Automated Polymer Purification Using Dialysis

Abstract

The automated dialysis of polymers in synthetic robots is described as a first approach for the purification of polymers using an automated protocol. For this purpose, a dialysis apparatus was installed within a synthesis robot. Therein, the polymer solution could be transferred automatically into the dialysis tube. Afterwards, a permanent running dialysis could be started, enabling the removal of residual monomer. Purification efficiency was studied using chromatography and NMR spectroscopy, showing that the automated dialysis requires less solvent and is faster compared to the classical manual approach.

Fully Automated Multi-Step Synthesis of Block Copolymers

“…Secondly, due to limited space in the synthesis robot, the reusability of a dialysis tubing was tested. Therefore, two typical automated dialysis approaches were performed each for 24 h in the same dialysis tubing utilizing the prior developed setup [35] and two different polymers synthesized for this approach (P5-P6). After each purification, the dialysis tubing was rinsed for four cycles by inserting and extracting THF.…”

“…The procedure was performed according to literature [35]. The polymer was dissolved in THF (100 mg/mL) and poured into dialysis tubing (3.5 kDa, d = 34 mm) using the 4-NH of the robot.…”

“…The first automated precipitation was performed in diethyl ether using poly(2-ethyl-2-oxazoline) synthesized via living cationic polymerization [31]. Prior to this study, we developed an automated continuous dialysis process, which is compatible to the automated synthesizer [35]. The system was investigated utilizing tetrahydrofuran (THF) as a solvent, which is commonly used in polymer purification [36][37][38][39] and resulted in a monomer removal up to the detection limit of the NMR-spectrometer in less than 48 h [39].…”

Improvement of High-Throughput Experimentation Using Synthesis Robots by the Implementation of Tailor-Made Sensors

“…For all UV experiments, poly(PEGMEMA) ( P1 ) and PMMA ( P2 ) were utilized since they are commonly used polymers [ 34 ]. Consequently, the working principle and effectiveness could be studied in detail.…”

Digital Transformation in Materials Science: A Paradigm Change in Material's Development

“…However, this procedure must be optimized so that a more efficient and faster analysis is possible and bottlenecks in the research can be eliminated. Variants for this are, for example, the online characterization during the reaction, [39] the combination of synthesis, purification, and characterization (see earlier) [31,32,40] and online/ inline flow-characterization approaches. [41] All of these strategies are already available to a certain extent, however, they are rarely utilized, (combined) expensive and need to further be developed.…”