrations of explosives in soil samples, but offers promise to detection of volatiles, semivolatiles, and pesticides. A method has been developed for the quantitative analysis of multicomponent mixtures with unknown individual spectra (D13). This method involves a twostep optimization procedure which allows for high precision results. A scanning IR polariscope with high spatial resolution has been developed for the inspection of residual strains in III-V compound wafers (D14). FT-IR has been used to determine quantitative equilibrium constants between CO2 and Lewis bases (D15). Step-scan FT-IR photoacoustic spectroscopy has been used to quantify the content of brivudine and dithranol in a petrolatum/ drug ointment (D16). The FT-IR extinction/scattering technique has been used to evaluate fuel vapor concentration in various spray conditions (D17). FT-IR has been used to quantitatively analyze levels of NH3 and HCN in hot combustion gases taken from the combustion chamber of boilers fueled by coal (D18). An FT-IR method has been developed for measuring norditerpenoid alkaloids in larkspurs. The method was calibrated using high-pressure liquid chromatography and gravimetric methods (D19). A combination of remote infrared differential absorption lidar experiments with a computational approach has been used to measure four organic gases (D20). A fully automated procedure has been developed for FT-IR determination of caffeine in soft drinks.
Detection limits with relative standard deviations were reported (D21). A calibration model based on DRIFT spectroscopy has been developed for the rapid estimation of the chemical composition of radiata pine wood samples. The model has been shown to predict extractives, lignin, and carbohydrates (D22). Attenuated total reflectance FT-IR spectroscopy has been used to monitor the epoxidation of indene to indene oxide using multivariate statistical methods (D23). A methodology has been developed for selection of the best calibration sample subset for principle component regression analysis (D24). This method has been applied to both UV-visible spectroscopy and near-IR spectroscopy effectively with a considerable reduction in cost. A calibration strategy has been proposed for dealing with difficult calibrations using NIR spectroscopy (D25). A preprocess step, dubbed piecewise mutiplicative scatter correction (PMSC), has been successfully applied to NIR calibration spectra for the analysis of homogenized beef samples (D26). This technique has shown up to 52% improvement on prediction error. A noninvasive NIR quantitative measurement instrument has been developed with removable finger inserts of various sizes to enable variable sample size insertion for analysis (D27). A method has been developed for the quantitative NIR spectroscopic analysis of biological liquids without the use of any detection reagents (D28). NIR spectroscopy with multivariate calibration has been used in the quantitative determination of glucose, fructose, sucrose, citric acid, and malic acid in dried orange juice samples (D29). An FT-NIR instrument equipped with a fiber-optic probe has been used to measure levels of resorcinol in water between 9 and 35% independent of temperature (D30). A PLS method has been developed for NIR in the analysis of orange juices (D31). Using NIR with a partial least-squares model, a method has been developed for the simultaneous determination of ethanol, glycerol, fructose, glucose, and residual sugars in botrytized grape sweet white wines (D32). A NIR method has been developed for the quantitative determination of resorcinol in aqueous solutions for industrial applications (D33). A NIR technique has been developed using artificial neural networks to study tobacco nicotine (D34). The application of FT NIR for quantitative and qualitative analysis has been discussed (D35). Quantitative determination of hemoglobin in turbid medium has been demonstrated using NIR spectroscopy (D36). Statistical and artificial network pattern recognition techniques have been applied to NIR spectra of soy sauce samples and related to differences in food flavorings (D37). A rapid FT-NIR spectroscopic method has been developed for quantitative determination of peroxides in edible oils. The method is based on a PLS calibration model and offers an alternative to the iodometric method, avoiding the solvent and reagent disposal problems (D38). A method and apparatus for the noninvasive measurement of intravascular ketone body concentration has been reported (D39). A patent application has been filed for a method to determine tissue hemoglobin levels using NIR spectroscopy (D40). A method of variable selection for quantitative NIR determination of glucose concentrations has been shown to reduce the number of calibration samples with no loss in reliability (D41). The combination of NIR and mid-IR spectra has been shown to provide improvements in calibration results in the assay of lignin, cell wall digestibility, and dry matter Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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digestibility on a variety of samples (D42). A PLS calibration method has been successfully applied to NIR spectroscopy for the measurement of malt quality constituents in whole grain (D43). The use of toluene as a test for the calibration of an FTNIR spectrometer in the analysis of the hydroxyl content of ethoxylated fatty acid produced a stable calibration over 120 days (D44). A procedure to standardize across a network of instruments has been proposed (D45). PCA has been applied to the study of the dissociation process of oleyl alcohol using FT-NIR spectroscopy (D46). A comparison of the quantitative properties of IR vibrational circular dichroism (VCD) and Raman optical activity (ROA) has been done in the analysis of trans-pinene, cis-pinane, R-pinene, and β-pinene (D47). Correlation was observed for the two techniques for the strongly chiral and strongly achiral vibrational modes. The use of quantitative VCD in the analysis of proteins has been discussed with specific reference to effects of spectral resolution, sample concentration, cell selection, and spectral normalization (D48). FT-IR with PLS techniques has been used in the simultaneous on-line determination of gases in smoke from burning textiles (D49). The compounds determined using this technology include the following: water, CO2, CO, NO, NO2, SO2, C3H4O, HCl, HBr, HCN, and HF. The shelf life of nitrocellulose containing singlebase propellants has been determined using FT-IR and PLS calibration techniques (D50). A PLS method has been developed using transmission FT-IR spectroscopy for the analysis of aldehyde formation and anisidine value of thermally stressed oils (D51). A PLS method has been developed for the quantitative FT-IR analysis of fatty acid esters (D52). A multiple model approach has been used to evaluate polyolefin formulations using discriminant analysis with process, chemistry, and spectroscopic information (D53, D54). Using principle component regression (PCR) and PCA, a classification method has been developed for the analysis of sugar cane juices (D55). This method allows for the qualitative classification of spectra without knowledge of their chemical composition. The effect of PCA on mid-IR spectroscopy data has been examined to determine the effects of instrumental instability on results (D56). FT-IR spectroscopy has been used to monitor gases generated during chemical inhibition of fuel pool fires burning in the air (D57). This technique was used in the analysis of acid gases formed when Halon 1301 was used to extinguish fires. FT-IR spectroscopy has been utilized in the study of nitric acid ices formed from vapors containing water (D58). Passive FT-IR remote sensing has been used in the analysis of effluent plumes, such as controlled gas releases, power plant emission stacks, and chemical manufacturing facilities (D59). Reflectance FT-IR spectroscopy has been used to examine the electrochemical mechanism for ethylene glycol oxidation by polycrystalline platinum (D60). IR spectroscopy has been used in the study of fullerene (D61). Information on intermolecular interactions are also discussed. Oxidation of mesocarbon microbeads has been followed by thermogravimetric and FT-IR spectroscopic techniques (D62). The quantitative determination of fluconazole has been demonstrated using KBr pellets of the material and the transmission technique 124R
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(D63). FT-IR spectroscopy has been used for the quantitative determination of dodecylbenzenesulfonate and tripolyphosphate in solid compound samples of detergents (D64). A gas flow equilibrium vapor cell has been shown to allow for the quantitative analysis of vapor-phase species using Beer’s law (D65). Using an equilibrated vapor cell with a closed-loop circulation, vapor-air mixtures of volatile organic compounds in water were examined. Mixtures of methanol, ethanol, 2-propanol, acetone, and 2-butanone were found to follow Beer’s law at less than 50 Torr (D66). An FT-IR classical computational method has been applied to the direct quantitation of multicomponent gas mixtures of organic compounds. The method has been used to characterize mixtures of up to 10 compounds (D67). FT-IR microspectroscopy has been used for the quantitative study of solid-phase resin-bound chemical reactions of species containing deuterium (D68). An artificial coalification series has been analyzed by FT-IR microscopy using a diamond anvil compression cell. The method has been applied to Mahakam coal (type III organic matter) (D69). FT-IR in conjunction with gravimetric methods has been used in the quantitative analysis of CO chemisorbed on Pt surfaces (D70). FT-IR spectroscopy has also been used in the study of antiepileptic medications (D71). A combination of IR and MS techniques have been used to determine the extinction coefficients of adsorbed CO on Rh/SiO2 catalyst (D72). Water adsorption on H-ZSM-5 zeolite has been evaluated using FT-IR spectroscopy (D73). IR spectroscopy analysis has been used in conjunction with nuclear reaction analysis in characterizing molar absorptivity of hydroxyl bands in high-hydroxyl-content silica glasses (D74). A nondestructive pulsed IR quantitative evaluation of defects in metal surfaces has been developed for the inspection of aluminum, steel, and turbine blades (D75). SPECTRA-STRUCTURE CORRELATION The SO2 stretching vibration in metal saccharinates for Na, Mg, Mn, Fe, Co, Ni, Zn, Cd, and Pb have been studied using IR spectroscopy (E1). An IR spectral study was made of kaolinite samples before and after dehydroxylation and rehydration. The surface areas of the samples were observed to effect the OH stretching frequencies (E2). IR spectroscopy has been used to interpret structural changes in silica glasses. Shifts in the Si-O stretching band was used to monitor changes in average Si-OSi bond angles (E3). IR and Raman spectroscopy have been used in the study of 1,3,5-tri-tert-butylpentalenes (E4). NMR and IR spectroscopies have been used to characterize the effects of physical surroundings and chemical structure information of carbonyl stretching frequencies in various solvents (E5). Density functional theory has been applied to the investigations of harmonic force fields, vibrational frequencies, and IR intensities of transition metal complexes (E6). The IR spectra of TiO2, sodium titanates, and natisite have been examined, and differences in the IR spectra have been correlated with structural features (E7). The IR bands of cis- and trans-CHdCH and vinyl CHdCH2 groups of model compounds and polybutadienes have been compared (E8). Group frequency assignments have been compiled for major IR bands observed in 20 common polymers (E9). In a review article, some methods of obtaining characteristic group frequencies, including empirical correlations, were discussed
(E10). Two-dimensional FT-IR correlation analysis was applied to both the mid-IR and NIR regions to investigate changes in the secondary structure of β-lactoglobulin in D2O solvent systems. A mechanism for the change from the β sheet to the R helix was proposed (E11). A review has been written on the twodimensional FT-IR and NIR correlation spectroscopies in the studies of temperature-dependent spectral variations of selfassociated molecules (E12). The theory of fuzzy sets has been applied to specific IR spectrum-structure correlations (E13). Grazing-angle FT-IR spectroscopy has been used to study the monolayer structure of self-assembly molecules with novel amido linkages (E14). The secondary structure of photosystem II reaction centers isolated from pea has been deduced from quantitative analysis of the component bands of the IR amide I spectral region determined by FT-IR (E15). A method for determining the orientation of individual bonds within complex macromolecules from polarized IR measurements on oriented single crystals has been described (E16). The peroxide bond of inorganic and organic peroxides have been studied by IR and Raman spectroscopies. The results of the study are a narrower range of frequencies for the vibration (845-875 cm-1) (E17). The experimental vibrational frequencies of s-trans-1,3-butadiene were used to determine the scale factors for its quantum mechanical force field. This information was then used to determine the location of the s-gauche rotamer band in the IR spectrum of the gas phase (E18). The spectral structure arising from the puckering vibration of perfluorocyclobutane has been modeled with a quadratic-quartic potential (E19). Two-electron correlation theories, second-order Moller-Plesset perturbation, and d functional methods have been adopted to obtain fully optimized structures of styrene, trans-stilbene, and cis-stilbene. The relationship of intermolecular and intramolecular forces was discussed (E20). The IR spectra of some hydroxy aromatic Schiff bases have been recorded. The bands due to CdN and OH groups were assigned and discussed in terms of molecular structure (E21). The structures of the size-selected hydrogen-bonded phenol-(H2O)n clusters were investigated by analyzing the OH stretching vibrational spectral in S0, S1, and the ionic states. The characteristics of the different states were discussed (E22). The spectral characteristics of absorption bands of free and bound H-bonded molecules of substituted anilines in solution were determined by FT-IR spectroscopy (E23). Solvent effects on N-(3-chloro-2-benzo[b]thienocarbonyl)-N′-ethylthiourea were studied by examining the changes in the IR bands belonging to the NH and CO bonds (E24). Spectral deconvolution, using a specially developed program, was used to characterize Co adsorbed onto aluminasupported bimetallic catalysts containing either Fe or Ni (E25). A review on matrix IR spectroscopy of intermediates with lowcoordinated carbon, silicon, and germanium atoms has been written (E26). An FT-IR study of the bonding of methoxy on Ni(100) has been used to evaluate the effects of coadsorbed sulfur, carbon monoxide, and hydrogen. Differences observed were attributed to changes in the metal-oxygen bond (E27). The FTIR spectra of six para-substituted aniline deriviatives and nine 1-paminophenylazoles and benzazoles have been recorded (E28). The fundamental IR absorption band for CO in solution in four chlorinated solvents has been reported. The changes in solutesolvent interaction were discussed (E29). The IR spectra of Fe
and Ru 5-cyclopentadienyl carbonylmetallocarboxylates were obtained in THF at -78 °C. The effect of the counterions on CO2 complexation was discussed (E30). HYPHENATED TECHNIQUES GC/FT-IR was used in the study of trimethylsilyl derivatives of 10 hydroxy- and methoxyhydroxyflavonoid compounds. The correlation between retention and gas-phase IR data was shown to be useful in structural identification of compounds with very similar chromatographic behavior. The carbonyl frequencies were shown to give information on the presence of substituting agents (F1). GC/MS and direct-deposition GC/FT-IR were applied at the same level of sensitivity to the study of minute concentrations of volatiles in green leaves (F2). The IR spectra of six monomeric gaseous aromatic N-methyleneamines were reported from GC/ FT-IR experiments (F3). Gas chromatography/matrix isolation/ FT-IR (GC/MI/FT-IR) were used to confirm the identities of trimethylsilyl derivatives of trichothecene mycotoxins found in grains (F4). A comparison of pyrolysis GC and FT-IR spectroscopy indicated the latter was able to discriminate fiber makeup better (F5). FT-IR and gas chromatography were used to study model samples containing various petroleum products and field samples of the Vltava River. This study showed IR and GC to be suitable to determine concentrations of 10-102 mg/L of lower and middle petroleum fractions in water (F6). GC/FT-IR has been used in the qualitative and quantitative determination of 1,2propanediol in Acyclovir cream (F7). Diffuse reflectance FT-IR spectroscopy has been used to qualitatively and quantitatively determine drugs (heroin, cocaine, codeine) separated by thinlayer chromatography (F8). GC/FT-IR has been used as a rapid method to distinguish cis and trans R,R-disubstituted piperidines and pyrrolidines (F9). GC/FT-IR has been used to identify 42 monosaccharides as their trimethylsilyl ethers (F10). GC/MS and GC/FT-IR have been used to determine ferrocenes (F11). GC/FT-IR has been successfully used in the identification of disaccharides after conversion to their methylsilyl ethers (F12). GC/FT-IR and CCD Raman spectroscopy has been used to differentiate cyclopentane- and cyclohexane-containing compounds. The GC/FT-IR was viewed as a method to determine individual naphthenes while the CCD Raman was viewed as a means to measure bulk mixture properties (F13). GC/FT-IR has been used to identify various fatty acids (F14). The total olefins in gasoline can be determined on-line by process GC or FT-IR spectroscopy. The FT-IR method uses PLS correlation calibration and takes approximately 0.2 min per determination (F15). Continuous FT-IR monitoring in conjunction with off-line pyrolysis GC/MS was used to evaluate the oxidation of fossil organic matter in Miocene and Silurian sediments. The oxidation of the organic matter in the two sediments was compared (F16). The identification of volatile organic compounds generated during polymer processing has been performed by the use of TG-GC/IR-MS spectroscopy (F17). A review on the application of multidimensional GC/MS and GC/FT-IR to the analysis of components in complex matrixes has been written (F18). The analysis of dimethylphenanthrenes by direct-deposition GC/FT-IR has been reported with quantitative procedures described (F19). GC/FTIR has been shown useful in the determination of the stereochemistry of carbon-carbon double bonds conjugated with a vinyl Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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group (F20). Off-line pyrolysis GC/MS/FT-IR was used to investigate oxidation of fossil organic matter in Miocene and Silurian sediments (F21). The photochemical degradation of dichoroprop and 2-naphthoxyacetic acid in water has been studied by GC/MS and GC/FT-IR. The photodegradation pathways were described (F22). An aqueous smoke flavoring employed in the food industry has been studied using GC/MS/FT-IR spectroscopy. The components were identified and discussed (F23). Headspace GC/FT-IR has been used to study the in situ thermal decomposition products of O-ethyldithiocarbonate on mineral surfaces (F24). DRIFTS has been coupled with GC to correlate changes in the IR spectrum of a zeolite with the composition of the gas phase (F25). On-line trace enrichment combined with column LC/FT-IR microspectroscopy has been used in the identification of herbicides in river water. The identification limits for the herbicides studied were reported (F26). Reversed-phase liquid chromatography has been used with FT-IR by means of a solvent elimination interface. Features studied included postcolumn band broadening, phase separation efficiency, evaporation efficiency, and extraction yield. This technique was applied to phenylureas and quinones. FT-IR detection was demonstrated at the submicrogram per milliliter level (F27). Reversed-phase liquid chromatography with solvent elimination and FT-IR microscopy have been applied to the characterization of additives in PVC and polypropylene at the low-nanogram range (F28). HPTLC/FT-IR has been used online to identify LSD, MBDB, and atropine in an in situ measurement (F29). A review on microcolumn liquid chromatography FT-IR has been written with attention to various approaches (F30). Size exclusion chromatography (SEC) has been used with FT-IR spectroscopy in studies of compositional distribution in copolymers, impurity profiling, and branching in polyolefins (F31). Film morphology of polymer systems (polyethylene-polystyrene blends) have been studied by SEC-FT-IR (F32). A particle-beam LC/FTIR interface has been employed in the investigation of the effect of chromatographic conditions, such as mobile-phase composition, elution process, and stationary phase, on protein secondary structure. Qualitative and semiquantitative measurements were possible (F33). The applicability of IR spectrometric detection in liquid chromatography, based on solvent elimination prior to IR scanning, has been enlarged to gradient separations by adaptation of a capillary column switching system and addition of a postcolumn makeup liquid (F34). A mobile-phase elimination interface originally designed for liquid chromatography IR spectroscopy has been shown to perform exceedingly well for packedcolumn SFC/FT-IR. The technique was used in the separation of Irganox 1076 (F35). Principle component analysis was applied to discriminate rapidly between extractable compounds that are indigenous to papers and nonindigenous compounds on the basis of their IR spectra. This method was applied with on-line SFE/ SFC/FT-IR spectroscopy to yield an automated analysis of compounds that can be extracted from very complex matrixes (F36). The orthogonal projection approach has been applied to the analysis of a reaction product by HPLC and LC/FT-IR in which overlapping peaks were observed. The resolution of the overlapping peaks into individual chromatograms and IR spectra were discussed (F37). 126R
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Thermogravimetric analysis (TGA) FT-IR spectroscopy has been used in the characterization of the reaction mechanism of Pb(Zr, Ti)O3 (F38). Thermogravimetric FT-IR methods were applied to characterization of used turbine engine lubricants during a reclamation effort. A themogravimetric/secondary oxidation/FT-IR method was developed to determine trace levels of chlorinated contamination. The detection limit was reported as 300 ppm (w/w) (F39). TGA/FT-IR has been used to study the thermal degradation of PMMA (F40). A review has been written on the applications of thermogravimetric analysis combined with FT-IR spectroscopy. This review covers characterization of coal, source rock, heavy hydrocarbons, biomass, waste materials, and plastics (F41). Thermogravimetry/IR/mass spectrometric analysis (TG/IR/MS), a relatively new technology, has been applied to the analysis of paper mill deposits as a rapid means of identifying contamination sources (F42). Thermogravimetry/ FT-IR spectroscopy have been used in the analysis of recycled cellulose pulps (F43). TC/FT-IR spectroscopy has been used in the study of the incineration and pyrolysis of polyethylene, PVC, and PET (F44). TG/MS/FT-IR has been applied to the study of post-cross-linking and decomposition of a phenolic resin (F45). A TG/FT-IR system was used in the study of modified phenolic hardeners and curing of an epoxy resin. The technique was used in the study of the evolved gases during the decomposition of 2,6-dimethylol-o-cresol and the product modification with hexahydrophthalic acid anhydride (F46). TIME-RESOLVED INFRARED SPECTROSCOPY A time-resolved IR double-resonance technique involving the use of two CO2 lasers was employed in a study of the transfer of vibrational energy between ozone and oxygen or nitrogen at 200300 K (G1). Oxidation of the lubricant in the ring pack of a running diesel engine was detected by time-resolved FT-IR (G2). Time resolution of 200 fs was achieved during time-resolved IR and UV-visible spectroscopy by means of an ultrafast laser apparatus (G3). Time-resolved FT-IR was used in a comparison between cytochrome P-450cam carbon monoxide complex bound with (1R)-camphor and same complex bound with (1S)-camphor (G4). A review was given on time-resolved diode laser IR reflection-absorption spectroscopy (G5). The reaction initiated by pulse radiolysis of SF6/NO gas mixtures was investigated by time-resolved IR and UV spectroscopy (G6). Femtosecond time-resolved IR spectroscopy was used to detect the reactive intermediates in an alkane C-H bond activation by organometallic compounds at room temperature (G7). A review of the application of time-resolved IR spectroscopy for the study of organometallic photochemicals in solution was presented (G8). The use of time-resolved IR spectroscopy to probe excited states of transition metals was discussed (G9). Time-resolved infrared spectroscopy was used to study the photolysis of 2-(methoxycarbonyl)phenyl azide and Cr(CO)4(2,2′-bipyridine) (G10, G11). The photochemistry of certain metal carbonyl species dissolved in supercritical noble gases or carbon dioxide was the focus of a study using time-resolved IR and UV spectroscopy (G12). Timeresolved IR spectroscopy was applied to the study of the photochemical rearrangement of a rhenium dimetallacyclobutene (G13). The propargyl radical produced by the UV photolysis of allene was detected by time-resolved IR diode laser spectroscopy
