Dataset Information

Automation of Controlled/Living Radical Polymerization.

ABSTRACT: Controlled/living radical polymerization (CLRP) techniques are widely utilized to synthesize advanced and controlled synthetic polymers for chemical and biological applications. While automation has long stood as a high-throughput (HTP) research tool to increase productivity as well as synthetic/analytical reliability and precision, oxygen intolerance of CLRP has limited the widespread adoption of these systems. Recently, however, oxygen-tolerant CLRP techniques, such as oxygen-tolerant photoinduced electron/energy transfer-reversible addition-fragmentation chain transfer (PET-RAFT), enzyme degassing of RAFT (Enz-RAFT), and atom-transfer radical polymerization (ATRP), have emerged. Herein, the use of a Hamilton MLSTARlet liquid handling robot for automating CLRP reactions is demonstrated. Synthesis processes are developed using Python and used to automate reagent handling, dispensing sequences, and synthesis steps required to create homopolymers, random heteropolymers, and block copolymers in 96-well plates, as well as postpolymerization modifications. Using this approach, the synergy between highly customizable liquid handling robotics and oxygen-tolerant CLRP to automate advanced polymer synthesis for HTP and combinatorial polymer research is demonstrated.

SUBMITTER: Tamasi M

PROVIDER: S-EPMC9113399 | biostudies-literature | 2020 Feb

REPOSITORIES: biostudies-literature

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Automation of Controlled/Living Radical Polymerization.

Tamasi Matthew M Kosuri Shashank S DiStefano Jason J Chapman Robert R Gormley Adam J AJ

Advanced intelligent systems (Weinheim an der Bergstrasse, Germany) 20191203 2

Controlled/living radical polymerization (CLRP) techniques are widely utilized to synthesize advanced and controlled synthetic polymers for chemical and biological applications. While automation has long stood as a high-throughput (HTP) research tool to increase productivity as well as synthetic/analytical reliability and precision, oxygen intolerance of CLRP has limited the widespread adoption of these systems. Recently, however, oxygen-tolerant CLRP techniques, such as oxygen-tolerant photoind ...[more]

PMID: 35586369

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Project description:In the present study, porous silica particles as well as impervious fused-silica wafers and capillary tubes were modified with hydrophilic polymers (hydroxylated polyacrylamides and polyacrylates), using a surface-confined grafting procedure based on atom transfer radical polymerization (ATRP) which was also surface-initiated from α-bromoisobutyryl groups. Initiator immobilization was achieved by hydrosilylation of allyl alcohol on hydride silica followed by esterification of the resulting propanol-bonded surface with α-bromoisobutyryl bromide. Elemental analysis, IR and NMR spectroscopies on silica micro-particles, atomic force microscopy, ellipsometry and profilometry on fused-silica wafers, as well as CE on fused-silica tubes were used to characterize the chemically modified silica substrate at different stages. We studied the effect of monomer concentration as well as cross-linker on the ability of the polymer film to reduce electroosmosis and to prevent protein adsorption (i. e., its non-fouling capabilities) and found that the former was rather insensitive to both parameters. Surface deactivation towards adsorption was somewhat more susceptible to monomer concentration and appeared also to be favored by a low concentration of the cross-linker. The results show that hydrophilic polyacrylamide and polyacrylate coatings of controlled thickness can be prepared by ATRP under very mild polymerization conditions (aqueous solvent, room temperature and short reaction times) and that the coated capillary tubes exhibit high efficiencies for protein separations (0.3-0.6 million theoretical plates per meter) as well as long-term hydrolytic stability under the inherently harsh conditions of capillary isoelectric focusing. Additionally, there was no adsorption of lysozyme on the coated surface as indicated by a complete recovery of the basic enzyme. Furthermore, since polymerization is confined to the inner capillary surface, simple precautions (e.g., solution filtration) during the surface modification process are sufficient to prevent capillary clogging.

Dataset Information

Automation of Controlled/Living Radical Polymerization.

Publications

Automation of Controlled/Living Radical Polymerization.

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