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Fourier transform Raman spectroscopic detector system for the analysis of polymers by gel permeation chromatography
Author(s) -
Edwards H. G. M.,
Johnson A. F.,
Lewis I. R.
Publication year - 1993
Publication title -
journal of raman spectroscopy
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.748
H-Index - 110
eISSN - 1097-4555
pISSN - 0377-0486
DOI - 10.1002/jrs.1250240709
Subject(s) - gel permeation chromatography , spectrometer , raman spectroscopy , analytical chemistry (journal) , polybutadiene , polymer , chemistry , fourier transform infrared spectroscopy , column chromatography , elution , chromatography , materials science , optics , copolymer , organic chemistry , physics
An attempt was made to use a Fourier transform (FT) Raman spectrometer as a detector with a gel permeation chromatograph which was otherwise configured in the usual way for the measurement of molar mass distribution in polymers. A low‐volume flow cell was constructed and the detector response tested both off‐line and, in a preliminary way, in‐line with the chromatograph. The particular objective was to establish whether it would be possible to measure the microstructural variation in polybutadiene with polymer molecular weight during the chromatographic process. The detector sensitivity was assessed for a range of polybutadienes with different cis ‐1,4‐, trans ‐1,4‐ and vinyl‐1,2‐ contents using tetrahydrofuran as solvent and eluent. Data obtained using visible Raman (488.0 nm) excitation and near‐infrared (1064 nm) excitation were compared. Although it has been established that the Raman spectrometer is one of the best instruments for the evaluation of the microstructure of polybutadiene when used in a conventional way, it lacks the necessary sensitivity to provide quantitative information on polydienes which elute from a chromatograph. However, there is no reason in principle why an FT‐Raman spectrometer should not be used as a concentration detector and for the simultaneous more detailed analysis of polymer composition or micro‐structure during the chromatographic process, provided that the scattering intensity of the solute is high relative to the eluent. The potential advantages and the observed problems of what appears to be a novel experiment with an FT‐Raman instrument are discussed.