(G14). The products produced by the photochemical ring opening of 1,3-cyclohexadiene were investigated by time-resolved step-scan FT-IR spectroscopy (G15). The experimental results for one- and two-dimensional time-resolved FT-IR spectroscopy of liquid crystals were presented (G16). Time-resolved FT-IR was used to monitor behavior of ferroelectric liquid crystals in an electric field (G17). A nematic solution of 2-naphthaldehyde in an electric field was studied by time-resolved step-scan FT-IR (G18). A multichannel FT-IR spectrometer for single-event time-resolved spectroscopy was described (G19). Attenuated total reflection surfaceenhanced IR absorption spectroscopy combined with time-resolved IR spectroscopy were used in monitoring electrochemical reactions (G20). Step-scan time-resolved FT-IR emission spectroscopy was used to study the photodissociation of ethylene at 193.3 nm (G21). A nanosecond time-resolved IR spectrometer with a photovoltaic MCT detector was described (G22). A review was published that encompasses both experimental and theoretical studies of the vibrational relaxation of small molecules in solution (G23). The bacteriorhodopsin photocycle was measured by time-resolved ATR/FT-IR spectroscopy (G24). Nanosecond time-resolved FTIR spectroscopy was also used to study the early stages of the bacteriorhodopsin photocycle (G25). Time-resolved FT-IR was applied to the investigation of the last steps of the photocycles of Glu-204 and Leu-93 mutants of bacteriorhodopsin (G26). Picosecond tunable IR pulses were used in a time-resolved spectroscopic experiment to study the vibrational energy transfer in nitromethane explosives (G27). Time-resolved impulse photoacoustic measurements of gases and solids were obtained with a step-scan FT-IR spectrometer (G28). Picosecond time-resolved near-IR was used to study the excited states of C70 (G29). The release of ATP from “caged ATP” and partial reactions of the Ca2+-pumping cycle of Ca2+-ATPase were followed by timeresolved FT-IR spectroscopy (G30-G32). A review discussed the use of time-resolved infrared spectroscopy to follow events in protein folding (G33). The IR chemiluminescence of the products for the NO + NCO reaction was monitored with time-resolved FT-IR (G34). The intermediates in the migratory insertion of CO into the metal-alkyl bond of manganese carbonyls were detected by time-resolved FT-IR spectroscopy (G35). REFLECTANCE TECHNIQUES Symmetry, selection rules, and nomenclature in surface spectroscopies was reviewed (H1). The application of FT-IR, diffuse reflectance, and attenuated total reflectance techniques toward the analysis of soil materials was discussed (H2). A review described the investigation of molecular chemisorption at single-crystal metal surfaces by reflection absorption IR spectroscopy (H3). Recent advances in the use of IR and Raman spectroscopies for the characterization of polymer/polymer and polymer/substrate interfaces was reviewed (H4). The theory and practice of external IR reflection absorption spectroscopy as applied to films at the air/water interface were described (H5). Time-resolved diode laser IR reflection-absorption spectroscopy and its application was discussed (H6). A book described the theory and practice of attenuated total reflectance spectroscopy of polymers (H7), while a review discussed the analysis of adhesives, sealants, and coatings by the same technique (H8). The use of diffuse reflectance FT-
IR spectroscopy in heterogeneous catalysis studies was reviewed (H9). The use of synchrotron radiation for reflection absorption studies of surfaces was described (H10). New data on water incorporation in glass as determined by IR reflectance spectroscopy were reviewed (H11). The Raman and IR reflection spectra of AlN (H12), BN (H13), GaN (H14) were reviewed. The analysis of photocopy toners by diffuse reflectance, attenuated total reflectance, microscopic reflection-absorption, and microscopic IR techniques was evaluated (H15). Single-Crystal and Bulk Analysis Applications. The crystal field transitions for Nd3+ were studied by Raman and farIR reflectance spectroscopies (H16). Polarization-dependent farIR reflectivity measurements were made on single crystals of anatase TiO2 (H17). The relaxation effect of IR reflectance spectra of nanocrystalline composite oxides was investigated (H18). Raman and IR reflectivity spectroscopies were used to study the TeO2 crystal (H19) and the GaN crystal (H20). Hexagonal barium titanate was studied by Raman and IR reflectivity spectroscopies (H21). Polarized IR reflection spectra of TlClO4, TlBF4, and NH4BF4 single crystals were analyzed (H22). Bismuth disproportionation in BaBiO3 was studied by infrared and visible reflectance spectroscopies (H23). Yttrium and lanthanide copper oxides were studied by X-ray diffraction and IR reflectance spectroscopy (H24). The far-IR reflectance spectra of bismuth cuprates were analyzed (H25). Phase transition dynamics in layered crystals were investigated by IR reflectance and Raman spectroscopies (H26). Cobaltite spinels were characterized by IR reflectance spectroscopy (H27). The formation and characterization of Si/SiO2 multilayer structures by oxygen ion implantation into silicon was studied by FT-IR reflectance spectroscopy (H28). Cofacially stacked phthalocyanines doped with iodine were studied by IR reflectance spectroscopy and X-ray diffraction (H29). The application of reflectance micro-FT-IR spectroscopy to analyze coal macerals was described (H30). Protonated and deuterated ices compressed under high pressure showed IR reflectance evidence of a phase transition (H31). The application of infrared reflectance spectroscopy to mineral exploration was described (H32). The coordination states of molybdenum and the nature of copper ion sites in superionic glasses was investigated (H33). Far-IR reflectance investigations of lead borate and lead aluminoborate glasses were described (H34). FT-IR microreflectance measurements of the CO32- ion content in glasses were discussed (H35). Polymer characterization by specular reflectance using an FT-IR microscope was evaluated (H36). Microreflectance FTIR techniques for the forensic examination of documents was discussed (H37). The application of real-time reflectance IR spectroscopy to the study of photopolymerization reaction rates of stereolithography resins was developed (H38). Aspects in interpreting results of reflectance and attenuated total reflectance spectra of semiconductor systems were discussed (H39). A method was developed for the in situ investigation of corrosion of copper in a gaseous environment (H40). The potential of IR reflection-absorption spectroscopy for the study of high-temperature oxidation of metals and alloys was demonstrated (H41). Thin-Film Applications. Reflectance FT-IR spectroscopy was used as a tool for surface inspection and contamination detection (H42, H43). A method was developed that eliminated the problem of interference fringes in reflection spectra of Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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photoresist films (H44). The current approach in using IR reflectance spectroscopy for thin-film measurement in the semiconductor industry was outlined (H45). Semiconducting iron silicide films were characterized (H46). Polarized IR reflection spectroscopy was used to identify boron nitride film phases (H47). FT-IR spectra of borophosphosilicate films obtained by metalbacked configurations were compared to those obtained by conventional transmission (H48). IR reflectance and transmittance spectra of chalcogenide glass layers were analyzed (H49). Cupric oxide in thin-film form was studied by IR reflectance spectroscopy (H50). Thin carbon films constructed from oriented carbon nanotubes were studied (H51). Molecular association in thin films of mesogenic cyanophenyl derivatives was investigated by reflection IR spectroscopy (H52). The infrared spectra of oxide films were modeled for microstructural analysis (H53). Silicon oxynitride thin films were characterized (H54). Thin films of lubricating oils on metal surfaces were examined by polarization modulation reflection-absorbance spectroscopy (H55). Iron oxide films deposited on a magnesium oxide substrate were examined (H56). IR reflection-absorption spectra of aluminum hydrides on a silicon oxide surface were done using a buried metal layer substrate (H57). A spectroscopic study was done on the self-assembling processes of organophosphates on evaporated silver films (H58). The optimization of IR reflection spectroscopy for the quantitative determination of borophosphosilicate glass parameters was described (H59). FT-IR reflection-absorption spectroscopy was used for in situ observation of photoinduced vapor deposition polymerization of N-vinylcarbazole (H60, H61). The redox-induced orientation change of a self-assembled monolayer of 11-ferrocenyl-1-undecanethiol was studied (H62). The role of hydrogen bond and metal complex formation in amino acid monolayers was investigated using IR reflection-absorbance spectroscopy (H63). The effects of substrates on the IR spectra of Langmuir-Blodgett films was discussed (H64). Structure disordering during surface pressure relaxation of Langmuir films of stearic acid was studied (H65). The structure and phase transitions in a Langmuir monolayer of tetracosanoic acid was measured (H66). Stearic acid and cadmium stearate films were characterized by external reflection IR at various angles of incidence (H67). Monolayer and multilayers of ferroelectric liquid crystals were characterized by polarization-modulated IR reflection-absorption spectroscopy (H68). The vibrational spectroscopy of thin films of water adsorbed on metal surfaces under ultrahigh vacuum were discussed (H69). Interfacial Applications. Samples at air/water and air/metal interfaces were measured by differential polarized reflectance spectroscopy (H70). The molecular order of chiral monolayers at the air/water interface was determined by infrared reflectionabsorption spectroscopy (H71). Monolayers of behenic acid methyl ester at the air/water interface and air/deuterated water interface were used for the quantitative determination of chain tilt angles (H72). Interfacial molecular interactions between ferroelectric liquid crystal and poly(vinyl alcohol) films were investigated by IR reflection-absorption spectroscopy (H73). Electromodulated FT-IR reflectance spectroscopy was used to investigate the interaction of tetramethylthiourea with a polycrystalline gold electrode (H74). Partial chain deuteration was used as a probe of conformational order of different regions in 128R
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hexadecanoic acid monolayers at the air/water interface (H75). The interfacial behavior of water molecules at a gold electrode surface was analyzed (H76). Adsorption and Surface Reaction Applications. Infrared reflection-absorption spectroscopy has been used extensively to characterize adsorbed molecules on a variety of substrates and to monitor surface reactions. Butene isomer reaction products evolved during the course of a surface reaction were identified (H77). The photolytic decarbonylation of iron pentacarbonyl adsorbed on a silica film was studied (H78). Adsorption and reactions of formic acid on nickel surfaces was investigated (H79). The reactions of water and ethanol with a silicon surface were studied (H80). Copper corrosion products formed by atmospheric corrosion were characterized (H81). Nitroglycerin photodecomposition on titania surfaces was measured (H82). The catalytic decomposition of 2-propanol was studied over molybdenum-iron oxide catalysts (H83). The chemisorption of hydrogen at a silicon surface was studied (H84). The mode of deactivation and coke formation in H-SSM-5 zeolite during ethylbenzene disproportionation was investigated (H85). The infrared spectra of neutral and ionic hydrogen-bonded complexes formed by interaction of a series of bases with H-Y, H-ZSM-5, and H-mordenite were compared with analogous adducts formed on H-Nafion (H86). The dehydrocyclization of submonolayer coverages of 1-hexene to benzene on a copper single-crystal surface was reported (H87). The nitridation of GaAs surfaces was observed (H88). The interaction of amyl xanthate with chalcopyrite, tetrahedrite, and tennantite was studied (H89). Nitrous oxide generated by the reduction of nitrite on a platinum electrode was monitored (H90). In situ infrared measurements of the reductive and oxidative removal of a nonanethiol monolayer from a gold single crystal were made (H91). The adsorption and oxidation of carbon monoxide on palladium was studied (H92). Kinetic studies of the reactivity of ethylene on platinum surfaces were done (H93). An in situ study was done of the electrooxidation of methanol on PtRu electrodes (H94). Mixed self-assembled monolayers were used as a model surface to study the adsorption of dimethylmethylphosphonate and water vapor (H95). Reflection-absorption IR spectroscopy was used to study the H/D scrambling reactions during the conversion of ethylene to ethylidyne in coadsorbed layers on platinum (H96). The melting of ordered monolayers of n-hexane, n-octane, and n-decane adsorbed on platinum was studied (H97). The chemical adsorption of 1-hexene on ruthenium was studied (H98). The bonding and orientation of L-alanine on copper was determined (H99). Adsorption of ethene on clean and ethylidyne-covered platinum surfaces was investigated (H100). The reflection-absorption IR spectra of chlorine adsorbed on a silver surface were characterized (H101). Several adsorbates on a copper surface were investigated at cryogenic temperatures (H102). The chemisorptive behavior of CO on several monometallic and bimetallic Pd, Cu, and Au catalysts was investigated (H103). The various phases occurring in dichlorodifluoromethane physisorbed on graphite were studied (H104). Thin films of nitric acid hydrates and ammonium nitrate adsorbed on gold foil were characterized (H105). Isotopic characterization was done of NO adsorption, dissociation, and coadsorption with CO on platinum (H106), as well as reduction of NO (H107). The spectrum of
iron pentacarbonyl adsorbed on gold surfaces was characterized (H108). The spectra of 1-prooxide and a set of deuterated 1-propoxides on a copper surface were obtained and characterized (H109). The adsorption of NO on a polycrystalline platinum foil was studied (H110). Two types of linear CO were observed adsorbed on a copper electrode, while only one type was observed on a silver electrode (H111). The adsorption and reactivity of NO on copper was studied (H112). In situ and ex situ infrared studies of the nature and structure of thiol monolayers adsorbed on cuprous sulfide were done (H113). Surface chemistry occurring during electroreduction of CO on electrodes modified with conducting polymer and inorganic conductor films was measured (H114). The spectrum of 2,5-dihydroxybenzyl mercaptan adsorbed on gold electrodes was obtained using attenuated total reflectance and reflection-absorption techniques (H115). Far IR spectra of copper and platinum electrode surfaces were studied (H116). The adsorption and reduction of nitrate ions on gold and platinum electrodes was studied (H117). The coordination, bonding, and configurational transitions for benzene and pyridine adsorbed on platinum and copper were studied by reflectionabsorption IR spectroscopy (H118). Silicon surfaces treated with an HF solution were used to study the behavior of adsorbed F atoms (H119). Reflectance absorbance spectra of methyl and ethyl formates chemisorbed on nickel were found to be consistent with surface coverage-dependent rotational isomerization (H120). The orientation of adsorbed deuterated and isotopic ethoxides on a copper surface was measured (H121). The adsorption of cyclohexane on clean and O-modified nickel surfaces was studied (H122). A study was done of D2O ice deposited on self-assembled alkanethiolate monolayers to measure cluster formation and substrate/adsorbate interaction (H123). A thin film of poly(ophenylenediamine) coated on a platinum electrode was characterized (H124). The molecular structures of self-assembled bimolecular films on gold and silicon surfaces were studied (H125). The orientation effects in physisorbed multilayers on copper were investigated (H126). An in situ study of 4-cyanopyridine adsorption on a gold electrode was done (H127). Propyne chemistry on nickel and copper surfaces was characterized, using analogies with ethyne adsorption (H128). A study was carried out on the coadsorption of D2O with preadsorbed K on cobalt (H129). Monolayers of octadecylsiloxane were formed on silicon and glass surfaces and studied by polarization- and angle-dependent external reflection IR spectroscopy (H130). An in situ study measured the coadsorption of perchlorate and bisulfate ions with adsorbed Tl on platinum (H131). In situ IR reflection spectroscopy was used in the qualitative and quantitative evaluation of heterogeneous adsorbed monolayers on a semiconductor electrode (H132). The adsorption of methanol on nickel oxide grown on nickel was studied (H133). The adsorption of ethylene on nickel was studied (H134). Attenuated Total Reflectance. A review was given on efforts to find spectroscopic evidence for or against the formation of bilayer islands of adsorbed surfactants (H135). A technique for depth profiling using multiple-angle ATR FT-IR was described (H136). A potential problem due to dispersion effects on infrared spectra in attenuated total reflectance was described (H137). Variable-angle ATR spectroscopy was used for depth profiling of stratified layers (H138). Spectra of copy toners were obtained
using microscopical internal reflection spectroscopy (H139). The use of diamond in an ATR design for analysis of highly corrosive liquids was reported (H140). The evaluation of collector adsorption phenomena by infrared internal reflectance spectroscopy of transferred Langmuir-Blodgett films (H141). A new chemical sensor based on ATR FT-IR spectroscopy was fabricated by coating an ATR crystal with a hydrophobic mesoporous silica film which can extract hydrophobic analytes (H142). ATR was used to monitor the decontamination reactions of chemical warfare agents (H143). The developmental changes in the content of carbohydrates and nitrogen-containing compounds in amaranth plants was measured (H144). The effects of pH and metal ions on the conformation of bovine serum albumin in aqueous solution was studied (H145). Diffusion coefficients of sodium p-aminosalicylate in sheep nasal mucosa and dialysis membranes were determined (H146). The skin barrier function was evaluated by measuring the rate of transepidermal water loss by an in vivo ATR method (H147). The kinetics of adenosine 5′-triphosphate hydrolysis was measured (H148). The infrared spectra of aqueous solutions of acetohydroxamic acid in soil and groundwater, and of suspensions of goethite with adsorbed acetohydroxamic acid, were measured (H149). Thin amorphous silicon layers on crystalline silicon substrates were characterized by infrared multiple internal reflection spectroscopy (H150). Surface processes occurring during chemical vapor deposition of silica through tetraethoxysilane onto GaAs were monitored by ATR (H151). Amorphous silicon monohydride films were characterized before and after reaction with atomic deuterium (H152). The hydrogen-bonding features of reacting film surfaces during hydrogenated amorphous silicon deposition were investigated (H153). Dissociative adsorption of methyl iodide on silicon was followed by multiple internal reflection spectroscopy (H154). In situ real-time measurements of chemical etching processes were made on silicon surfaces in ammonium fluoride solution (H155). The interfacial water near the hydrophilic surface of a silicon single-crystal internal reflection element, and the hydrophobic surface of a polymer-coated germanium single-crystal reflection element was characterized (H156, H157). An FT-IR ATR method was described for quantitative in situ analysis of the adsorption and rinsing removal of surfactants from silicon surfaces (H158). In situ ATR investigations of water, HSiCl3, and Co2(CO)8 on zinc selenide surfaces were done (H159). The nature of acid sites present in cation-exchanged montmorillonite was studied by ATR (H160). Bonding mechanisms of salicylic acid adsorbed onto illite clay were examined (H161). Hydration processes at the bentonite surface were studied (H162). The adsorption of polyamine, poly(acrylic acid), and poly(ethylene glycol) on montmorillonite was investigated (H163). The interaction mechanism of sodium dodecyl sulfonate with mineral fluorite was studied by ATR (H164). The chelation of titanium oxide, zirconium oxide, and aluminum oxide surfaces by catechol, 8-quinolinol, and acetylacetone was studied by a new in situ ATR spectroscopic method (H165). Real-time monitoring of electrochemical reactions by attenuated total reflectance/surface-enhanced IR spectroscopy was described (H166). An order-disorder process in LangmuirBlodgett films of dioctadecyldimethylammonium chloride was studied (H167). Trace levels of organic impurities in hydrofluoric Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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acid solutions were measured using a clean silicon ATR crystal to extract the organic impurities (H168). DMSO self-association in acetonitrile solutions was investigated (H169). The hydrolysis of trimethyl phosphate in aqueous solutions was studied (H170). Polarized infrared ATR spectroscopy was used for the threedimensional structural analysis of long-chain compounds (H171). The adsorption of acetic acid on n-CdTe photoelectrodes in aqueous and nonaqueous solutions was studied (H172). Realtime in situ ATR monitoring of mesoporous silicate syntheses was performed (H173). The extent of adsorption and the spatial chain orientation of adsorbed alkyl phosphate surfactants on alumina were studied (H174). The poly(p-phenylene vinylene)/chromium interface was characterized by ATR (H175). The electrochemical doping and protonation processes of polyaniline were described using in situ FT-IR-ATR (H176). In situ FT-IR-ATR spectroscopy was used to characterize the reduced form of polyaniline (H177, H178). Diffuse Reflectance. An investigation was done to determine whether increasing the scanned sample area would improve results obtained by diffuse reflectance FT-IR spectroscopy (H179). Diffuse reflectance was combined with gas chromatography as a coupled technique for the characterization of catalysts (H180). Diffuse reflectance was used to evaluate cleanliness of rough surfaces (H181). Solid-phase reactions of solid resin beads were investigated using diffuse reflectance spectroscopy (H182). The surface composition of AlN samples exposed to atmospheric air was analyzed as a function of their preparation method (H183). The structure of hydroxylated alumina surfaces were characterized (H184). The use of diffuse reflectance for the nondestructive inspection of organic films on sandblasted metals was discussed (H185). The application of diffuse reflectance in the preservation of historical monuments by monitoring salt migration was described (H186). Determination of the anti-sap-stain chemical didecyldimethylammonium chloride on wood surfaces by diffuse reflectance was shown to be effective (H187). In situ analysis was performed on catalytic surfaces of membrane electrode assemblies in working fuel cells (H188, H189). A study was done on the reversibility of CdGeON sensors toward oxygen (H190). The modifications afforded by chemical treatments to the main functional groups of a bituminous coal were characterized (H191). The catalytic removal of soot from diesel exhaust gases was studied (H192). Diffuse reflectance spectra of explosives were studied (H193). A comparison of several FT-IR sampling techniques, including diffuse reflectance, was investigated for the characterization of cement systems (H194). The structural nature of polyacrylates adsorbed on alumina from aqueous solution was investigated (H195). Adsorption interactions of bipyridines with the surfaces of different aluminapillar interlayered clays were studied (H196). The photochemistry of nitrates with alkali halides was studied (H197). The thermal derivatization of porous silicon was measured using diffuse reflectance spectroscopy (H198). The formation of ethyl tert-butyl ether on H-modenite was measured (H199). A series of dealuminated hydrogen mordenites were investigated with and without probe molecules CO and H2 (H200). The analysis of volatile organic chemicals adsorbed onto bentonitic clays was discussed (H201). 130R
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The application of diffuse reflectance FT-IR spectroscopy toward heterogeneous catalyst studies was reviewed (H202). The state of palladium on the surface of titanium dioxide-based carriers was investigated (H203). The interaction of cobalt cations with coordinated molecular oxygen species on Co-ZSM-5 emission control catalysts was studied (H204). The adsorption of paraffins on simple oxides was studied (H205). Acid-base properties of the surface of zirconia and zirconia modified with yttria were studied (H206). A kinetics and diffuse reflectance study of lowtemperature carbon monoxide oxidation over Au-TiO2 catalysts was done (H207). In situ temperature-programmed diffuse reflectance studies of V2O5/TiO2 catalysts were described (H208). The active surface species and the reaction mechanism were studied in the vapor-phase hydroformylation of ethene over Co/ SiO2 promoted with various noble metals (H209). The reaction mechanism of catalytic reduction of nitrogen oxides by propene in the presence of oxygen has been studied (H210). TiO2supported W- and Mo-selective catalytic reduction catalysts were studied before and after poisoning with As3+ oxide (H211). Colloidal hematite adhered onto silver and mercury electrodes was studied (H212). Evidence of alloy formation was observed in a study of CO adsorption on a bimetallic Pt-Pd catalyst supported on NaY zeolite (H213). The direct thermal interaction of elemental fluorine with hydrogenated and oxidized diamond surfaces was investigated (H214). Diffuse reflectance spectroscopy was used to characterize the adsorbed species when zirconia is exposed to aqueous oleate and oleic acid over a range of pH (H215). Adsorption complexes of triacylglycerol and oleic acid on silica gel and synthetic magnesium silicate were observed (H216). The thermal and adsorbed-water effects of a (3-aminopropyl)triethoxysilane layer modified onto the surface of silica gel were examined (H217). Boron nitride films deposited on steels from borazine were investigated (H218). The properties of different chromium oxide phases in the catalytic reduction of NO by NH3 was studied (H219). EMISSION The use of FT-IR emission spectroscopy as a tool for the study of chemical reactions was reviewed (I1). Another review discussed the use of FT-IR emission spectroscopy in observing electronic, rotational-vibrational, and pure rotational transitions (I2). The potential of near-IR emission spectroscopy for real-time monitoring of gas-phase molecules was described (I3). The means to detect, visualize, and survey different kinds of gases within industrial and energy processes, technological infrastructure, landfill bodies, and indoor and outdoor environments were discussed (I4). Exhaust gases from aircraft engine plumes were analyzed through remote sensing using FT-IR emission spectroscopy (I5-I7). A new technique was described that makes possible the laboratory IR emission study of gases of atmospheric interest, specifically CFC-12 (I8). A design for an open-path atmospheric monitor that uses both emission and absorption spectroscopies was discussed (I9). Remote sensing FT-IR emission spectroscopy was applied to the study of Freon12 thermal fragmentation in an alcohol/air flame (I10). FT-IR emission spectroscopy was used to measure nitric acid and ozone in the winter polar atmosphere (I11).
