Acrylamide polymerization kinetics in gel electrophoresis capillaries.  A Raman microprobe study

Rapp, Tracey L.; Kowalchyk, Will K.; Davis, Kevin L.; Todd, Elizabeth A.; Liu, Kei Lee; Morris, Michael D.

doi:10.1021/ac00044a023

Cited by 37 publications

(12 citation statements)

References 13 publications

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“…Upon grafting with MAA, bands assignable to polyMAA (indicated with an asterisk in Fig. and summarized in Table S1, Supporting Information, together with their assignments) appeared with increasing intensity at increasing grafting yield. The band at 731 cm −1 appeared the most sensitive to polymer incorporation.…”

Section: Resultsmentioning

confidence: 96%

Stability toward alkaline hydrolysis ofB.morisilk fibroin grafted with methacrylamide

Taddei

Pavoni

Tsukada

2016

J. Raman Spectrosc.

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Bombyx mori silk fibroin fibers were grafted with methacrylamide (MAA) and characterized by Raman and infrared (IR) vibrational spectroscopy before and after hydrolysis in NaOH 5% to elucidate the possible interactions between the two components and the stability of the fibers toward alkaline hydrolysis.Upon grafting, the fibers underwent conformational rearrangements toward a more unordered state and lost orientation at weight gains higher than 60%. Vibrational spectroscopy disclosed the occurrence of intermolecular interactions (mainly hydrogen bonds) between B. mori silk fibroin and polyMAA in the grafted fibers, and the formation of covalent bonds has been explored.These strong interactions made the grafted fibers as a whole more stable toward alkaline hydrolysis because they prevented the solubilization of the polymer upon hydrolysis and made slower the transformation of its CONH 2 groups into COOH and COO À groups.Upon hydrolysis, silk fibroin underwent an enrichment in the β-sheet crystalline domains, because of the preferential removal of the unordered domains, which were more prone to the OH À attack. IR and Raman spectroscopy proved valid techniques to investigate the degradation mechanism and kinetics of grafted silk fibroin fibers and so for designing high-performing silk-based materials. The A 731 /A 1004 Raman intensity ratio was proposed to spectroscopically evaluate the composition of the grafted samples; its value was found to linearly increase with weight gain (R 2 = 0.998), envisaging the possibility of using Raman spectroscopy as a routine analytical technique for qualitative and quantitative characterization of grafted industrial samples.

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Section: Resultsmentioning

confidence: 96%

Stability toward alkaline hydrolysis ofB.morisilk fibroin grafted with methacrylamide

Taddei

Pavoni

Tsukada

2016

J. Raman Spectrosc.

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“…There were no details of the nature of the polymer phase reported in the above mentioned study. Polymer obtained by chemical methods (using ammonium persulfate as reaction initiator and tetramethyl‐ethylenediamine as a catalyst) with crosslinker was found to be a gel and the one without the crosslinker was a solid linear polymer. The polyacrylamide retrieved through pressure‐induced polymerization is found to be a solid polymer rather than a gel as it is an addition polymerization.…”

Section: Resultsmentioning

confidence: 99%

“…Polymerization of acrylamide (C 3 H 5 NO) by chemical methods, shear deformation, x‐ray irradiation and shock wave loading, etc, have been reported in the literature . Solid‐state polymerization under x‐ray irradiation are reported to be brought about by the absorption of radiation and generation of free radicals which react further to form polymer .…”

Section: Introductionmentioning

confidence: 99%

Hydrogen bonds and polymerization in acrylamide under pressure

Sharma

Murli

Sharma

2013

J Raman Spectroscopy

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Acrylamide (C3H5NO), a hydrogen‐bonded amide, is an important compound from the point of view of basic and material research. It can be used as a model system for studying hydrogen bonding interactions in amides under pressure. As it is a monomer of polyacrylamide, an important polymer, high pressure investigation of polymerization in this material is also of interest. Our in‐situ high pressure Raman spectroscopic investigations of acrylamide carried out up to 17 GPa under quasi‐hydrostatic conditions indicate possible structural variations through the reconstruction of the N‐H‐‐‐O hydrogen bonds at pressures above 2.6 GPa. Emergence of several new spectral features at higher pressures indicate onset of polymerization. The characteristic polymer band becomes discernible at ~17 GPa. The increase in the relative intensity of the polymer peaks with respect to the monomer peaks on release to ambient conditions suggests that higher fraction of polymer is obtained on decompression. Copyright © 2013 John Wiley & Sons, Ltd.

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“…In studies of acrylamide/bisacrylamide copolymerization, the degree of cyclization was found to be as high as 80%, with average reactivity of pendant vinyl groups decreasing with increasing crosslinker concentration [30,31]. Polymerization conditions such as temperature [32] and monomer reactivity [33], as well as monomer concentration [34], cross-linker concentration [35], swelling behavior [36], and confinement within capillary tubes [37] also influence reaction kinetics and gel pore structure.…”

Section: Introductionmentioning

confidence: 99%

Usingin situ rheology to characterize the microstructure in photopolymerized polyacrylamide gels for DNA electrophoresis

Jian

Ugaz

2006

Electrophoresis

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Photopolymerized cross-linked polyacrylamide hydrogels are attractive sieving matrix formulations for DNA electrophoresis owing to their rapid polymerization times and the potential to locally tailor the gel pore structure through spatial variation of illumination intensity. This capability is especially important in microfluidic systems, where photopolymerization allows gel matrices to be precisely positioned within complex microchannel networks. Separation performance is also directly related to the nanoscale gel pore structure, which is in turn strongly influenced by polymerization kinetics. Unfortunately, detailed studies of the interplay among polymerization kinetics, mechanical properties, and structural morphology are lacking in photopolymerized hydrogel systems. In this paper, we address this issue by performing a series of in situ dynamic small-amplitude oscillatory shear measurements during photopolymerization of cross-linked polyacrylamide electrophoresis gels to investigate the relationship between rheology and parameters associated with the gelation environment including UV intensity, monomer and cross-linker composition, and reaction temperature. In general, we find that the storage modulus G' increases with increasing initial monomer concentration, cross-linker concentration, and polymerization temperature. The steady-state value of G', however, exhibits a more complex dependence on UV intensity that varies with gel concentration. A simple model based on rubber elasticity theory is used to obtain estimates of the average gel pore size that are in surprisingly good agreement with corresponding data obtained from analysis of DNA electrophoretic mobility in gels cast under identical polymerization conditions.

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Acrylamide polymerization kinetics in gel electrophoresis capillaries. A Raman microprobe study

Cited by 37 publications

References 13 publications

Stability toward alkaline hydrolysis ofB.morisilk fibroin grafted with methacrylamide

Stability toward alkaline hydrolysis ofB.morisilk fibroin grafted with methacrylamide

Hydrogen bonds and polymerization in acrylamide under pressure

Usingin situ rheology to characterize the microstructure in photopolymerized polyacrylamide gels for DNA electrophoresis

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