Gel Permeation

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Isao Noda - One of the best experts on this subject based on the ideXlab platform.

Alan Brookes - One of the best experts on this subject based on the ideXlab platform.

  • polyolefin characterization in dibutoxymethane by high temperature Gel Permeation chromatography with a new evaporative light scattering detector
    Polymer Testing, 2017
    Co-Authors: Adrian Boborodea, Alan Brookes
    Abstract:

    Abstract A new evaporative light scattering detector (ELSD) for the analysis of polyolefins by high temperature Gel Permeation chromatography (GPC) was recently introduced by Agilent Technologies. For the first time, we investigated the possibility to use this detector to measure the molecular weight distributions (MWD) of different types of polyolefins (polypropylene, linear and low-density polyethylene) in dibutoxymethane (DBM, butylal). These samples were previously characterized by GPC in trichlorobenzene (TCB) with a differential refractive index (DRI) detector in an interlaboratory study conducted by the International Union of Pure and Applied Chemistry (IUPAC) [1], and in a recent publication by GPC with the new ELSD in TCB [2]. The signal to noise of ELSD using DBM is about 10 times lower than that for TCB. However, the ELSD signal power exponent for DBM was measured as 1.35, which is much closer to unity than the value of 1.61 for TCB. After applying the required corrections to linearize the response of the ELSD signal as a function of concentration, similar average molecular weights to those measured in the interlaboratory study using DRI, were obtained for the analyzed resins.

  • investigation of sample preparation for high temperature Gel Permeation chromatography using a low solvent consumption method
    Polymer Testing, 2017
    Co-Authors: Adrian Boborodea, Alan Brookes
    Abstract:

    Abstract The study explored the optimum conditions for sample preparation of polyolefins for high temperature Gel Permeation chromatography (GPC) recommended by ASTM D 6474, and the potential for reducing solvent consumption by using columns with reduced internal diameter. A polypropylene sample with high crystallinity and high molecular weight was selected, because this is one of the most difficult polyolefins to analyze by GPC. Sequences of injections covering 20 h showed that, at 160 °C, 2 h is enough to dissolve this sample, and that the antioxidant concentration is the critical parameter in obtaining reproducible GPC results. By using one column with an internal diameter (ID) of 4.6 mm and a flow rate of 0.3 mL/min, instead of the classical set of 3 columns of 7.5 mm ID and a flow rate of 1 mL/min, the solvent consumption can be reduced to about 10%.

  • Gel Permeation chromatography atmospheric pressure chemical ionization mass spectrometry for characterization of polymer additives
    International Journal of Polymer Analysis and Characterization, 2017
    Co-Authors: Adrian Boborodea, Alan Brookes
    Abstract:

    ABSTRACTThe study presents the possibility to use Gel Permeation chromatography (GPC) with atmospheric pressure chemical ionization (APCI)-mass spectrometry for the analysis of polymer additives having molecular weights up to 2,000 g mol−1. Irganox 1010, Irganox 1035, Irganox 1076, and Irganox 3114 were analyzed in chloroform using 2.1-mm-internal-diameter GPC columns at the optimum flow rate of 50 µL min−1. Based on the chemical formula, the APCI interface combined with chlorine ionization enabled us to predict the expected mass spectrum and to build libraries without needing to inject each additive separately. Quantification limits of about 100 µg of additive in 1 g of polymer (100 ppm) can be reached using single-ion-monitoring methods based on the calculated isotope distribution.

Adrian Boborodea - One of the best experts on this subject based on the ideXlab platform.

  • polyolefin characterization in dibutoxymethane by high temperature Gel Permeation chromatography with a new evaporative light scattering detector
    Polymer Testing, 2017
    Co-Authors: Adrian Boborodea, Alan Brookes
    Abstract:

    Abstract A new evaporative light scattering detector (ELSD) for the analysis of polyolefins by high temperature Gel Permeation chromatography (GPC) was recently introduced by Agilent Technologies. For the first time, we investigated the possibility to use this detector to measure the molecular weight distributions (MWD) of different types of polyolefins (polypropylene, linear and low-density polyethylene) in dibutoxymethane (DBM, butylal). These samples were previously characterized by GPC in trichlorobenzene (TCB) with a differential refractive index (DRI) detector in an interlaboratory study conducted by the International Union of Pure and Applied Chemistry (IUPAC) [1], and in a recent publication by GPC with the new ELSD in TCB [2]. The signal to noise of ELSD using DBM is about 10 times lower than that for TCB. However, the ELSD signal power exponent for DBM was measured as 1.35, which is much closer to unity than the value of 1.61 for TCB. After applying the required corrections to linearize the response of the ELSD signal as a function of concentration, similar average molecular weights to those measured in the interlaboratory study using DRI, were obtained for the analyzed resins.

