Attenuated total reflectance FTIR polymers

The most widely available technique for identifying mainly polymer, but also additives in plastics, is Fourier Transform Infrared (FTIR) spectroscopy. Samples are exposed to infrared light (4000-400 wavelengths per centimetre or cm ) causing chemical bonds to vibrate at specific frequencies, corresponding to particular energies. In the last 5 years, an accessory for FTIR has been developed, which enables non-destructive examination of surfaces and so is ideal for analysis of plastics in museum collections. Attenuated Total Reflection-FTIR (ATR-FTIR) requires samples to be placed on a diamond crystal with a diameter of 2 mm through which the infrared beam is reflected... 

Specific interactions in binary blends of ethylene-vinyl acetate copolymer with various low molecular weight terpene-phenol tackifying resins (TPR) were systematically investigated, as a function of the composition of the blend and of the electron acceptor ability of the resin, by using attenuated total reflection FTIR spectroscopy. Molecular acid-base were evidenced between TPR hydroxyl groups and EVA carbonyl groups. Quantitative information on the fraction of acid-base bonded entities, the enthalpy and equilibrium constant of pair formation were obtained. A crystalline transition of the EVA copolymer was observed and discussed in terms of enthalpy and entropy considerations based on FTIR and calorimetric DSC investigations. Fundamental results are then summarised to predict the interfacial reactivity of such polymer blends towards acid or basic substrates. 16 refs. 

FTIR instrumentation is mature. A typical routine mid-IR spectrometer has KBr optics, best resolution of around 1cm-1, and a room temperature DTGS detector. Noise levels below 0.1 % T peak-to-peak can be achieved in a few seconds. The sample compartment will accommodate a variety of sampling accessories such as those for ATR (attenuated total reflection) and diffuse reflection. At present, IR spectra can be obtained with fast and very fast FTIR interferometers with microscopes, in reflection and microreflection, in diffusion, at very low or very high temperatures, in dilute solutions, etc. Hyphenated IR techniques such as PyFTIR, TG-FTIR, GC-FTIR, HPLC-FTIR and SEC-FTIR (Chapter 7) can simplify many problems and streamline the selection process by doing multiple analyses with one sampling. Solvent absorbance limits flow-through IR spectroscopy cells so as to make them impractical for polymer analysis. Advanced FTIR... 

Always based on the use of IR spectrophotometry, a novel attenuated total reflection-Fourier-transform infrared (ATR-FTIR) sensor [42] was proposed for the on-line monitoring of a dechlorination process. Organohalogenated compounds such as trichloroethylene (TCE), tetrachloroethylene (PCE) and carbon tetrachloride (CT) were detected with a limit of a few milligrams per litre, after extraction on the ATR internal-reflection element coated with a hydro-phobic polymer. As for all IR techniques, partial least squares (PLS) calibration models are needed. As previously, this system is promising for bioprocess control and optimization. 

X-ray photoelectron spectroscopy (XPS) was used for elemental analysis of plasma-deposited polymer films. The photoelectron spectrometer (Physical Electronics, Model 548) was used with an X-ray source of Mg Ka (1253.6 eV). Fourier transform infrared (FTIR) spectra of plasma polymers deposited on the steel substrate were recorded on a Perkin-Elmer Model 1750 spectrophotometer using the attenuated total reflection (ATR) technique. The silane plasma-deposited steel sample was cut to match precisely the surface of the reflection element, which was a high refractive index KRS-5 crystal. 

This study addresses the question of how bulk polymer chemistry and surface energy affect the amount and the conformation of FN adsorbed to a series of polyurethaneureas. The technique of Fourier transform infrared spectroscopy (FTIR) coupled with attenuated total reflectance (ATR) optics was used to continuously and non-invasively measure the kinetics of FN adsorption, as well as to monitor conformational changes occuring during adsorption. 

The polymer properties in thin films are then compared with the bulk as measured by FTIR attenuated total reflection spectroscopy (ATR). A modest refractive index of the internal reflection element (IRE made of ZnSe, n=2.43 at 2000 cm ) and an incident angle of 65° - still low but well above the critical angle of total reflection - are chosen for the p-polarized light in order to obtain an information depth of several microns. Hence, the ATR spectra provide the bulk properties of the polymer sample. 

The FTIR spectra were recorded with a Nexus instrument (Nicolet, USA) using the ATR (attenuated total reflectance, 45° angle of incidence) technique with a diamond or a Ge cell ( Golden Gate, Specac, Kent, UK). The IR signal comes from a near-surface layer of the polymer film. The information depth de-... 

A cell for characterising the diffusion of small molecules through thin polymer films using attenuated total reflectance (ATR) FTIR spectroscopy was described. The cell was designed to be used with precast (commercially extruded) polymer films, thus enabling the as-processed transport properties of the film to be studied. The cell was used to measure the diffusion of carbon dioxide, amyl acetate and limonene, and simultaneous diffusion of the individual components from a 50/50 mixture of amyl acetate and limonene through the thin polymer films (HDPE, LDPE and PS). Diffusion coefficients measured with the ATR technique compared favourably with values obtained from gravimetric measurements with the same penetrants and polymer samples. 20 refs. 

This section introduces a novel application of IR spectroscopy, namely IR imaging, and the specific sampling technique of attenuated total reflectance (ATR). FTIR imaging in ATR mode allows one to visualize the spatial distribution of different components in polymeric materials and to study directly the effect of high-pressure CO2 on this distribution. This novel approach should benefit polymer scientists studying polymer blends and their processing with SCCO2. 

Infrared spectroscopy, including Fourier-transform infrared (FTIR) spectroscopy, is one of the oldest and most widely used analytical techniques in adhesion-related research. Transmission infrared spectroscopy has been used to identify compounds used in formulating adhesives and to follow curing reactions. Attenuated total reflection (ATR) (see Infrared spectroscopy attenuated total reflection) has been used to probe the surface composition of polymers that have been surface modified by an etching process or by deposition of a film. More recently, reflection-absorption infrared spectroscopy (see Infrared spectroscopy RAIR) has been used to characterize thin films on the surfaces of reflecting substrates. 

Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) method can be used for spectral characterization of the physical properties of the synthetic mbber nanocompounds, as well as other complex samples such as polymer... 

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