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Characterizing batch reactions with in situ spectroscopic measurements, calorimetry and dynamic modeling
Author(s) -
Ma Bei,
Gemperline Paul J.,
Cash Eric,
Bosserman Mary,
Comas Enric
Publication year - 2003
Publication title -
journal of chemometrics
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.47
H-Index - 92
eISSN - 1099-128X
pISSN - 0886-9383
DOI - 10.1002/cem.793
Subject(s) - chemistry , batch reactor , analytical chemistry (journal) , spectrometer , in situ , energy balance , spectral line , chromatography , thermodynamics , optics , organic chemistry , physics , astronomy , catalysis
A method for fully characterizing consecutive batch reactions using self‐modeling curve resolution of in situ spectroscopic measurements and reaction energy profiles is reported. Simultaneous measurement of reaction temperature, reactor jacket temperature, reactor heater power and UV/visible spectra was made with a laboratory (50 ml capacity) batch reactor equipped with a UV/visible spectrometer and a fiber optic attenuated total reflectance (ATR) probe. Composition profiles and pure component spectra of reactants and products were estimated without the aid of reference measurements or standards from the in situ UV/visible spectra using non‐negative alternating least squares (ALS), a type of self‐modeling curve resolution (SMCR). Multiway SMCR analysis of consecutive batches permitted standardless comparisons of consecutive batches to determine which batch produced more or less product and which batch proceeded faster or slower. Dynamic modeling of batch energy profiles permitted mathematical resolution of the reaction dose heat and reaction heat. Kinetic fitting of the in situ reaction spectra was used to determine reaction rate constants. These three complementary approaches permitted simple and rapid characterization of the reaction's rate of reaction, energy balance and mass balance. Copyright © 2003 John Wiley & Sons, Ltd.