The cure chemistry and kinetics of aerospace epoxy resins and prepregs were measured in real-time by FT-IR emission spectroscopy (I12). The in situ analyses of reaction intermediates and adsorbed species during chemical vapor deposition of siliconbased films by infrared emission spectroscopy were described (I13). The sulfidation of molybdenum oxide has been studied by XPS and IR emission spectroscopy (I14). The dehydroxylation of a series of the kaolinite clay minerals has been investigated by FT-IR in situ emission spectroscopy (I15, I16). The FT-IR emission spectra of several different molecular species have been studied. These include the OH and OD stretch of HOI and DOI (I17), the vibration-rotation bands of ND (I18), the vibration-rotation bands of the CD radical (I19), and the spectra of ScH and ScD (I20). Similarly, the emission spectra of CoH (I21), BN (I22), Ge-As-S and Ge-Ga-S glasses doped with Dy3+ (I23), and LaH and LaD (I24) were studied. The emission spectrum of FeF was observed in the near-infrared region (I25), while the radiative decay of hot two-dimensional plasmons in AlO‚3GaO‚7As/GaAs heterostructures was studied by farinfrared emission spectroscopy (I26). The far-infrared laser emission spectra of ammonia isotopomers were reported (I27). The blackbody infrared radiative dissociation of bradykinin and its analogues was measured (I28). The vibrational relaxation of isomerizing alkyl halide complexes of perylene were measured by stimulated emission spectroscopy (I29). Plasmas of fluorinated hydrocarbons under conditions similar to those used in semiconductor surface processing were analyzed using time-resolved FT-IR emission (I30). The timeresolved FT-IR absorption and emission spectra of species produced in hollow cathode molecular discharges were characterized (I31). A new method was described that obtains time- and energy-resolved emission spectra using a step-scan FT spectrometer combined with correlational analysis techniques, providing superior dynamics and signal-to-noise ratios (I32). The quantitative aspects of FT-IR emission spectroscopy and the simulation of emission-absorption spectra were reviewed (I33). PROCESS AND IN SITU ANALYSIS FT-IR spectroscopy has been used in conjunction with in situ ellipsometry to characterize the deposition of amorphous hydrogenated silicon from a remote argon/hydrogen plasma. The FTIR results indicated a hydrogen content of 9-25 atom % (J1). IR transmission spectra with submonolayer resolution of the initial growth of amorphous hydrogenated Si deposited by F2 laser chemical vapor deposition (CVD) have been reported. The technique allows for the evolution of the H content and bonding configuration on a Si substrate to be monitored during nucleation and growth (J2). The H content and stoichiometry of silicon suboxides in a plasma parallel PECVD system have been determined by FT-IR spectroscopy (J3). In situ IR spectroscopy has been used to confirm the formation of gold-tetramethylthiourea (TMTU) complexes from the etching of Au(111) electrode surfaces in the presence of TMTU (J4). In situ FT-IR spectroscopy has been used in the study on the nature of the metal compleximmobilized polyaniline/Prussian blue-modified electrode in the electroreduction of CO2 in an aqueous solution (J5). Neutral H2O and H3O+ adsorbed on a Pt(111) electrode from acid solutions have been identified by in situ IR spectroscopy (J6). The
interfacial oxides formed under steady-state anodic polarization of p-silicon in fluoride electrolytes has been studied using difference in situ IR spectroscopy (J7). The promoted electrooxidation of aqueous sulfur dioxide at platinum electrodes has been studied in acidic medium with the aid of cyclic voltammetry and in situ FT-IR spectroscopy (J8). The five oxidation states of osmium carbonyl clusters have been characterized in the electrochemical redox processes using in situ FT-IR (J9). The activation and reduction of CO2 on a functional dual-film electrode has been studied by in situ FT-IR spectroscopy (J10). In situ farIR spectra of the surface films on Cu and Pt in aqueous solutions have been obtained using a synchrotron source (J11, J12). A comparison of static linear polarization selection and a new realtime technique has been done for the in situ FT-IR spectroelectrochemical studies of copper electrodes. The species analyzed in this comparison were the thiocyanate ion, imidazole, and glucose (J13). In situ FT-IR spectroscopy has been employed in the study of the electrode/electrolyte solutions at pH values of 1.2-3.4. The adsorbate associated with the anomalous peaks in the cyclic voltammetry of Pt(111) in sulfate- and bisulfatecontaining solution was examined (J14). In situ FT-IR has been used to examine the effects of incorporating redox-active pendant [Ni(tetraazamacrocycle)]2+ in poly(3-methylthiophenol) on Pt electrodes (J15). The underpotential deposition (UPD) of copper and thallium on a Pt(111) electrode in a sulfuric acid solution was studied by time-resolved in situ IR spectroscopy and electrochemical scanning tunneling microscopy. Surface changes were reported (J16). In situ electrochemical FT-IR spectroscopy has been extended to the study of a real carbon-supported platinumruthenium catalyst. Results of the electrooxidation of methanol at bulk Pt, Pt particles, and carbon black-supported Pt-Ru electrodes were discussed (J17). The oxidation of propene in aqueous HClO4 solution was studied on polycrystalline Au electrodes using differential electrochemical mass spectroscopy (DEMS) and in situ FT-IR spectroscopy. Reaction pathways and products were discussed (J18). In situ FT-IR spectroscopy has been used in the study of the oxidation of 2-propanol on Pt(111), Pt(110), and Pt(100) electrodes. The reaction intermediates were characterized for functional groups (J19). Linear polarization absorption ratios were determined from data for carbon monoxide and bisulfate anion adsorbed on Pt single-crystal electrodes (J20). The adsorption of sulfate species at polycrystalline gold electrodes were studied with in situ FT-IR spectroscopy in a HF/KF buffer solution of pH 2.8. This method allowed for the clear distinction between adsorbate and solution features (J21). The redox processes of poly(thiophene-3-methanol)-modified Pt electrodes were studied by cyclic voltammetry, in situ optical beam deflection, and FT-IR techniques. FT-IR results were used to study the insertion and release of ions into and from the polymer films (J22). The electrochemical oxidation of thiourea on a Pt electrode was studied at different potentials using voltammetry and in situ FTIR spectroscopy. The chemical changes during the reaction were discussed (J23). The coadsorption of nitriles and CO on CuZSM-5 were studied using in situ FT-IR spectroscopy (J24). The vibrational properties of CN-pseudohalide ions adsorbed on a Pt(110) single-crystal electrode in aqueous neutral solution were studied using in situ visible-IR sum frequency generation. The adsorption behavior of both ions depends drastically on the Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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electrode potential and on the immersion potential (J25). The adsorption of nitrate ions on Au and Pt electrodes in acid solutions was studied in acidic solution using in situ FT-IRS. Coordination on the Au electrodes and reaction products was discussed (J26). Under- and overpotential deposition of hydrogen on polycrystalline platinum, Pt(100), Pt(110), and Pt(111) surfaces in sulfuric acidic medium was monitored by IR-visible sum-frequency generation (J27). The urea adlayers formed at the surface of Pt(100) electrodes immersed in urea-containing solutions were characterized in situ by cyclic voltammetry and FT-IR spectroscopy. The bonding orientation of the urea at the surface of the electrode was discussed (J28). The ethanol electrooxidation on a coelectrodeposited Pt-Ru catalyst was studied by in situ FT-IR spectroscopy. Only CO2 was detected under the experimental conditions that produced acetaldehyde, acetic acid, and CO2 for a Pt catalyst (J29). In situ FT-IR spectroscopy was used to characterize doped films of poly(5-amino-1-naphthol) electrodes. These electrodes were effective in the reduction of chlorate anions (J30). The electrosorption of CO and CO2 from aqueous solutions of various pH values on polycrystalline Ni and Pd electrodes has been studied using in situ IR spectroscopy techniques. Various adsorbed species were identified (J31). With the help of in situ multistep FT-IR spectroscopy, two types of adsorbed geminal CO have been observed for the first time at an electrochemically modified Rh electrode (J32). The adsorption of CO and intermediate species in the electrochemical reduction of CO2 to hydrocarbons on a Cu electrode was examined using in situ IR spectroscopy (J33). The interaction of hydrogen with ZrO2 at high temperatures has been studied by in situ FT-IR spectroscopy. A proposed mechanism for the uptake of hydrogen by the surface of the zirconia was proposed (J34). The role of surface hydrides and fluorides in the Si-CVD process was studied by in situ FT-IR spectroscopy (J35). The electrochemical reduction of CO2 by electrogenerated 4,4′-dimethyl-2,2′-bipyridine-Ni and 1,10-phenanthroline-Ni complexes was studied by in situ FT-IR spectroscopy. The reactions of the carbonyl species with these complexes were discussed (J36). In situ FT-IR has been employed to study the formation of NH3 during reduction of NOx with propane on H/CuZSM-5 in the presence of excess oxygen (J37). A photogravimetric analyzer with FT-IR has been developed for the monitoring of removal of nitroglycerin from a reaction process. The FT-IR was used to analyze the nitroglycerin photodecomposition products on the surface of immobilized titania (J38). In situ FT-IR spectroscopy has been used for the investigation of the interaction of chlorinated ethylenes (vinyl chloride, 1,1-dichloroethylene, trichloroethylene, and perchloroethylene with the surface of chromium-exchanged zeolite Y (Cr-y) catalyst. The analysis was performed at different temperatures between 25 and 300 °C (J39). In situ FT-IR spectroscopy has been used to study the effect of temperature on the acid-bridged OH groups of mordenite zeolite with Si/Al ratios between 5.56 and 23.60 (J40). The initial activity of chromia/alumina catalyst in butane dehydrogenation was studied in a flow reactor using on-line FT-IR gas analysis. The time resolution for this analysis was on the order of seconds (J41). The mixed-valence isopolyanion Mo6O193- was investigated by means of cyclic voltammography, in situ FT-IR, and UV-visible/ near-IR spectroelectrochemical methods. The characteristics of 132R
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the anionic species were discussed (J42). The decomposition reaction of methyltrichlorosilane was investigated by an in situ IR spectroscopic method. The decomposition products were characterized (J43). In situ IR spectroscopy has been used to study the interaction of polypeptides and proteins with monomolecular films of phospholipids (J44). FT-IR spectroscopy has been used in the study of new molecular precursors of titanium oxide for the sol-gel process (J45). In situ FT-IR has been applied to the study of the conversion of methane to methanol in a gas mixture with Fe-Al-P-O catalysts (J46). The absorptions of SO2 and CO2 to fresh and aged forms of CaO and Ca(OH)2 have been investigated using in situ IR spectroscopy. This study focused on the chemistry of SO2 with the deterioration of calcareous stone monuments (J47). In situ time-resolved FT-IR spectroscopy was used to study particulate formation in radio frequency discharges in mixtures of silane, Ar, and N. An explanation of the results was discussed (J48). FT-IR was used to probe the nanostructures of novel polymer/organically modified silicon oxide hybrids obtained from sol-gel reactions of mixtures of tetraethoxysilane and diethoxydimethylsilane in perfluorosulfonic acid films (J49). FT-IR spectroscopy was used to study the gas-phase thermal decomposition of [Y(TMHD)3], [CU(TMHD)2], and [Ba(TDFND)2‚tetraclyme] under vacuum and at high temperatures (J50). In situ IR spectroscopy has been used in the determination of high-pressure phase diagrams of methane/heavy hydrocarbon mixtures (J51). In situ FT-IR spectroscopy has been employed in the monitoring of the SiC deposition in an industrial CVI/CVD reactor. The gaseous species observed were discussed (J52). In situ FT-IR spectroscopy was used to study syndiotactic poly(methyl methacrylate) films exposed to high pressure and supercritical CO2. The effect of mobility changes on spectral features was discussed (J53). The electrochemical reduction of CO2 by electrogenerated LNi(0), where L was 4,4′-dimethyl-2,2′bipyridine or 1,10-phenanthroline, was studied using in situ FTIR spectroscopy (J54). Activation and reduction of CO2 on the bis(1,8-dihydroxynaphthalene-3,6-disulfonato)iron(II) complexfixed polyaniline/Prussian blue-modified electrode was studied by in situ FT-IR spectroscopy. The site of attachment of the CO2 was discussed (J55). FT-IR has been integrated with a sampling system and control software as a continuous emission monitor for the analysis of volatile organic materials and some inorganic compounds (J56). In situ FT-IR has been used to characterize the oxidative degradation of working polymeric light-emitting devices with active layers of poly[2-methoxy-5-(2′ethoxyhexoxyl)1,4-phenylenevinylene] (J57). The electrooxidation of methanol on single-crystal surfaces was characterized by the formation of strongly adsorbed intermediates. Adsorbed species from this reaction were detected by in situ FT-IR spectroscopy (J58). The reactions of acetaldehyde on the surface of CeO2, Pd/CeO2, Co/ CeO2, and Pt/Co/CeO2 were examined by FT-IR spectroscopy. Identification of the reaction products was discussed (J59). IR spectroscopy has been used in the analysis of the uniform drying process of the paper process. This analysis gives information about temperature distributions along the paper track, supplying better process control (J60). Toluene alkylation with methanol over zeolites has been studied using FT-IR (J61). FT-IR spectroscopy of CO adsorbed at liquid nitrogen temperatures on zeolite K-L has aided in the understanding of the interaction of the CO
with the zeolite surface (J62). IR measurement of single layers and coextruded plastic films has been reported. The application of this to measure film thickness has been discussed (J63). ATR FT-IR was used in the analysis of the in situ adsorption of alkyl- and (perfluoroalkyl)trichlorosilane molecules on Si substrates. The information from this analysis was used to determine the Gibbs surface excess of adsorbed surfactants (J64). Real-time ATR FT-IR monitoring of M41S-type mesoporous silicate syntheses were performed which allowed the observation of simultaneous changes in both the organic and inorganic phases of the mixtures (J65). The chemistry of Si(100) and -(111) surfaces during immersion in dilute HF solutions was studied by multiple internal reflection IR spectroscopy (J66). In situ realtime ATR IR measurements of chemical-etching processes on Si(111) and Si(100) surfaces in NH4F solutions have been carried out for the first time (J67). The chemical nature of the Si(100) and Si(111) surfaces during immersion in dilute HF solution was investigated using ATR FT-IR spectroscopy (J68, J69). The dissolution of silicon oxides in hydrofluoric acid at the surface of a chemically oxidized silicon surface has been characterized by ATR IR with a spectrochemical cell (J70). A new ATR FT-IR setup has been used for the in situ spectroscopic study on the ZnSe crystal surfaces in the range of 600-4000 cm-1. This technique was used to study very thin water films on the crystal surface and the formation of polysiloxane films with Si-H bonds at the surface (J71). The vibrational properties of 2,5-dihydroxybenzyl mercaptan irreversibly adsorbed on gold electrodes were examined in 0.1 M HClO4 by ATR FT-IR and by FT-IR RAS techniques. The surface features were discussed (J72). In situ FT-IR/internal reflection spectroscopy has been used to study interfacial water near the hydrophilic surface of a Si single-crystal internal reflection element. A depth profile of the H2O structure was examined and reported (J73). In situ ATR FT-IR spectroscopy was used the examine the extent of adsorption and spatial chain orientation of adsorbed alkyl phosphate surfactant molecules on alumina. The effects on surface properties were discussed (J74). In situ cylindrical internal reflection FT-IR (CIR-FT-IR) was used to examine the behavior of subcritical and supercritical hydrocarbons processing over a Y-type zeolite at high temperatures and pressures (J75). The effect of coke formed by the conversion of ethylbenzene as well as ethylene on the sorption capacity and diffusivity of benzene and ethylbenzene in H-ZSM-5 was investigated by an in situ FT-IR technique. The coke species formed during this test were characterized (J76). Using in situ FT-IR ATR spectroscopy, the electrochemical polymerization process of 2,2′thienylpyrrole monomer in electrolytes containing LiClO4, Bu4NClO4, Bu4NBF4, and Bu4NPF6 was studied (J77). The investigation of the base-acid transition process of emeraldine (polyaniline) has been carried out by in-situ FT-IR spectroscopic methods (J78). ATR FT-IR spectroscopy, in conjunction with FTRaman, was used to elucidate the mechanism of the reaction of benzonitrile and hydrogen peroxide in alkali medium (J79). In situ high-resolution FT-IR spectroscopy was used to study the photopolymerization of C60 film. A C60 dimer structure was postulated from the results of this analysis (J80). In situ highresolution FT-IR spectroscopy was used to study the orientation phase transition of a H2O-free C60 film by examining the temperature dependence of line shift, half-width, and integrated
absorbance of the four fundamental IR-active modes in the highresolution IR spectrum (J81). In situ FT-IR spectroscopy was used to monitor the production of air toxics during the pyrolysis and combustion of benzene and o-dichlorobenzene. The effects of temperature and Cl concentration on the formation of polynuclear aromatic hydrocarbons were discussed (J82). In situ FT-IR was used to study the polynuclear peroxo complexes formed in a H2O2- cerium(IV) decatungstate ion-reacting system. The effect of H2O2 concentration on complexes and reactions was discussed (J83). The polymerization of 2,2′-thienylpyrrole and the redox behavior of the resulting polymer film electrodes were studied by FT-IR ATR experiments. The polymerization process was studied in aqueous solutions of different pH containing NaClO4, LiClO4, and NaBF4 (J84). The electrochemical redox processes of poly(thienylpyrrole) in acetonitrile solutions containing Bu4NClO4 or Bu4NPF6 were investigated using FT-IR-ATR spectroscopy (J85). The effect of moisture on a model silane coupling agent-modified adhesive bond was studied using FT-IR ATR spectroscopy. The silane studied was vinylbenzyl(trimethoxysilyl)propylethanediamine hydrochloride (J86). In situ FT-IR ATR spectroscopy has been used to gain a picture of the base-acid transition of leucoemeraldine, the reduced form of polyaniline in electrolytes containing KPF6/HPF6, NaClO4/HClO4, and NaReO4/ HReO4 (J87, J88). The electrochemical doping and protonation process of polyaniline processes have been described using insitu FT-IR-ATR spectroscopy (J89). In situ FT-IR MIR spectroscopy has been used in the study of the electrosynthesis and redox process of poly(1,5-diaminonaphthalene) (J90). Analytical expressions have been derived within the Leveque approximation, for the steady-state concentration profile of a reactant or stable product generated via first-order kinetics at an electrode in a channel-type electrochemical cell under fully developed laminar flow. This study has implications on the application of quantitative ATR FT-IR in a channel-type spectrochemical cell (J91). The adsorption of acetic acid on the n-CdTe photoelectrode in aqueous and nonaqueous solutions has been studied using ATR FT-IR spectroscopy (J92). Theoretical aspects of the application of insitu attenuated total reflectance infrared spectroscopy to the study of a channel-type spectrochemical cell have been developed (J93). The in situ FT-IR internal reflectance spectroscopy (FT-IR IRS) analysis of interfacial water near hydrophilic and hydrophobic surfaces has led to a better understanding of the water structure near these regions (J94). In situ ATR FT-IR spectroscopy has been used to investigate the polymerization of aniline on the p-Si electrode. From this work, a mechanism of the polyaniline synthesis has been proposed (J95). An ATR IR sensor has been developed and constructed to monitor the progression of chemical reactions during processing (J96). A model-assisted feedback control algorithm was developed to manipulate the mold temperature and control the curing during liquid composite molding of siloxane (J97). In situ IR spectroscopy has been used to study and model the hydrogenation steps in ethylene hydroformylation on 4 wt % Rh/SiO2 (J98). The adsorption of phosphate species on the well-ordered Au(111) single-crystal surfaces has been studied with in situ FTIR spectroscopy. The spectral features of the adsorbed H2PO4-, HPO42-, and PO43- have been identified (J99). The surface roughness and porosity during the photoelectrochemical etching Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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process has been studied by in situ FT-IR spectroscopy using multiple internal reflection techniques (J100, J101). TiO2 single crystals were studied in aqueous electrolyte with in situ FT-IR. Both photoinduced evolution of oxygen from the water and the oxidation of model organic compounds can be followed with this technique (J102). The role of surface hydrides and fluorides in the Si CVD process has been studied by in situ FT-IR spectroscopy. The conditions for replacement of hydrides by fluorides and subsequent etching were reported (J103). The anodic dissolution of p-Si in fluoride media has been studied using in situ IR spectroscopy for various compositions of the electrolyte. The IR spectra of the oxide layer revealed information on the disorder of the oxide in the current plateau (J104). In situ FT-IR spectroscopy was used to study the adsorption of NO and the reaction of NO with O2 on H-, NaH-, CuH-, and Cu-ZSM-5 zeolites. Decomposition of NO was observed for all catalysts, but the rates were observed to differ significantly for the different materials (J105). The adsorption of acetone and its coadsorption with CO were studied on a solid-state ion-exchanged Cu-ZSM-5 catalyst using in situ FT-IR spectroscopy. Changes in the C-O stretching vibrational frequencies of the adsorbed species were characterized (J106). The adsorption of MeCN and its coadsorption with CO on a solid-state ion-exchanged Cu-ZSM-5 catalyst were studied by FT-IR spectroscopy (J107). In situ IR absorbance spectra of NaVO3 was obtained at pressures up to 300 kbar. Two distinct phase transformations were observed (J108). In situ FTIR microscopy has been utilized in the study of the nature, strength, and reactivity of the sorption sites of single crystals of the microporous gallophophate cloverite. Two kinds of structural hydroxyl groups were identified (J109). Dehydrated Cd-exchanged zeolite HY reacted with H2S to give (CdS)4 in zeolite hosts has been studied by IR spectroscopy. The coordination around the Cd atoms was discussed (J110). The characterization of the coordination geometry or Cu ions included within zeolites was carried out with in situ XAFS, photoluminescence, and IR measurements (J111). The adsorption of phosphate species on Pt(111) and Pt(100) has been monitored by FT-IR spectroscopy (J112). The adsorbed residue originating from the contact of SO2 with smooth platinum electrodes was characterized by in situ FTIR and cyclic voltammtery in 1 M HF solutions. A potential dependent spectral feature ranging between 980 and 1020 cm-1 was reported (J113). FT-IR spectroscopy has been employed to investigate the effect of both the deposition parameters and subsequent thermal processing on phosphosilicate glass (J114). In situ IR has been used to study ethylene hydroformylation catalyzed by silica-supported [Rh12(CO)3O]2- cluster anions. The counterions in the study were Li+, Na+, K+, and Zn2+ (J115). In situ IR studies of the oxydehydrogenation reaction of propane over VPO/TiO2 catalyst indicated the Lewis acid sites are linked to COx formation and Brønsted sites to propene formation (J116, J117). The reactivity of adsorbed CO toward H on Rh/SiO2 catalyst has been examined by IR spectroscopy. The effect of linear CO and bridged CO on the reaction was discussed (J118). In situ FT-IR was used to study the oxygen adspecies on SrF2/ La2O3 catalyst during the oxidative coupling of methane (J119). The electrooxidation of CO adsorbed on polycrystalline Pt, Ru, Pt0.5Ru0.5, and Pt0.7Ru0 was studied by in situ IR spectroscopy (J120). Internal reflection spectroscopy has been used to obtain 134R
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the in situ IR spectra of ruthenium(II) bipyridyl dicarboxylic acid adsorbed to Degussa P25 and sol-gel TiO2 films. The site adsorption structure was discussed (J121). The adsorption of CO on the Au(332) surface was studied by LEED, surface potential measurements, temperature-programmed desorption, and IR spectroscopy. The IR band at 2120 cm-1 was observed to move to lower wavenumbers with increasing coverage (J122). The adsorption and reaction of CO on La2O3 has been examined with UV reflectance and FT-IR spectroscopy. The structural features of this interaction were discussed (J123). The stretching frequency of adsorbed CO (IR) and the 195Pt NMR of Pt catalysts on zeolite-NaY have been correlated. The chemisorption results of this study indicate that a steric effect as well as an electronic effect was operating (J124). FT-IR spectroscopy has been used to study the protonic sites of HXSM-5 zeolite effects on adsorption of methane at low temperatures. These sites are the active sites for methane conversion at high temperatures (J125). The physisorption of CO at low temperatures on a catalyst of H-mordenite embedded into an amorphous silica alumina matrix was investigated by FT-IR. The technique provides a means of characterizing the porosity of the catalyst (J126). The low-temperature methane adsorption and coadsorption of methane and CO on HZSM-5 and Mo/HZSM-5 were investigated by FT-IR spectroscopy. The assignment of observed bands was discussed (J127). The coordination geometry of Cu ions within zeolites was studied using photoluminescence and IR spectroscopy (J128). Gravimetric measurements with FT-IR analysis were used in the quantitative analysis of CO chemisorption on Pt/H zeolites (J129). The reactivity of Pt metal clusters supported on KL zeolite toward CO was studied by FT-IR spectroscopy at various pressures (J130). The interaction of CO and N2 with ferrisilicate MFI-type zeolites has been studied by FT-IR spectroscopy. The surface chemistry of the interaction was discussed (J131). The chemistry of the interaction of dimethyl ether with H-ZSM-5 zeolites has been studied using in situ IR spectroscopy (J132). The effects of structural defects and alloying of Pt/ZnO on adsorbed CO chemistry have been studied using FT-IR spectroscopy (J133). The surface reactions of CCl4 with zeolites have been examined by FT-IR spectroscopy. The Fermi resonance observed was explained by reaction intermediates (J134). The IR spectra of CO adsorbed at 77 K on ZnO ex-carbonate, on CoO and on CoOZnO solid solutions have been characterized (J135). The adsorption and oxidation of CO over gold supported on ZnO and TiO2 were studied by FT-IR and mass spectroscopy. Two kinds of sites on the particles were identified (J136). The structure of adsorbed CO on nanostructured Pt-Ru electrode surfaces has been examined by FT-IR spectroscopy (J137). IR spectroscopy has been used in the study of metal support interactions in the adsorption of CO on supported platinum in Pt/LTL and Pt/SiO2 catalysts (J138). CO adsorption on high-loading Ni/MgO samples treated at 800 and 900 °C was studied by IR spectroscopy. Linear and bridged monocarbonyls were characterized (J139). IR spectroscopy was used in the study of the CO stretching mode with respect to Brønsted and Lewis acidity of dealuminated acid ZSM 5, ultrastable Y, fluorinated USY, and Y zeolites. Changes in the OH IR bands on the surface of the zeolites were discussed (J140). The measurement of the shift in the stretching frequency of Brønsted hydroxyl groups on adsorption of a weak base has
been proposed as a quantitative measurement of the strength of acid sites in zeolites. This information might prove useful in the development of catalysts (J141). The IR spectrum of CO adsorbed on Ni(100) has been shown to display an additional high-frequency band at approximately 2200 cm-1. This absorbance has been attributed to the internal stretching mode of CO molecules weakly bonded to the Ni surface atoms (J142). The picosecond mid-IR pump-probe experiments were used to study vibrational relaxation of CO bound to synthetic metalloporphyrins with different metal atoms (Fe, Ru, Os), different axial nitrogenous ligands, and differently substituted porphyrins (J143). Ag clusters were prepared by either gas aggregation or matrix aggregation. The clusters were embedded in CO and CO/Ar matrixes, and the CO stretch frequency of the monolayer coverage was discussed (J144). The structure and hydrogen bonding of solid N1-alkylarylthioureas was studied by 13C CP/MASS and IR spectroscopy. It was concluded that, with the exception of cyclic dimers of N1 propenethioureas, hydrogen bonding occurs at N1 and N2 of the structure (J145). The electrooxidation of CO adsorbed on polycrystalline Pt, Ru, and Pt-Ru alloys has been studied by in situ IR spectroscopy. The effects of increased Ru content on the IR spectrum of the CO stretch vibration were discussed (J146). The Cu2+ ion sites in copper-exchanged ZSM-5 for activation and methanol synthesis have been studied by XPS and FT-IR spectroscopy (J147). The adsorption of CO and the coadsorption of CO and H2 on Ni/Al2O3 catalyst were studied by FT-IR. The interaction of the CO molecules with the surface was described (J148). The adsorption of CO2 and CO2/H2 on SiO2-supported Cs-doped Cu catalyst has been examined by FT-IR spectroscopy. Two forms of adsorbed carboxylate were identified also (J149). The adsorption of CO, NO, and C2H4 and reaction of CO+H2 on well-dispersed FeOx/TIO2 and FeOx/Al2O3 catalysts were studied with pulse adsorption and temperature-programmed desorption of NO and FT-IR. The adsorption properties and reaction products of the study were discussed (J150). Some Ru and Co carbonyl clusters in zeolite pores were prepared by a ship-in-bottle technique and characterized by FT-IR and EXAFS (J151). Some Cu and Cu-Ni-on-silica catalysts were characterized by IR spectroscopy of adsorbed CO. The interactions of surface species were discussed (J152). The adsorption of CO and CO2 on two series of palladium-based catalysts was compared by IR spectroscopy (J153). The adsorption of Co on CuO/SiO2 and Cu-ZSM-5 catalysts was studied by IR spectroscopy (J154). The vibration frequencies of adsorbed CO molecules on Pd/MgO(100) have been examined by fast FT-IR spectroscopy (J155). Both linear and bridged forms of adsorbed CO on Pt/ZrO2 catalyst have been observed using FT-IR spectroscopy (J156). IR spectroscopy has been used to study the decomposition of CO2 on a coppercontaining methanol catalyst (J157). The transient nature of adsorbates for the reaction of NO with CO over a 4 wt % Rh/SiO2 catalyst has been studied by in situ IR spectroscopy combined with pulse transient techniques (J158). The reactivity of adsorbed CO toward H has been studied using a temperature-programmed reaction technique coupled with IR spectroscopy. This combination provided information on the structure and reactivity of adsorbates, activation energy, and kinetic data for the CO hydrogenation reaction (J159). The adsorption of CO on the MgO(100) surface prepared in situ was studied using polarization
