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Figure 5.16. Effects of (A) reaction volume and (B) ratio A/B under optimized reaction conditions of 6-L/min ow rate of inert gas and 20-minute dwell time. Intra-array materials parameters: (A) Ratio A/B = 1.0, catalyst concentration C = 1.0; (B) reaction volume = 200 mL, catalyst concentration C = 1.0. From ref. 73.
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Figure 5.17. Spatially resolved uorescence emission spectra of solid bisphenol-A polycarbonate in a melt-polymerization microreactor before (A) and after (B) optimization of processing conditions. (Inset) Microreactor cross section and locations of spectral measurements. From ref. 73.
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the combinatorial scale. This variability is determined as differences in measured uorescence spectra which are caused by the spatial variation in the chemical composition in the formed polymer within each microreactor. Figure 5.17 illustrates the uorescence spectra of polymers within individual microreactors under nonoptimized and optimized polymerization conditions. The evaluations were performed by measuring multiple regions of
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polymer in each microreactor. The small beam size (ca. 1 mm in diameter) permitted the detailed evaluation of the spatial distribution of polymer formation in each of the microreactors in the array. These measurements of variability can be provided only on a solid material directly in each microreactor because this information is lost after dissolving the polymer for traditional GPC analysis. 5.5.4. Determination of Contributing Factors to Combinatorial-Scale Chemical Reactions
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Monitoring of melt-polymerization reactions of bisphenol-A polycarbonate was performed in individual microreactors intended for combinatorial screening. Fluorescence spectroscopy coupled with the multivariate analysis of kinetic data provided previously unavailable combinatorial and highthroughput screening capabilities for tracking the progress of the reaction in real time and without sample preparation steps and determination of critical contributing factors to combinatorial reactions. Spectral data were generated using a UV light source coupled via a ber-optic probe to microreactors and to a portable spectro uorometer based on a linear CCDarray detector described in Section 5.5.1.The data collected during the reaction was analyzed using two chemometric tools to learn about the nature and concentrations of chemical species participating in the reaction. First, the contributing chemical factors in the reaction were determined using evolving factor analysis.79,80 Second, pure spectra and concentration pro les of these contributing factors were estimated using the multivariate curve resolution method.81,82 The evolving factor analysis is useful for processing of multivariate data produced by dynamic systems. In the monitored chemical reactions the measured spectra evolved with time because of the consumption of starting products during the reactions and because of a generation of intermediate and nal products. The evolving factor analysis was used to estimate the number of independent factors in the spectral data set at each time step that contributed to the spectral variation observed during a polymerization reaction. For this analysis uorescence data were baseline-corrected and spectral range was limited to 340 to 600 nm to reduce noise in the data (Figure 5.18A). Results of the forward analysis are presented in Figure 5.18B. As the rst step in the forward analysis, the eigenvalue of the rst measured spectrum was calculated. Then eigenvalues were calculated of matrices as new measured spectra were appended. The forward analysis suggests that several independent factors have evolved into the data set. In the reverse analysis (see Figure 5.18C), eigenvalues were calculated for the last spectra rst, and subsequent eigenvalues were calculated as spectra
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