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Coupling of NMR and liquid chromatography at critical conditions: A new tool for the block length and microstructure analysis of block copolymers

dc.contributor.authorHiller W.
dc.contributor.authorPasch H.
dc.contributor.authorSinha P.
dc.contributor.authorWagner T.
dc.contributor.authorThiel J.
dc.contributor.authorWagner M.
dc.contributor.authorMullen K.
dc.date.accessioned2011-05-15T15:59:55Z
dc.date.available2011-05-15T15:59:55Z
dc.date.issued2010
dc.identifier.citationMacromolecules
dc.identifier.citation43
dc.identifier.citation11
dc.identifier.issn249297
dc.identifier.other10.1021/ma902359e
dc.identifier.urihttp://hdl.handle.net/10019.1/11431
dc.description.abstractThe online coupling of liquid chromatography at critical conditions (LCCC) and NMR was used for the analysis of block copolymers. Polyisoprene-b- poly(methyl methacrylate) (PI-b-PMMA) copolymers synthesized by living anionic polymerization were separated regarding chemical composition by LCCC using single solvents as mobile phases. The analysis of the chemically different LCCC fractions was conducted by on-flow 1H NMR. To separate the copolymers from the respective homopolymers, critical conditions of polyisoprene (PI) and poly(methyl methacrylate) (PMMA) were used. Critical conditions were obtained by varying the column temperature. The comprehensive chemical composition and microstructure analysis by 1H NMR revealed that quantitative information on the PI/PMMA content as well as the microstructure of PMMA (isotactic, atactic, and syndiotactic triads) and PI (1,2-PI, 1,4-PI, 3,4-PI) was obtained. For the first time the determination of the true molar masses and true chemical compositions of the block copolymers was achieved by determining the microstructure distribution. © 2010 American Chemical Society.
dc.subjectAtactic
dc.subjectBlock lengths
dc.subjectChemical compositions
dc.subjectColumn temperature
dc.subjectCritical condition
dc.subjectHomopolymers
dc.subjectIsotactics
dc.subjectLiquid chromatography at critical conditions
dc.subjectLiving anionic polymerization
dc.subjectMicrostructure analysis
dc.subjectMobile phasis
dc.subjectNew tools
dc.subjectOn-line coupling
dc.subjectQuantitative information
dc.subjectSingle solvents
dc.subjectSyndiotactics
dc.subjectAcrylic monomers
dc.subjectAnionic polymerization
dc.subjectBlock copolymers
dc.subjectCopolymerization
dc.subjectEsters
dc.subjectLiquid chromatography
dc.subjectLiquids
dc.subjectLiving polymerization
dc.subjectMicrostructure
dc.subjectPlastic products
dc.subjectChemical analysis
dc.titleCoupling of NMR and liquid chromatography at critical conditions: A new tool for the block length and microstructure analysis of block copolymers
dc.typeArticle
dc.description.versionArticle


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