FT-IR spectroscopy. The IR spectra from p- and s-polarization were discussed (J160). Physically adsorbed acetonitrile, THF, diethyl ether, and methanol-d in supercritical SO2 on silica gel were studied by FT-IR at pressures up to 15 MPa (J161). The acid properties of pure and sulfated zirconias were studied by FTIR spectroscopy of adsorbed CO and NH3 probe molecules. Two types of Brønsted acidic centers and two types of Lewis acid centers were identified (J162). The oxidation state of Rh/Al2O3 catalyst was investigated by XPS and IR spectroscopy of adsorbed CO (J163). The dynamics of adsorbed species on Rh/SiO2 catalyst during CO hydrogenation to form methane was studied by in situ IR spectroscopy combined with steady-state isotopic transient and pulsing CO methods (J164). In situ MIR IR studies of semiconducting electrode surfaces have provided information of surface chemistry of HF-rinsed silicon (J165). The adsorption and decomposition of N2O over ZrO2 has been studied in situ by in situ diffuse reflectance IR Fourier transform DRIFT, TPD, TPR, and XPS. The surface chemistry was discussed (J166). An in situ DRIFTS technique was used in the study of the active surface species and the reaction mechanism of the vapor-phase hydroformylation of ethene over Co/SiO2 promoted with various noble metals (J167). DRIFT spectra of two humic sodium salts have been recorded to study structural changes caused by heating (J168). In situ DRIFT spectroscopy has been introduced as a method for studying the catalytic surfaces of membrane electrode assemblies in working fuel cells (J169). The catalytic surfaces of membrane electrode assemblies in direct methanol/oxygen fuel cells were investigated in situ by FT-IR diffuse reflection spectroscopy. Possible mechanisms for methanol, formaldehyde, and formic acid oxidation at the anode surfaces were discussed (J170). In situ DRIFT spectroscopy was used to study both the adsorbed and desorbed species produced on highsurface-area anodes (Pt-Ru, Pt black) and cathodes (Pt black) of direct methanol/oxygen fuel cells (J171). In situ DRIFT spectroscopy has been used in the study of chromia on titania catalysts containing different chromium oxide phases used for the low-temperature selective catalytic reduction of nitric oxide by ammonia (J172). In situ DRIFT spectroscopy has been utilized in the high-temperature study of OD stretching vibrations on the surface of various Li ceramics. The frequency of the stretching vibration of the OD group has a strong correlation with the LI/O ratio of the ceramics (J173). Hydroxyl groups on the surface of Li2O were studied by DRIFTS at high temperatures under controlled D2O and D2 partial pressures (J174). Temperatureprogrammed DRIFT spectroscopy has been proposed to follow in situ temperature-programmed reduction and the temperatureprogrammed programmed desorption experiments of catalyst systems. TPDRIFTS studies of desorption and reduction of a conventional V2O5/TiO2 catalyst have been carried out (J175). The reaction mechanism of catalytic reduction of nitrogen oxides by propene in the presence of O2 has been studied by in situ DRIFT spectroscopy (J176). In situ FT-IR ATR spectroscopy with mass spectroscopy were used in the kinetic investigation of the reaction mechanism of CO2 methanation over a catalyst (J177). The oxygenation functions issued from the oxidative thermal treatment of mesocarbon microbeads at 320 °C were investigated by DRIFTS. Some information about the reaction kinetics and mechanism were discussed (J178). Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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In situ reflection IR spectroscopy with electrochemical modulation was used to study the coadsorption of anions for the system Tlads/Pt(111) in dilute H2SO4 and HClO4. Possible structures of the Tl-ClO4 and Tl-HSO4 adlayers at Pt(111) were discussed (J179). The potential-dependent structural change and irreversible anodic decomposition of the self-assembled monolayers of 3-mercaptopropanenitrile and of 8-mercaptooctanenitrile on gold electrode were studied by SNIFTIRS (J180). SNIFTIRS has been used in the study of the structure of the double layer for the system Pt(hkl)/acetonitrile with tetraethylammonium perchlorate and sodium perchlorate electrolytes (J181). The SNIFTIRS results obtained on polyaniline films containing heteropoly anions in acidic solutions have been reported. The report focused on the behavior of the anions during the redox switching of the polymer (J182). SNIFTIRS has been used to probe the concentration change of the perchlorate anion in the electrochemical double layer at Au(100) (J183). SNIFTIRS and two internal reflectance modes have been used in the study of the surface chemistry of Li electrodes and nonactive electrodes polarized to low potentials in LiC(SO2CF3)3 solutions in 1,3-dioxolane and THF (J184). The electrooxidation of hypophosphite ions on polycrystalline nickel in alkaline solutions was studied using cyclic voltammetry, chronoamperometry, and in situ IR spectroscopy (J185). SNIFTIRS studies on the electrooxidation of hypophosphite at polycrystalline and single-crystal Ni electrodes indicated a process dependent upon the structure of the crystal plane exposed for the electrolyte (J186). The subtractively normalized interfacial FT-IR technique has been applied to the in situ IR spectroscopic study of electrochemical doping of poly(N-vinylcarbazole). The doping of ClO4- anion was shown to be limited by cross-linking of the polymer (J187). Subtractive normalized FT-IR spectroscopy studies were performed on the electroreduction of CO2 at a Cu electrode, using isotopically labeled CO2 and HCO3- in H2O and D2O (J188). In situ external reflection FT-IR spectroscopy was performed during cyclic voltametric polymerization of poly(p-phenylene) films (J189). Nitridation of GaAs(001) surfaces grown by MBE was observed by detection of reflectance change caused by the formation of Ga-N and As-N bonds by reflection FT-IR spectroscopy (J190). In situ external reflection absorption FT-IR spectroscopy was used to understand the dynamics of the organic/ inorganic interface during crystal growth. The dynamics of template-directed calcite crystallization were studied (J191). In situ reflectance FT-IR spectroscopy has been used to study the adsorbed species, reactive intermediates, poisoning intermediates, and reaction products of the electrocatalytic oxidation of methanol on Pt-Ru electrodes (J192). In situ IR reflectance spectroscopy combined with spectral simulation has been applied to the study of the supramolecular structure of ethyl xanthate (C2H5OCS2-) species on cuprous sulfide. The identity of adsorption products was discussed (J193). External reflectance FT-IR spectroscopy was used to study the electrochemical deposited poly(o-phenylenediamine) on a Pt electrode. The film was doped with ClO4and the resulting features were characterized (J194). IR reflectance spectroscopy for thin-film measurement has been applied in the semiconductor industry. This technique has been used for the multilayer thickness and doping concentration determinations (J195). 136R
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The potential-dependent structure change and irreversible anodic decomposition reaction of a 2-(11-mercaptoundecyl)hydroquinone monolayer on a gold electrode surface in 0.1 mol/L HClO4 solution was studied by electrochemical in situ FT-IR reflectance absorbance spectroscopy (J196). The effects of Ar, H2/AR, and H2/O2/Ar downstream microwave plasmas on the surface structure and properties of poly(vinyl chloride) films have been studied using in situ IR reflection-absorption spectroscopy (J197). Real-time IR reflectance spectroscopy has been employed to identify the hydrogen incorporation and release process that control the final hydrogen content of hydrogenated amorphous silicon films (J198). In situ IR reflectance absorbance spectroscopy has been used to detect reaction products resulting from the etching of Si in Cl2 plasmas. The species in the gas phase and at the surface were characterized (J199). The electrochemical behavior of an azobenzene containing a self-assembled monolayer, 10-[4-(phenylazo)phenoxy]decane-1-thiol, was examined by in situ FT-IR reflection absorption spectroscopy. The process and architecture were discussed (J200). In situ reflectance IR spectroscopy was used in the real-time monitoring of the metallorganic vapor-phase epitaxy growth of InGaAsP films (J201). In situ IR ellipsometry was used to demonstrate the efficiency of several plasmas in the removal of hydrocarbon contamination from metallic surfaces prior to film deposition (J202). In situ IR reflection spectroscopy has been combined with spectral simulation in the study of monolayers of ethyl xanthate formed at a controlled potential on cuprous sulfide (J203). An approach to the use of IR reflectance spectroscopy for thin-film measurement in the semiconductor industry has been described. The multilayer thickness and doping concentration of IC wafers can be determined by a single-angle, unpolarized IR reflectance measurement using an FT-IR spectrometer (J204). Reflectance IR spectra of tungsten oxide films have been used to determine the refractive index and extinction coefficients (J205). The behavior of diethyl carbonate electrolyte on lithium with a surface film was examined by in situ FT-IR spectroscopy. Solvent penetration of the film and reaction with the lithium was observed (J206). In situ IR absorption spectroscopy was measured for a hot-filament diamond growth process. Absorptions of CH4 and C2H2 were detected (J207). In situ IR absorption was used to monitor diamond films prepared by hot-filament CVD. The presence of C2H2 in the diamond film was proposed as the active radical in diamond growth (J208). The enhancement of copper growth in the chemical vapor deposition of Cu(II) by auxiliary reagents has been monitored by FT-IR spectroscopy (J209). In situ IR reflectionabsorption spectroscopy has been used for conformational analysis of different regions of partially deuterated fatty acid and phospholipid Langmuir films (J210). A versatile, thin-layer cell to perform in situ IR spectroelectrochemistry has been used to monitor the electrochemical reaction of oxyhalide electrolytes (J211). The interaction of hydrophobic and hydrophilic species at the surface of minerals has been studied using in situ FT-IR reflection spectroscopy and ATR FT-IR spectroscopy (J212). In situ IR spectroscopy was used to monitor the adsorptive and catalytic events occurring at the gas/solid interfaces during 2-propanol decomposition over pure and MnOx-modified aluminas (J213). The atomic layer controlled deposition of silicon nitride has been studied by FT-IR reflection absorption spectroscopy
(J214). The real-time in situ observation of deposition and reevaporation of N-vinylcarbazole polymer on a Ag-coated glass plate was performed using FT-IR RA spectroscopy (J215). Real-time in situ FT-IR RA spectroscopy has been used to evaluate the vapor deposition polymerization of N-vinylcarbazole (J216). Reflectance FT-IR spectroscopy was used to study the abnormal optic properties of adsorbed CO on a dispersed Pt layer on different substrates (J217). Reflectance absorbance IR spectroscopy has been used to study the adsorption and oxidation of CO on Pt(110) (J218). Reflectance absorbance IR spectroscopy has been used to observed the reversible phase transition between chemisorbed CO on Cu(100) with physisorbed overlayers (J219). FT-IR RA spectra obtained for a set of D- and isotopic carbon-labeled ethoxides adsorbed on the Cu(111) surface have been used to determine the orientation of the adsorbed ethoxide (J220). The thermal desorption of CO and NO on MO2C has been studied using reflectance absorbance IR spectroscopy (J221). The adsorption and desorption of CO and hydrogen on K-modified Ir(111) has been studied using reflectance absorbance IR spectroscopy (J222). Polarization modulation IR reflectance absorption spectroscopy has been applied for the first time to the study of the adsorption of CO on Co(001) (J223). RAIRS has been used to identify and characterize three distinct coverage-dependent phases for CO on Co(1010). The orientation of the CO on the surfaces was discussed (J224). The adsorption of cyclohexane on clean and O-modified Ni(111) surfaces was studied by RAIRS. The orientation of the cyclohexane at the surface was discussed (J225). Adsorption of CO on Ni(100) surfaces has been studied by reflectance absorption IR spectroscopy (J226). In situ reflectance FT-IR has been used for the evaluation of the photoinduced reaction at an aqueous solution/semiconductor interface of a (S)lysine solution (J227). The coadsorption of H2O and SO3 molecules on Pt(111) has been studied by reflectance-absorption IR spectroscopy. The structure at the surface of the electrode was shown to be a double layer (J228). Reflectance-absorbance IR spectroscopy in conjunction with scanning tunneling microscopy has been used to study the structure of irreversibly adsorbed cyanide adlayers on a Pt(111) electrode (J229). The nitrous oxide generated by the electrochemical reduction of nitrite on a polycrystalline platinum electrode in aqueous HClO4 was monitored by in situ FT-IR reflection adsorption spectroscopy. IR observations were found to agree with on-line mass spectrometry (J230). The interfacial behavior of water molecules at a polycrystalline gold electrode surface in aqueous sodium halide solutions was studied by in situ FT-IR reflection absorption spectroscopy. Frequency shift dependence on the electrolyte anion was observed (J231). The acidity of cloverite was studied by in situ FT-IR microscopy of sorption of probe molecules with varying basicity. Changes in the cloverite lattice were discussed (J232). Spatially resolved IR microscopy was used in conjunction with the contact method to conduct in situ diffusion experiments of photocured polymerdispersed liquid crystals (J233). In situ diffusion and miscibility studies of polymer-dispersed liquid crystals dissolved in a polymer matrix were carried out using FT-IR microscopy. This technique was used to study the miscibility of a liquid crystal (E7) in poly(butyl methacrylate) (J234). Single-bead FT-IR microscopy was used for the real-time monitoring of the catalytic oxidation of
alcohol to aldehydes and ketones on resin support (J235). Methodology for the in situ IR monitoring and analysis of solidphase organic reactions has been developed. This technique has been applied to the analysis of solvent diffusion into and subsequent washout from aminomethyl polystyrene beads (J236). The interaction of allylbenzene with oxide catalyst surfaces having different surface characteristics has been investigated by FT-IR spectroscopy (J237). A prototype FT-IR-based measurement system designed for continuous emission monitoring has been tested in full-scale and pilot plant-scale fossil fuel-fired combustors. The results of these applications are discussed (J238, J239). IR absorption spectra of molecular clusters formed in a supersonic free jet expansion were measured at various conditions. Cluster size and distribution were discussed (J240). Emission IR spectroscopy has been demonstrated to be an effective technique for in situ analysis of reaction intermediates and adsorbed species during chemical vapor deposition of Si-based films at high temperatures (J241). In situ IR spectroscopy was used to study the intermediates of the reaction of NOx reduction with propane in excess O2 on Cu-ZSM5- zeolites (J242). FT-IR technology has been successfully applied to the monitoring of emission gases from an oil refinery. This technique monitors CO2, SO2, NOx, NH3, and HCl in the presence of H2O (J243). Gas-phase FT-IR has been applied to the on-line analysis of effluents containing trimethylamine and methanol quantitatively using PLS (J244). NIR spectroscopy has been used to develop a method for the determination of lubrication properties of oils (J245). On-line NIR monitoring to a polyol process resulted in a decrease in production of out-of-specification material and increased the plant throughput (J246). A proposal for the use of mid-IR spectroscopy to provide linear calibration numbers to calibrate on-line NIR monitors with nonlinear features has been suggested (J247). On-line NIR in hostile environments has been shown to be advantageous in many incidents. The calibration problems have been noted, but the highly precise results from the NIR is a strong drawing point (J248). A report has been written on the practicality of keeping NIR working in an industrial environment. Calibration model transfer and maintenance were two topics covered (J249). NIR spectroscopy has been applied to the noninvasive on-line detection of cortical spreading depression in the pentobarbital-anesthetized rat (J250). An automated system for the on-line monitoring of powder blending processes has been developed and applied to give a realtime determination of blend homogeneity (J251). NIR spectroscopy has been evaluated as an on-line technique to monitor the homogeneity of a pharmaceutical blend containing 10% sodium benzoate, 39% microcrystalline cellulose, 50% lactose, and 1% magnesium stearate. The experiments were carried out using fiber optics, a commercially available NIR spectrometer, and a blender (J252). The suitability of diffuse reflectance NIR spectroscopy as an on-line method to monitor process streams was tested in a pilot plant-scale oil sand extraction plant. The feasibility of monitoring feed stream conditions was demonstrated by principal component analysis of the measured spectra (J253). Diffuse reflectance NIR spectroscopy was applied in an at-line process analytical interface to determine moisture content in bulk hard gelatin capsules. No Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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sample pretreatment was required, and the analytical time was 1-2 min (J254). The need for stable, high-quality process NIR and IR spectroscopic analysis has been discussed. Steps to condition the samples prior to analysis have been presented (J255). A method has been developed for the NIR monitoring of the cracking property of a feed to a steam cracking process (J256, J257). NIR using a ripple calibration technique has been described and applied to the characterization of web thickness and coating monitoring (J258). A new on-line process control spectrometer for measurements from the UV to the IR has been developed and tested in combustion gas analysis of a waste incineration plant (J259). A high-pressure and temperature in situ transmission IR reactor cell has been developed and applied to the study of adsorbates in CO hydrogenation and NO-CO reaction on Rh/ SiO2 (J260). A transmission IR cell of simple construction has been developed to study heterogeneous catalysis in situ. The cell was demonstrated on the catalytic NOx removal (J261). A generalized mathematical treatment has been developed that enables the quantitative analysis of various in situ spectroscopic experiments involving detection of solution-phase species generated at the surface of a rotating disk and ring disk, channel, and tube-type electrodes under steady state (J262). An attempt at application of modern IR spectroscopy as a noncontact-nondestructive technique for evaluation of chemical processes has led to an improved sample handling system. Use of this has been recommended for off-line as well as on-line applications (J263). A fixed-volume sample of a reaction mixture of a chemical process has been injected into a liquid carrier stream. The stream was passed through an IR detector which was used to monitor a species of the reaction mix (J264). Chemometrics has been applied to the NIR monitoring of the manufacturing of ethyl glucoside fatty ester (J265). A closed loop on-line NIR spectrometer has been used in the analysis of the gasoline blending process. This has enabled the operation to gain tighter control of the octane number of their process (J266). On-line prediction of 10 gasoline properties including research and motor octane numbers, vapor pressure, API gravity, and aromatic contents were carried out using NIR spectroscopy and fiber optics (J267). NIR spectroscopy with fiber optics has been used in on-line determination of hydrocarbon gases at a petrochemical plant in mixtures of ethane, ethene, propane, and propene (J268). Fiber-optic FT-IR spectroscopy has been applied to the in situ monitoring of input partial pressures of organometallic precursors in a vertical rotating-disk OMVPE reactor (J269). A novel H2O-cooled mid-IR fiber-optic probe with calcogenide fibers and a ZnSe internal reflection element has been use in the in situ analysis of an acid-catalyzed esterification reaction in toluene at 110 °C (J270). An IR fiber-optic sensor has been developed for the in situ detection of chlorinated hydrocarbons and other pollutant species in water (J271). NIR process applications focused on the use of fiber optics and probes to interface to the process have been carried out in single-point and multiplepoint NIR process analysis. The technique has been reported to produce a result in 45 s or less (J272). NIR spectroscopy using fiber optics has been applied as a monitor of homogeneous and heterogeneous reactions. This technique has been applied directly to full-size chemical reactors (J273). 138R
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Imaging NIR radiometry has been employed successfully for radiance measurements of the closed coupled atomization of nickel base superalloys. The technique provides opportunities for realtime process control feedback (J274). A spatially resolved IR imaging technique has been developed to monitor the linear adsorbed CO coverage on supported catalyst surface to better understand the dynamics of spatitemporal patterns on heterogeneous catalyst (J275). NIR spectroscopy has been used as a process monitor for the anionic polymerization of styrene and isoprene in cyclohexane and in THF (J276). In situ real-time NIR monitoring has been demonstrated in the reaction of phenyl glycidyl ether with aniline and bisphenol A diglycidyl ether with 1,8-diaminonaphthalene in and epoxy resin-amine reactions (J277). The esterification reaction between acid or anhydride and an alcohol has been monitored by NIR spectroscopy for both small molecules (J278) and polyesters (J279). NIR has been used to measure and control properties of polyamide formation in the manufacturing of polyamide yarn (J280). The application of IR and UV photometers in the continuous monitoring of product purity has been discussed (J281). The thermal elimination of NaCl from sodium chloroacetate, a polymerization reaction that takes place between 150 and 200 °C in the solid state, has been monitored by in situ IR spectroscopy. The polymerization process, intermediates, end groups, and byproducts have been explained from these results (J282). Direct control of fermentation by on-line NIR spectroscopy has been described (J283). NIR spectroscopy has been shown to provide tighter process control, greater process knowledge, and improved product quality assurance in fermentation process analysis (J284). NIR spectroscopy has been applied to the process control of antithrombin III production using a partial least-squares algorithm (J285). NIR spectroscopy has been applied to the postconsumer package identification. A correct classification rate of better than 97% for six major types of packages in household garbage was reported (J286). An aqueous supercritical fluid extraction (SFE) FT-IR spectroscopy technique was used to monitor dodecane in water ranging from 200 to 12.5 ppm (J287). A simple on-line SFE FTIR transmission cell has been used to obtain both qualitative and quantitative information about analytes in supercritical fluids (J288). A review has been written on the available spectroscopic techniques for the in situ study of combustion chemistry occurring in an internal combustion engine chamber (J289). FT-IR spectroscopy has been used in the study of fluorine dopant levels in plasma-enhanced chemical-deposited fluorinated silica glasses. The effects of dopant levels on peak positions, areas, film thickness, and physical properties were reported (J290). FT-IR spectroscopy has been used to monitor exhaust gases produced from the plasma-supported gas-phase cleaning of PECVD facilities (J291). A list of Internet sites has been presented which may be of interest to anyone dealing with IR and near-IR spectrochemical analysis (J292). A new mathematical correction method has been developed for on-line film thickness determination for FT-IR analysis incorporating both optical interference and absorption methods (J293). FT-IR spectroscopy has been applied to the analysis of pollution prevention systems in ceramic processing
(J294). FT-IR has been applied to the determination of chemical concentrations of constituent classes of hydrocarbon feed to a catalytic cracking process (J295). Discriminant analysis using principle components of mid-IR spectral data has been shown to be a powerful quality validation tool for manufacturing processes (J296). Initial studies on open-path FT-IR for measurements at a refinery, chemical plant, and natural gas processing facility have proven promising. The effects of water vapor interference have been reduced using software algorithms (J297). The open-path FT-IR technology was applied for a four-week period around the process area of an industrial chemical facility. Methods for dealing with background collection, quality assurance techniques, prediction modeling, and data storage, presentation, and retrieval were discussed (J298). The translational energy of CO2 produced from CO oxidation on Pd foil at 600 K was studied using high-resolution IR chemiluminescence spectroscopy. The rotational structure of certain vibrational transitions was fully resolved using a FT-IR spectrometer operating at 0.006-cm-1 resolution (J299). This technique has also been applied to the catalytic oxidation of CO on Pt(110), Pt(111), and polycrystalline Pt surfaces. The vibrational temperatures of the resulting products were discussed (J300). A combined IR and MS technique has been used to determine extinction coefficients of adsorbed CO on the 4% Rh/ SiO2 catalyst. The procedure provides a fast and accurate method for the determination of extinction coefficients of adsorbed surface species (J301). The structure of a triruthenium ketenylidene cluster deposited on MgO, SiO2, and SiO2-Al2O3 has been examined by FT-IR and Raman spectroscopy (J302). A cell and optics design for in situ far-IR spectroscopy study of electrode surfaces using synchrotron radiation has been discussed. Precautions necessary for good results were also discussed (J303). Explanations on application of interferometer- and grating-based IR spectrometers on process analysis with calibration strategies have been published (J304). Octane number has been calibrated successfully with accuracy and precision sufficient for ASTM conformance using an acoustooptic process spectrometer (J305). Oxidation of CO over a palladium/zirconia catalyst obtained from an amorphous Pd25Zr75 precursor was investigated by time-resolved FT-IR spectroscopy (J306). Two types of adsorbed geminal CO have been observed for the first time at an electrochemically modified Rh electrode using in situ multistep FT-IR spectroscopy (J307). The reaction of dimethylaluminum hydride with photochemically deposited hydrogenated amorphous silicon was studied in situ with polarization modulation IR spectroscopy (J308, J309). ENVIRONMENTAL ANALYSIS A review of the environmental applications of near-IR spectroscopy was presented (K1). The use of FT-IR for monitoring processes at coal-fired power plants was reviewed (K2). FT-IR was included along with other spectroscopic techniques in a review of methods for studying combustion chemistry in an internal combustion engine chamber (K3). The use of IR techniques such as DRIFT and ATR for soil analysis was described in a review (K4). FT-IR, NMR, and chromatographic techniques were used in the differentiation of chlorinated dibenzo-p-dioxin isomer pairs (K5). Seven tetrachlorobutadiene isomers were identified using
ab initio calculations and GC/MS/FT-IR (K6). The absorption of SO2 and CO2 on CaO and Ca(OH)2 was studied by in situ IR (K7). Results from this study may aid in understanding how polluted air can lead to the deterioration of stone monuments and buildings. IR and X-ray diffraction methods for determination of quartz in coal and airborne dust were compared (K8). Motor oil contamination in sandy loam was determined using near-IR reflectance spectroscopy (K9). Hazardous organic compounds were detected in sandy soil using IR fiber-optic sensors (K10). An IR method to screen soil samples from waste sites for explosives, pesticides, and some volatile or semivolatile organics was discussed (K11). Explosives in soils were detected via the pyrolysis products using tunable infrared laser differential absorption spectroscopy (TILDAS) (K12). An FT-IR spectrometer and fiber-optic probe were used for real-time analysis of soil for organic contaminants (K13). FT-IR was among the techniques used to investigate the inorganic compounds present in coal ash from power plants (K14). The use of a polypropylene filter and IR for the quantitative determination of respirable cristobalite in airborne dust was reported (K15). Chemometrics and a near-IR analyzer that uses acoustooptic tunable filter (AOTF) spectrometry were employed to identify organic contaminants in pretreated wastewater (K16). Volatile organic compounds (VOCs) were detected in water using solidphase microextraction of the VOCs into Parafilm and IR analysis of the Parafilm (K17). Chlorinated pesticides in water were concentrated into a chloroparaffin-plasticized PVC coating on an ATR element or optical fiber and analyzed by FT-IR (K18). A Teflon-coated silver halide optical fiber was evaluated as a sensor for the FT-IR analysis of chlorinated hydrocarbons in water (K19). Herbicides in river water were identified by liquid chromatography/FT-IR (K20). Low concentrations of hydrocarbons in water were detected by coupling an aqueous supercritical fluid extraction vessel to an FT-IR spectrometer (K21). An evanescent field absorbance sensor operating in the near-IR region was used for the detection of hydrocarbons in water (K22). A filter-based infrared analyzer for measurement of oil contaminants in water was described (K23). Reports were published on the evaluation of IR sensors capable of detecting oil spills on water at night (K24, K25). The nondispersive IR organic carbon analyzer and the CO2 coulometer were compared as methods for the determination of dissolved inorganic carbon (DIC) in water (K26). Examples were given to illustrate how process analysis monitors can be used for pollution control (K27). The desorption of greenhouse gases (CO2, N2O, H2O) from a thin film of poly(methyl methacrylate) was followed by FT-IR (K28). The impact of the ban on the manufacture of Freon 113 was discussed in relation to the IR analysis of water or soil for hydrocarbons (K29). A paper was published that describes the design and use of a micromachined, integrated optical bench for a carbon dioxide IR sensor (K30). Quality assurance measurements for consistent instrument operation and performance prediction of passive FTIR data collection systems for air analysis were developed (K31). In another paper, the quality assurance aspects for FT-IR analysis using a short cell and high concentrations of gases were considered (K32). Gas analysis is an important aspect of monitoring the environment. A number of devices for the analysis of gases by IR Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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spectroscopy were described in various papers. These include a tubular IR waveguide sensor with a functionalized self-assembled monolayer (K33), fiber-optic sensors for on-line gas monitoring (K34), a portable FT-IR, real-time, gas analyzer (GASMET) (K35), an IR imaging volatile organic carbon field sensor (K36), an intercavity diode laser near-IR spectrometer (K37), and a dualcell extractive FT-IR ambient air monitor (K38). Sources of noise in FT-IR instruments used for trace gas analysis were the subject of an investigation (K39). Heated extractive FT-IR was used for the analysis of volatile emissions from production facilities (K40). Fugitive emissions (carbon tetrachloride, 1,3-butadiene, propane) from piping components were analyzed with a portable IR analyzer (K41). Trace gas analysis was carried out by means of a Midac FT-IR equipped with a multipass cell and Grams/386 software (K42). FT-IR was used for time-resolved air monitoring for methyl bromide concentrations after fumigation of buildings (K43). Ammonia and HCl were detected in flue gases using a GASMET gas analyzer (K44). The IR spectra of 18 hydrochlorofluorocarbons and hydrofluorocarbons were measured and used to calculate radiative forcing and global warming potentials (K45). A portable FT-IR was used for the measurement of hexahydrophthalic anhydride in air at a manufacturing site (K46). Volatile organic compounds and some inorganic compounds were detected on-line using an FT-IR spectrometer as a continuous emission monitor (K47). IR spectroscopy and gas correlation techniques were used for the visualization of gas flows (K48). FT-IR was used for the determination of consumer exposure to solvents during paint stripping operations (K49). An algorithm was developed for quantitative analysis of the FT-IR spectrum of a chemical plume (K50). Several papers outlined the use of FT-IR spectroscopy for the analysis of emissions from the burning of coal (K51-K54). FTIR has also been used as a continuous emission monitor for stack gas at an oil refinery (K55) and incinerator (K56). In situ and extractive FT-IR techniques for the analysis of compounds from incineration of chlorinated hydrocarbons were discussed (K57). Quantitative analysis of the toxic gases produced during chemical quenching of JP-8 fuel fires was performed using FT-IR spectroscopy (K58). FT-IR spectroscopy and a chemometric technique (partial least squares) were investigated as a means to obtain the concentrations of compounds in the smoke from burning textiles (K59). Sampling techniques and FT-IR methods for analysis of nonmethane organic gases in automotive exhaust were presented (K60). The gases from aircraft engine exhaust were analyzed by an on-board FT-IR spectrometer (K61). An emission FT-IR technique was used to detect water, carbon dioxide, and carbon monoxide in aircraft engine exhaust (K62). Nitric oxide, nitrogen dioxide, and water were measured in aircraft engine exhaust with a tunable IR diode laser system (K63). FT-IR spectroscopy was used in a study of vehicle exhaust emissions from oxygenated fuel blends (K64). Four analyzers are normally used to test vehicle emissions for CO, CO2, NOx, and total hydrocarbons for the IM240 inspection test. The results from an FT-IR analyzer were compared to those of the four analyzers (K65). FT-IR was used in studying the catalytic conversion of NOx (K66). The use of IR spectrometry for the analysis of certain gases (such as ClO, NO, and HCl) in the upper atmosphere was 140R
