A gel permeation chromatograph (GPC) was obtained using a TOSOH EcoSEC HLC-8320GPC system (TOSOH Bioscience, Japan) gel permeation chromatograph calibrated with polystyrene standards. ESS solution was prepared in THF at a concentration of 5 mg/mL.
Ecosec hlc 8320gpc system
Manufactured by Tosoh
Sourced in Japan
The EcoSEC HLC-8320GPC system is a high-performance gel permeation chromatography (GPC) instrument developed by Tosoh. It is designed for the analysis of molecular weight distribution and other macromolecular properties of polymers and other large molecules.
Automatically generated - may contain errors
Lab products found in correlation
S 4800 sem, by Hitachi (1 mentions)
208hr sputter coater, by Cressington (1 mentions)
Tsk gel pwxl guard column, by Tosoh (1 mentions)
Tsk gel gmpwxl column, by Tosoh (1 mentions)
500 mhz nmr spectrometer, by Bruker (1 mentions)
Mixed d 300 7.5 mm columns, by Agilent Technologies (1 mentions)
Pl gpc 50 plus system, by Agilent Technologies (1 mentions)
8 protocols using ecosec hlc 8320gpc system
1
Polystyrene-Calibrated GPC Analysis
2
Characterization of Polypeptide Polymers
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The structures of the monomers and
their respective polymers were characterized by 1H NMR
and 13C NMR. A Bruker Avance 400 Hz NMR was used for the
structure determination. All samples were analyzed in CDCl3, and the residual solvent peak was used as the reference (δ
= 7.26 ppm or δ = 77.16 ppm).
The molecular weight (Mn) and dispersity (Đ)
of the synthesized polypeptides were determined by size exclusion
chromatography using a TOSOH EcoSEC HLC-8320 GPC system equipped with
3 columns (PSS PFG 5 μm; Microguard, 100 and 300 Å) from
PSS GmbH and an EcoSEC RI detector. The eluent was 0.01 M LiBr in
DMF (0.2 mL/min), and the measurements were performed at 50 °C.
Broad and linear poly(methyl methacrylate) standards were used for
the calibration, and toluene was used as the internal standard.
The morphology of the particles was determined by scanning electron
microscopy (SEM) using a Hitachi S-4800 SEM. The samples were sputter-coated
with Ag/Pd (Cressington 208HR sputter-coater). An accelerating voltage
of 0.7–1.0 kV was used. The size of the particles is reported
as the mean diameter of 10 particles.
their respective polymers were characterized by 1H NMR
and 13C NMR. A Bruker Avance 400 Hz NMR was used for the
structure determination. All samples were analyzed in CDCl3, and the residual solvent peak was used as the reference (δ
= 7.26 ppm or δ = 77.16 ppm).
The molecular weight (Mn) and dispersity (Đ)
of the synthesized polypeptides were determined by size exclusion
chromatography using a TOSOH EcoSEC HLC-8320 GPC system equipped with
3 columns (PSS PFG 5 μm; Microguard, 100 and 300 Å) from
PSS GmbH and an EcoSEC RI detector. The eluent was 0.01 M LiBr in
DMF (0.2 mL/min), and the measurements were performed at 50 °C.
Broad and linear poly(methyl methacrylate) standards were used for
the calibration, and toluene was used as the internal standard.
The morphology of the particles was determined by scanning electron
microscopy (SEM) using a Hitachi S-4800 SEM. The samples were sputter-coated
with Ag/Pd (Cressington 208HR sputter-coater). An accelerating voltage
of 0.7–1.0 kV was used. The size of the particles is reported
as the mean diameter of 10 particles.
3
Molecular Weight Determination of γ-PGA
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Concentration and mass average molecular weight (Mw) of γ-PGA was determined by gel permeation chromatography (GPC). The GPC was equipped with a TSKgel GMPWxl column (300 × 7.8 mm, Tosoh Bioscience GmbH, Griesheim, Germany) and a TSKgel PWxl guard column (40 × 6 mm, Tosoh Bioscience GmbH, Griesheim, Germany). The column was eluted with 30 mM KNO3 at 40 °C at a flow rate of 1.0 mL min−1. Peaks were detected with the RI detector of the integrated EcoSEC HLC-8320GPC system (Tosoh Bioscience GmbH, Griesheim, Germany). Data analysis was performed with the software WinGPC UniChrom (PSS Polymer Standards, Service GmbH, Mainz, Germany). Poly(ethylene oxide) standards with peak molecular weights (Mp) in the range of 56 to 1015 kDa (PSS Polymer Standards, Service GmbH, Mainz, Germany) were used to create a calibration curve for molecular weight. γ-PGA sodium salt (cosmetic grade; kindly provided by Henkel AG & Co. KGaA, Düsseldorf, Germany) was used to create a calibration curve to determine concentrations. Culture broth was diluted 1:50 with distilled water and filtered with 0.2 μm filters (Bulk GHP Acrodisc 13 mm syringe filter, GHP membrane, N° 4567, Pall Life Sciences, Dreieich, Germany). 30 μL of the standards and of the filtrated samples were injected.
