Onflow liquid chromatography at critical conditions coupled to 1H and 2H nuclear magnetic resonance as powerful tools for the separation of poly(methylmethacrylate) according to isotopic composition

被引：7

作者：

Hehn, Mathias ^{[1
]}

Sinha, Pritish ^{[2
]}

Pasch, Harald ^{[2
]}

Hiller, Wolf ^{[1
]}

机构：

[1] TU Dortmund, Dept Chem & Chem Biol, D-44227 Dortmund, Germany

[2] Univ Stellenbosch, Dept Chem & Polymer Sci, ZA-7602 Matieland, South Africa

来源：

JOURNAL OF CHROMATOGRAPHY A | 2015年 / 1387卷

基金：

新加坡国家研究基金会;

关键词：

Liquid chromatography at critical conditions; Onflow LCCC-NMR; H-2; NMR; Deuterated PMMA; Protonated PMMA; CRITICAL ADSORPTION POINT; SIZE-EXCLUSION CHROMATOGRAPHY; POLYMER OPTICAL-FIBER; ONLINE HPLC-NMR; PS-B-PMMA; POLY(ETHYL METHACRYLATE)S; DEUTERATED POLYSTYRENE; BLOCK-COPOLYMERS; MOLAR-MASS; BLENDS;

D O I：

10.1016/j.chroma.2015.02.012

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

The present work addresses a major challenge in polymer chromatography by developing a method to separate and analyze polymers with identical molar masses, chemical structures and tacticities that is solely based on differences in isotope composition. For the first time, liquid chromatography at critical conditions (LCCC) was used to separate PMMA regarding the H and D isotopes. At critical conditions of H-PMMA, D-PMMA eluted in the adsorption mode and vice versa. By online onflow LCCC-NMR, both PMMA species were clearly identified. Different from other detectors, NMR can distinguish between H and D. Onflow LCCC-H/NMR and LCCC-D/NMR measurements were carried out and the H/D-blend components were detected. H-1 and C-13 NMR provided the tacticity of protonated PMMA. Double resonance C-13{H} and triple resonance C-13{H,D} provided the tacticity of the deuterated samples. Samples with similar tacticities were used to ensure that separation occurs solely regarding the isotope labeling. (C) 2015 Elsevier B.V. All rights reserved.

引用

页码：69 / 74

页数：6

共 30 条

[1] Separation of poly(methyl methacrylate)s according to their tacticity II. Chromatographic investigations of poly(methyl methacrylate)s with different tacticity at the critical adsorption point [J].

Berek, D ;

Janco, M ;

Hatada, K ;

Kitayama, T ;

Fujimoto, N .

POLYMER JOURNAL, 1997, 29 (12) :1029-1033

[2] Demonstrating the feasibility of monitoring the molecular-level structures of moving polymer/silane interfaces during silane diffusion using SFG [J].

Chen, CY ;

Wang, J ;

Loch, CL ;

Ahn, D ;

Chen, Z .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2004, 126 (04) :1174-1179

[3] Different molecular structures at polymer/silane interfaces detected by SFG [J].

Chen, CY ;

Loch, CL ;

Wang, J ;

Chen, Z .

JOURNAL OF PHYSICAL CHEMISTRY B, 2003, 107 (38) :10440-10445

[4] Controlling the Location of Nanoparticles in Polymer Blends by Tuning the Length and End Group of Polymer Brushes [J].

Chung, Hyun-Joong ;

Kim, Jinyong ;

Ohno, Kohji ;

Composto, Russell J. .

ACS MACRO LETTERS, 2012, 1 (01) :252-256

[5] Chemical structures of liquid poly(ethylene glycol)s with different end groups at buried polymer interfaces [J].

Even, Mark A. ;

Chen, Chunyan ;

Wang, Jie ;

Chen, Zhan .

MACROMOLECULES, 2006, 39 (26) :9396-9401

[6] HPLC-NMR of fatty alcohol ethoxylates [J].

Hiller, W ;

Brüll, A ;

Argyropoulos, D ;

Hoffmann, E ;

Pasch, H .

MAGNETIC RESONANCE IN CHEMISTRY, 2005, 43 (09) :729-735

[7] On-line HPLC-NMR of PS-b-PMMA and blends of PS and PMMA:: LCCC-NMR at critical conditions of PS [J].

Hiller, Wolf ;

Sinha, Pritish ;

Pasch, Harald .

MACROMOLECULAR CHEMISTRY AND PHYSICS, 2007, 208 (18) :1965-1978

[8] Online Coupling of Two-Dimensional Liquid Chromatography and NMR for the Analysis of Complex Polymers [J].

Hiller, Wolf ;

Hehn, Mathias ;

Sinha, Pritish ;

Raust, Jacques-Antoine ;

Pasch, Harald .

MACROMOLECULES, 2012, 45 (19) :7740-7748

[9] On-line fractionated size exclusion chromatography-nuclear magnetic resonance of polymers with 1H and 2H nuclear magnetic resonance detection [J].

Hiller, Wolf ;

Hehn, Mathias ;

Hofe, Thorsten ;

Oleschko, Kirsten ;

Montag, Peter .

JOURNAL OF CHROMATOGRAPHY A, 2012, 1240 :77-82

[10] Separation Analysis of Polyisoprenes Regarding Microstructure by Online LCCC-NMR and SEC-NMR [J].

Hiller, Wolf ;

Sinha, Pritish ;

Hehn, Mathias ;

Pasch, Harald ;

Hofe, Thorsten .

MACROMOLECULES, 2011, 44 (06) :1311-1318

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