Surface‐Functionalized, Ring‐Opening Metathesis Polymerization‐Derived Monoliths for Anion‐Exchange Chromatography

Eder, Karoline; Huber, Christian G.; Buchmeiser, Michael R.

doi:10.1002/marc.200700467

Cited by 22 publications

(4 citation statements)

References 34 publications

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“…Star polymers containing multiple linear arms connected at a central branched core represent one of the simplest nonlinear polymers, , and synthetic approaches the using atom transfer radical polymerization via the “core-first”, “coupling-onto”, or “arm-first” approach has thus been actively investigated recently. The approaches for synthesis of cross-linked polymers by ROMP were also known, − especially in terms of application as monolith materials for separation reported by Buchmeiser; , however, reports for precise syntheses of star (ball) shape polymers that are highly soluble in common organic solvents have not so far been reported. Since exclusive preparation of the end-functionalized ring-opened polymers can be easily achieved by a living ROMP of norbornene derivatives especially using the Schrock type molybdenum alkylidene initiator, , we thus explored a possibility to prepare soluble star (ball) shape ROMP polymers via the “core-first” approach in a precise manner.…”

Section: Introductionmentioning

confidence: 99%

Facile Controlled Synthesis of Soluble Star Shape Polymers by Ring-Opening Metathesis Polymerization (ROMP)

et al. 2009

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Section: Introductionmentioning

confidence: 99%

Facile Controlled Synthesis of Soluble Star Shape Polymers by Ring-Opening Metathesis Polymerization (ROMP)

et al. 2009

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“…By applying this method, the amounts of grafted monomers exceeded 1 mmol/g [75]. Recently, ROMP-derived, NBE-based monoliths were subject to in situ surface functionalization using 2-(N,N-dimethylaminoethyl)norborn- resulting functionalized monoliths were successfully used in anion-exchange chromatography of oligodeoxynucleotides [76]. Figure 17 illustrates the separation of oligodeoxythymidylic acids dT 8 , dT 16 , and dT 24 .…”

Section: Functionalized Romp-derived Polymeric Monolithsmentioning

confidence: 98%

Stationary phases for chromatography prepared by ring opening metathesis polymerization

Buchmeiser

2008

J of Separation Science

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The chemistry of metathesis polymerization-derived stationary phases is summarized. Since both ring-opening metathesis and 1-alkyne polymerization triggered by well-defined transition metal alkylidenes are living polymerization methods, they allow for the controlled and highly reproducible synthesis of stationary phases in terms of both the nature and total content of the functional group(s) of interest. In addition, the high functionality tolerance of these polymerization techniques allows for creating chromatographic supports with an unprecedented diversity in terms of functional groups that may be introduced. Their applications in various areas of separation science such as SPE, ion-chromatography, RP chromatography, chiral chromatography, and the high-performance liquid chromatographic separation of biomolecules are summarized. Within the context of the latter topic, special attention will be given to metathesis polymerization-derived monolithic supports. Consideration will also be given to those aspects of polymer chemistry that are relevant to the separation performance of these supports.

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“…The preparation, characterization, and application of monoliths in microscale separation have consequently been the subject of numerous reviews, with both electrochromatography 2–5 and capillary HPLC 6–11 as target techniques. A variety of precursor recipes and polymerization approaches such as thermally 12, 13 and UV‐initiated free radical polymerization 14, “living” ring opening metathesis polymerization 15, 16, electron‐beam curing 17, controlled radical polymerizations mediated by stable nitroxides 18–20, atom transfer 21, reversible addition‐fragmentation chain transfer 22 and organotellurium compounds 23 and recently also epoxy/amine polycondensation 10, 24–29 have been reported for synthesizing organic monoliths. Add to this the recently described scheme of controlled dissolution/precipitation of polyamides 30, 31 and the spectrum of structures and surface functionalities synthesized for liquid‐phase separation purposes is now very wide.…”

Section: Introductionmentioning

confidence: 99%

Differences in porous characteristics of styrenic monoliths prepared by controlled thermal polymerization in molds of varying dimensions

Byström

Viklund

Irgum

2010

J of Separation Science

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Nitroxide-mediated polymerization was used as a model system for preparing styrenic monolithic materials with significant mesopore contents in different mold formats, with the aim of assessing the validity of pore characterization of capillary monoliths by analysis of parallel bulk polymerized precursor solution. Capillary monoliths were prepared in 250 microm id fused silica tubes (quadruplicate samples, in total 17 m), and the batch polymerizations were carried out in parallel in 100 microL microvials and regular 2 mL glass vials, both in quintuplicate. The monoliths recovered from the molds were characterized for their meso- and macroporous properties by nitrogen sorptiometry (three repeated runs on each sample), followed by a single analysis by mercury intrusion porosimetry. A total of 14 monolith samples were thus analyzed. A Grubbs' test identified one regular vial sample as an outlier in the sorptiometric surface area measurements, and data from this sample were consequently excluded from the pore size calculations, which are based on the same nitrogen sorption data, and also from the mercury intrusion data set. The remaining data were subjected to single factor analyses of variance analyses to test if the porous properties of the capillary monoliths were different from those of the bulk monoliths prepared in parallel. Significant differences were found between all three formats both in their meso- and macroporous properties. When the dimension was shrunk from conventional vial to capillary size, the specific surface area decreased from 52.2+/-4.7 to 34.6+/-1.7 m(2)/g. This decrease in specific surface area was accompanied by a significant shift in median diameter of the through-pores, from 310+/-3.9 to 544+/-13 nm. None of these differences were obvious from the scanning electron micrographs that were acquired for each sample type. The common practice of determining the mesopore characteristics from analysis of samples prepared by parallel bulk polymerization and looking for changes in the macropore structure by visual assessment of SEMs are therefore both rather questionable, at least for monoliths of the kind used in this study.

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Surface‐Functionalized, Ring‐Opening Metathesis Polymerization‐Derived Monoliths for Anion‐Exchange Chromatography

Cited by 22 publications

References 34 publications

Facile Controlled Synthesis of Soluble Star Shape Polymers by Ring-Opening Metathesis Polymerization (ROMP)

Facile Controlled Synthesis of Soluble Star Shape Polymers by Ring-Opening Metathesis Polymerization (ROMP)

Stationary phases for chromatography prepared by ring opening metathesis polymerization

Differences in porous characteristics of styrenic monoliths prepared by controlled thermal polymerization in molds of varying dimensions

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