4
Determining Purity and Molecular Weight of Hulless Barley Grass Polysaccharide
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The determination of the purity of hulless barley grass polysaccharide was performed according to the method of Liu et al. [28 (link)]. HBGP (5 mg, d.b.) was dissolved in distilled water (1 mL) and passed through a filter (0.45 μm). The purity of HBGP was analyzed on a Waters Alliance e2695 High Performance Liquid Chromatography (HPLC) system equipped with a Waters 2414 differential detector and SUGAR KS-805 Shodex® sugar column (8.0 mm ID × 300 mm L).
The molecular weight of HBGP was analyzed according to a previously described procedure [28 (link)]. The molecular weight of soluble HBGP was analyzed on an EcoSEC HLC-8320 GPC system (TOSOH Co., Tokyo, Japan), equipped with an EcoSEC refractive index detector. Dextran with different molecular weights (4400, 9900, 21,400, 43,500, 12,400, and 805,000 Da) was used to produce a standard curve to calculate the molecular weight of HBGP.
The molecular weight of HBGP was analyzed according to a previously described procedure [28 (link)]. The molecular weight of soluble HBGP was analyzed on an EcoSEC HLC-8320 GPC system (TOSOH Co., Tokyo, Japan), equipped with an EcoSEC refractive index detector. Dextran with different molecular weights (4400, 9900, 21,400, 43,500, 12,400, and 805,000 Da) was used to produce a standard curve to calculate the molecular weight of HBGP.
5
Polymer Analysis by GPC-RI
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All polymer samples were analysed using a Tosoh EcoSec HLC 8320GPC system with two SuperHM-M columns in series at a flow rate of 0.350 mL min−1. THF was used as the eluent and all number-average molecular weights (Mn), weight-average molecular weights (Mw), dispersities (Đ), asymmetry factors (As), Mz and Mz+1 for the first polystyrene block were calculated from refractive index chromatograms against TSKgel polystyrene standards. Conversions were determined by 1H nuclear magnetic resonance (NMR) spectra obtained on a Bruker 500 MHz NMR spectrometer in CDCl3, as were the Mns for the diblock and triblock copolymers.
6
Oligomer Characterization by GPC
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The number average molar mass (Mn) and dispersity (Đ) of the acetic acid quenched oligomers prior to RCD were analyzed with a Verotech PL-GPC 50 Plus system, equipped with a PL-RI detector and two Mixed-D (300 × 7.5 mm) columns (Varian, Santa Clara). An injection rate of 1 mL min−1 at 30 °C was used with chloroform as the mobile phase. Toluene was used as the internal standard for flow rate fluctuation corrections. Polystyrene standards with a narrow mass distribution and a molecular weight of 160–371 000 g mol−1 were used for calibration.
The product from the condensation reaction between the longer diols and DEC was analyzed with a TOSOH EcoSEC HLC-8320GPC system equipped with a RI detector, and two PSS columns (100 and 300), using N,N-dimethylformamide (DMF) with 0.01 M LiBr as the eluent. The analysis was conducted at 50 °C with a flow rate of 0.2 mL min−1. The results were plotted against linear PMMA standards.
The product from the condensation reaction between the longer diols and DEC was analyzed with a TOSOH EcoSEC HLC-8320GPC system equipped with a RI detector, and two PSS columns (100 and 300), using N,N-dimethylformamide (DMF) with 0.01 M LiBr as the eluent. The analysis was conducted at 50 °C with a flow rate of 0.2 mL min−1. The results were plotted against linear PMMA standards.
7
Polymer Melt Compounding Analysis
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Analysis was performed to assess changes in the molecular weight distribution after melt-compounding. SEC was performed with a TOSOH EcoSEC HLC-8320GPC system equipped with an EcoSEC RI detector and three PSS PFG 5 μm columns (microguard, 100 Ã…, and 300 Ã…). A calibration curve was created using narrow, linear poly(methyl methacrylate) standards ranging from 700 to 2000000 g mol â€"1 . Typical sample concentration was 3 mg/mL, and the flow rate was 1 mL/min at 30 °C. Corrections for flow-rate fluctuations were made using toluene as an internal standard. PSSWinGPC Unity software version 7.2 was used to process data. Each sample was analyzed twice, and the average value was selected.
8
Molecular Weight Distribution Analysis
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The molecular weight distribution was measured at 40 °C with a TOSOH EcoSEC HLC‐8320GPC system (Japan), equipped with an EcoSEC RI detector and three PSS PFG 5 µm columns (microguard, 100, and 300 Å; USA). Poly(methyl methacrylate) (PMMA) standards were used for calibration and toluene was used as an internal standard.
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