Keiichiro Kimura

Carbon-13 nuclear magnetic resonance study of ethylene-1-octene and ethylene-4-methyl-1-pentene copolymers

Abstract Detailed assignments of 13 C n.m.r. signals of ethylene-1-octene and ethylene-4-methyl-1-pentene copolymers, members of the linear low-density polyethylene (LLDPE) family, are presented. The equations relating signal intensities to the monomer sequences are given. Using these equations, the characterization of these copolymers by the triad monomer sequences is possible. From the analysis by the triad sequence, it is suggested that these 1-olefins have a tendency to be present isolated in the copolymer chain.

Structural change of a polymeric hindered amine light stabilizer in polypropylene during UV-irradiation studied by reactive thermal desorption-gas chromatography

Abstract The structural changes of a polymeric hindered amine light stabilizer (HALS), Adekastab LA-68LD (MW=1900) added in PP materials during UV-irradiation were investigated by reactive thermal desorption-gas chromatography (RTD-GC) in the presence of tetramethylammonium hydroxide [(CH3)4NOH, TMAH]. Not only the products formed from the residual intact HALS, but also those from its oxidized moiety (nitroxyl radical) were observed on the resulting chromatograms without the use of any troublesome sample pretreatment such as solvent extraction. The changes in the yields of these key products were then examined as a function of UV-exposure time. As a result, it was revealed that the amount of the nitroxyl radical increased in the initial stage of UV-irradiation but then slightly decreased mainly because of further decomposition into the smaller compounds, whereas that of the intact HALS monotonously decreased during exposure.

Highly sensitive determination of a polymeric hindered amine light stabilizer in polypropylene by reactive thermal desorption–gas chromatography using nitrogen-specific detection

Highly sensitive and specific determination of trace amounts of a polymeric hindered amine light stabilizer (HALS) in polypropylene (PP) materials could be established by improving reactive thermal desorption-gas chromatography (RTD-GC) in the presence of an organic alkali, tetramethylammonium hydroxide. By using nitrogen-phosphorus detection, highly selective detection of the HALS-related components was attained. In addition, the use of a polar poly(ethylene glycol) separation column alleviated the adsorption of minor specific pyrolysis products. This modified RTD-GC method allowed the determination of the polymeric HALS (Mr 1900) in PP even for trace concentrations between 100 and 500 ppm, through observing selectively the characteristic products containing a tetramethylpiperidine moiety, which had been impossible to detect under the previous RTD-GC conditions using a non-polar separation column and conventional flame ionization detection.