In-line monitoring
of polymerization via Raman spectroscopy is
standard for batch reactors but yet to be manifested for flow reactors.
When transferring the in-line Raman spectroscopy from batch to flow
reactors, the aim is to maintain the measurement precision. We present
a customized Raman measurement cell for in-line monitoring in a tubular
flow reactor and a systematic accuracy analysis of the obtained measurement.
The accuracy analysis involves comparing three calibration models
and measurements of flowing solvent, monomer solution, and microgel
solution. The evaluation of the measurements reveals that multimolecular
analyte solutions most significantly influence the quantification
accuracy. From these investigations, we derive a quality criterion
for the Raman measurements based on the root mean square error, and
apply the criterion to the monitoring of precipitation polymerization
of poly(N-iso-propylacrylamide) (PNIPAM) microgels.
The results compare the predictions from the Raman measurements of
the microgel synthesis in the flow and batch reactor. Applying the
quality criterion enables high-quality measurements and allows the
functional detection of outliers during the synthesis. The identification
and exclusion of outliers eliminate several potential errors to cause
the difference in measurement results from the flow and batch reactors.
This contribution serves as a guideline for transferring in-line monitoring
from batch to flow reactors as the example of precipitation polymerization.
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