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reviewed for the period from 1969 to 1992 (K67). Chlorine monoxide was detected in the lower stratosphere via FT-IR measurements (K68). Ground-based FT-IR was used in the determination of the concentration of ozone in the atmosphere (K69-K71). A passive remote IR sensing system for monitoring atmospheric pollution was discussed (K72). The CO column abundance in the atmosphere over Tokyo was measured by IR (K73). Column densities of various trace gases were obtained by high-resolution FT-IR solar absorption spectrometry (K74). Considerations for using IR to determine the distributions of nitric acid and nitric oxides in the Earth’s atmosphere were discussed (K75). The use of a ground-based FT-IR spectrometer as a remote monitoring device for pollutants such as CFCs was reported (K76). The influence of aerosols and cloud absorption on the FT-IR determination of atmospheric pollutants was studied (K77). MidIR measurements of the atmosphere above the South Pole yielded information about water vapor content, trace gases, temperature profiles, and aerosols (K78). Trace gases in the atmosphere (including HCl and ClONO2) were detected from a high-resolution FT-IR spectrometer operating from a stabilized balloon gondola (K79). A high-resolution FT-IR spectrometer carried on an aircraft and used for remote sensing of atmospheric emission was described (K80). The HBr profile in the stratosphere was measured via far-IR emission spectroscopy (K81). A review covered the remote sensing of Earth’s atmosphere from space via IR (K82). Another review discussed far-IR remote monitoring of the atmosphere (K83). An FT-IR that will be placed on a satellite (CESAR) and used to monitor trace gases in the atmosphere was described (K84). A review discussed the use of mid-IR tunable diode lasers for monitoring trace gases in the atmosphere and remote sensing of exhaust gases (K85). An airborne tunable diode laser IR spectrometer (FLAIR) was used in the measurement of trace gases in the troposphere (K86). NIR tunable diode laser systems that use fiber optics were described. The instruments can be used for stack monitoring (K87). An IR emission spectrometer carried on an aircraft was used to monitor a number of gases from wildfires in the western United States (K88). Methods for achieving background suppression to facilitate FT-IR monitoring of volatile organic compounds were discussed (K89). Fourier transform near-IR spectroscopy was used for remote monitoring of volatile organic compounds (K90). Remote sensing of smoke stack plumes was achieved with high-resolution FT-IR spectroscopy (K91, K92). The feasibility of remote measurement of HNO3 and SO2 in aircraft exhaust gases was investigated through computer modeling of the IR spectra of the exhaust plume (K93). Industrial fugitive emissions of hydrocarbons were measured by the FT-IR tracer method (FTM) (K94). A new remote optical fiber sensor for nearIR detection of CO2 was reported (K95). Near-IR vapor sensors were developed that depend on the detection of compounds adsorbed on thin-layer chromatography plates (K96). An in situ monitor for underground waste sites uses an FT-IR system and a fiber-optic reflectance probe (K97). A fiber-optic IR reflectance probe was also used in the remote detection of trichloroethylene in soil (K98). Band-pass digital filtering and linear discriminant analysis were applied to portions of the interferogram data from a passive FT-IR system in order to detect trichloroethylene vapor in the presence of other chemicals (K99). The reactions of
alumina powder with halomethanes were studied by in situ FTIR as part of an investigation of the impact of alumina from solidpropellant rocket motors on the chemistry of the stratosphere (K100). The application of open-path FT-IR at three Shell Oil sites was discussed (K101). An automated open-path FT-IR system was used to monitor volatile organics from a wastewater treatment plant (K102). The gases produced from controlled biomass fires were detected by open-path FT-IR at 0.12-cm-1 resolution (K103). The use of open-path near-IR tunable diode lasers for the detection of fugitive emissions was reported (K104, K105). Air pollutants in a petrochemical industrial park were measured with open-path FT-IR remote sensing techniques (K106, K107). Indoor tracer gas concentration profiles were obtained with an open-path FTIR spectrometer and computed tomography (K108). These two techniques were also used to obtain two-dimensional maps of air pollutants (K109). Open-path FT-IR analysis of emissions from volcanoes and extractive FT-IR analysis of gases from polluted groundwater were discussed in a study describing the use of FTIR for environmental monitoring (K110). Open-path FT-IR in combination with synthetic calibration was found to be useful for the analysis of smoke from biomass fires (K111). The effects of spectral resolution on open-path FT-IR measurements were investigated (K112-K114). The U.S. EPA has contracted the development of standardized procedures (document TO-16) for obtaining quantitative data from FT-IR remote sensors. The contents of these procedures were described (K115). Details were provided on methods for estimating emission rates from nonhomogeneous fugitive sources using open-path FT-IR (K116). The results of an open-path FT-IR field study of air pollutants by the API and U.S. EPA were presented (K117). Both FT-IR and UV systems were used at a Superfund site in an evaluation of open-path fenceline monitoring and emission rate estimation (K118). Open-path FT-IR and UV were also used to monitor volatile organics during excavation at a petroleum refining site (K119). Modeling techniques to estimate emissions from air pollution sources by open-path FT-IR were reported (K120). Quality assurance programs for open-path FT-IR air monitoring at 20 U.S. industrial plants and waste sites were reviewed (K121). A fence line FT-IR monitoring system around the perimeter of an industrial facility was described (K122). An exposure chamber was used in the evaluation of the accuracy of an open-path FT-IR spectrometer (K123). The use of open-path FT-IR for measurement of air pollutants in industry and agriculture was discussed (K124). The design of an open-path atmospheric monitor containing an acoustooptic tunable filter for emission spectroscopy and lasers for mid-IR and far-IR absorption spectroscopy was described (K125). The methodology used in open-path FT-IR monitoring of a process area was presented along with recommendations for improvement (K126). The results of open-path FT-IR measurements at a Kodak industrial complex and the Hanford site were reported (K127, K128). A paper detailed the use of a program to calculate open-path FT-IR reference spectra for temperatures at which no spectra are available (K129). A report was presented on the methods used in a training course in Taiwan on open-path FT-IR technology (K130). Calibration of an open-path FT-IR spectrometer via multipass cells was described (K131, K132).
CARBON AND CARBON COMPLEXES Carbon cluster anions, trapped in an Ar matrix, were studied spectroscopically. New bands found in the IR spectra were assigned to asymmetric stretching modes of the C3, C5, C7, and C9 anions (L1). The IR spectra of neutral linear carbon clusters were studied in Ne, Ar, and Kr matrixes. Thermal annealing and high-level ab initio and density functional theory calculations were used to locate unknown bands of C8 and C9 clusters (L2). The n7 stretching mode of the linear C9 carbon cluster has been observed at 1601.0 cm-1. Comparison to isotopic shifts and theoretical calculations confirm the assignment (L3). Two previously identified fundamentals, n4 of the linear C7 cluster, were confirmed using 13C isotopic shifts and theoretical calculations (L4). New assignments for the silent-mode vibrational frequencies in C60 are proposed that are consistent with the Raman and IR spectra, isotopically induced frequency shifts, and theoretical calculations (L5). The room-temperature IR and Raman spectra for the pressure-induced rhombohedral, tetragonal, and orthorhombic C60 polymers and the C60 photopolymer have been explored (L6-L8). Fluorinated C60 fullerenes were examined spectroscopically (L9). A quantitative IR method has been established for the determination of C60/C70 concentrations in mixtures (L10). The influence of the method of deposition on the atomic scale structure of amorphous hydrogenated carbon has been analyzed using IR spectroscopy and inelastic neutron spectroscopy (L11). The bonding configurations of hydrogen in hydrogenated amorphous carbon (a-C:H) has been studied using IR spectroscopy and thermal effusion experiments (L12). IR spectroscopy was used to examine thin solid films of hydrogenated amorphous carbon under conditions near decomposition (L13). Structural changes induced by nitrogen doping amorphous hydrogenated carbon films hacw been investigated using IR and photoluminescence spectroscopy (L14). An IR analysis of amorphous hydrogenated carbon films has been performed to determine the sp3/ sp2 ratio (L15). Infrared and Raman spectroscopies were used to characterize the structural changes that occurred in hydrogenated diamondlike carbon film upon implantation with heavy energetic ions (L16). The interactions of hydrogen and methyl radicals with diamond (C111) surfaces were examined using IR-visible sumfrequency vibrational spectroscopy (L17). The interactions between acetone and pure carbon surfaces and carbon surfaces doped with cations (Ni2+, Cu2+, Cr3+) were explored. The IR spectra indicate that acetone can be both physisorbed and chemisorbed on the pure carbon surfaces. Acetone can also be used to probe the surface for Lewis acidic sites (L18). The measurement of C13/C12 ratios in carbon samples converted to CO2 gas can be accomplish using IR spectroscopy (L19). Pressure broadening of the 2350-cm-1 band permitted isotope ratio differences of 0.02 at. % above the natural abundance of 1.11 at. % to be detected (L20). The far-IR spectra of carbon disulfide under high pressure in a diamond anvil cell did not reveal a solid-state phase transition. The intramolecular bonding weakens at high pressure and the intermolecular bonding increases at the pressures studied (L21). Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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The distribution of functional groups in coal macerals can be examined using reflectance IR microspectroscopy. The technique yielded information on the character of aliphatic chains of vitrinite and liptinite macerals from high-volatile bituminous coal and can be used to study the degree of oxidation and reactivity of vitrinite and semifusinite (L22). Specular reflectance IR microspectroscopy was also used to account for reflectance anomalies seen in the Brent coal series of the North Sea. The variations in the chemistries of the vitrinites and oxidation biased the reflectance measurements (L23). Self-deconvolution and curve-fitting of the IR spectra of coal varying in rank were used to gain additional information on structural changes that occur during coalification (L24). Chemical treatment modification of coal samples was followed using diffuse reflectance IR spectroscopy (L25). The weathering process in stockpiled coals, including zones where signs of high oxidation and self-ignition, were studied using IR spectroscopy (L26). The coal properties of volatile matter, fixed carbon, ash, carbon, hydrogen, and vitrinite reflectance could be successfully determined from models based on derivative diffuse reflectance IR spectroscopy (L27). Compressed infrared data from osculating polynomials gave slightly better correlations for these same properties of coal (L28). The middle oil fractions of high-temperature coal tar were examined and chemical components identified using gas chromatography/infrared spectroscopy (L29). Chemical changes that occurred during thermal decomposition of rockrose to produce char and activated carbon have been examined using IR spectroscopy (L30). IR spectroscopy has been used in a comprehensive program to elucidate the structure and reactivity of carbon black (L31). Multicomponent absorption kinetics of gases in activated carbon was studied by a batch absorber IR technique and compared to a model for predicting multicomponent dynamics in a differential adsorption bed system (L32). CHEMICAL REACTIONS/ORGANIC CHEMISTRY Hydrogen-Bonding Studies. Infrared studies of the hydration of di-, tri-, tetra-, and pentamethonium halides supported the formation of planar hydrate clusters (M1, M2). The hydrogenbonded complexes between N-methylsuccinimide and phenols were investigated (M3). The associative interactions of hydroperoxides to form hydrogen-bonded dimers and complexes with cycloalkanones were studied (M4). Hydrogen bonding in imidazolium salts was studied, and the implications for the structure and solvent properties of the ionic liquids were discussed (M5). The infrared spectra of associated molecules of N-methylacetamide were calculated and compared with experimental data (M6). The intra- and intermolecular H bonds between the H on the N and the ferrocenyl for N-methylferrocene aniline compounds were studied (M7). The FT-IR spectra of the H-bonded complexes between HCl and substituted pyridines, benzimidazole, purine, and 4-aminopyrimidine were investigated (M8). Crown ether complexes with urea and thiourea showed significant differences in their respective interactions (M9). The influence of hydrogen bonding in 3-hydroxyazabicyclo[2.2.2]octane pentachlorophenolate was described (M10). The geometry and complexing ability of 142R
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aminoquinolines in carbon tetrachloride solutions were examined (M11). Near-infrared was used to study the hydrogen bonding between thioacetamide and N,N-disubstituted benzamide derivatives in CCl4 (M12). The hydrogen-bonding influence on the molecular vibrational spectra of liquid methanol was studied by molecular dynamics simulation (M13). The IR bending vibrational band of water in aqueous haloethanol mixtures was studied as a measure of hydrogen-bonding strength (M14). FT-IR studies of hydrogen bonding between unsaturated esters and several alcohols were correlated with the enthalpy of hydrogen bond formation (M15). The infrared absorption spectra of acetone and methanol mixtures in a solid argon matrix showed H-bond interactions (M16). The integrated intensities of bent hydrogen bonds in o-dialkylaminomethyl phenols and deuterated analogues were measured (M17). An infrared study was done of intramolecularly hydrogen-bonded aromatic carbonyl-containing compounds in various solvents (M18). The hydrogen bonds in different crystal phases and melts were determined for a group of alcohols derived from 2,2-dimethylpropane (M19). Substituent effects on hydrogen bonding were measured for ortho-substituted nitrobenzenes and 2,4-dinitrobenzenes in chloroform and acetonitrile (M20). Complexes of five pyridines and nine pyridine N-oxides with 2,6-dichloro-4-nitrophenol were studied by infrared spectroscopy (M21). The far-infrared hydrogen bond vibration was studied as a function of the pKa of the donor or acceptor molecules for systems of complexes (M22). The self-assembling properties of pyridone and the structurebreaking effects of organic solvents were investigated (M23). The self-association of several N-urethanyl-L-amino acids in carbon tetrachloride was investigated by FT-IR (M24). A potassium salt of acetylenedicarboxylic acid was used as a model to study a strongly hydrogen-bonded system (M25). The hydrogen bond structure in benzoic acid solutions was investigated (M26). The influence of intramolecular hydrogen bonding on the structure and photoisomerization of urocanic acid derivatives was studied (M27). The hydrogen bond energies of crystalline carboxylic acid salts were determined (M28). Differences in the types of hydrogen bonding occurring in oxamic, malonamic, and succinamic acids in the solid state were investigated (M29, M30). Hydrogen bond structures of partially methylated p-tert-butylcalix[6]arenes were investigated in both solution and the solid state by FT-IR (M31). Infrared was used to characterize the crystal and molecular structure of new diketone enols designed to have known packing features (M32). The interaction by hydrogen bond formation of 1,1,1-trichloro-2-methyl-2-propanol with some ethers and acetone in CCl4 was investigated (M33). An infrared study was done in the region of the fundamental NH stretching vibration for six N-methylbenzamide-aromatic donor systems (M34). The infrared spectra of butyl halides dissolved in CCl4 and deuterated DMSO were investigated to determine the degree of hydrogen bonding occurring (M35). Intramolecular hydrogen bonding in 8-hydroxy-N,N-dimethyl-1naphthylamine was studied (M36). An FT-IR study of the proton polarizability and Fermi resonance effects as a function of temperature for hydrogen-bonded systems in Mannich bases of 2,2′-biphenol was done (M37). The temperature effects on hydrogen-bonded complexes of NH donors with proton acceptors
were studied (M38). Peak shifts in the infrared spectrum of benzoic acid crystals when compressed with methylated additives were investigated (M39). The equilibrium kinetics and vibrational energy transfer between the free acid Et3SiOH and its 1:1 hydrogen-bonded complex with acetonitrile were studied using picosecond time-resolved IR double-resonance spectroscopy (M40). Catalysis Studies. The infrared spectral methods of studying catalysis mechanisms were reviewed (M41). Acetonitrile adsorption onto hydroxylated zirconium dioxide and the mechanism of hydrolysis were studied by in situ FT-IR spectroscopy (M42). The hydration of acetonitrile toward acetamide by a silica-supported rhodium catalyst was investigated (M43). A study was made of the interconversion of isomeric unsaturated C4 nitriles over strongly basic Na/NaY (M44). The cracking of 1,3,5-triisopropylbenzene over deeply dealuminated Y zeolite was monitored by infrared spectroscopy (M45). The IR spectra of species formed from the adsorption of butene isomers on 12-tungstophosphoric acid showed primarily saturated C-C bonds (M46). The selective synthesis of 2-methylnaphthalene over a variety of zeolites was studied (M47). Infrared was used to characterize zinc-promoted H-ZSM-5 catalysts used for conversion of propane to aromatics (M48). A diffuse reflectance study was used to monitor the state of an H-mordenite catalyst during ethyl tert-butyl ether synthesis (M49). Methanol adsorption and dehydrogenation over stoichiometric and nonstoichiometric hydroxyapatite catalysts were characterized (M50). IR spectroscopic investigations were performed of the adsorption and surface reactions of CH3Cl over acidic, basic, and neutral zeolite catalysts (M51). Kinetic studies using in situ FT-IR characterized the mechanism of methanol synthesis over a zirconia-supported catalyst (M52). The H/D isotope-exchange reactions of adsorbed formate and methoxy species with D2 on zirconia were investigated (M53). The lowtemperature adsorption of methyl chloride and methyl iodide on silica-supported Pt catalysts was studied (M54). The conversion of methyl radicals to methanol and formaldehyde over vanadium oxide catalysts was confirmed by infrared spectroscopy (M55). Infrared spectroscopy and temperature-programmed desorption were used to investigate the chemistry of methyl iodide adsorbed on silica-supported copper nanoparticles (M56). The interaction of propene and butenes with a butene oxydehydrogenation catalyst was studied (M57). The decomposition of perfluorodiethyl ether on alumina was studied at 300 and 500 K (M58). An infrared study of chromium carbonyl complexes on silica-alumina showed ligand loss resulting in an active ethene polymerization catalyst (M59). Infrared studies of methylation of pyridine over zeolites were performed to understand the correlation between catalyst acidity and activity/selectivity for the reaction (M60). The reaction products from acetone decomposition on silver were identified by infrared spectroscopy (M61). Infrared was used to study the interaction of Ge(n-C4H9)4 with the surface of partially dehydroxylated alumina and silica-alumina (M62). The adsorption of 4,4′-bipyridine on the surfaces of silica, alumina, and titania was characterized by infrared spectroscopy (M63). The mechanisms in the oxidation and dissociative chemisorption of ethanol on platinum electrodes were characterized by infrared spectroscopy (M64). Infrared was used to study the adsorption and oxidation of propene on multiphase Bi, Mo, and Co catalysts (M65). The mechanisms of light alkane catalytic
oxidation and oxydehydrogenation for n-butane conversion over magnesium chromate and a magnesium-vanadate catalyst were characterized (M66). The interaction of propane and propene and of C1-3 oxygenates on cobalt oxide surfaces was studied (M67). In situ FT-IR spectroscopy was used to study oxygen-adsorbed species over SrF2/Nd2O3 (M68). The selective oxidation of nitrosobenzene to nitrobenzene by metal oxides was studied (M69). The adsorption, decomposition, and oxidation of methyl chloride on tin oxide catalysts were investigated (M70). Infrared spectroscopy was used in characterizing the bonding geometry of the carbonyl group during hydrogenation on Pd/SiO2 catalysts (M71). The hydrogenation of propyne on a range of supported palladium catalysts was investigated (M72). The hydrogenation and dehydrogenation of isobutene on platinum were monitored (M73). Several infrared studies have characterized the adsorption, reaction mechanism and products of NO and NOx reduction over a variety of catalysts (M74-M83). The products and mechanism of the gas-phase reaction of NO3 radicals with 2-butyne in purified air were investigated (M84). The chemical transformations of silica-supported iron rhodium complexes and the catalysis of propylene hydroformylation were investigated (M85). The interactions of supported RhO and Co- and Fe-promoted RhO with the silica surface were studied by infrared spectroscopy (M86). The adsorption of methanol and formaldehyde on rhodium-containing catalysts was studied (M87). The skeletal isomerization of butene by alumina-supported tungsten oxide catalysts was studied (M88). Infrared studies characterized the isomerization of methyl formate and ethyl formate chemisorbed on nickel (M89). Solvent/Matrix Effects. The conformational behavior of trimethyl phosphate was studied by infrared spectroscopy in the liquid phase and as 1% solutions in a wide range of solvents (M90). Rotational isomerism of desyl chloride in solvents of varied dielectric constants was examined by infrared spectroscopy (M91). Conformational isomerism and self-association of calixarene in nonpolar solution were studied by FT-IR (M92). The molecular states of alkali metal acetates in glacial acetic acid were investigated (M93). Solvation of lauric acid was investigated in different solvents by infrared and Raman (M94). Aqueous ATR FT-IR spectra of 24 aliphatic monocarboxylates were correlated with the pKa values of these acids (M95). An infrared study of R-haloacetic acids in solution was done (M96). The infrared spectra of cyclic and noncyclic ureas in solution were interpreted with respect to structures and interactions with a variety of solvents (M97). Using model spectra of toluene and cyclohexane and variable-temperature spectra of chlorocyclohexane, curve resolution of infrared profiles from nonconformational mixtures and conformational equilibria is discussed (M98). The tautomeric (enol-keto) and dimeric equilibria of 2-hydroxypyridines and 1,3-cyclohexanediones in chloroform and/or CCl4 solutions were studied by FT-IR (M99). The interactions in binary mixtures of acetone and chloroform-d were studied by infrared and Raman spectroscopies (M100). The dynamics of the carbonium ion solvated by molecular hydrogen was studied (M101, M102). The solvent-induced shift of the fundamental vibrational mode of the carbonyl group in 2-butanone was measured in 27 solvents (M103). Selfassociation of medium-chain alcohols in n-decane solutions was studied by the infrared absorption of the fundamental OH Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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stretching vibration (M104). An experimental and theoretical study of the structure and aggregation of diphenylguanidine in nonpolar and low-polarity solvents was performed (M105). Infrared measurements of N-acetyl- and N-benzoylaminopyridines in a set and in mixtures of solvents were discussed in terms of bulk and solute-solvent interactions (M106). The solvation of 2-hydroxypentylphosphonates was studied (M107). Liquid mixtures of pyridine with carbon disulfide, benzene, and carbon tetrachloride were studied in the far-infrared region as a function of concentration and temperature (M108). The solvation of amides and peptides was studied by infrared and NMR (M109). Solute/solvent interactions of 1-substituted 2-pyrrolidinones and related compounds in a variety of solvents were studied by infrared spectroscopy (M110). Infrared spectroscopy of the OH stretching vibrations of hydrogen-bonded tropolone complexes was discussed (M111). Tautomerism of thioguanine was studied using matrix isolation infrared spectroscopy (M112). The infrared spectra of some hydrogen halide salts of methamphetamine were observed to display significant variations dependent upon the alkali halide matrix in which the salt was dispersed for analysis (M113). Organic Reactions/Characterization. A review described the use of ab initio infrared spectra in the identification of highly reactive organic molecules and intermediates (M114). Changes occurring in the infrared spectrum of ethylene-CO alternating copolymer as a function of temperature were analyzed (M115). The reaction products generated by pulsed flash pyrolysis of 2-ethynyl-1,1,1-trimethyldisilane were characterized by matrix isolation IR spectroscopy (M116). Isomeric silylenes were generated by pulsed flash pyrolysis and identified by matrix isolation IR spectroscopy (M117). The methane elimination during silation of partially dehydroxylated alumina was studied (M118). The kinetics and products of the gas-phase reactions of silanes and siloxanes with hydroxyl radical and atomic chlorine were studied by FT-IR and mass spectrometry (M119). The highly substituted cyclohexane derivatives synthesized from the Michael-Michael aldol condensation of chalcones with cyanoacetylurea and cyanoacetylpiperidine were characterized by IR and NMR (M120). The interconversion of isomeric unsaturated C4 nitriles in the presence of butyllithium was investigated by means of FT-IR and UV-visible spectroscopy (M121). FT-IR spectroscopic studies were performed on the mechanisms of the halogen atom-initiated oxidation of haloacetaldehydes (M122). The products and mechanisms for the gas-phase reactions of the nitrate radical and haloethenes were studied (M123). The hydrothermolysis kinetics and pathways of guanidinium nitrate and urea in were described as examples of the use of IR spectroscopy for determining the rates and pathways of hydrolytic decomposition reactions of organic and inorganic compounds in aqueous media in conditions up to 400 °C and 350 atm (M124). Quantitative characterization of protolytic reactions of o,o′-dihydroxyphenylazonaphthyls using IR spectroscopy was described (M125). The reaction of ketenes in pyridine matrixes to form ketene--yridine ylides was observed by IR spectroscopy (M126). The decomposition products of ethylenediammonium dinitrate through hydrothermal reactions were studied (M127). The results of studies on the protonation of a series of sulfinamides using IR and NMR were reported (M128). 144R
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The ab initio MO method was used to study the decomposition of carbamic acid and its thio and sila derivatives (M129). Diffuse reflectance FT-IR was used to study two humic sodium salts and structural changes caused by heating (M130). The thermal decomposition of acetic anhydride was monitored by vacuum-UV absorption and IR emission (M131). The evolved products from the melting, vaporization, and thermal decomposition of alkyl- and arylureas were analyzed by IR spectroscopy (M132). The decomposition reaction of methyltrichlorosilane was investigated by in situ IR spectroscopy (M133). The analytical capacity of FTIR for the analysis of works of art was discussed (M134). The mineralization of cellulose and protein fibers was investigated using FT-IR microscopy (M135). Motor oil degradation was characterized by IR spectroscopy (M136). The stabilization of water-soluble surfactants at the air/water interface with gegenion complexation was studied by IR spectroscopy (M137). A Raman/IR spectroscopic study investigated the stoichiometry and conformation of the azacrown moiety in sodium complexes of azacrown ethers (M138). Near-infrared absorption was used to characterize and measure the association constants of the inclusion complexes between aromatic compounds and cyclodextrins (M139). IR spectroscopy was used in establishing the structure of complexes of phenols with compounds containing SOx groups (M140). The formation of complexes of picric acid with hexamethylbenzene, 2-iodoaniline, and 1-aminoanthracene was examined using FT-IR spectroscopy (M141). The interaction of 2-chloro-3,5-dinitropyridine with aniline and its derivatives and the structure of the formed complexes were studied using IR and electronic absorption spectroscopy (M142). Several 1:1 chloranilic acid-amine complexes were studied by IR, UV, and NMR (M143). The complex formation between o-cresol and propionitrile was investigated by FT-IR (M144). Complexes formed by phenols with 1,3,4,6,7,8-hexahydro-1-methyl2H-pyrimido[1,2-a]pyrimidine were studied as a function of the pKa of the phenols by FT-IR (M145). Infrared measurements of the kinetics and decomposition pathways of aqueous urea and guanidinium nitrate were described (M146). Infrared spectroscopic studies of photoinduced reactions of methyl radical in solid para-hydrogen were described (M147). The ultraviolet photolysis of acetyl and propionyl radicals was studied by infrared emission spectroscopy (M148). The composition of aerosol generated in the photooxidation of 1,3,5-trimethylbenzene was investigated in a smog chamber experiment using IR spectroscopy (M149). IR characterization of the UV photoinduced reactions of matrix-isolated 1-diazido-1-germacyclopent-3-ene was described (M150). The photochemistry of phenyl azides bearing 2-hydroxy and 2-amino groups was studied by matrix isolation spectroscopy (M151). FOOD AND AGRICULTURE Near-IR spectroscopy continues to be a focus of application in the food and agricultural industries. The proceedings from two conferences provide a good review of the varied applications (N1, N2). A review of infrared spectroscopy and microspectroscopy as related to food applications has been presented (N3). Application of photoacoustic spectroscopy in the near-IR and mid-IR regions to determination of the principal components of food has also been reviewed (N4).
