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Chemeorheology: a new design for simultaneous rheological and Fourier transform
near infrared analysis S. Benali,a,c J. Boucheta,d and G. Lachenalb aIngénierie des Matériaux Polymères /
Laboratoire des Matériaux Macromoléculaires, INSA de Lyon (CNRS, UMR 5627), 20 Avenue Albert Einstein, F-69621 Villeurbanne Cedex, France bLaboratoire
des Matériaux Plastiques et des biomatériaux, UCBL, (UMR CNRS 5627), 43, bd du 11 novembre 1918, 69622 Villeurbanne Cedex, France
ABSTRACT:
In this paper we present a new
laboratory-made system which allows the combination of rheometer dynamical analysis (RDA) and Fourier transform near infrared (FT-NIR) spectroscopy. Dynamic rheological
data and NIR spectra were simultaneously collected. Previous studies of thermosetting systems and, more particularly, polyurethane studies, manufactured by the reaction
injection moulding (RIM) process, emphasised the need for simultaneous rheological and kinetic measurements. The rheological measurements, performed using RDA, were
obtained using oscillatory shear experiments at variable angular frequencies between two parallel plates. In-situ monitoring of the extent of reaction of the investigated
polyurethane was carried out at room temperature using fibre-optic FT-NIR spectroscopy. Multivariate analysis of transmittance spectra was performed to calculate the degree of
conversion. The appliance for simultaneous measurement is described and their advantages and limitations are briefly discussed. The viscoelastic behaviour and the extent of
reaction were studied during reactive blending of polyurethane formation, especially at the critical moment of gelation. A good agreement is observed, between separate and
simultaneous rheological-FT-NIR measurements. Indeed, rheological experiments (up to 100 Hz) are not perturbed by the increase of the weight of the RDA plates. The RDA-FT-
NIR technique may provide a powerful tool for studying curing reactions of polymers for both industrial and academic communities.
Keywords: reaction injection moulding, near infrared
spectroscopy, polyurethane reactive system, kinetic, gel point, viscosity
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