Size exclusion chromatography – A blessing and a curse of science and technology of synthetic polymers

Berek, Dušan

doi:10.1002/jssc.200900709

Cited by 152 publications

(134 citation statements)

References 89 publications

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“…Whereas silica packed columns are preferred over polymer packed columns in HPLC, polymer particles are mainly used in size exclusion chromatography (SEC) due to their 'configurable' pore size and pore size distribution. In SEC, smaller polymer chains spend more time in pores of packed beads compared to the larger chains, which is the basis for the separation [426]. For a batch of higher MW polymer to be analyzed, beads with a higher pore size are necessary for better separation.…”

Section: Spe and Chromatographymentioning

confidence: 99%

Porous polymer particles—A comprehensive guide to synthesis, characterization, functionalization and applications

Gökmen

Prez

2012

Progress in Polymer Science

446

309

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Section: Spe and Chromatographymentioning

confidence: 99%

Porous polymer particles—A comprehensive guide to synthesis, characterization, functionalization and applications

Gökmen

Prez

2012

Progress in Polymer Science

446

309

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“…Only a handful of techniques can measure the absolute molecular mass distribution [3]. The gold standard is size exclusion chromatography (SEC) using universal calibration [4], which does not always work [5,6]. New techniques must be developed to aid in the advancement of polymer science.…”

Section: Introductionmentioning

confidence: 99%

Scaling exponent and dispersity of polymers in solution by diffusion NMR

Williamson

Röding

Miklavcic

et al. 2017

Journal of Colloid and Interface Science

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Molecular mass distribution measurements by pulsed gradient spin echo nuclear magnetic resonance (PGSE NMR) spectroscopy currently require prior knowledge of scaling parameters to convert from polymer self-diffusion coefficient to molecular mass. Reversing the problem, we utilize the scaling relation as prior knowledge to uncover the scaling exponent from within the PGSE data. Thus, the scaling exponent-a measure of polymer conformation and solvent quality-and the dispersity (M w /M n ) are obtainable from one simple PGSE experiment. The method utilizes constraints and parametric distribution models in a two-step fitting routine involving first the mass-weighted signal and second the number-weighted signal. The method is developed using lognormal and gamma distribution models and tested on experimental PGSE attenuation of the terminal methylene signal and on the sum of all methylene signals of polyethylene glycol in D 2 O. Scaling exponent and dispersity estimates agree with known values in the majority of instances, leading to the potential application of the method to polymers for which characterization is not possible with alternative techniques. Keywords:Pulsed gradient spin echo, pulsed field gradient, Nuclear Magnetic Resonance spectroscopy, Molecular weight distribution, Polymers, DOSY, Polydispersity Index, Self-diffusion, Molar mass, Flory exponent, Lognormal distribution, Gamma distribution, End-group analysis, Scaling law Synthetic polymers have distributions of molecular masses determined by their synthesis [1]. Measuring the molecular mass distribution rather than its average is important because the dispersity can influence polymer properties [2]. Absolute as opposed to relative measurements are needed when using polymer physics to fully realize the potential applications of a polymer [3]. Only a handful of techniques can measure the absolute molecular mass distribution [3]. The gold standard is size exclusion chromatography (SEC) using universal calibration [4], which does not always work [5,6]. New techniques must be developed to aid in the advancement of polymer science.Pulsed gradient spin echo nuclear magnetic resonance (PGSE NMR) [7,8] is a powerful technique for obtaining the distribution of polymer self-diffusion coefficients D [9], from which the distribution of molecular masses M can be obtained by the scaling law [10] ration give PGSE NMR a competitive edge with respect to SEC. Chemical shift information [7], e.g. in a diffusion ordered spectroscopy (DOSY) plot [11], provides the ability to observe chemical heterogeneity and impurity. Sample preparation generally does not require filtration because contaminates from large particles such as dust do not impact the experiment. However, the scaling parameters of Eq. (1) specific to that polymersolvent system must be found by measuring ⟨D⟩ on fractionated samples of the polymer with known M. Therefore, currently all PGSE NMR-based methods which convert from D to M cannot independently measure the absolute molecular mass distribution [...

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“…For example, size-dependent migration and partition, controlled by steric interactions in nanoporous media, provide the basis for macromolecular separations in gel electrophoresis [24] and size-exclusion chromatography. [25] Electrostatic prevention of the entry of charged species from charged pores with radii close to the electrical doublelayer thickness leads to the development of permselective membranes/films used for fuel cells, [26] reverse osmosis, [27] and electrochemical sensors. [28] Unfortunately, structurally polydisperse and deformable nanopores of conventional nanoporous media limit their sensing/separation selectivity and also obstruct quantitative studies on the molecule-nanopore interactions.…”

Section: Introductionmentioning

confidence: 99%

Block Copolymer‐Derived Monolithic Polymer Films and Membranes Comprising Self‐Organized Cylindrical Nanopores for Chemical Sensing and Separations

Ito

2014

Chemistry An Asian Journal

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Microphase separation of block copolymers (BCPs) has been extensively studied because it leads to the self-assembled formation of periodic structures controlled on the scale of tens of nanometers. In particular, BCP-derived cylindrical microdomains have attracted considerable interest for various applications owing to their well-defined shapes of uniform and tunable diameters. This focus review highlights recent efforts to apply BCP-derived monolithic films/membranes comprising cylindrical nanopores for chemical sensing and separations. The nanopores provide confined molecular pathways that exhibit enhanced selectivity based on steric, electrostatic, and chemical interactions, and thus, enable us to design unique electrochemical sensors and highly efficient separation membranes.

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Size exclusion chromatography – A blessing and a curse of science and technology of synthetic polymers

Cited by 152 publications

References 89 publications

Porous polymer particles—A comprehensive guide to synthesis, characterization, functionalization and applications

Porous polymer particles—A comprehensive guide to synthesis, characterization, functionalization and applications

Scaling exponent and dispersity of polymers in solution by diffusion NMR

Block Copolymer‐Derived Monolithic Polymer Films and Membranes Comprising Self‐Organized Cylindrical Nanopores for Chemical Sensing and Separations

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