Mass spectrometry in polymer chemistry: a state-of-the-art up-date

Gruendling, Till; Weidner, Steffen M.; Falkenhagen, Jana; Barner‐Kowollik, Christopher

doi:10.1039/b9py00347a

Cited by 223 publications

(189 citation statements)

References 169 publications

(191 reference statements)

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“…To obtain reference spectra, the 4 acrylates as given in the scheme were reacted with the RAFT polymer following the procedure of Boyer et al 21 with subsequent full characterization of the products. Disappearance of the RAFT-characteristic UV absorption is in all cases observed and a clear shift of the product peaks observed in ESI-MS analysis 22 with unambiguous assignment of all product peaks (for details see ESI †).…”

mentioning

confidence: 95%

Use of a continuous-flow microreactor for thiol–ene functionalization of RAFT-derived poly(butyl acrylate)

Vandenbergh

Junkers

2012

Polym. Chem.

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This study describes the synthesis of functionalized RAFT-derived poly(n-butyl acrylate) polymers via the use of a continuous-flow microreactor, in which aminolysis as well as thiol-ene reactions are executed in reaction times of just 20 minutes. Poly(n-butyl acrylate) (M n ¼ 3800 g mol À1, PDI ¼ 1.10) with a trithiocarbonate end group was prepared via a conventional RAFT process. The polymer was then functionalized via aminolysis/thiol-ene reactions in the micro-flow reactor with isobornyl acrylate, propargyl acrylate, poly(ethylene glycol) methyl ether acrylate and pentaerythritol tetraacrylate. To optimize the reaction time and reaction temperature of the micro-flow reactor, freshly collected samples were studied with soft ionization mass spectrometry. With this technique, efficient and very fast aminolysis and subsequent thiol-ene reactions take place on the RAFT-precursor polymer, yielding quantitative end group conversion within 20 min and functionalized polymers of 3700-4000 g mol À1, depending on the type of acrylate coupled. The use of a continuous-flow microreactor opens the pathway towards upsizing lab scale methods into larger processes without suffering from problems associated with reproducibility and tedious optimization issues.An often less valued key aspect of contemporary polymer synthesis, be it in the realm of controlled polymerization, click-like modifications or polymer analogous reactions, is the ability to upscale existing synthesis protocols. The adaption of procedures from microgram scale to significant production of materials on gram scale or larger is often tedious and accompanied with a loss in reaction efficiency or unreasonable reaction volumes. A convenient solution to this problem is the employment of microreactor technology.1 Miniaturized flow reactors offer the ability to optimize reaction conditions on a small scale while concomitantly allowing for simple upscale of reactions by going from small reactors to massive parallelization in reactor arrays or simply longer runtimes of the individual reactors. Also accelerations of the reactions can often be achieved by the rapid mixing of the components due to short diffusion lengths inside the microreactor, 2 as well as employing unconventional temperature regimes making microreactors in that respect comparable to the use of microwave reactors. The improved heat transfer of microreactors is a distinct advantage of these devices making their use especially interesting for highly exothermic reactions.3 While a wide array of commercial microreactors already exists, only a few studies have been reported so far on applications from the polymer field. Recently, Bally et al. described the synthesis of branched polymers from atom transfer radical polymerization (ATRP), 4 in a tubular microreactor. 5Also, polymerizations following the reversible addition fragmentation transfer (RAFT) 6 protocol have been described lately 7,8 as well as end group modifications 9 . Some earlier work on polymerizations in flow microreactors is summarized in a re...

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confidence: 95%

Use of a continuous-flow microreactor for thiol–ene functionalization of RAFT-derived poly(butyl acrylate)

Vandenbergh

Junkers

2012

Polym. Chem.

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“…[555] Two reviews contain significant reference to RAFT synthesized polymers. [556,557] The first details recent applications of mass spectrometry, in particular the matrix-assisted laser desorption/ionization (MALDI) and electrospray ionization (ESI) techniques, in polymer chemistry. The other is on application of multidimensional chromatography to polymers.…”

Section: Characterization Of Raft Agents and Raft-synthesized Polymersmentioning

confidence: 99%

Living Radical Polymerization by the RAFT Process – A Third Update

2012

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This paper provides a third update to the review of reversible deactivation radical polymerization (RDRP) achieved with thiocarbonylthio compounds (ZC(¼S)SR) by a mechanism of reversible addition-fragmentation chain transfer ( Chem. 2009Chem. , 62, 1402. This review cites over 700 publications that appeared during the period mid 2009 to early 2012 covering various aspects of RAFT polymerization which include reagent synthesis and properties, kinetics and mechanism of polymerization, novel polymer syntheses, and a diverse range of applications. This period has witnessed further significant developments, particularly in the areas of novel RAFT agents, techniques for end-group transformation, the production of micro/nanoparticles and modified surfaces, and biopolymer conjugates both for therapeutic and diagnostic applications.

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“…Several attempts of sample fractionation relying on a the size of the analytes in solution namely LC in SEC mode 44 , b the end-groups of the analytes namely LC in adsorption mode LAC or at the critical condition LCCC 37 39 and c the shape of the analytes in the gas phase IM 40 as well as alternative ionization mode namely ESI have been conducted to check at the representativeness of the direct MALDI-MS results reported above and interpreted with a HRKMD analysis. In spite of a size-based separation process with no chemical interaction with the stationary phase, the SEC-MALDI-MS analysis of PEO monostearate Fig.…”

Section: Representativeness Of a Direct Maldi-hrms / Hrk-md Analysismentioning

confidence: 99%

High-resolution Kendrick Mass Defect Analysis of Poly(ethylene oxide)-based Non-ionic Surfactants and Their Degradation Products

et al. 2017

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Mass spectrometry in polymer chemistry: a state-of-the-art up-date

Cited by 223 publications

References 169 publications

Use of a continuous-flow microreactor for thiol–ene functionalization of RAFT-derived poly(butyl acrylate)

Use of a continuous-flow microreactor for thiol–ene functionalization of RAFT-derived poly(butyl acrylate)

Living Radical Polymerization by the RAFT Process – A Third Update

High-resolution Kendrick Mass Defect Analysis of Poly(ethylene oxide)-based Non-ionic Surfactants and Their Degradation Products

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