Determination of Chemical Composition Distribution and Molecular Weight Distribution of Poly(2-(perfluoroalkyl)ethyl acrylate-<i>co</i>-alkyl acrylate) by High Performance Liquid Chromatography and Size Exclusion Chromatography

Isemura, Tsuguhide; Sato, Takatoshi; Kawahara, Kengo; Otsuka, Koji

doi:10.1080/10236660801905718

Cited by 5 publications

(2 citation statements)

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“…Size-exclusion chromatography (SEC) was conducted on a Younglin GPC system (YL9100) equipped with a refractive index detector by eluting AsahiKlin AK225G at 35 °C. 35 Monodisperse poly(methyl methacrylate) (PMMA; molecular weight of 860−2,200,000 g mol −1 ; Showa-Denko) was used as a reference standard. The current, voltage, and luminance characteristics of the OLED were measured using a source measurement unit (Keithley 2400) and a spectroradiometer (Minolta, CS-2000).…”

Section: Methodsmentioning

confidence: 99%

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Photoinduced Solubility Modulation in the Copolymers of Fluoroalkyl, Spiropyranyl, and Isobornyl Methacrylates

Park

Choi

et al. 2023

ACS Appl. Polym. Mater.

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This article reports photoinduced solubility modulation in copolymer thin films derived from spiropyranyl, perfluoroalkyl, and isobornyl methacrylates. A random copolymer of spiropyranyl methacrylate (SPMA) and 1H,1H,2H,2H-perfluorooctyl methacrylate (FOMA) was first prepared in the absence of isobornyl methacrylate (IBMA). The resulting as-prepared thin film could be dissolved in highly fluorinated or fluorous solvents but became insoluble following exposure to UV light (λ = 365 nm) via the photoisomerization transformation of spiropyran units into merocyanine moieties. On the other hand, the incorporation of IBMA into the copolymer structure above a certain threshold resulted in copolymers exhibiting the opposite dissolution behavior. UV–vis spectroscopic measurements on the copolymer films and solutions indicated that dipolar attraction between the photoisomerized merocyanine moieties contributed to the decrease in solubility. The incorporation of IBMA into the copolymer chains diluted the merocyanine moieties and increased their glass-transition temperature, resulting in the disruption of the intermolecular attraction and an increase in the solubility of the UV-exposed polymer chains. These results suggested that stencils could be developed without additives to generate strong acid molecules or free radicals in polymer thin films. The proposed processing technique for fluoroalkylated copolymers was thus tested in the fabrication of orthogonal copolymer stencils and demonstrated to be a useful tool for the pixel patterning of chemically vulnerable organic light-emitting diodes.

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Section: Methodsmentioning

confidence: 99%

“…Size-exclusion chromatography (SEC) was conducted on a Younglin GPC system (YL9100) equipped with a refractive index detector by eluting AsahiKlin AK225G at 35 °C . Monodisperse poly(methyl methacrylate) (PMMA; molecular weight of 860–2,200,000 g mol –1 ; Showa-Denko) was used as a reference standard.…”

Section: Methodsmentioning

confidence: 99%

Photoinduced Solubility Modulation in the Copolymers of Fluoroalkyl, Spiropyranyl, and Isobornyl Methacrylates

Park

Choi

et al. 2023

ACS Appl. Polym. Mater.

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Non‐size‐exclusion Chromatography Analysis of Synthetic Polymers

