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23 protocols using pl gel 5 μm mixed c columns

1

Molecular Weight Characterization of PGMA-PTFEMA Polymers

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The molecular weights
and polydispersities of the PGMA macro-CTAs and selected PGMAx–PTFEMAy diblock copolymers were determined by DMF GPC operating at 60 °C.
The setup comprised two Polymer Laboratories PL gel 5 μm Mixed
C columns connected in series to a Varian 390 LC multidetector suite
(refractive index and ultraviolet detector) and a Varian 290 LC pump
injection module. The GPC eluent was HPLC-grade DMF containing 10
mmol of LiBr with a flow rate of 1.0 mL min–1. DMSO
was used as a flow rate marker, and six near-monodisperse PMMA standards
(Mp = 625–489 000 g mol–1) were used for calibration. Chromatograms were analyzed
using Varian Cirrus GPC software (version 3.3).
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2

Molecular Weight Analysis of Macro-CTAs and Diblock Copolymers

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The molecular weights and dispersities of the three
macro-CTAs and diblock copolymers were determined by DMF GPC at 60
°C. The GPC setup consisted of two Polymer Laboratories PL gel
5 μm Mixed C columns connected in series to a Varian 390 LC
multidetector suite (refractive index detector) and a Varian 290 LC
pump injection module. The mobile phase was HPLC-grade DMF containing
10 mmol of LiBr at a flow rate of 1.0 mL min–1.
Copolymer solutions (1.0% w/v) were prepared in DMF using DMSO as
a flow rate marker. Ten near-monodisperse poly(methyl methacrylate)
standards (PMMA; Mn = 625–618 000
g mol–1) were used for calibration. Data were analyzed
using Varian Cirrus GPC software (version 3.3). The PMAA85–PNMEPx diblock copolymers were
methylated prior to GPC analysis.
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3

PMMA Molecular Weight Characterization

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Molecular weights and dispersities were determined using either DMF or THF GPC. The DMF GPC set-up comprised two Polymer Laboratories PL gel 5 μm Mixed C columns operating at 60 °C and connected in series to a Varian 390 LC multi-detector suite (only the refractive index detector was utilised) and a Varian 290 LC pump injection module. The GPC eluent was HPLC-grade DMF containing 10 mM LiBr at a flow rate of 1.0 mL min–1. DMSO was used as a flow-rate marker. Calibration was conducted using a series of ten near-monodisperse poly(methyl methacrylate) standards (Mn = 645–618 000 g mol–1). Chromatograms were analysed using Varian Cirrus GPC software (version 3.3) provided by the instrument manufacturer (Agilent). The THF GPC set-up comprised two 5 μm (30 cm) Mixed C columns and a WellChrom K-2301 refractive index detector operating at 950 ± 30 nm. The mobile phase contained 2.0% v/v triethylamine and 0.05% w/v butylhydroxytoluene (BHT) and the flow rate was 1.0 mL min–1. A series of ten near-monodisperse poly(methyl methacrylate) standards (Mp values ranging from 645 to 2 186 000 g mol–1) were used for calibration.
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4

Polymer Molecular Weight Determination

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Polymer molecular
weights and polydispersities were determined using a DMF GPC setup
operating at 60 °C and comprising two Polymer Laboratories PL
gel 5 μm Mixed-C columns connected in series to a Varian 390-LC
multidetector suite (only the refractive index detector was utilized)
and a Varian 290-LC pump injection module. The GPC eluent was HPLC-grade
DMF containing 10 mM LiBr at a flow rate of 1.0 mL min–1. DMSO was used as a flow-rate marker. Calibration was conducted
using a series of 10 near-monodisperse poly(methyl methacrylate) standards
(Mn = 625–2 480 000
g mol–1). Chromatograms were analyzed using Varian
Cirrus GPC software (version 3.3).
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5

Molecular Weight Analysis of Polymers

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Molecular weight distributions
were assessed for the PGMA50 precursor, the PGMA50-PMMA80 diblock copolymer by GPC analysis, and the PGMA50-PTFEMA80 diblock copolymer at 60 °C using
DMF eluent (containing 10 mM LiBr), two Agilent PL gel 5 μm
Mixed-C columns connected to a Varian 290-LC pump injection module,
and a Varian 390-LC multidetector suite (refractive index detector).
A series of near-monodisperse poly(methyl methacrylate) standards
ranging from Mn = 645 g mol–1 to 618 000 g mol–1 were used for calibration
at a flow rate of 1.0 mL min–1.
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6

