Front-surface external reflection infrared spectroscopy was used to study a set of samples of poly(ethylene terephthalate) (PET) corresponding to various states of order: highly amorphous, drawn at 80 °C to different draw ratios, and thermally crystallized under different conditions. Kramers-Kronig transformation provided high-quality spectra that included an accurate representation of the most intense bands in the spectrum, which are generally saturated or distorted in transmission and internal reflection spectra. Factor analysis indicated the presence of three principal components in the spectra, and by taking linear combinations of the three principal factors, it was possible to generate three distinct physically meaningful basis spectra designated G, TC, and TX. The G spectrum corresponds to a gauche conformation of the ethylene glycol moiety, which is predominant in the amorphous state, while the other two correspond to a trans glycol conformation. The TC spectrum corresponds to the true crystalline state of PET, in which the carbonyl groups are coplanar with and in an all trans arrangement with respect to the benzene rings. The TX spectrum, on the other hand, corresponds to a less ordered trans structure in which the peaks associated with the terephthaloyl moiety of the molecule resemble those observed for the amorphous phase, where the carbonyl groups are either noncoplanar or cis and trans with respect to the benzene rings. However, the TX spectrum is a major contributor in the spectra of the drawn samples. This indicates that drawing at 80 °C produces a structure in which gauche conformers are converted into extended trans sequences, but the terephthaloyl conformation remains rather disordered. In other words, the development of order involves two processes that do not necessarily occur simultaneously. This provides new insight into the nature of the widely reported "intermediate" phase in PET and into the complex behavior of some of the trans peaks in the infrared spectrum. Detailed analysis of the basis spectra, including curve fitting, has also made it possible to suggest more precise assignments for some of the bands in the IR spectrum.
/npsi/ctrl?lang=en http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/ctrl?lang=fr Access and use of this website and the material on it are subject to the Terms and Conditions set forth at http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/jsp/nparc_cp.jsp?lang=en NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur.Applied Spectroscopy, 50, 6, pp. 774-780, 1996 New approach to quantitative analysis of two-component polymer systems by infrared spectroscopy Cole, K. C.; Thomas, Y.; Pellerin, E.; Dumoulin, M. M.; Paroli, R. M. January 1996A version of this document is published in / Une version de ce document se trouve dans:Applied Spectroscopy, 50, (6), pp. 774-780, 1996 The material in this document is covered by the provisions of the Copyright Act, by Canadian laws, policies, regulations and international agreements. Such provisions serve to identify the information source and, in specific instances, to prohibit reproduction of materials without written permission. For more information visit http://laws.justice.gc.ca/en/showtdm/cs/C-42Les renseignements dans ce document sont protégés par la Loi sur le droit d'auteur, par les lois, les politiques et les règlements du Canada et des accords internationaux. Ces dispositions permettent d'identifier la source de l'information et, dans certains cas, d'interdire la copie de documents sans permission écrite. Pour obtenir de plus amples renseignements : http://lois.justice.gc.ca/fr/showtdm/cs/C-42 A new treatment is proposed for quantitative analysis of two-component polymer systems by infrared spectroscopy. Like much previous work, it is based on a ratio involving two peaks in the same spectrum. The relationship between such a ratio and the concentration of a given polymer is inherently nonlinear. It is shown that this nonlinearity can be well described by a simple equation derived from the laws of optical transmission. This equation has the form Xl = m 1 + mzR/(l + ュ セ I where Xl is the weight fraction of polymer 1, the m i are adjustable coefficients, and the ratio R is equal to Aj(A u + A b ). The quantities An and A b are the absorbances (peak heights or areas) at two frequencies a and b of which the first is associated mainly with polymer 1 and the second with polymer 2. This equation has been applied to various peak combinations in spectra of miscible blends of poly(phenylene ether) with polystyrene (both mid-IR and near-IR data) and immiscible blends. of polypropylene with polyethylene (mid-IR data). It is shown that the equation is valid in all cases, covering the full concentration range from 0 to 100% even when the peaks used for the analysis involve absorption by both polymers. It is therefore believed to be of broad general usefulness for the analysis of polymer blends and copoly...
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