Mid-IR and near-IR spectroscopy techniques have been applied in the dairy industry. By using the second derivative of the IR spectrum, simplified models could be developed to determine the fat and protein contents of raw milk (N5). Determination of fat, protein, casein, and noncasein in milk by near-IR (N6) is reported. Fermented milk composition was also examined using near-IR spectroscopy (N7). Mid-IR techniques have been adapted to determine microorganisms (especially Clostridium) in dairy (N8). The composition of cheese was examined using optothermal nearIR and mid-IR attenuated total reflectance (N9) and near-IR reflectance spectroscopy (N10). The examination of sugars for composition and quantitation using mid-IR and near-IR has been reported. A multivariate analysis of the infrared spectra of biological samples allows for the quantitation of a mixture of sucrose, fructose, and glucose (N11). The theoretical recoverable sugar (TRS) can be predicted from near-IR spectra and can be used to assess the quality of cane and beet sugar sources (N12). Sucrose can be determined in raw sugar cane juices using spectral data from mid-IR attenuated total reflectance (N13). The thermal degradation of sugar cane bagasse through to carbonization has been studied using mid-IR spectroscopy (N14). Sugar refinery streams can be analyzed using near-IR spectroscopy (N15, N16). Edible oils and fats have been analyzed using IR spectroscopies. A review of the application of mid-IR to edible oil analysis stresses key elements associated with developing suitable fat and oil analysis (N17). IR spectroscopy is compared to chromatographic techniques for the determination of trans fatty acids in oils and fats (N18-N20). Supercritical fluid extraction of oils in food samples coupled to a high-pressure flow cell has been used to monitor the vinylic C-H band to determine the amount of unsaturated fat (N21). Near-IR spectroscopy is demonstrated for determination of palmitic, oleic, and linoleic acids in edible oils (N22). Classification of edible oils and fats with regard to their origin can be accomplished using mid-IR spectroscopy (N23). A mid-IR spectroscopic technique for determining the solid fat index of oils and fats was developed (N24). Fruit, fruit juices, and vegetables have received the attention of mid-IR and near-IR spectroscopies. Determination of sugars and acid in a variety of fruit juices has been accomplished (N25N28). Sesquiterpene hydrocarbons in citrus essential oils have been identified using cryofocusing GC/IR (N29). Adulteration of raspberry purees can be detected using mid-IR spectroscopy and attenuated total reflectance sampling (N30). A nondestructive method for determination of soluble solids in tomatoes based on near-IR spectroscopy has been demonstrated (N31). The growth period of Japanese pear fruit was monitored using the constituent sugar concentrations (N32). Biochemical changes in peaches associated with ripening during storage were followed using midIR (N33). Identification and detection of adulteration of coffees using both mid-IR and near-IR spectroscopy have been reported. DRIFT and ATR sampling techniques are suggested as alternatives to wet chemical methods (N34, N35). Partial success was demonstrated in using near-IR to discriminate between coffees prepared from several different beans (N36). The components of sausage products were simultaneously determined using near-IR transmission with precision as good as
reference methods (N37). Near-IR spectroscopy can also be applied to the analysis of oil and moisture (N38) and fat content of salmon (N39). The prediction of total dietary fiber in cereal and grain products (N40) and the effect of residual moisture on total dietary fiber in cereals (N41) have been examined using near-IR reflectance spectroscopy. Infrared microspectroscopy has been used to elucidate the microstructural details of phase-separated polysaccharide-protein mixtures (N42). Near-IR reflectance spectroscopy can provide a nondestructive method to predict the solubility and digestibility of protein heated under high pressure (N43). Determination of heme and nonheme iron in raw muscle meats is possible using near-IR spectroscopy (N44). Pressure-induced changes in food components measured using a diamond anvil cell and mid-IR spectroscopy were compared to temperature-induced gel formation (N45). The adsorption of triacylglycerol and oelic acid on synthetic magnesium silicate was studied using diffuse reflectance FT-IR spectroscopy and compared to magnesium silicates used to treat degraded frying oil (N46). It is possible to perform starch content determination on digestive samples using near-IR spectroscopy (N47). The temperature effects and calibration methods have been studied to demonstrate the feasibility of using mid-IR spectroscopy for determination of major compounds of alcoholic fermentation (N48). The ability to differentiate meat speciation, the detection of frozen or thawed meat, and semiquantitative analysis of meat mixtures using mid-IR ATR have been demonstrated (N49). NearIR is also suggested as a technique for differentiating frozen and unfrozen beef (N50). The phospholipid content of intramuscular fat can be determined using the band between 1282 and 1020 cm -1 (N51). Polarized IR microspectroscopy can be used to assess the orientation of the mineral and matrix components of calcified tissue (N52). Near-IR spectroscopy has been used to screen the crude glycinin fraction and the effects of growing temperature and genotype on this fraction (N53). The effects of bound water on the mid-IR spectrum of glycinin was also studied (N54). The ruminal protein content in roasted soybeans can be estimated from the near-IR spectrum (N55). Near-IR spectroscopy can be used to quantitate moisture, protein, and starch in buckwheat flours but failed to correlate with the amylose and tannin content (N56). Several quality characteristics in rice by analysis of whole-grain milled samples can be measured using near-IR reflectance spectroscopy (N57). Determination of forage composition was not improved by using models based on a combination of both mid-IR and near-IR spectra over models based on just a single spectral range (N58). The value of Leucaena, a fast-growing tree used in the tropics for forage, can be evaluated using near-IR spectroscopy with differences observed between species, varieties, and hybrids (N59). The prediction of energy value of compound feeds for swine and ruminants based on near-IR spectroscopy is slightly better than other analytical methods (N60). Partial success in determining the composition of biomass feedstock has been accomplished using near-IR spectroscopy (N61). Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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Near-IR spectroscopy can be used as a rapid-scanning technique for the determination of chemical compositions of plantation eucalypti woods (N62). Residues and extracts from eucalyptus wood have been characterized by IR spectroscopy, UV spectroscopy, and HPLC (N63). It is possible to determine the resistance of sugarcane to sugarcane borer infestation using predictive models based on the near-IR spectrum of stalk surface wax (N64). External and internal insect infestation in stored wheat grain could be detected using near-IR reflectance spectroscopy (N65). Mid-IR spectroscopy has shown that significant differences may exist within the plasma membrane ATPase of corn roots (N66). A sensor based on a polymer-coated attenuated total reflectance element of a silver halide optical fiber and mid-IR spectroscopy has achieved a 2 ppm limit of detection for atrazine and alachlor in water (N67). The use of infrared techniques applied to organic and inorganic soil materials has been reviewed (N68). BIOCHEMISTRY To determine the effects of age on bone quality, human bone tissue taken from adult subjects deceased from violent death was analyzed by means of FT-IR in the diffuse reflectance mode (O1). FT-IR and FT-Raman spectra of human brain tissue are presented in this article (O2). This paper describes a nondispersive IR spectrometer for the measurement of the 13CO2/12CO2-ratio in breath samples (O3). Untreated and bleached hair samples were analyzed by FT-IR spectroscopy for cysteic acid and cysteine S-thiosulfate using different data manipulations and various sampling techniques (O4). Absorption spectra of human teeth sections were measured by FT-IR to identify absorption peaks for amides I, II, and III, carbonate, and phosphate (O5). To establish age-related lipid composition-membrane structure relationships, the hydrocarbon chain structure of lipid membranes from the human lens cortex and nucleus was examined by infrared and near-infrared spectroscopies (O6). The feasibility of obtaining reproducible spectra of skin oils from individuals with a very simple, noninvasive technique is reported (O7). Direct vapor generation FT-IR spectrometry is a new procedure proposed for a direct determination of ethanol in plasma and whole blood (O8). The secondary structure of myelin basic protein in reconstituted central nervous system myelin was studied FT-IR spectroscopy (O9). A new method of IR spectroscopic imaging is described and applied to the instantaneous, noninvasive mapping of the molecular constituents of unprocessed brain tissue (O10). A simple and rapid method for the analysis of poly(ethylene glycol)400 (PEG-400) in human urine is described using FT-IR spectrometry (O11). Mid- and near-IR spectra of viable and clipped human finger nails are presented (O12). Toluene and a mixture of the isomeric xylenes are common organic solvents that have been implicated in false ethanol results produced by older models of the Intoxilyzer 5000, a breath alcohol analyzer that uses IR spectrophotometry to quantitate ethanol in breath samples (O13). This review with 87 references is of experiments in which the photoreactions of the visual pigments rhodopsin and octopus rhodopsin were investigated by FT-IR spectroscopy (O14). This paper reviews a study to analyze the IR spectra of a liquidsimulating simulating food and an artificial saliva following exposure to resin composites (O15). 146R
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This symposium report with three references discusses the molecular structure of penicillin transition metal complexes (O16). This paper describes the interference of volatile anesthetics with infrared analysis of carbon dioxide and nitrous oxide tested in the Draeger Cicero EM using sevoflurane (O17). From the two wagging frequencies of the para amino group identified by IR and laser Raman spectroscopy in the local anesthetic benzocaine, the inversion barrier height and optimum inversion angle of this group were calculated and reported (O18). The interaction of calf thymus DNA with aspirin is investigated in aqueous solution, and FT-IR and laser Raman difference are used to determine drug binding sites, sequence preference, and DNA secondary structure, as well as the structural variations of aspirin-DNA complexes in aqueous solution (O19). This paper discusses in situ FT-IR and calorimetric studies of the preparation of a pharmaceutical intermediate (O20). Raman and FT-IR were used to analyze the interaction of the antibiotic lasalocid with DPPC membranes (O21). The mechanism of action of Timolor, used in the treatment of ocular hypertension in glaucoma, was studied using FT-IR spectroscopy (O22). The equilibria and structures of some azobarbiturate and benzylidene barbituate compounds were investigated based on different spectral and pH-metric methods (O23). This work presents FT-IR spectra of tetracycline and ampicillin, the major drugs used for the treatment of fatal bacillary and coccal infections (O24). FT-IR, along with DCS, has been used to study the interaction between a new antineoplastic drug and diastearoylphosphatidylcholine bilayers (O25). FT-IR spectroscopy has been applied to the investigation of synovial fluids aspirated from arthritic joints (O26). Glycogen levels in the tissue samples obtained from carcinomas and normal sections of the human lungs were studied by measuring the IR band intensities due to glycogen (O27). This review with 44 references has been written on the use of IR spectroscopy for diagnosis and determination of prognosis of malignant neoplasia such as breast and endometrial carcinomas (O28). This paper describes the analysis of urinary calculi by infrared spectroscopy (O29). Tumor progression to the metastatic state involves structural modifications in DNA markedly different from those associated with primary tumor formation. These modifications alter vibrational and rotational motion and are discussed in this article (O30). FT-IR microscpectroscopy, combined with principal component analysis, was applied in the study of exfoliated cervical cells to investigate the techniques feasibility as a biodiagnostic tool for cervical cancer (O31). Newly developed FT-IR spectroscopic analysis techniques were applied to the diagnosis of adulthood disease and to reveal the role of unsaturated fatty acids in neuronal function (O32). Determination of whewellite, uric acid, weddellite, dahllite, and struvite in their mixtures was studied by X-ray diffraction and IR spectroscopy (O33). The IR spectra of organic constituents of urine from cancerous bladders of some patients were recorded and classified (O34). The secondary structure and the thermal stability of human liver and heart fatty acid-binding proteins were analyzed, in the absence and in the presence of oleic acid, by FT-IR spectroscopy (O35). The authors determined the structural changes in the bladder carcinoma cell line J82-NVB induced by navelbine using FT-IR spectroscopy (O36). The anticoagulant effect of tungstophosphoric acid salt was studied by IR spectroscopy (O37). FT-IR spectra of 75
biopsies from 55 cases of breast carcinoma were studied in comparison with histomorphometry and were found to be very different from the spectra of normal tissues (O38). The transmission IR spectra of exfoliated endocervical mucin-producing columnar epithelial cells and the ATR IR spectra of the singlecolumnar cell layer on the endocervical tissues has been measured and compared with the corresponding IR spectra of the ectocervical squamous cells and squamous epithelium (O39). The authors report the conformation of intersubunit region from three serotypes of influenza A virus and the MAP-1 peptide, with and without the fusion peptide, as revealed by comparative CD and FT-IR spectroscopy measurements (O40). FT-IR and laser Raman difference spectroscopic techniques were used to establish correlations between spectral modifications and drug binding mode, sequence specificity, DNA melting, and conformational changes, as well as structural variations of calf thymus drug-DNA complexes in aqueous solution (O41). The secondary structure of P2 protein, isolated from bovine peripheral nervous system myelin, in reconstituted myelin was studied using FT-IR spectroscopy (O42). Unoriented films of calf thymus Na DNA were prepared and studied by Raman and IR spectroscopy (O43). FT-IR spectroscopy, along with X-ray diffraction and electron microscopy, was used to study apatite crystals isolated from chicken and bovine calcified cartilage (O44). This article describes the spectroscopic analysis of the FT-IR spectra of pig citrate synthase using the factor analysis method (O45). Aqueous dispersions of dipalmitoyl phosphatidylcholine, calf lung surfactant, and an organic solvent extract of calf surfactant were examined by FT-IR spectroscopy in the presence and absence of calcium (O46). This paper discusses the possibility of detecting in a semiquantitative manner alterations in the collagen content of heart tissue following myocardial infarction (O47). Infrared was used to study the effects of pH and KCl on the conformations of creatine kinase from rabbit muscle (O48). The authors apply high-fidelity FT-IR imaging to noninvasively generate image contrast in sections of monkey brain tissue and to relate these data to specific lipid and protein fractions (O49). The interaction of diethylstilbestrol with calf thymus DNA was investigated with FT-IR and Raman spectroscopy (O50). The interaction of calf thymus DNA was studied with Al and Ga cations using FT-IR spectroscopy (O51). FT-IR spectroscopy was used to investigate the secondary structure of boar sperm proacrosin to determine structural changes following protein autoactivation to β-acrosin and to study the effect of suramin binding on protein secondary structure (O52). FT-IR was used to study the conformational differences of ovine and human corticotropin releasing hormone (O53). FT-IR was used to obtain conformational data on the monomeric form of insulin, which is believed to be the physiologically active form of the hormone (O54). The secondary structure of human fibrin from normal donors and from bovine and suilline plasma was studied by FT-IR and a quantitative analysis of its secondary structure was suggested (O55). FT-IR spectroscopy combined with a resolution enhancement technique has been used to characterize pressure-induced structural changes in bovine pancreatic trypsin inhibitor (O56). The goal of this work was to develop a portable and rapid laserbased air sampler for detection of specific chemical contraband and to compile a spectral database in both the near- and mid-IR
of sufficiently high quality to be useful for gas-phase spectroscopic identification of chemical contraband (O57). A review with 13 references has been written on technique, drug distribution and sampling homogeneity for drug hair analysis (O58). FT-IR was used to survey and compare heroin seized throughout Israel in 1992 to detect salt forms and additives and compare the powders for intelligence and investigation purposes (O59). A review has been written on the use of IR spectrometry in the analysis of narcotics (O60). Preliminary investigations of solvent and temperature effects upon the IR spectra of organophosphorus pesticides were carried out and are discussed in this article (O61). This article discusses the use of IR spectrometry to determine the configurations of water molecules absorbed in isolated plant cuticles (O62). The authors discuss FT-IR and Raman spectroscopic evidence for the incorporation of cinnamaldehydes into the lignin of transgenic tobacco plants with reduced expression of cinnamyl alcohol dehydrogenase (O63). The IR absorption characteristics of a highly alkaline soil and its derivatives were studied, and efforts were made to detect polluting metals in the soil by studying the characteristics of their IR curves (O64). This article discusses a FT-IR investigation of the structural differences between two lipid binding proteins extracted from plants (O65). Eleven actinomycete melanins from Brazilian soils were characterized by IR analysis (O66). This paper focuses on the increasing use of FT-IR spectroscopy for the analysis of biomacromolecules (O67). The effect of temperature on the secondary structure of β-lactoglobulin was studied by FT-IR (O68). The polymorphic phase behavior of a homologous series of saturated 1,2-diacylphosphatidylglycerols was studied by FT-IR, DSC, and NMR (O69). The secondary structure of apolipoprotein B-100 in low-density lipoprotein subfractions was analyzed by FT-IR spectroscopy (O70). FT-IR difference spectroscopy with self-deconvolution and secondderivative methods as well as curve-fitting procedures are applied to the interaction of Al and Ga cations with proteins of the photosystem II-enriched membranes in order to determine the cation binding mode, the protein conformational changes, and the structural properties of metal-protein complexes (O71). The FTIR spectra of adenosine in the polycrystalline state were recorded as part of a series of normal coordinate analyses of nucleic acid components and their analogues (O72). A review has been written with 20 references on bioorganometallic chemistry in receptorology and analysis (O73). FT-IR and molecular modeling have been used to characterize the interaction of Ca2+ with hydroxy and non-hydroxy fatty acid species of cerebroside sulfate (O74). FT-IR spectroscopy has been used to determine the cation content of alginate thin films (O75). The FT-IR spectrum of the oxygen-evolving center was analyzed by using spinach PSII membranes perturbed in various ways such as calcium depletion, chloride depletion, H-D exchange, and 15N-labeling (O76). Comparison of the effects of amikacin and kanamycins A and B on dimyristoylphosphatidylglycerol bilayers was investigated by FT-IR spectroscopy (O77). The QA and the QB binding sites of Rhodobacter sphaeroides R26 reaction centers have been investigated by FT-IR spectroscopy (O78). A review with many references has been written covering applications of the separation and characterization of peptides and proteins by liquid chromaAnalytical Chemistry, Vol. 70, No. 12, June 15, 1998
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tography, mass spectrometry, FT-IR spectroscopy, CD, and NMR (O79). A review with 30 references has been written on the potentially powerful technique for determining the interaction configurations of water molecules in macromolecular systems (O80). The aim of this study was to analyze the Raman and IR spectra of eight common mammalian bile acids in order to identify intermolecular interactions between hydroxyl and carbonyl groups (O81). An infrared spectroscopic study was conducted on the conformational fluctuation and ion permeation of lipid bilayers doped with azobenzene derivative (O82). The reconstitution of the retinal-containing protein bacteriorhodopsin from the apoprotein and retinal has been studied by FT-IR difference spectroscopy (O83). This article focuses on the recent advances in IR spectroscopy that have made it possible to study structural and dynamic properties of biomembranes and model systems at the molecular level by spectral analysis (O84). Conformational studies of the cyclic L,D-lipopeptide surfactin were investigated by FT-IR spectroscopy (O85). Structural changes of R-lactalbumin in response to pH, ionic strength, sugars, and heat treatment were investigated by DSC and FT-IR spectroscopy (O86). FT-IR spectroscopy was used to characterize the stretching vibrations of the ester carbonyl groups and the amide I vibration of the amide group of N-acylphosphatidylethanolamine bilayers (O87). FT-IR spectroscopy of dry, multilayer films has been used to study γ radiation and UV-C light-induced lipid peroxidation in 1,2dilinoleoyl-sn-glycero-3-phosphocholine liposomes (O88). The secondary structures of two forms of Saccharomyces cerevisiae palsma membrane H+-ATPase were examined by FT-IR spectroscopy (O89). The vibrational modes of photoactive yellow protein and its photoproduct were studied by FT-IR spectroscopy (O90). FT-IR spectroscopy was used to identify the molecular sites in vesicles constituted of phosphatidylglycerol (PGV) and photosystem II (PSII) that determine the formation of the PSII-PGV complex and the sites affected by Mg(II) (O91). The kinetic behavior of human serum albumin adsorbed on a reversed-phase support was studied by FT-IR spectroscopy and chromatographic methods (O92). The results of Raman and IR spectroscopic investigations of the vibrational model of dimethyl phosphorothioate anion are reported (O93). This review with 32 references presents different techniques of FT-IR spectroscopy to investigate microorganisms in biofilms (O94). This review has many references and summarizes the main conformation-sensitive regions of phospholipid IR spectra and details three recent applications of new FT-IR methods that provide quantitative information about phospholipid microphase separation and acyl chain conformation (O95). Two computer programs were designed for helping in library handling and microbial identification by means of their IR spectra (O96). The hydration of ω-gliadins and partially deamidated and esterified ω-gliadins was studied by FT-IR spectroscopy (O97). Results obtained by FT-IR spectroscopy on the influence of Ca2+ binding on the secondary structure of calsequestrin are reported (O98). FT-IR spectra were reviewed for glycine oligomers and polyglycine (O99). The conformational variability of the basic subdomain of c-Jun was assessed through the study of the secondary structure of its N-terminal peptide and C-terminal peptide fragments using FT-IR spectroscopy (O100). FT-IR spectroscopy using principal component analysis and principal component regression were used for the determination of K+ ions 148R
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in biological solutions by investigating interactions between the cation and sucrose molecules (O101). The secondary structure of native D-glyceraldehyde-3-phosphate dehydrogenase was compared with its partially folded intermediate and aggregated states obtained during guanidine hydrochloride denaturation using transmission FT-IR and micro-FT-IR measurements (O102). Environmental chemicals are known to induce a higher degree of hydroxyl radical-mediated damage in DNA. FT-IR and principal components analysis were used to test the hypothesis that this exposure leads to new forms of DNA (O103). FT-IR spectroscopy was applied to cytochrome P 450 to analyze the protein secondary structure (O104). FT-IR spectra have been obtained from solid egg white lysozyme (O105). An IR spectroscopic study has been conducted on the structure and phase behavior of long-chain diacylphosphatidylcholines in the gel state (O106). Pilot experiments were performed to analyze the potential of FT-IR spectroscopy for classification and identification of actinomycetes (O107). The author has recently reported the use of a combination of multidimensional statistical analysis and FT-IR spectroscopy for the quantitative determination of sugars in a biological sample (O108). A spectroscopic study was conducted on polymer/protein interactions in composite films (O109). FT-IR studies have been carried out to investigate the secondary structure and thermal stability of hen egg white avidin and its complexes with biotin and with a biotinylated lipid derivative (O110). A review with 32 references has been written on the use of FT-IR spectroscopy in determining analytes in blood and characterization of disease states (O111). Differences in conformational dynamics of bovine pancreatic RNase A and RNase S were investigated using 1H-2H exchange in conjunction with FT-IR spectroscopy (O112). The secondary structure of the black-eyed pea trypsin/chymotrypsin inhibitor was analyzed from the FT-IR spectrum of the protein in D2O solution (O113). The conformation and stability of recombinant tetrameric human tryrosine hydroxylase isoenzyme 1 was studied by IR spectroscopy (O114). Highly purified adenylate kinase was characterized by FT-IR spectroscopy. Analysis of the FT-IR spectra and estimation of secondary structure revealed a global protein structure similar to that of other adenylate kinase enzymes (O115). This paper reports the spectroscopic characterization of two de novo peptides (O116). The effect of H/D exchange on a FT-IR difference spectrum between the S1 and S2 states of the oxygen-evolving center in photosystem II has been investigated (O117). A review with many references has been written discussing the main conformation-sensitive regions of phospholipid FT-IR methods that provide quantitative information about phospholipid microphase separation and acyl chain conformation (O118). A three-component model for the lipid barrier of the stratum corneum consisting of ceramide III, cholesterol, and perdeuterated palmitic acid has been characterized by FT-IR spectroscopy (O119). FT-IR spectroscopy demonstrates that lyophlization alters the secondary structure of recombinant human growth hormone (O120). Thermal denaturation processes of chicken egg white ovomacroglobulin and human serum R-2macroglobulin with and without chymotrypsin have been studied (O121). An FT-IR spectroscopic study was conducted to determine protonation, conformation, and hydrogen bonding of nicotinamide adenine dinucleotide (O122). Grouping of Spherobacter mitis strains grown on two different growth media was made by
