Analysis of chemical composition distribution of styrene-methyl methacrylate copolymer by high-performance liquid chromatography (original) (raw)
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The separation of a mixture of three poly(styrene-block-t-butyl methacrylate) copolymers (PS-b-PtBMA), consisting of polystyrene (PS) blocks of similar length and t-butyl methacrylate (PtBMA) blocks of different lengths, was performed using various chromatographic techniques, that is, a gradient liquid chromatography on reversed-phase (C18 and C8) and normalphase columns, a liquid chromatography under critical conditions for polystyrene as well as a fully automated two-dimensional liquid chromatography that separates block copolymers by chemical composition in the first dimension and by molar mass in the second dimension. The results show that a partial separation of the mixture of PS-b-PtBMA copolymers can be achieved only by gradient liquid chromatography on reversed-phase columns. The coelution of the two block copolymers is ascribed to a much shorter PtBMA block length, compared to the PS block, as well as a small difference in the length of the PtBMA block in two of these copolymers, which was confirmed by SEC-MALS and NMR spectroscopy.
e-Polymers, 2005
Ethylene - methyl methacrylate block copolymers are semicrystalline polymers that dissolve in organic solvents only at high temperatures. Accordingly, microstructure analysis by solution methods must be conducted at temperatures above 130°C. For the analysis of block copolymers of different compositions several analytical techniques were used, including high-temperature size-exclusion chromatography (SEC), hyphenated SEC-FTIR, and CRYSTAF (crystallisation analysis fractionation). While SEC with refractive index detection indicated a certain multimodality of the samples, SEC coupled with FTIR revealed that the samples were chemically inhomogeneous and may contain homo- and copolymer fractions. The presence of polyethylene and poly(methyl methacrylate) homopolymers in the copolymer samples was confirmed by CRYSTAF analysis, when the total concentration as well as the carbonyl group distribution were monitored separately. Chromatographic separation of the different sample components wa...
Use of high-performance liquid chromatography for the characterization of synthetic copolymers
Journal of Chromatography A, 1990
The evaluation of copolymer distribution as a function of molecular weight and chemical composition requires two separations, knotin as cross-fractionation. This procedure can be substantially improved by using high-performance liquid chromatographic (HPLC) techniques, including size-exclusion chromatography for the separation by molecular size. The separation by chemical composition can be achieved by gradient HPLC. Examples are given for copolymers of styrene and ethyl methacrylate (SEMA). Gradient HPLC of these and similar copolymers can be performed in both normal-phase and reversed-phase modes with inversion of elution order. In isooctane-tetrahydrofuran (THF) mixtures on polar columns, the elution of SEMA samples occurs at a higher THF concentration than required by solubility, i.e., with a distinct contribution of adsorption to retention. In contrast, reversedphase elution with methanol-THF mixtures takes place almost exactly at the solubility borderline of the system.
e-Polymers, 2005
The development of high-throughput liquid chromatographic techniques for the analysis of styrene-butyl acrylate (SBA) copolymers is discussed. The analysis time in size-exclusion chromatography (SEC) can be reduced to about 3 min per sample when high-throughput SEC columns and high flow rates are used. In gradient HPLC, small columns with improved separation efficiencies can be applied. The time requirements can be decreased to less than 2 min per sample. Using the high-throughput HPLC technique, the chemical composition distribution of high-conversion SBA copolymers can be analyzed in a fast and efficient way. The calibration of HPLC separation is conducted by coupling the HPLC system with FTIR through the LC-transform interface. A comparison of the chemical compositions of the copolymers obtained by 1 H NMR, off-line FTIR and coupled HPLC-FTIR verifies the accuracy of the high-throughput copolymer analysis approach.
Characterization of complex copolymers by two-dimensional Liquid Chromatography
Procedia Chemistry, 2010
Complex polymers were characterized by combinations of different chromatographic separation mechanisms: liquid adsorption chromatography (LAC), liquid chromatography under critical conditions (LCCC), and liquid exclusion-adsorption chromatography (LEAC). These techniques were combined off-line and on-line in two-dimensional separations. Fatty acid ethoxylates, fatty esters of polyethylene glycol (PEG) and polysorbates were analyzed by two-dimensional liquid chromatography with normal phase LAC as the first and liquid chromatography at critical conditions (LCCC) or liquid exclusion adsorption chromatography (LEAC) as the second dimension. A full separation of all oligomers to the baseline could be achieved in both dimensions. In two-dimensional separations, the offline approach is compared to comprehensive chromatography, and the scope and limitations of both techniques are discussed.
European Polymer Journal, 2005
Statistical copolymers of styrene and methyl methacrylate of different compositions were synthesized by the radical solution copolymerization in a batch isothermal reactor. Copolymers were characterized by the size exclusion chromatography (SEC), elemental analysis and dilute solution viscometry. Experimental limiting viscosity numbers were described by the Mark-Houwink-Kuhn-Sakurada correlation as the function of the molar mass and by the Mendelson correlation as the function of both the molar mass and copolymer composition. A new correlation of the intrinsic viscosity number, molar mass and composition was developed, based on semiempirical considerations. The correlation takes into consideration all the effects which affect the dimensions of random linear copolymer coils in solvents. The new equation was found to be superior to the MendelsonÕs one in correlating the experimentally obtained intrinsic viscosities.