Lee

Chang

2010

Encyclopedia of Analytical Chemistry

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While nature is capable of producing uniform macromolecules as found in complex biosystems, man‐made polymers are hardly homogeneous. They exhibit inherent distributions at least in molecular weight, and often come with multivariate distributions in chemical composition, functionality microstructure, chain architecture, and so on. Size‐exclusion chromatography (SEC) has been the most widely employed chromatographic technique for the characterization of molecular weight and its distribution of synthetic polymers since its inception about half a century ago. Compared to conventional molecular weight characterization methods, SEC is an excellent method with regard to precision, analysis speed, required amount of samples, etc. Nonetheless, SEC separates the polymer molecules in terms of their chain size, which is not only a function of molecular weight but also depends on other molecular characteristics such as composition, branching, and microstructure. Therefore, SEC cannot characterize nonlinear polymers or copolymers effectively. In contrast to SEC, in which the different pore accessibility of the macromolecules is the major separation mechanism, interaction chromatography (IC) fractionates the polymer sample by enthalpic interaction between the polymer solutes and the stationary phase. As a result, IC is sensitive to the chemical nature as well as the molecular weight of the polymers, whereas it is less sensitive to long‐chain branching than SEC. By judiciously selecting the IC separation condition, one can characterize specific molecular properties of polymers with much higher resolution than SEC. Furthermore, one can access the chromatographic critical condition (CC) for a given polymer system by adjusting the solute interaction strength with the stationary phase until the exclusion and interaction contributions to the solute retention are exactly compensated. Liquid chromatography at the critical condition (LCCC) can be used as a unique tool for the characterization of polymers. Of late, 2D liquid chromatography (LC) separations by a rational combination of SEC, IC, and LCCC has become more and more popular for the characterization of multivariate polymers. In this article, recent advances in non‐SEC analysis methods of a variety of synthetic polymers are reviewed.

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Separation of Polymers by Chromatography

Chang

2022

Macromolecular Engineering

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While mother nature can produce uniform macromolecules as found in many biological systems, man‐made polymers are hardly homogeneous. Synthetic polymers are usually complex mixtures of molecules differing in various molecular characteristics such as molecular weight (MW), chemical composition, functionality, microstructure, and chain architecture. For precise characterization of polymers, the multivariate distributions in all these molecular characteristics need to be measured, which is an extremely difficult task, if not impossible. In practice, however, it is often sufficient to analyze a limited number of molecular characteristics. For the purpose, liquid chromatography is the most widely used method that has made a remarkable progress during the last several decades in both instrumentation and understanding of the separation mechanism. Size exclusion chromatography (SEC) has been the most widely employed chromatographic separation technique for the characterization of synthetic polymers since its inception about a half‐century ago. Compared to traditional fractionation methods of polymers, SEC is an excellent method in precision, analysis speed, required amount of a sample, etc. Nonetheless, SEC separates the polymer molecules according to the chain size that depends on not only MW but also other molecular characteristics such as composition, chain architecture, and microstructure. Therefore, for instance, SEC cannot separate nonlinear homo‐polymers according to MW or copolymers according to the composition. In contrast to SEC in which the different pore‐accessibility of macromolecules is the main separation mechanism, interaction chromatography (IC) fractionates polymers according to the interaction strength between the polymer molecules and the sorbent. In results, IC is more sensitive to the chemical nature of the polymers than SEC. By judiciously selecting the IC separation condition, it is possible to separate polymers according to specific molecular properties with higher resolution than SEC. Furthermore, one can access to the chromatographic critical condition for a given polymer system by adjusting the solute interaction strength with the sorbent until the exclusion and interaction contributions to the solute retention are exactly compensated. At the critical condition, polymers of different MW coelute. Therefore, LC at the critical condition (LCCC) can be used as a unique tool for the characterization of polymers since one can suppress the peak dispersion by MW distribution and focus on other molecular characteristics. Recently, polymer separations using two‐dimensional LC by a rational combination of SEC, IC, or LCCC have become more and more popular for the characterization of polymers with multivariate distributions. In this article, chromatographic separation methods of synthetic polymers are reviewed with an emphasis on non‐SEC methods.

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Determination of Chemical Composition Distribution and Molecular Weight Distribution of Poly(2-(perfluoroalkyl)ethyl acrylate-co-alkyl acrylate) by High Performance Liquid Chromatography and Size Exclusion Chromatography

Cited by 5 publications

References 23 publications

Photoinduced Solubility Modulation in the Copolymers of Fluoroalkyl, Spiropyranyl, and Isobornyl Methacrylates

Photoinduced Solubility Modulation in the Copolymers of Fluoroalkyl, Spiropyranyl, and Isobornyl Methacrylates

Non‐size‐exclusion Chromatography Analysis of Synthetic Polymers

Separation of Polymers by Chromatography

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