FT-IR spectroscopy (O123). Effects of R-tocopherol and R-tocopheryl acetate on dipalmitoylphosphatidylcholine multilayers have been investigated by FT-IR and Raman spectroscopies (O124). Changes in conformation of oligosaccharides, and the constraints imposed by hydrogen bonding with the solvent, were studied by means of FT-IR and Raman (O125). A review with many references has been written outlining four approaches, FT-IR, Raman, CD and calorimetry, to probing protein and peptide properties (O126). This paper describes a spectrophotometer dedicated to the polarization modulation IR reflection-absorption spectroscopic study of monolayers spread at the air/water interface (O127). FT-IR measurement disclosed formation of a thiol ester bond between a cysteine of arylmalonate decarboxylase and an active site-directed inhibitor strongly suggesting that the enzyme initially activates the substrates in a similar mechanism (O128). The thermotropic phase behavior of aqueous dispersions of dipalmitoylphosphatidylcholine and its analogues was examined by DSC, and the organization of these molecules in those hydrated bilayers was studied by FT-IR spectroscopy (O129). This review with 83 references was written on the properties of lipid vesicles studied by FT-IR spectroscopy (O130). Examination of L-tyrosine spectra by various IR techniques allows some conclusions on the molecular interactions in the examined systems (O131). A review with 23 references has been written on the relative advantages and disadvantages of various spectroscopic techniques for identifying and measuring concentrations of multicomponent mixtures (O132). The authors discuss infrared spectroscopic studies of vancomycin and its interactions with N-acetyl-D-Ala-D-Ala and N,N′diacetyl-L-Lys-D-Ala-D-Ala (O133). This paper discusses spectroscopic characterization of the interferon-γ and analogue II in hydroorganic solution or adsorbed on an hydrophobic chromatographic support (O134). The secondary structures of staphylococcal nuclease have been assigned and semiquantitatively estimated from the deconvoluted FT-IR spectrum (O135). FT-IR spectroscopy has been used to investigate the structure and temperature stability of the acetylcholinesterase from Torpedo californica (O136). The cyanide complex of iron(II) myoglobin was studied by FT-IR spectroscopy and compared with complexes of microperoxidase and hemoglobin (O137). FT-IR spectroscopy has been used to investigate the structural properties of the channel-forming integral membrane protein present in phospholipid vesicles suspended in aqueous media (O138). The plant growth hormone auxin and its natural analogue, as well as their synthetic congeners, were studied by FT-IR spectroscopy (O139). FT-IR spectroscopy was used to investigate the local structure around the chromophore of rhodopsin and its change upon photoisomerization (O140). Chemical changes in the medium, induced by the fermentative species Lactobacillus plantarum and Lactobacillus brevis and by the enzymic action of a proteolytic, spoilage species, were analyzed using FT-IR spectroscopy (O141). A complete set of vibrational spectra obtained from several spectroscopic techniques has been used in order to assign the vibrational modes of uracil on the basis of an ab initio scaled quantum mechanical force field (O142). FT-IR has been used to analyze protein conformational stability on surfaces (O143). Structural differences between two genetic variants of bovine β-lactoglobulins in aqueous solutions were characterized using FT-IR and CD spectroscopies (O144). The FT-IR spectra of
several coiled coil proteins have been shown to possess unusual features in the amide I′ region (O145). The authors of this paper used FT-IR to measure secondary structures of isolated domains of types III and IV intermediate filament proteins and of the solution tetramers and the filaments formed by type III intermediate filament proteins (O146). A review with 142 references has been written on the determination of protein secondary structure, IR spectrometry measurement of H-D exchange in proteins, and probing protein structure at the level of individual chemical groups (O147). This article discusses the use of 13C-labeled molecules in the conformational analysis of proteins by FT-IR spectroscopy (O148). FT-IR spectroscopy has been used to compare S-cis and S-trans conformations of planar dithiooxamides (O149). A review with 20 references has been written on an IR spectroscopy-based multicomponent assay of biofluids such as whole blood, urine, and synovial fluid (O150). The redox reactions of the cytochrome c oxidase from Paracoccus denitrificans were investigated in a thinlayer cell designed for the combination of electrochemistry under anaerobic conditions with UV-visible and IR spectroscopies (O151). Hydrated sites in biogenic amorphous calcium phosphates have been studied by infrared spectroscopy (O152). Similarities in the architecture of the active sites of Ni hydrogenases and Fe hydrogenases have been detected by means of infrared spectroscopy (O153). The adsorption of a membrane protein of flagellar FliF and its derivatives onto chemically modified surfaces has been studied by FT-IR spectroscopy (O154). FT-IR spectra of a dilute solution of N-acetyl-Pro-Leu-Gly-NH2 have been measured and reported (O155). Changes in the secondary structure of adsorbed IgG and F(ab′)2 was studied by FT-IR spectroscopy (O156). An unusually high hydrogen-deuterium exchange of the CHIP28 protein (aquaporin) from red blood cells was observed by FT-IR spectroscopy (O157). Cyanide binding to the heme-copper binuclear center of bo-type ubiquinol oxidase from Escherichia coli was investigated with FT-IR and EPR spectroscopies (O158). A combination of CD and IR spectroscopy helps to build a molecular picture of the thermal denaturation and conformational changes of β-lactoglobulin (O159). An FT-IR spectroscopy study was conducted to determine conformational order of phospholipids incorporated into human erythrocytes (O160). A new method for the determination of R-amylase activity in aqueous solutions and human serum by FT-IR spectroscopy is proposed (O161). The authors of this paper synthesized and studied by FT-IR spectroscopy monosalts of diamides as models for the active site of aspartic proteinases (O162). In situ and ex situ structural analysis of phospholipid-supported planar bilayers was studied using infrared spectroscopy and atomic force microscopy (O163). A comparative study using IR spectroscopy was conducted to determine the interaction of two lipid binding proteins with membrane lipids (O164). FT-IR and FT-Raman spectra of 5′-dAMP were determined and a normal coordinate analysis of the mononucleotide was carried out (O165). The aim of this study is to demonstrate the reliability of the use of FT-IR spectroscopy to monitor conformational changes when a protein is adsorbed under chromatographic conditions on silica material (O166). Variants of recombinant staphylokinase were investigated by FT-IR spectroscopy for a correlation between thermal stability and structural features of staphylokinase and the selected mutants (O167). FT-IR spectroscopy studies of lipoxygenase showed Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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changes in the amide I′ band which correlate to structural changes of the enzyme (O168). Free amphipathic peptides and peptides bound to dimyristoylphosphatidylcholine were studied directly at the air/water interface using polarization modulation IR reflection absorption spectroscopy (O169). The possibility of using FT-IR spectroscopy to detect subtle differences in the molecular dynamics in biomembranes is discussed (O170). This paper reports the spectroscopic characterization of two de novo peptides (O171). Mid-IR pump-probe experiments were used to study vibrational relaxation of CO bound to synthetic heme and porphyrin complexes with different metal atoms and different promixal ligands (O172). Mitochondrial F1 ATPase from beef heart was treated with different buffers to modulate the nucleotide content of the enzyme and then analyzed by FT-IR spectroscopy (O173). The interaction between superoxide dismutase and dipalmitoylphosphatidylglycerol bilayer was studied with FT-IR spectroscopy (O174). The structure, water absorbability, and mechanical properties of the blend membranes of regenerated silk fibroin in poly(vinyl alcohol) were studied by FT-IR spectroscopy (O175). The detection and structure of water molecules inserted in biomembranes by FT-IR spectroscopy is discussed and an example is given of the study of the structures of the two main types of water molecules that are found in leaf cuticles (O176). The use of isotope-enhanced FT-IR spectroscopy and ESR spin-labeling to examine the conformation of the 23-residue peptide of the N-terminal fusion peptide of the HIV-1 gp41 protein were examined (O177). FT-IR spectroscopy was used to study the effects of Triton X-100 treatment on the purple membrane of Halobacterium halobium ET1001 (O178). FT-IR and optical spectroscopy have been used to characterize the binding of NO to the oxidized form of the heme cd1 nitrite reductase from Pseudomonas stutzeri JM300 (O179). FT-IR spectroscopy was used to study thermally induced H exchange in RNase A, RNase T1, and various RNase T1 mutants in relation to the melting transition of the protein (O180). FT-IR and surface plasmon resonance spectroscopy were used to study the interaction of C-reactive protein from Limulus polyphemus with phosphorylcholine groups both in aqueous solution and immobilized on solid supports (O181). FT-IR spectroscopy is shown to be a rapid method for the identification of Candida at the species level (O182). FT-IR has been used to study the thermotropic phase behavior of mixed vesicles made up by lipopolysaccharides and phospholipids (O183). The FT-IR difference spectra of 4-amidinophenylmethanesulfonyl-thrombin and -trypsin complexes are discussed (O184). The interaction of cisplatin and its analogues with the phospholipid molecules of human erythrocyte membranes was studied using IR and NMR methods (O185). The authors discuss a method for the classification of biological FTIR spectra prior to quantitative analysis (O186). The secondary structure of calmodulin from Brassica campestris pollen was studied by FT-IR spectroscopy and the CD method (O187). The application of IR to an analysis of yeast cytochrome oxidase is discussed (O188). This review with four references discusses a study of enzyme-ligand binding of chymotrypsin with amino acid derivatives using infrared spectroscopy (O189). The thermally induced denaturation of three chymotrypsin complexes, acylenzyme cinnamoyl chymotrypsin, phenylmethylsulfonyl chymotrypsin, and proflavin chymotrypsin, was examined (O190). Short linear peptides were synthesized and studied to investigate the 150R
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influence of conformational equilibrium of the matrixes on excitedstate processes, which in turn can provide information on the structure and dynamics in solutions of these materials (O191). FT-IR spectroscopy was used to investigate the kinetics of secondary structure formation during refolding of small globular proteins triggered by temperature jump or fast denaturant dilution (O192). FT-IR difference spectroscopy was used to study the behavior of native rhodopsin and its mutants expressed in DOS cells solubilized in dodecyl maltoside and reconstituted into lipids (O193). FT-IR spectroscopy has been used to study the thermally induced exchange characteristics of those backbone amide protons which persist in H-D exchange at ambient conditions in RNase A, in wild-type RNase T1 and some of its variants, and in the histone-like protein Hbsu (O194). This review with 51 references is of the development over the past thirty years of IR spectroscopic investigations of natural and synthetic melanins (O195). Vibrational CD and FT-IR methods for prediction of protein secondary structure are systematically compared using selective regression analysis (O196). FT-IR spectra were obtained for mammalian calmodulin and two of its fragments produced by limited proteolysis (O197). The authors investigated Raman and IR spectra of the Watson-Crick type of the guanine‚cytosine base pair and of the individual guanine and cytosine nucleic acid bases by ab initio Hartree-Fock theory (O198). The effect of the nature of the third-strand sugar on the geometry and stability of triple helixes with a pyrimidine motif was studied by FT-IR spectroscopy (O199). FT-IR was used to study the proper orientation of membranes containing nicotinic acetylcholine receptors on crystals (O200). FT-IR spectroscopy has been used to investigate the secondary structure, disulfide reduction, and thermal behavior of recombinant human granulocyte-macrophage colony-stimulating factor in aqueous solution (O201). This review with 149 references is of applications of FT-IR spectroscopy to the structural study on the function of bacteriorhodopsin (O202). Highresolution two-dimensional NMR complemented by FT-IR and CD has been employed for the elucidation of three-dimensional solution structure of several synthetic peptides corresponding to the calcium binding domains of the 148 residue protein calmodulin (O203). IR spectra of helical poly(β-phenethyl-L-aspartate) in 1,1,2,2-tetrachloroethane were observed as a function of temperature (O204). This paper discusses the selective enhancement and subsequent subtraction of atmospheric water vapor contributions from FT-IR spectra of proteins (O205). The conformation of puroindoline-a and -b, two basic lipid-binding proteins isolated from wheat seedlings, has been studied for the first time by IR and Raman spectroscopy (O206). FT-IR spectroscopic studies of hydration of such as phosphatidylcholines are discussed (O207). FT-IR spectra of collagen films set in a vacuum chamber have been measured as a function of time (O208). Resonance Raman and FT-IR spectra are reported for free-base tetraphenylbacteriochlorin and its isotopomers (O209). FT-IR has been used to quantitatively examine the secondary structure of imprinted proteins in anhydrous media (O210). This review with 135 references discusses the IR spectroscopy of lipids (O211). The metastability of dimyristoylphosphatidylethanolamine has been studied by FT-IR spectroscopy, both in the absence and in the presence of R-tocopherol (O212). Structural changes in the complex formation between transducin and metarhodopsin II, the
activated form of photolyzed rhodopsin, in the visual transduction process were analyzed by FT-IR spectroscopy (O213). The photooxidation of the primary electron donor in several photosystem I-related organisms has been studied by light-induced FTIR difference spectroscopy (O214). FT-IR spectroscopy was used to quantitatively assess the secondary structure of proteins in aqueous-organic mixtures ranging from pure water to a pure solvent (O215). The influence of hydration and hydrostatic pressure on the conformation and local interactions of phosphatidylinositol has been investigated using IR spectroscopy (O216). The FT-IR spectra of photocycle intermediates of sensory rhodopsin II from Natronobacterium pharaonis were measured (O217). FT-IR spectra indicate that the pressure-induced liquid crystal-togel transition of dioleoylphosphatidylglycerol involves a conformational change making the glycerol Csn-1-Csn-2 bond more parallel to the bilayer surface and resulting in increased carbonyl group hydrogen bonding (O218). FT-IR spectroscopy has been used to characterize Langmuir-Blodgett films of purple membranes deposited on Ge crystals at different surface pressures (O219). The secondary and tertiary structures of the cholinedependent major pneumococcal autolysin LytA amidase and of its COOH-terminal domain have been investigated by CD and FTIR spectroscopy (O220). A selective solubilization process of behenic acid in mixed Langmuir films by 2-propanol was demonstrated by IR spectroscopy (O221). A review with 24 references focuses on FT-IR and Raman spectroscopies in the study of proteins and other biological molecules (O222). This paper discusses the IR analysis of protein unfolding caused by disulfide reduction (O223). Infrared studies of the types of coordination of the side-chain carboxylate anion to a metal cation have been studied for protein-metal interactions (O224). The authors discuss the first systematic structural and conformational characterization of a complete family of diribonucleotide analogues in aqueous solution by Raman and IR spectroscopies (O225). The authors studied the spectral variation of mixed and separated homopolymeric RNA and DNA systems under conditions that lead to conformational variation using FT-IR and CD (O226). Hydrogenbonding formation between guanine and cytosine was studied by vibrational spectroscopy (O227). Fluorescence and FT-IR spectroscopic studies were used to define the role of the disulfide bond in the calcium binding in the 33-kDa protein of photosystem II (O228). Light-induced FT-IR difference spectra of P840 upon its oxidation have been measured with the reaction center complex from the green sulfur bacterium Chlorobium tepidum (O229). MidIR spectra of pure sucrose solutions and of biological solutions containing sucrose and potassium ions were investigated by principal component analysis (O230). Conformational disorder in liquid alkenes and in the L R and H phases of some unsaturated phospholipids has been monitored by FT-IR spectroscopy (O231). Upon the removal of water, proteins undergo a major, reversible rearrangement of their secondary structure, as revealed by FTIR spectroscopy (O232). The hydration of 1,2-dioleoyl-sn-glycerophosphoethanolamine has been studied by FT-IR spectroscopy applied to macroscopically oriented films in comparison to related phospholipids (O233). FT-IR (ATR) was used to probe the kinetics of hydrogen/deuterium exchange in Manduca sexta apolipophorin-III (O234). IR spectroscopy was applied to the investigation of normal and oxidatively modified hepatic nuclei
(O235). This review is of structures of cell surface polysaccharides as determined by FT-IR spectroscopy (O236). A review has been written of the use of IR spectroscopy in identifying the base composition of nucleic acids, polymorphism of duplex DNA, etc. (O237). A review with references has been written of various applications of FT-IR spectroscopy to the study of hydrated lipid assemblies and biomembranes (O238). This review is of a computational IR procedure for simulating the amide I band envelopes in globular proteins, transition dipoles, etc. (O239). A review with 75 references is presented on the use of FT-IR spectroscopy for the study of enzyme systems (O240). This article is the first one of a series aimed at determining the numerous interaction configurations adopted by water molecules in macromolecular systems using FT-IR spectrometry (O241). Model systems for the hydrogen-bonded chain in the active center of maltodextrinphosphorylase are synthesized and studied by FTIR spectroscopy (O242). FT-IR was used with other analytical techniques to analyze the structural organization and thermal stability of two spermhesins (O243). A study was undertaken of the interaction of the Mg ion with the anionic phosphatidylglycerol, and FT-IR was used to identify the Mg(II) binding sites (O244). FT-IR and site-directed isotope labeling has been used as a probe of local secondary structure in the transmembrane domain of phospholamban (O245). The experimental and theoretical investigation of the vibrational spectra of cytosine and protonated cytosine was performed (O246). IR spectroscopy has been used to determine gel-state miscibility in long-chain phosphatidylcholine mixtures (O247). FT-IR and EXAFS spectroscopic techniques have been used to characterize Cu and Zn complexes with deoxycholate, a derivative of deoxycholic acid which is an important physiological bile acid (O248). FT-IR spectroscopy was applied to investigate the conformational aspects of synthetic polynucleotides upon binding of berenil and pentamidine (O249). FT-IR spectra have been recorded both as a function of time and after prolonged exposure to buffer to study the structural changes that lead to both the ligand- and lipid-dependent channel-inactive states of the nicotinic acetylcholine receptor (O250). FT-IR spectroscopy was used to investigate interactions of the cryoprotective agents glycerol and DMSO with Bradyrhizobium japonicum (O251). Gas chromatography/Fourier transform infrared spectroscopy was used to examine a selection of 42 monosaccharides and related compounds obtaining unambiguous identification (O252). The results of an international trial proficiency test are described. Compounds relevant to the Chemical Weapons Convention were analyzed in rubber, paint and two soil samples using GC, GC/ MS, and GC/FT-IR (O253). Direct-deposition GC/FT-IR, along with GC/MS, was used to identify trace components of plant substances (O254). GC/FT-IR, along with other chromatography techniques, was used to identify R-phenylethylamine in judicial samples (O255). Purge-and-trap PLOT capillary GC/FT-IR was used to identify volatile organic compounds in blood samples (O256). The use of GC/FT-IR of methylsilyl ethers of disaccharides to positively identify disaccharides is reported (O257). This paper examines the photochemical transformations of dichloroprop and 2-naphthoxyacetic acid in aqueous solution by combined GC/MS and GC/FT-IR analyses (O258). Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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This paper focuses on the time-resolved infrared and steadystate Fourier transform infrared spectroscopy of native and mutant reaction centers of R. sphaeroides (O259). Time-resolved FT-IR spectroscopy was used to characterize the structure and dynamics of the last step in the photocycle of the light-driven proton pump bacteriorhodopsin (O260). Two bathointermediates of the bacteriorhodopsin photocycle were distinguished by nanosecond timeresolved FT-IR spectroscopy (O261). Rapid-scan FT-IR spectroscopy and time-resolved single-wavelength IR spectroscopy have been applied to study the mechanism of the photochemical release of ATP from its P3-[1-2-nitrophenyl)ethyl] ester (caged ATP) (O262). Infrared absorbance changes of the sarcoplasmic reticulum Ca2+-ATPase arising from three partial reactions of its Ca2+pumping cycle were triggered by the photochemical release of ATP from caged ATP and were followed in real time using rapidscan FT-IR spectroscopy (O263). Changes in the vibrational spectrum of sarcoplasmic reticulum Ca2+-ATPase in the course of its catalytic cycle were followed in real time using rapid-scan FT-IR spectroscopy (O264). This paper details a comparative analysis of the refolding kinetics of RNAse A by time-resolved FT-IR spectroscopy (O265). This review and discussion focuses on fast events in protein folding initiated by laser-induced temperature jump and probed by time-resolved infrared spectroscopy (O266). Time-resolved FT-IR difference spectroscopy was used to characterized the amplitude, frequency, and kinetics of the absorbance changes induced in the IR spectrum of sarcoplasmic reticulum Ca2+-ATPase by Ca2+ binding at the high-affinity transport sites (O267). A review and discussion has been written that covers applications to biological membranes and to surface chemistry (O268). ATR was used to investigate the structure of purified P-glycoprotein functionally reconstituted into liposomes. A quantititative evaluation of the secondary structure and kinetics of 2H/H exchange of the P-glycoprotein were performed both in the presence and in the absence of Mg-ATP, Mg-ATP-verapamil, and Mg-ADP (O269). Examination of intact living bacterial cells was made by ATR spectroscopy. Typical examples demonstrate that ATR FT-IR spectroscopy makes it possible to classify and differentiate between microorganisms in vivo (O270). ATR was used to elucidate the hydration behavior and molecular order of phospholipid/ganglioside bilayers (O271). A method of measuring fecal lipids by ATR that requires no solvents was developed using partial least squares (O272). The secondary structure and orientation of the viral fusion protein hemagglutinin reconstituted in planar members was found to assume a tilted conformation during membrane fusion as determined by ATR (O273). Polarized attenuated total internal reflectance was applied to study the IR dichroism of the amide I transition moment in gramicidin A in a supported phospholipid monolayer and Ac-Lys2-Leu24-Lys2-amide in oriented multibilayers (O274). ATR was used to investigate the secondary structure of the plasma membrane H+-ATPase of corn roots and compare it to the FT-IR spectra of the Neurospora crassa plasma membrane H+-ATPase and the H+-ATPase and the H+/K+-ATPase from hog stomach (O275). This paper describes a new analytical technique for the study of adsorption of sarcosinate surfactants on live human skin as evidenced by the presence of spectral bands at frequencies characteristic of C-D bonds from the deuterio surfactant upon examination by ATR IR (O276). ATR 152R
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difference spectroscopy was combined with the step-scan technique and compared to conventional transmission spectra of biological matter (O277). ATR FT-IR was used to study the effect of phosphatidylglycerol on the percutaneous penetration of drugs through the dorsal skin of guinea pigs in vitro and analysis of the molecular mechanism (O278). The secondary structure of fibronectin (FN) adsorbed to polymer surfaces was investigated in a quantitative manner using FT-IR ATR techniques (O279). Amide hydrogen/deuterium exchange rates were recorded on thin lysozyme films by ATR FT-IR spectroscopy as a function of the pH of the solution from which the films were prepared (O280). The stratum corneum structure was examined by ATR FT-IR and X-ray scattering after prolonged in vitro iontophoresis. ATR FTIR studies showed that iontophoresis induced an important and reversible increase in the hydration of the outer layers of stratum corneum, but no increase in lipid fluidity could be detected (O281). Representative values for amide I absorptivities were obtained for 15 different films of globular proteins spread from water solutions (O282). Attenuated total reflection FT-IR spectroscopy was used to follow the adsorption of the globular protein lysozyme from aqueous (D2O) solution onto a silicon surface (O283). This paper discusses and illustrates amide hydrogen/ deuterium exchange kinetics in protein films recorded by attenuated total reflection infrared spectroscopy (O284). An ATR FTIR spectroscopic technique was developed for the estimation of the methoxy poly(ethylene glycol) 5000 content of the methoxy poly(ethylene glycol) 5000-modified protein bovine copper-zinc superoxide dismutase (O285). Attenuated total reflectance FTIR difference spectroscopy was used in the study of the formation of metarhodopsins (O286). A combination of ATR and FT-IR was used to measure the bacteriorhodopsin photocycle (O287). This paper discusses the influence of gangliosides on phospholipid model membranes as studied by ATR FT-IR spectroscopy and the structural information obtained (O288). ATR FT-IR, along with angle-dependent XPS and AFM, was used to investigate mussel adhesive protein adsorption on polystyrene and poly(octadecyl methacrylate) (O289). ATR FT-IR was used to investigate the effects of 10 phospholipids on the in vitro percutaneous penetration of prednisolone through the dorsal skin of guinea pigs (O290). The sorption of the plasma proteins human serum albumin (HSA) and human fibrinogen (FIB) onto hemodialysis cellulose substrates was investigated by the surface sensitive ATR FT-IR spectroscopy (O291). The effects of pH and the presence of metal ions An2- and Cd2+ on the conformation of bovine serum albumin were investigated using ATR FT-IR spectroscopy (O292). Fourier transform IR horizontal-attenuated total reflectance (FT-IR/IR/ H-ATR) spectroscopy was employed to determine the diffusion coefficients of sodium p-aminosalicylate (PAS) in sheep nasal mucosae and dialysis membranes (O293). Attenuated total reflection FT-IR spectroscopy in conjunction with statistical methods has been used as a new approach to rapidly discriminate three isogenic strains of Pseudomonas aeruginosassusceptible, less susceptible, and highly resistant to imipenemsand to follow the structural modifications related to an outer membrane impermeability (O294). DRIFTS was used as an in situ detection method for the qualitative and quantitative analysis of heroin, cocaine, and codeine after separation by thin-layer chromatography (O295). DRIFTS,
