Polyesters chromatography methods

Specifications and Analytical Methods. Butanediol is specified as 99.5% minimum pure, determined by gas chromatography (gc), sohdifying at 19.6°C minimum. Moisture is 0.04% maximum, determined by Kad-Fischer analysis (dkecdy or of a toluene a2eotrope). The color is APHA 5 maximum, and the Hardy color (polyester test) is APHA 200 maximum. The carbonyl number is 0.5 mg KOH/g maximum the acetal content can also be measured dkecdy by gc. 

Klingsberg (jf.S.D.C., 1954, 70, 563) describes a method specially designed for the chromatographic examination of vat dyes. Owing to the insolubility in virtually all solvents of the pigment form, the separation must be carried out in the leuco state. The reduced vat dyes, however, have such a marked affinity for cellulose that paper chromatography must be ruled out, but strips of material made of hydrophobic synthetic fibres, of which polyesters are the best, may be substituted. Rao, Shah, and Venka-... 

A sensitive method for the detection and separation of micro quantities of cyclic acetals of sugars by means of gas-liquid, partition chromatography has been described by Jones and coworkers. The column packing consisted of an intimate mixture of Apiezon M grease on Cromosorb W and butanediol succinate polyester on Cromosorb W, which was packed on top of a column of SE-30 methylsilicone polymer and glass beads. The column temperatme was maintained at 200°. Some cyclic acetals of sugars have been fractionated by gas-liquid chromatography as their (trimethyl-silyl) ethers. These derivatives are conveniently prepared and the method is especially suited to the less volatile monoacetals. 

On-line coupling of pyrolysis, gas chromatography, and mass spectrometry is a quick and elegant method for the qualitative detection of monomer units in many resins (e.g., polyesters, polyurethanes, phenolic resins, and polyacrylates). Identification of comonomers of polyacrylates, including hydroxy-functional and carboxy-functional monomers, is facilitated if the sample is silylated before pyrolysis [10.30]. 

Glycol ethers have a flexibilizing action on saturated polyester resins that crosslink with melamine-formaldehyde resins some functional groups in the melamine resin are apparently blocked by the glycol ether. The flexibilization of paint films by retention of solvents occurs in copolymer paints and has been investigated by gas chromatography [14.232] and radiotracer methods [14.233]. Dry, hardened paint... 

Driffield M, Bradley EL, Castle L. A method of test for residual isophorone diisocyanate trimer in new polyester-polyurethane coatings on light metal packaging using liquid chromatography with tandem mass spectrometric detection. J Chromatogr A 2007 1141(l) 61-6. 

METHOD 43 - DETERMINATION OF ACID AND GLYCOL UNITS IN TERYLENE AND OTHER POLYESTERS. HYDROLYSIS - GAS CHROMATOGRAPHY. 

METHOD 44 - DETERMINATION OF WATER IN POLYESTERS. DERIVATIVIZATION - GAS CHROMATOGRAPHY. ... 

This book covers all aspects of the analysis of plastics by chemical and physical methods. It is divided into eight chapters which each deal with a particular polymer or group of polymers - polyolefins, polypropylene, higher alkene polymers, styrene polymers, chlorine-containing polymers, methacrylates, polybutadienes, polyesters and polyethers. The techniques discussed include spectroscopy, chromatography, fractionation,. X-ray diffraction, autoradiography, DTA, TGA and DSC. 

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