Lakshani J. Weerarathna, Oliver Weismantel and Tanja Junkers*,
{"title":"嵌段共聚物纳米聚集体形成条件的自动DLS综合筛选","authors":"Lakshani J. Weerarathna, Oliver Weismantel and Tanja Junkers*, ","doi":"10.1021/acs.macromol.4c0317110.1021/acs.macromol.4c03171","DOIUrl":null,"url":null,"abstract":"<p >A fully automated robotic synthesizer for the screening of amphiphilic block copolymer (BCP) nanoparticle synthesis is presented. To reach this aim, BCP solutions are mixed in continuous flow with water, allowing for the automated variation of overall polymer concentration, mixing ratio of the water and organic solvent phase, and the overall flow rate of the system. Particle sizes are monitored online via a commercial dynamic light scattering instrument, and the obtained data are automatically analyzed. While the machine generally allows us to produce particles with a 10% standard deviation, the control software performs automatic outlier detection based on measurement of data in triplicates and repeats experiments until a statistically robust result is obtained. The synthesis platform was tested on 5 individual block copolymers, namely, poly(ethyl methacrylate)-<i>block</i>-poly(2-(dimethylamino)ethyl acrylate) (PEMA<sub>75</sub>-<i>b</i>-PDMAEA<sub>50</sub>), polystyrene-<i>block</i>-poly(2-(dimethylamino)ethyl acrylate) (PS<sub>50</sub>-<i>b</i>-PDMAEA<sub>25</sub>), polystyrene-<i>block</i>-poly(poly(ethylene glycol) methyl ether acrylate) (PS<sub>40</sub>-<i>b</i>-PPEGMEA<sub>35</sub>, PS<sub>90</sub>-<i>b</i>-PPEGMEA<sub>23</sub>), and polystyrene-<i>block</i>-poly(2-hydroxy ethyl acrylate) (PS<sub>90</sub>-<i>b</i>-PHEA<sub>14</sub>), which were obtained from reversible addition-fragmentation chain transfer polymerization. The screening revealed complex interdependencies of the synthesis parameters on the obtainable particle sizes. Generally, smaller particles were obtained at high water contents, high flow rates, and low polymer concentrations.</p>","PeriodicalId":51,"journal":{"name":"Macromolecules","volume":"58 11","pages":"5465–5476 5465–5476"},"PeriodicalIF":5.2000,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Comprehensive Screening of Conditions for Block Copolymer Nanoaggregate Formation via Automated DLS\",\"authors\":\"Lakshani J. Weerarathna, Oliver Weismantel and Tanja Junkers*, \",\"doi\":\"10.1021/acs.macromol.4c0317110.1021/acs.macromol.4c03171\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >A fully automated robotic synthesizer for the screening of amphiphilic block copolymer (BCP) nanoparticle synthesis is presented. To reach this aim, BCP solutions are mixed in continuous flow with water, allowing for the automated variation of overall polymer concentration, mixing ratio of the water and organic solvent phase, and the overall flow rate of the system. Particle sizes are monitored online via a commercial dynamic light scattering instrument, and the obtained data are automatically analyzed. While the machine generally allows us to produce particles with a 10% standard deviation, the control software performs automatic outlier detection based on measurement of data in triplicates and repeats experiments until a statistically robust result is obtained. The synthesis platform was tested on 5 individual block copolymers, namely, poly(ethyl methacrylate)-<i>block</i>-poly(2-(dimethylamino)ethyl acrylate) (PEMA<sub>75</sub>-<i>b</i>-PDMAEA<sub>50</sub>), polystyrene-<i>block</i>-poly(2-(dimethylamino)ethyl acrylate) (PS<sub>50</sub>-<i>b</i>-PDMAEA<sub>25</sub>), polystyrene-<i>block</i>-poly(poly(ethylene glycol) methyl ether acrylate) (PS<sub>40</sub>-<i>b</i>-PPEGMEA<sub>35</sub>, PS<sub>90</sub>-<i>b</i>-PPEGMEA<sub>23</sub>), and polystyrene-<i>block</i>-poly(2-hydroxy ethyl acrylate) (PS<sub>90</sub>-<i>b</i>-PHEA<sub>14</sub>), which were obtained from reversible addition-fragmentation chain transfer polymerization. The screening revealed complex interdependencies of the synthesis parameters on the obtainable particle sizes. 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Comprehensive Screening of Conditions for Block Copolymer Nanoaggregate Formation via Automated DLS
A fully automated robotic synthesizer for the screening of amphiphilic block copolymer (BCP) nanoparticle synthesis is presented. To reach this aim, BCP solutions are mixed in continuous flow with water, allowing for the automated variation of overall polymer concentration, mixing ratio of the water and organic solvent phase, and the overall flow rate of the system. Particle sizes are monitored online via a commercial dynamic light scattering instrument, and the obtained data are automatically analyzed. While the machine generally allows us to produce particles with a 10% standard deviation, the control software performs automatic outlier detection based on measurement of data in triplicates and repeats experiments until a statistically robust result is obtained. The synthesis platform was tested on 5 individual block copolymers, namely, poly(ethyl methacrylate)-block-poly(2-(dimethylamino)ethyl acrylate) (PEMA75-b-PDMAEA50), polystyrene-block-poly(2-(dimethylamino)ethyl acrylate) (PS50-b-PDMAEA25), polystyrene-block-poly(poly(ethylene glycol) methyl ether acrylate) (PS40-b-PPEGMEA35, PS90-b-PPEGMEA23), and polystyrene-block-poly(2-hydroxy ethyl acrylate) (PS90-b-PHEA14), which were obtained from reversible addition-fragmentation chain transfer polymerization. The screening revealed complex interdependencies of the synthesis parameters on the obtainable particle sizes. Generally, smaller particles were obtained at high water contents, high flow rates, and low polymer concentrations.
期刊介绍：
Macromolecules publishes original, fundamental, and impactful research on all aspects of polymer science. Topics of interest include synthesis (e.g., controlled polymerizations, polymerization catalysis, post polymerization modification, new monomer structures and polymer architectures, and polymerization mechanisms/kinetics analysis); phase behavior, thermodynamics, dynamic, and ordering/disordering phenomena (e.g., self-assembly, gelation, crystallization, solution/melt/solid-state characteristics); structure and properties (e.g., mechanical and rheological properties, surface/interfacial characteristics, electronic and transport properties); new state of the art characterization (e.g., spectroscopy, scattering, microscopy, rheology), simulation (e.g., Monte Carlo, molecular dynamics, multi-scale/coarse-grained modeling), and theoretical methods. Renewable/sustainable polymers, polymer networks, responsive polymers, electro-, magneto- and opto-active macromolecules, inorganic polymers, charge-transporting polymers (ion-containing, semiconducting, and conducting), nanostructured polymers, and polymer composites are also of interest. Typical papers published in Macromolecules showcase important and innovative concepts, experimental methods/observations, and theoretical/computational approaches that demonstrate a fundamental advance in the understanding of polymers.
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