title: Spectra and concentration profiles throughout the reaction of curing epoxy resins from near-infrared spectroscopy and multivariate curve resolution methods.
abstract: When applied to near-infrared (NIR) data, multivariate curve resolution methods, in particular alternating least squares (ALS), make it possible to calculate the concentration profiles and the spectra of all species involved in the reaction of curing epoxy resins. In this paper, the model reaction between phenyl glicidyl ether and aniline (2:1) was studied at 95 degrees C. A NIR spectrum was recorded every five minutes throughout the eight-hour reaction process. The data display rank deficiency. This problem was overcome by supplying additional information to the system in the form of known spectra of some reactants. The recovered spectra and concentration profiles satisfactorily reproduced the experimental data. In this way, 99.99% of the variance associated with the experimental matrix was reproduced. A value of 0.87% was obtained for lack of fit while the similarity coefficient r between the spectra recovered and the spectra corresponding to the three pure species involved in the reaction were PGE (r = 0.994), aniline (r = 0.994), and tertiary amine (r = 0.999). The maximum and minimum limits associated with the ALS solutions were calculated, which made it possible to limit to a considerable extent the ambiguity that is characteristic of these curve resolution methods.
authors.affiliation: Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili, Pl. Imperial Tàrraco, 1, 43005 Tarragona, Spain. larrechi@quimica.urv.es
authors.forename: M S
authors.initials: MS
authors.lastname: Larrechi
authors.forename: F X
authors.initials: FX
authors.lastname: Rius
mesh_terms: D000465:Algorithms; D000814:Aniline Compounds / Q000032:analysis / Q000737:chemistry; D002484:Cementation / Q000379:methods*; D004853:Epoxy Resins / Q000032:analysis* / Q000737:chemistry*; D015999:Multivariate Analysis; D010647:Phenyl Ethers / Q000032:analysis / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013055:Spectrophotometry, Infrared / Q000379:methods*
chemical_list: D000814:Aniline Compounds; D004853:Epoxy Resins; D010647:Phenyl Ethers; C016050:phenylglycidyl ether; C023650:aniline