along with scanning electron microscopy and other chemical analyses, was used to study the fungal degradation of Eucalyptus grandis (O296). Fourier transform powder diffuse reflectance infrared spectroscopy was used to evaluate particle size of bulk powders in pharmaceutical preparations (O297). This study reports a quantitative correlation between specific FT-IR absorption peak intensity of phenytoin to its particle size in the bulk as well as in powder blends of pharmaceutical preparations (O298). This paper reports the use of DRIFTS to determine the concentrations of surface-adsorbed organics present as mixtures on bentonitic clays (O299). DRIFTS was used to rapidly identify Streptococcus and Enterococcus species (O300). This paper describes the quantitation of cefepime‚2HCl dihydrate in cefepime‚ 2HCl monohydrate by DRIFTS and powder X-ray diffraction techniques (O301). A review with 140 references has been written of biomedical applications of FT-IR and Raman microspectroscopy, spectral imaging, and mapping (O302). Fourier transform IR microscopy was used to monitor spatial variations in the quality and quantity of the mineral phase in calcified turkey tendon (O303). A method has been developed to obtain large red crystals of cytochrome bc1 complex from beef heart mitochondria and the structure of the complex by micro-FT-IR spectroscopy has been investigated (O304). Synchrotron FT-IR microspectroscopy has been used for in situ characterization of β-amyloid in human Alzheimer’s disease tissue (O305). Fourier transform IR microspectroscopy was applied to in situ detection of cholesterol ester stored in atherosclerotic plaques in New Zealand white rabbits (O306). This paper details the FT-IR microspectroscopy of three distinct types of plant tissues, nutshells, bamboo, and potato tubers (O307). The ability of FT-IR microscopy to analyze crystal deposits in tissues, especially in biopsy samples, was test and reported (O308). This paper details the use of FT-IR microscopy to study solute (drug and protein)/polymer interactions that affect solute diffusion in and subsequent release from swellable dosage forms based on environmentally responsive, pH-sensitive polymer networks (O309). A newly developed microscopic FT-IR spectrometry combined with differential scanning calorimetry has been used to investigate simultaneously the thermal response and IR spectral changes in protein structure in porcine stratum corneum after pretreatment with skin enhancers (O310). FT-IR microspectroscopy has been used to study the changes in mineral and matrix content and composition replicate biopsies of nonosteoporotic human osteonal bone (O311). Using FT-IR microspectroscopy, the average translational diffusion coefficients of bile salt-lecithin mixed micelles diffusing in amylopectin gel of varying concentration were measured (O312). FT-IR microscopy was used to detect mineral changes in a mouse model of osteogenesis imperfecta, an inheritable disease characterized by skeletal deformities and brittle bones (O313). FT-IR microscopy has been used to deduce the role of type X collagen in endochondral ossification (O314). This paper reports a completely noninvasive measurement of blood glucose using near-infrared waves (O315). In this article, near-IR spectroscopic measurements of hemoglobin concentration in whole blood, which are potentially useful in a pulse oximeter modified for noninvasive hemoglobinometry, are presented (O316). This paper discusses the hemoglobin content of whole blood being measured with a simple light-transmittance procedure using a
single-term derivative ratio calibration (O317). The authors of this paper discuss their investigation of the development of a sensor suitable for continuous noninvasive monitoring of blood glucose concentrations in diabetic patients (O318). This paper focuses on selective calibration models generated for glucose over the 1-20 nM concentration range by use of partial least-squares regression analysis of near-IR spectra from 5000 to 4000 cm-1 (O319). Calibration models have been generated and evaluated for the measurement of glucose, glutamine, ammonia, lactate, and glutamate in aqueous solutions by near-infrared spectroscopy (O320). The authors of this article describe a multivariate calibration procedure that is based on the use of a genetic algorithm to guide the coupling of band-pass digital filtering and partial least-squares regression (O321). This paper explores the complications of determining the concentration of glucose in vivo by near-IR spectroscopy due to the effects of optical changes caused by fluctuations in temperature, tissue water content, and concentration of other analytes. An investigation was conducted to determine the magnitude of the changes in diffuse reflectance and transmittance from changes in glucose (O322). A variable selection method that reduces prediction bias in single factor partial least-squares regression models was developed and applied to near-IR absorbance spectra of glucose (O323). Near-IR reflectance spectra of numerous frozen sections of carcinomatous tissue and frozen sections of normal surrounding fibroglandular tissue from patients with breast cancer are presented and discussed (O324). The authors of this study demonstrate the possibility of using near-IR absorption and excitation spectroscopy as accurate and rapid techniques to distinguish between normal and cancer breast tissues (O325). This paper illustrates how near-IR spectroscopy can discriminate between normal and carcinomatous human breast tissues (O326). In this study, the authors have attempted to use near-IR reflectance to map the variability in water content across the stratum corneum in vivo (O327). A new NIR technique based on a pseudorandom modulation/correlation method is being developed for noninvasive tissue diagnosis applications (O328). This paper discusses the characterization of biological tissues using Fourier transform nearinfrared spectroscopy. Changes in the skin due to sunlight and other environmental factors are reported (O329). The results of this study clarify the influence of probe geometry on near-infrared spectroscopic measurements obtained from the surface of a turbid biological tissue (O330). This paper focuses on determining the feasibility of near-IR analysis for quantitating urea, creatinine, and protein in urine (O331). Using continuous near-IR spectroscopy, the oxygenated state of hemoglobin and the redox state of cytochrome c oxidase in the cerebral tissue of newborn piglets were studied (O332). This paper examines noninvasive methods for determination of the hemoglobin content of arterial blood and the water content of skin (O333). The authors of this paper used near-IR spectroscopy to study noninvasive changes in cerebral hemoglobin oxygenation in the frontal and parietal cortex during performance of a verbal fluency task in patients with Alzheimer’s disease (O334). Acute responses of brain oxygenation were studied during postural change using near-IR spectroscopy. NIRS is shown to be useful to monitor cerebral oxygenation during postural change in humans (O335). This paper focuses on the use of a combination Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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of near-IR spectroscopy and discrete wavelength near-IR imaging to noninvasively monitor the forearm during periods of restricted blood outflow and interrupted blood inflow (O336). A review has been written that discusses the relationship between spectral data and β-lipoprotein content determined by routine turbidimetry (O337). The objective of this study was to explore whether measurements in the near-IR spectral region can be related to hemoglobin content of the human whole blood (O338). This paper focuses on a clinical study comparison where near-IR spectra and analyte reference data were collected on serum samples from a mixed diabetic/nondiabetic population. The objective of the study was to compare calibrations developed from spectral data sets collected by different operators under the same experimental conditions but separated in time (O339). This investigation focuses on the availability of oxygen in the human vastus medialis muscle and the tympanic, skin forehead, quadriceps, and rectal temperatures during exercise test and postexercise with noninvasive near-IR spectroscopy (O340). Near-IR was used to study noninvasively the influence of aging on changes in the local concentration of oxygenated hemoglobin, reduced hemoglobin, and total hemoglobin during activation of brain function (O341). This study focuses on the assessment by near-IR on the consumption of oxygen for the vastus medialis muscle that works supporting the weight of the human body (O342). The authors of this paper have used second-differential near-IR spectroscopy of water to determine the mean optical path length of the neonatal brain (O343). This report outlines the use of near-IR spectroscopy to measure cerebral hemoglobin oxygenation after hepatic transplantation (O344). The aim of this study was to evaluate the efficiency, validity, and practicability of near-IR reflectance analysis compared with standard methods for measurement of fecal carbohydrates (O345). This paper describes a novel, noninvasive method for measuring peripheral venous oxygen saturation in newborn infants using near-IR spectroscopy with venous occlusion (O346). The principle and possibility of bone tissue analysis by near-IR spectroscopy are described (O347). This paper explores the potential of near-IR spectroscopy in the clinical laboratory. Potential in vitro applications of NIR spectroscopy include analysis of serum, whole blood, plasma, breast milk, feces, bone, urine, cerebrospinal fluid, and tissue for analytes. In vivo applications of NIR spectroscopy include measurement of brain and tissue oxygenation and cerebral blood volume and flow characteristics, oximetry measurements, quantitation of cytochrome, and body fat composition. The possibility of measuring blood analytes noninvasively is also discussed (O348). Investigation of rapid near-IR spectroscopy in combination with fiber optics for biomedical sensing is presented in this paper (O349). This review with 16 references focuses on biological and medical applications of near-IR spectrometry (O350). This paper describes functional brain mapping using multichannel NIRS by applying motor stimulation in humans (O351). The authors of this paper studied cerebral oxygen metabolism during hypoxia to demonstrate whether the redox state of cytochrome aa3, as measured by nearIR spectrophotometry, reflects the brain energy level (O352). FTNIR spectra have been measured for native and thermal denatured pepsin in a solid state to find a marker band for the secondary structure of proteins (O353). Near-IR spectroscopy has been investigated as a tool for determining the amount of nitrogen in 154R
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feces since the well-known Kjeldahl method is rather complex, time-consuming, and expensive (O354). The purpose of this study was to determine whether the initial rate of hemoglobin and myoglobin deoxygenation during immediate postexercise ischemia, a reflection of muscle O2 consumption, can be a quantitative measure of muscle oxidative metabolism (O355). This paper compares three methods for fecal fat measurement in the presence of long- and medium-chain triglycerides and fatty acids (O356). This paper describes a method for estimating the cerebral blood volume and transit time in neonates from quick oxygen increases measured by near-infrared spectrophotometry (O357). The authors of this paper describe the use of second derivative nearIR spectroscopy to measure absolute deoxyhemoglobin concentrations in tissue (O358). The authors of this paper explore the potential sources of discrepancies between living tissue near-infrared spectroscopy algorithms (O359). The analytical strategies are described for the ferrylmyoglobin/ABTS radical monocation assay for measuring total antioxidant activity, which is a measure of the collective H-donating abilities of the antioxidants in the samples and is based on the interaction between antioxidants in the sample with the 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) radical monocation, which is highly chromogenic (O360). Asparagine and glutamine concentrations were determined in binary aqueous solutions with near-IR absorption spectroscopy and are described in this paper (O361). This paper explores structure-base calculations of the optical spectra of the LH2 bacteriochlorophyllprotein complex from Rhodopseudomonas acidophila (O362). Conflicting patterns of change in cytochrome c oxidase redox status have been obtained between different near-IR spectrophotometers when measurements were made during tissue ischemia. This study identifies possible sources of error that could be the cause of the discrepancy (O363). The potential of near-IR reflectance spectroscopy for nondestructively probing structural changes in protein during the process of denaturation was investigated (O364). This review with 111 references focuses on the photobiological application of nonlinear visible/NIR spectroscopic techniques, exemplified by the primary processes of bacterial photosynthesis (O365). A multichannel reflectance measurement system was developed that uses near-IR measurements for topographic imaging inside biological tissue (O366). Near-IR reflectance spectroscopy has been used for rapidly and reproducibly measuring the NIR spectra of mainstream smoke collected on Cambridge filter pads and quantifying the chemical composition from the spectral data (O367). The authors continuously measured hepatic absorbance of indocyanine green using near-IR spectroscopy after iv bolus injection in rabbits and their study suggests the advanced utility as a comprehensive liver function test (O368). The aim of this study was to examine the possibility for predicting purine nitrogen and total nitrogen content as a marker of microbial protein in duodenal digesta samples of sheep by near-IR spectroscopy (O369). To examine the feasibility of optical monitoring of cellular energy states with tissue-transparent near-IR light, the absorptions and fluorescence characteristics of Rhodamine 800 in isolated rat liver mitochondria and hepatocytes were investigated (O370). This paper focuses on the simultaneous prediction of the concentrations
of glucose, glutamine, lactic acid, ammonia, and antibody in the culture broth of mouse-mouse hybridoma by near-infrared reflectance spectroscopy (O371). The objective of this work was to determine whether the Dy content of ruminal digesta samples labeled by pulse-dosing intraruminally with Dy-labeled forages could be determined by near-IR reflectance spectroscopy (O372). Rat carcass characteristics were determined by classical chemical analyses, near-IR reflectance, and total body electrical conductivity, with the aim to establish a rapid, reliable, and soft method for numerous body composition predictions (O373). Near-IR spectroscopy was applied to rat liver allografts for assessing nitric oxide synthesis and tissue oxygenation as a means of monitoring the refection response following liver transplantation (O374). In this study, near-IR spectroscopy was applied to the prediction of the concentration of nutrients and products in culture broth of a mouse-mouse hybridoma (O375). Near-IR transmission spectroscopy has proven to be a more efficient and convenient analytical method for the determination of poly(ethylene glycol) used as a flow rate marker for the liquid phase in rumen digestion kinetics studies (O376). Cortical spreading depression (CSD) has been implicated in the migraine aura and in stroke. This study demonstrates near-IR spectroscopy for the first time as capable of noninvasive on-line detection of CSD in the pentobarbitalanesthetized rat (O377). A continuous-wave near-IR spectroscopy system co-operated with an NMR spectrometer has been developed for the regional correlation of nitrosyl hemoglobin formation in gerbil head under hypoxia (O378). Near-IR, in conjunction with measurement of cerebral blood flow, was used in rabbits with experimental bacterial meningitis to determine whether there was evidence for cerebral energy depletion and alterations in the cerebral vascular bed with infection (O379). Cortical spreading depression was monitored noninvasively by near-IR spectroscopy in male Wistar rats (O380). The authors of this paper have shown that an inexpensive dual wavelength near-IR tissue oxygen monitor may be very useful to detect myoglobin oxygenation in a volume of tissue as small as the isolated buffer-perfused rat heart (O381). The paper discusses near-IR depth-resolved measurement of drug concentrations during diffusion through a matrix (O382). This paper is a description of the analytical applications of nearIR spectroscopy in the pharmaceutical industry (O383). A study was performed on the pharmaceutical components in tablets. NearIR spectroscopy was shown to measure with satisfactory accuracy and reliability within the validity limits of calibration (O384). NearIR spectroscopy was used for the on-line measurement of moisture during granulation and drying of pharmaceuticals (O385). NearIR spectroscopy was used to qualitatively assess the homogeneity of a typical direct compression pharmaceutical powder blend consisting of hydrochlorothiazide, Fast-flo lactose, croscarmellose sodium, and magnesium stearate (O386). The authors of this paper discuss a calibration line adjustment to facilitate the use of synthetic calibration samples in near-infrared spectrometric analysis of pharmaceutical production samples (O387). Near-IR spectrometry was used to quantify metoprolol succinate in controlled-release tablets (O388). The viability of using principal component analysis and soft independent modeling of class analogy analysis of the near-IR reflectance spectra of illicit methaqualone tablet formulations as an aid in sample differentiation was investigated (O389). This investigation focused on the
possibility of applying near-IR reflectance spectrometry to the control of the production cycle of ranitidine hydrochloride tablets (O390). Investigation of rapid near-IR spectroscopy in combination with fiber optics for biomedical sensing is investigated (O391). This review with 15 references was written on reflection and transmission NIR spectrometry direct analyses of pharmaceuticals without the need of forming aqueous solutions (O392). This paper demonstrates the use of near-infrared reflectance spectroscopy to identify pharmaceutical products by the direct measurement of tablets or capsules in a blister packing (O393). The authors demonstrate the use of near-IR spectroscopy for assessing the progress of reactions leading to compounds for evaluation as antituberculosis drugs (O394). This overview is given of the use of near-IR spectrometry for screening characteristics of corn and soybean (O395). Near-IR transmission spectroscopy was explored for single-seed oil determination of meadowfoam (Limnanthes spp.) (O396). The mimosine contents of Leucaena foliage, Acacia tannins, and total phenols from leaf, bark, and pod were analyzed by a near-IR reflectance spectrophotometer (O397). The purpose of this study was to investigate whether near-IR reflectance spectroscopy and chemometric methods can be used as a rapid and simple procedure to predict the leachability of pesticides from soil samples (O398). A near-IR spectroscopic assay has been developed for in situ monitoring of lipolysis in water-in-oil microemulsions stabilized by soybean lecithin (O399). The authors of this paper describe a method of control of fermentations by means of on-line near-infrared spectrometry (O400). The authors of this paper describe the applications of near-IR spectroscopy to fermentation process analysis (O401). By use of near-IR spectroscopy, simultaneous, multiple-constituent estimation of important bioprocess parameters can be obtained in a time frame that was previously unattainable (O402). This article discusses the potential use of near-IR spectroscopy for analyzing strongly absorbing highly light scattering samples for bioprocess analysis (O403). The dynamics of electronic and thermal relaxation of the heme in myoglobin have been determined from subpicosecond time-resolved near-IR absorbance spectra of photoexcited myoglobin (O404). Near-IR is used to determine cerebral blood volume and cerebrovascular CO2 reactivity (O405). Light-induced release of ADP and ATP from respective caged nucleotides produced small distinct difference IR spectra of creatine kinase (CK), indicating that ADP and ATP binding to CK promoted different structural alteration (O406). FT-IR difference spectroscopy has been used to probe structural changes in membrane proteins (O407). The effects of both neutral and anionic lipids on the structure of the nicotinic acetylcholine receptor have been probed using IR difference spectroscopy (O408). This paper examines FT-IR difference spectra of tyrosine D oxidation and plastoquinone QA reduction in photosystem II (O409). Redox FT-IR difference spectroscopy using caged electrons reveals contributions of carboxyl groups to the catalytic mechanism of heme-copper oxidases (O410). FT-IR difference spectroscopy and 13C-labeled bicarbonate techniques investigate bicarbonate binding to the none-heme iron of photosystem II (O411). The photocycle of 124-kDa phytochrome A from Avena sativa was studied by FT-IR at low temperatures. Difference spectra between the parent and the intermediates were obtained Analytical Chemistry, Vol. 70, No. 12, June 15, 1998
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and show characteristic spectral features which allow a clear distinction between the different intermediates (O412). The tyrosine D radical FT-IR difference spectrum obtained in photosystem II membranes has been compared to FT-IR difference spectra of tyrosine and phenol radicals generated by UV irradiation at low temperature (O413). The photocycle of bacteriorhodopsin (BR) regenerated with all-trans-9-demethylretinal was investigated by time-resolved rapid-scan FT-IR difference spectroscopy (O414). A review with 54 references has been written of light-induced FTIR difference spectroscopy of the quinone vibrations in protein/ quinone interactions in the bacterial photosynthetic reaction center (O415). FT-IR difference spectroscopy was used to investigate Z,E isomerization of the R-84 phycoviolobilin chromophore of phycoerythrocyanin from Mastigocladus laminosus (O416). Lightinduced FT-IR difference spectroscopy was used to investigate protein and bacteriopheophytin response to QA reduction in photosynthetic bacterial reaction centers from R. sphaeroides and Rhodopseudomonas viridis (O417). Difference FT-IR spectra were recorded for the formation of the photointermediates and isorhodopsin from octopus rhodopsin at low temperatures (O418). Time-resolved FT-IR difference spectroscopy was used to characterize the amplitude, frequency, and kinetics of the absorbance changes induced in the IR spectrum of sarcoplasmic reticulum (SR) Ca2+-ATPase by Ca2+ binding at the high-affinity transport sites (O419). Low-temperature FT-IR difference spectroscopy has identified a pH-dependent polarity change at the heme-copper binuclear center of the aa3-type cytochrome c oxidase from R. sphaeroides (O420). Molecular reaction mechanisms of proteins have been monitored by nanosecond step-scan FT-IR difference spectroscopy (O421). This paper details the light-induced QA/ QA FT-IR difference spectrum of the photoreduction of the primary quinone (QA) in reaction centers from R. spaeroides (O422). An infrared difference spectroscopy investigation was conducted of the conformational changes of arginine kinase induced by photochemical release of nucleotides from caged nucleotides (O423). FT-IR spectroscopy has been used to assess the bonding interactions of the quinone carbonyls of QA (asymmetric binding) and QB (more symmetric) and compared to those proposed in the X-ray structures (O424). A combination of protein electrochemistry and spectroscopy was used to determine the midpoint potentials of the cofactors and the redox-induced difference spectra of cyt b and cyt c1 (O425). The authors of this paper report the first TyrDo/TyrD FT-IR difference spectrum obtained in spinach PS II membranes (O426). RNA/diethylstilbestrol interactions were studied by FT-IR difference spectroscopy (O427). This paper examines the analysis of the polymer/ antibody/antigen interaction in a capacitive immunosensor by FTIR difference spectroscopy (O428). This review has been written with many references related to light-induced FT-IR difference spectroscopy of the primary electron donor in photosynthetic reaction centers (O429). This review with references is of techniques and applications of ultrafast IR spectroscopy to biomolecules, pulse-probe methods in biology, etc. (O430). This article discusses the rapid advances in the generation of intense tunable ultrashort mid-IR laser pulses which allow the use of ultrafast IR pump-probe and vibrational echo experiments to investigate the dynamics of the fundamental vibrational transition of CO bound to the active site of heme 156R
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proteins (O431). An ultrafast laser apparatus was developed that allows time-resolved UV-visible and IR spectroscopy to be performed with a time resolution of 200 fs (O432). The authors of this paper present data from mutated photosynthetic reaction centers where a change in the energetics of the special pair P leads to a speed up of the electron-transfer step away from P (O433). Picosecond IR vibrational echo experiments on a protein, myoglobin-CO, are described in this article (O434, O435). In this article, picosecond IR vibrational echo experiments on a mutant protein, H64V myoglobin-CO, are described and compared to experiments on wild-type myoglobin-CO (O436). The authors of this paper discuss the application of step-scan FT-IR spectroscopy with nanosecond time resolution to the photocycle of carbonylHb (O437). A nanosecond step-scan FT-IR investigation of the KL to L transition in the bacteriorhodopsin photocycle is discussed in this article (O438). Femtosecond IR spectroscopy of low-lying excited states in the reaction center of R. sphaeroides are discussed in this paper (O439). These authors discuss femtosecond IR studies of photosynthetic reaction centers (O440). The authors of this paper present transient absorbance spectra of the reaction centers from the bacterium R. sphaeroides (O441). Marianne L. McKelvy is a Research Leader in the Spectroscopy Group of the Analytical Sciences Laboratory of the Dow Chemical Co., U.S.A. She received her B.S. degree from the University of Detroit, Detroit, MI (1979) and the M.S. (1982) and Ph.D. (1985) degrees in polymer chemistry from Polytechnic University, Brooklyn, NY. She joined the Dow Chemical Co. in the Analytical Sciences Laboratory in 1984, where she is involved in solving polymer problems using infrared spectroscopy. Her research interests involve the characterization of polymers using vibrational spectroscopy and infrared microspectroscopy. She is a member of the Coblentz Society, the Society for Applied Spectroscopy, and the American Chemical Society. Thomas R. Britt is a Project Leader in the Analytical Science Group of the Louisiana Division of Dow Chemical Co., U.S.A. He received his B.S. (1976) from Millsaps College, Jackson, MS, M.S. (1981) from the University of Southern Mississippi, Hattiesburg, MS, and the Ph.D. (1981) from the University of Southern Mississippi, Hattiesburg, MS. He joined Dow in 1982 and has worked in new polymer development and on-line analyzer development. For the past 9 years, he has worked in the Instrumental Analysis group, applying FT-IR and FT-Raman spectroscopies in the solution of production and research problems. His interests are polymer characterization and the application of FT-IR and FT-Raman microspectroscopies to understanding polymers and their processes. Bradley L. Davis is a Research Leader in the Materials Science Group of the Analytical Sciences Laboratory, The Dow Chemical Co., U.S.A. He received a B.A. degree from Rice University in 1972 and a M.A. from The University of Texas at Austin in 1974. He joined Dow in 1974 where he has been involved primarily in the application of infrared spectroscopy toward solving production and research problems. His research interests include polymer characterization, determination of molecular structure, and characterization of polymer surfaces. He is a member of the Society for Applied Spectroscopy and the Coblentz Society. J. Kevin Gillie is a Research Scientist in the Research and Development group at AET Films, located in New Castle, DE. His current responsibilities include directing the analytical sciences laboratory at AET Films. Since joining AET Films, he has focused on applying a variety of analytical techniques to the complex development, manufacturing, and application of oriented polypropylene films. He received a B.S. in chemistry from James Madison University in 1983 and a Ph.D. in physical chemistry from Iowa State University in 1989. Prior to joining AET Films, he worked in the Analytical Sciences Laboratory for The Dow Chemical Co. He has eight years of experience applying vibrational spectroscopy to solve complex industrial and materials problems. Felicia B. Graves is a Research Specialist in the Molecular Spectroscopy Group with The Dow Chemical Company, U.S.A. She received her B.S. from Jackson State University, Jackson, MS in 1982, and M.S. (1988) and Ph.D. (1991) from the University of Southern Mississippi, Hattiesburg, MS. She joined the Dow Chemical Co. in the Separation Sciences group in 1991 and, in 1993, joined the Molecular Spectroscopy group, where she has been involved primarily in applications of infrared and UV-visible spectroscopy. Her research interests included the development and applications of GC-IR-MSD for materials characterization. She is a member of the American Chemical Society, the Society for Applied Spectroscopy, and the National Organization for the Professional Advancement of Black Chemists and Chemical Engineers.
L. Alice Lentz retired from the Analytical Sciences Laboratory, The Dow Chemical Co., U.S.A. on December 31, 1997, with the title of Research Associate. She received a B.A. in chemistry from Rice University in Houston, TX and joined Dow in 1961. Her career was focused on the fields of infrared and ultraviolet spectroscopy. While at Dow, her interests included polymer analysis and the use of hyphenated techniques (gas chromatography/FT-IR and liquid chromatography/FT-IR) for the elucidation of molecular structure. In 1995, she received the Richard A. Nyquist Award from Dow for long-term contributions to analytical chemistry. She is a member of the American Chemical Society, the Society for Applied Spectroscopy, and the Coblentz Society.
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