Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate)

Jiang, Xulin; Lima, Vincent; Schoenmakers, Peter J.

doi:10.1016/j.chroma.2003.08.035

Cited by 37 publications

(24 citation statements)

References 33 publications

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“…This study extends previous observations, which proved little effect of the eluent composition changes on the LC LCD behavior [3,21] as well as high sample recovery of the method. [4,5] LC LCD column efficiency does not affect results substantially.…”

Section: Resultssupporting

confidence: 76%

“…[1] For example, Jiang et al [20,21] have successfully applied the LC LCD approach (by error designated as LC CC) to the separation of carboxy-and hydroxy-terminated poly(n-butyl acrylate)s and PMMAs, respectively. They employed bare silica gel and dichloromethane (adsorli)/ acetonitrile (desorli)-mixed eluents.…”

Section: Practical Application Of Lc Lcdmentioning

confidence: 99%

“…For PMMA, the above system was rather insensitive to eluent composition changes. [21] The decreased stability of similar chromatographic systems for poly(nbutyl acrylate)s as well as some unexpected results [20] were likely caused by the break-through phenomena, because their sample volume was only 10 ml.…”

Section: Practical Application Of Lc Lcdmentioning

confidence: 99%

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Liquid Chromatography of Polymers under Limiting Conditions of Desorption, 3

Šnauko

Berek

2005

Macro Chemistry & Physics

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Summary: Liquid chromatography under limiting conditions of desorption (LC LCD) enables the elution of adsorbing macromolecules independent of their size in solution. In this way, polymer species with different adsorptivities can be separated without mutual interference. It is shown on systems of bare silica gel, a tetrahydrofuran/toluene‐mixed eluent and poly(methyl methacrylate)s (PMMA) that LC LCD produces narrow, focused peaks with retention volumes independent of not only polymer molar mass but also, to a large extent, the concentration and volume of the injected sample. Sample capacity of LC LCD is very high, and sample volume can reach as much as 80% of the column pore volume. Reduced sample dilution or even its re‐concentration within the column is important for two‐dimensional separations. Changes in temperature as large as 40 °C only slightly affected retention volumes of the LC LCD‐eluted PMMA. Consequently, the LC LCD method is rather robust and user‐friendly. A practical application of LC LCD for the separation of model polymer blends has been demonstrated. Polystyrene and PMMA of similar molar masses were easily separated in less than four minutes using a small LC LCD column of low efficiency. The LC LCD fractions were successively transported into an on‐line SEC column either directly or after storage in the LC LCD column. The SEC system was equipped with a refractive index detector and a multi‐angle light scattering (MALS) detector. The MALS detector proved a good reproducibility of the molar masses for polymer blend components determined with a combination of LC LCD and SEC. Storage of the fractions within the LC LCD column even for several hours exhibited only a negligible effect on the determined molar mass averages.Scheme of the two‐dimensional chromatograph used. The capillary resistor had a flow resistance similar to that of the SEC column. For further details, see text.imageScheme of the two‐dimensional chromatograph used. The capillary resistor had a flow resistance similar to that of the SEC column. For further details, see text.

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Section: Resultssupporting

confidence: 76%

Section: Practical Application Of Lc Lcdmentioning

confidence: 99%

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Liquid Chromatography of Polymers under Limiting Conditions of Desorption, 3

Šnauko

Berek

2005

Macro Chemistry & Physics

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“…For binary blends of polymethacrylates it was shown that, depending on the polarity of the components, polar or non-polar phases can be used [13,14]. Among other applications, LC-CC can also be used efficiently for the separation of homopolymers with regard to their functional groups as has been shown by Schoenmakers et al [15].…”

Section: Introductionmentioning

confidence: 87%

Development of Fast Gradient Separations for Different Polymethacrylates

Brüll¹,

Pasch

Bashir³

2006

E-Polymers

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Liquid chromatography of polymers is traditionally a slow technique with analysis times of typically 30 min per sample. To adapt liquid chromatographic techniques to combinatorial materials research the sample throughput must be significantly increased. Preferably, the analysis time per sample is to be reduced to a few minutes. Short analysis times can be achieved using high resolution stationary phases, high flow rates, and fast gradients. The present work demonstrates that gradient HPLC of polymethacrylates can be accomplished in less than 2 min. The fast separation of poly(methyl methacrylate), poly(i-propyl methacrylate), poly(n-butyl methacrylate), poly(tbutyl methacrylate), and poly(n-decyl methacrylate) is conducted on a short monolithic stationary phase using a flow rate of up to 7 mL/min. The optimization of the gradient is conducted by running a number of linear gradients and by simulating an optimum step gradient. Further modification of the simulated gradient results in the desired short analysis times.

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“…Under this mode, the elution volume of the block copolymer increased exponentially with the length of the ''visible'' block, which limits the application to only analysis of short ''visible'' block (or end-group analysis). [23,41,42] In the other mode, the block copolymer elutes in size exclusion regime, i.e. before the system peak, when the ''visible'' block is less interactive with the column.…”

Section: Establishment Of Lccc For Polyma Homopolymersmentioning

confidence: 99%

Characterization of Linear and 3‐Arm Star Block Copolymers by Liquid Chromatography at Critical Conditions

Gao

Min

Matyjaszewski

2006

Macro Chemistry & Physics

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Summary: LCCC for polyMA homopolymers was established in order to analyze the polyMA‐polySt linear and star block copolymers. The validity of the assumption that under the LCCC for polyMA, the polyMA segment in the polyMA‐containing block copolymer is chromatographically “invisible” was verified. It was found that within the scale of investigation ($\overline M _{{\rm n},{\rm polyMA}} \leq 5\;\overline M _{{\rm n},{\rm polySt}}$), the molecular weight and architecture of the polyMA segments had no evident influence on the retention behavior of the polySt‐polyMA block copolymers and the polyMA block in the copolymer was “invisible”. The critical conditions of polyMA were used for quantitative analysis of the polySt block in the linear and 3‐arm star polyMA‐polySt block copolymers, which were synthesized by AGET ATRP in miniemulsion. It was shown that the copolymer had completely different elution peak from its MI. The calculated molecular weights of polySt blocks in the block copolymers were similar to those obtained from normal SEC analysis. Transferring the eluates from the LCCC (the first dimension) column to a SEC column (the second dimension) produced LCCC × SEC two‐dimensional chromatogram, which contained information on both chemical composition and molecular weight of the synthesized copolymers. The combination of these liquid chromatography methods clearly confirmed the high initiation efficiency of the polyMA MIs during the synthesis of block copolymers and the presence of a byproduct formed by radical‐radical coupling. magnified image

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Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate)

Cited by 37 publications

References 33 publications

Liquid Chromatography of Polymers under Limiting Conditions of Desorption, 3

Liquid Chromatography of Polymers under Limiting Conditions of Desorption, 3

Development of Fast Gradient Separations for Different Polymethacrylates

Characterization of Linear and 3‐Arm Star Block Copolymers by Liquid Chromatography at Critical Conditions

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