Infrared reflectance-absorption experimental methods

Chapter 1 summarizes methods for the stabilization of artificial lipid membranes. They include synthesis of new types of polymerizable lipids and polymerization of membranes. Creation and characterization of novel poly(lipid) membrane systems, as well as their functionalization for biotechnological applications, are also described. Chapter 2 addresses experimental studies on the design and characterization of lipopolymer-based monolayers at the air-water interface. Thermodynamic and structural data collected with X-ray and neutron reflectrometry, infrared reflection absorption spectroscopy, and sum frequency generation spectroscopy provide... 

The infrared reflection-absorption spectroscopy was performed on a Bruker IFS 66 spectrometer (Karlsruhe, Germany) equipped with a MCT detector and a modified external reflection attachment P/N 19650 of SPECAC (Orpington, UK). This included a miniaturized Langmuir-trough, permitting thermostatic measurements. An extensive description of the method can be found in Gericke et al. (1993). The IRRAS set-up as well as the experimental approach can be inferred from the schematic sketch shown in Fig. 2. 

The experiments which provide direct infonnation on the vibrations of one- and tridimensional lattices are infrared absorption (reflection) spectra, Raman scattering and neutron scattering. For a general discussion on the theoretical principles and experimental methods the reader is referred to the abundant literature on these... 

Surface analytical techniques. A variety of spectroscopic methods have been used to characterize the nature of adsorbed species at the solid-water interface in natural and experimental systems (Brown et al, 1999). Surface spectroscopy techniques such as extended X-ray absorption fine structure spectroscopy (EXAFS) and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) have been used to characterize complexes of fission products, thorium, uranium, plutonium, and uranium sorbed onto silicates, goethite, clays, and microbes (Chisholm-Brause et al, 1992, 1994 Dent et al, 1992 Combes et al, 1992 Bargar et al, 2000 Brown and Sturchio, 2002). A recent overview of the theory and applications of synchrotron radiation to the analysis of the surfaces of soils, amorphous materials, rocks, and organic matter in low-temperature geochemistry and environmental science can be found in Fenter et al (2002). 

Single crystal studies of solid hydrates are scarce. There are two experimental procedures possible (i) transmission spectra of thin crystal plates (see, for example. Refs. 16, 17) and (ii) reflection spectra of crystal faces . Using polarized infrared radiation, the species (symmetry) and other directional features of the water bands can be determined. In the case of reflection measurements, the true transverse and longitudinal optic phonon frequencies can be additionally computed by means of Kramers-Kronig analyses and oscillator fit methods, respectively. Both experimental techniques, however, are relatively difficult because of the lack of suitable monocrystals, the requirement of preparing sufficiently thin, i.e., <0.1 mm, crystal plates (except for studying overtone bands, see Sect. 4.2.6), and the efflorescence or absorption of water at the crystal surfaces. In favorable cases, thin sheets of orientated powdery material can be obtained . ... 

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