Polymer Molecular Weight Characterization

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Copolymer molecular
weights and polydispersities were determined using a DMF GPC setup
operating at 60 °C and comprising two Polymer Laboratories PL
gel 5 μm Mixed C columns connected in series to a Varian 390
LC multidetector suite (only the refractive index detector was utilized)
and a Varian 290 LC pump injection module. The GPC eluent was HPLC
grade DMF containing 10 mM LiBr at a flow rate of 1.0 mL min–1. DMSO was used as a flow-rate marker. Calibration was conducted
using a series of ten near-monodisperse poly(methyl methacrylate)
standards (Mn = 625–618 000
g mol–1). The chromatograms were analyzed using
Varian Cirrus GPC software (version 3.3) provided by the instrument
manufacturer (Polymer Laboratories).
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7

Molecular Weight Characterization of Copolymers

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Copolymer molecular weights and polydispersities were determined using a DMF GPC set-up operating at 60 °C and comprising two Polymer Laboratories PL gel 5 μm Mixed C columns connected in series to a Varian 390 LC multi-detector suite (only the refractive index detector was utilized) and a Varian 290 LC pump injection module. The GPC eluent was HPLC grade DMF containing 10 mM LiBr at a flow rate of 1.0 mL min–1. DMSO was used as a flow-rate marker. Calibration was conducted using a series of ten near-monodisperse poly(methyl methacrylate) standards (Mn = 625–618 000 g mol–1). The chromatograms were analyzed using Varian Cirrus GPC software (version 3.3) provided by the instrument manufacturer (Polymer Laboratories).
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8

Polymer Molecular Weight Analysis by GPC

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Polymer molecular
weights and polydispersities were determined using a DMF GPC setup
operating at 60 °C and comprising two Polymer Laboratories PL
gel 5 μm Mixed-C columns connected in series to a Varian 390-LC
multidetector suite (with only the refractive index detector being
used) and a Varian 290-LC pump injection module. The GPC eluent was
HPLC-grade DMF containing 10 mM LiBr at a flow rate of 1.0 mL min–1. DMSO was used as a flow-rate marker. Calibration
was conducted using a series of ten near-monodisperse poly(methyl
methacrylate) standards (Mn = 625–2 480 000
g mol–1). Chromatograms were analyzed using Varian
Cirrus GPC software (version 3.3).
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9

Polymer Molecular Weight Analysis by GPC

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Polymer molecular weights and dispersities were determined using a DMF GPC set-up operating at 60 °C and comprising two Polymer Laboratories PL gel 5 μm Mixed-C columns connected in series to a Varian 390-LC multidetector suite (only the refractive index detector was utilized) and a Varian 290-LC pump injection module. The GPC eluent was HPLC-grade DMF containing 10 mM LiBr at a flow rate of 1.0 mL min–1. Calibration was conducted using a series of ten near-monodisperse poly(methyl methacrylate) standards (Mn = 625–2 480 000 g mol–1). Aqueous copolymer dispersions were freeze-dried overnight to obtain powders. Copolymer solutions (0.70% w/w) were prepared in DMF containing DMSO (1.0% v/v) as a flow rate marker. Chromatograms were analyzed using Varian Cirrus GPC software (version 3.3).
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10

Molecular Weight Distribution Analysis

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Molecular weight distributions were determined using a DMF gel permeation chromatography (GPC) instrument operating at 60 °C that comprised two Polymer Laboratories PL gel 5 μm Mixed C columns and one PL polar gel 5 μm guard column connected in series to a Varian 390 LC multidetector suite (only the refractive index detector was utilized) and a Varian 290-LC pump injection module. The GPC eluent was HPLC grade DMF containing 10 mM LiBr and was filtered prior to use. The flow rate was 1.0 mL min–1 and DMSO was used as a flow-rate marker. Calibration was conducted using a series of 10 near-monodisperse poly(methyl methacrylate) standards (Mn = 625–618 000 g mol–1). Chromatograms were analyzed using Varian Cirrus GPC software.
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