Infrared analysis solids

The most common methods for monitoring solid phase reacdons udlized in normal research laboratories are Infrared analysis of resin... 

The reaction mixture was removed from the vessel and distilled at a pressure of 30-60 mm, and a bath temperature of 30°C to 50°C until the methanol had all been removed. The extremely viscous tarry residue remaining in the still pot was given a very crude distillation, the distillate boiling at B2°C to 1 32°C/2 mm. In an attempt to purify this distillate by a more careful distillation, 5.3 g of a liquid distilling from 53°C to 150°C/5 mm was collected. At this point, much solid sublimate was noted not only in this distillate but in the condenser of the still. 7 g of the solid sublimate was scraped out of the condenser of the still. Recrystallization of the sublimate from ethyl acetate containing a small amount of petroleum ether gave beautiful crystals melting at 175°C to 177°C (5 g). Infrared analysis confirmed that this compound was hydroquinone (9% conversion). 

Reaction of K3Co(CN) with PMMA. A 1.0 g sample of PMMA and 1.0g of the cobalt compound were combined in a standard vessel and pyrolyzed for 2 hrs at 375°C. The tube was removed from the oven and the contents of the tube were observed to be solid (PMMA is liquid at this temperature). The tube was reattached to the vacuum line via the break-seal and opened. Gases were determined by pressure-volume-temperature measurements on the vacuum line and identified by infrared spectroscopy. Recovered were 0.22g of methyl methacrylate and 0.11 g of CO and C02. The tube was then removed from the vacuum line and acetone was added. Filtration gave two fractions, 1.27g of acetone insoluble material and 0.30g of acetone soluble (some soluble material is always lost in the recovery process). The acetone insoluble fraction was then slurried with water, 0.11 g of material was insoluble in water. Infrared analysis of this insoluble material show both C-H and C-0 vibrations and are classified as char based upon infrared spectroscopy. Reactions were also performed at lower temperature, even at 260°C some char is evident in the insoluble fraction. 

Harbour JR, Hopper MA, Marchessault RH, Dobbin CJ, Anczurowski E (1985) Photoacoustic spectroscopy of cellulose, paper and wood J Pulp Pap Sci 11 J42-J47 Hauser M, Oelichmann J (1988) A critical comparison of solid sample preparation techniques in infrared spectroscopy Microchim Acta (Wien), Spec Issue, I 39-43 Hergert HL (1971) Infared spectra In Sarkanen KV, Ludwig CH (eds) Lignins Occurrence, formation, structure and reactions Wiley-Interscience, New York, 267-293 Hirschfeld T (1987) In McClure GL (ed) Computerized quantitative infrared analysis ASTM, Philadelphia, 169-179... 

The liquid reaction mixture was extracted with CC14. Infrared analysis of the extract did not indicate any additional products. The aqueous residue was evaporated to dryness at room temperature, and a few needle crystals were recovered. The infrared spectrum of this solid showed only absorptions owing to water. Attempts to dehydrate the small amount of product which remained were unsuccessful. 

Infrared analysis of water associated with a solid centers on an assessment of the degree to which the... 

Micro-IR spectra were used for real-time monitoring of solid phase reactions (12,15,16) and, utilizing deuterium isotope containing protecting groups, for quantitative infrared analysis of solid phase, resin-bound chemical reactions (13). 

There are many other characterization methods (e.g., small-angle X-ray scattering, solid-state nuclear magnetic resonance, and Fourier-transformed infrared analysis) for investigating nanocomposite structure. These techniques are extensively reviewed in Ray and Okamoto. ... 

SR Culler. Sampling techniques For Qualitative/Quantitative Analysis of Solids. In PB Coleman, ed. Practical Sampling Techniques Techniques for Infrared Analysis. Boca Raton CRC Press, 1993, pp. 107-144. 

General solid sampling technique can be used in the infrared analysis. However, improvement has been made in actual operation based on the features of the polymer. Mr. 

Solid films have been examined frequently for infrared analysis in biochemical work, for example, in structural studies of proteins, polypeptides, and polysaccharides. Such films have been of particular value for studying polarization spectra of macromolecules in intact films and in oriented ones (stretched, rolled, or stroked), thereby permitting knowledge to be gained concerning spatial arrangements within the molecule and conformational effects among molecules. (See The Use of Polarized Infrared Radiation and the Measurement of Dichroism, p. 73, for a detailed discussion.) A few workers have discussed the film technique (Lecomte, 1948 Randall et al., 1949 Hacskaylo, 1954). 

G. Lucazeau, Infrared, Raman and neutron scattering studies of p- and p"-alumina a static and dynamic structure analysis, Solid State Ionics 8... 

---