Surface analytical techniques Nuclear magnetic resonance

Analytical techniques are conveniently discussed in terms of the excitation-system-response parlance described earlier. In most cases the system is some molecular entity in a specific chemical environment in some physical container (the cell). The cell is always an important consideration however, its role is normally quite passive (e.g., in absorption spectroscopy, fluorescence, nuclear magnetic resonance, electron spin resonance) because the phenomena of interest are homogeneous throughout the medium. Edge or surface effects are most often negligible. On the other hand, interactions between phases are the central issue in chromatography and electrochemistry. In such heterogeneous techniques, the physical characteristics of the sample container become of critical... 

Chemiluminescence is a very sensitive and selective technique. Reagent types, analytes, and detection limits have been summarized in a review by Imai.56 Chemiluminescence has been applied to the analysis of compounds that exhibit low UV absorbance, including metal ions, amino acids, fatty acids, and bile acids. Other detectors include detectors for radioactivity, nuclear magnetic resonance (NMR), and surface-enhanced Raman spectroscopy. Radioactivity detection is one of the most selective detectors, as only components that have been radiolabeled will be detected. The interface of NMR with HPLC and has been discussed in detail by Grenier-Loustalot et al.57 Surface-enhanced Raman spectroscopy is another technique that... 

Many of these requirements are met by INS spectroscopy, and INS investigations of catalysts have been carried out for more than 30 years (7-9). INS has emerged as an attractive technique to extend and supplement characterizations by surface science techniques, such as high-resolution electron energy loss spectroscopy (HREELS), X-ray photoelectron spectroscopy (XPS), and secondary ion mass spectrometry (SIMS). INS complements infrared (IR), Raman, and nuclear magnetic resonance (NMR) spectroscopies, especially when the electrical conductivity and absorption of visible and IR light by metals or supports, hinders, or prevents, the use of the full analytical power of these methods. 

Scientists have used a wide arsenal of analytical techniques to monitor chemical and physical transformations of polymers following exposure to laser radiation, among which UV-Vis absorption, nuclear magnetic resonance (NMR) spectroscopy, electron spin resonance (ESR) spectroscopy for detection of free radicals, GC/MS analysis, FTIR for detection of various functional groups and bonds, X-ray photoelectron spectroscopy (XPS) for the chemical composition of surfaces, optical, and fluorescence microscopy, atomic force microscopy (AFM) for surface topography, quartz crystal microbalance (QCM) for in situ mass loss measurements, and so forth. 

The stmctural and conformational analysis of proteins adsorbed to solid surfaces is difficult because most common analytical methods are not compatible with the presence of the interacting solids. With recent developments in instrumentation and techniques, our understanding of protein adsorption behavior has improved considerably [4, 14]. The most commonly used techniques include attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), radiolabeling techniques, immunofluorescence enzyme-linked immunosorbent assay (ELISA), ellipsometry, circular dichroism (CD) spectroscopy, surface plasmon resonance (SPR), and amide HX with nuclear magnetic resonance (NMR). Atomic force microscopy (AFM) and scanning... 

A glance at the table of contents, in volume 10, will show that some topics merit a large number of articles, a reflection of their importance in current analytical science. Several techniques, for example, mass spectrometry, nuclear magnetic resonance spectroscopy, atomic emission spectrometry, microscopy, the various chromatographic techniques (e.g., gas, liquid and thin-layer), and electrophoresis, merit a series of articles, as do areas such as food and nutritional analysis, forensic sciences, archaeometry, pharmaceutical analysis, sensors, and surface analysis. Each of these collections of articles, written by experts in their fields, provides at least as much up-to-date information on that particular subject as a complete textbook. 

Other analytical techniques have less frequently been used nuclear magnetic resonance spectroscopy (NMR) (e.g., tocopherols in toothpaste by hyphenated LC-NMR), energy dispersive X-ray fluorescence (ED-XRF) (e.g., heavy metals determination), surface enhanced Raman scattering (e.g., determination of 4-aminobenzoic acid or PABA, in sunscreens), neutron activation analysis (e.g., determination of iron and zinc), and thermometric analysis (e.g., fluoride in toothpaste). 

Several surface-sensitive techniques can provide details about bonding in amorphous materials. Such information complements structural analyses obtained by traditional bulk analytical techniques like Raman and infrared spectroscopy, solid state nuclear magnetic resonance spectroscopy, and Mossbauer spectroscopy. 

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