  • investigation of sample preparation for high temperature Gel Permeation chromatography using a low solvent consumption method
    Polymer Testing, 2017
    Co-Authors: Adrian Boborodea, Alan Brookes
    Abstract:

    Abstract The study explored the optimum conditions for sample preparation of polyolefins for high temperature Gel Permeation chromatography (GPC) recommended by ASTM D 6474, and the potential for reducing solvent consumption by using columns with reduced internal diameter. A polypropylene sample with high crystallinity and high molecular weight was selected, because this is one of the most difficult polyolefins to analyze by GPC. Sequences of injections covering 20 h showed that, at 160 °C, 2 h is enough to dissolve this sample, and that the antioxidant concentration is the critical parameter in obtaining reproducible GPC results. By using one column with an internal diameter (ID) of 4.6 mm and a flow rate of 0.3 mL/min, instead of the classical set of 3 columns of 7.5 mm ID and a flow rate of 1 mL/min, the solvent consumption can be reduced to about 10%.

  • new evaporative light scattering detector for high temperature Gel Permeation chromatography
    International Journal of Polymer Analysis and Characterization, 2017
    Co-Authors: Adrian Boborodea, Stephen Odonohue
    Abstract:

    ABSTRACTA new evaporative light scattering detector (ELSD) for the analysis of polyolefins by high temperature Gel Permeation chromatography (GPC) was recently introduced by Agilent Technologies. For the first time, we investigated the possibility to use this detector in order to measure the molecular weight distributions (MWD) of different type of polyolefines (polypropylene, linear and low density polyethylene). These samples were previously characterized by GPC with a differential refractive index (DRI) detector by several companies, in an interlaboratory study conducted by International Union of Pure and Applied Chemistry (IUPAC) [1]. The excellent baseline stability of ELSD as compared with DRI was reflected in a better reproducibility of the measured average molecular weights. More importantly, after applying required corrections to linearize the response of the ELSD as a function of concentration, we obtained similar results as previously obtained with DRI for the MWD of analyzed resins, covering t...

  • assessing the suitability of a green solvent for Gel Permeation chromatography mass spectrometry analysis
    International Journal of Polymer Analysis and Characterization, 2017
    Co-Authors: Adrian Boborodea, Stephen Odonohue
    Abstract:

    ABSTRACTThe study presents the possibility of performing the analysis of oligomeric structures and polymer additives by Gel Permeation chromatography (GPC) with atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) in dibuthoxymethane (DBM, butylal), a halogen-free and less hazardous solvent than typically used chloroform and tetrahydrofuran. Polystyrene oligomers and Irganox® additives were analyzed in DBM using 2.1 mm internal diameter GPC columns, allowing to decrease the flow rate down to 50 µL/min, compatible with APCI–MS interface. The ionization was controlled by adding 1% chloroform in DBM to obtain (M+Cl)− adducts, allowing a fast optimization of method parameters.

  • Gel Permeation chromatography atmospheric pressure chemical ionization mass spectrometry for characterization of polymer additives
    International Journal of Polymer Analysis and Characterization, 2017
    Co-Authors: Adrian Boborodea, Alan Brookes
    Abstract:

    ABSTRACTThe study presents the possibility to use Gel Permeation chromatography (GPC) with atmospheric pressure chemical ionization (APCI)-mass spectrometry for the analysis of polymer additives having molecular weights up to 2,000 g mol−1. Irganox 1010, Irganox 1035, Irganox 1076, and Irganox 3114 were analyzed in chloroform using 2.1-mm-internal-diameter GPC columns at the optimum flow rate of 50 µL min−1. Based on the chemical formula, the APCI interface combined with chlorine ionization enabled us to predict the expected mass spectrum and to build libraries without needing to inject each additive separately. Quantification limits of about 100 µg of additive in 1 g of polymer (100 ppm) can be reached using single-ion-monitoring methods based on the calculated isotope distribution.

Kenichi Izawa - One of the best experts on this subject based on the ideXlab platform.

Brice Bouyssiere - One of the best experts on this subject based on the ideXlab platform.