Separate Epoxy Resin Oligomers with Agilent Preparative Gel Permeation Chromatography

Separate Epoxy Resin Oligomers with Agilent Preparative Gel Permeation Chromatography
Separate Epoxy Resin Oligomers with
Agilent Preparative Gel Permeation
Chromatography
Application Note
Materials Testing and Research
Author
Introduction
Graham Cleaver
Preparative gel permeation chromatography (GPC) can be used to separate and
isolate individual components of a sample based on size exclusion. By scaling up
analytical separations, preparative GPC isolates practical quantities of individual
components that can be used in further analysis. The Agilent OligoPore preparative
GPC column is ideally suited to the separation and isolation of individual oligomers
from oligomer distributions and complex mixtures. In this example, the columns are
employed for the fractionation of epoxy oligomers.
Agilent Technologies, Inc.
Verified for Agilent
1260 Infinity
GPC/SEC System
Epoxy Resin Olgomer Analysis
Figure 1 shows the general structure of an epoxy oligomer
such as Epikote 828. This commercial epoxy resin is composed
of two main epoxy oligomers where n = 0 and n = 1, and small
amounts of the mono- and di-epoxy water adducts.
OH
O
O
H3C
O
CH3
CH3
H3C
O
O
O
10
Figure 2.
Figure 1.
General structure of Epikote 828 epoxy resin oligomers.
Initially, the optimum loading of Epikote 828 on the OligoPore
columns was analyzed on an analytical scale. Figure 2 shows
analytical chromatograms at concentrations of 0.5% to
2.0% (w/v). They indicate that Epikote 828 could be analyzed
at a concentration of 2.0% (w/v) without serious loss of
reduction.
Epikote 828, 0.5-2.0% (w/v)
Columns
2 × Agilent OligoPore, 7.5 × 300 mm
(p/n PL1113-6520)
Eluent
THF
Flow rate
1.0 mL/min
Inj vol
100 µL
Detector
UV
System
Agilent PL-GPC 50
18
OligoPore preparative columns were then used to fractionate
and purify the two oligomers from the resin. A preparative
GPC system was set up with a 2 mL injection loop, two
Agilent OligoPore 25 × 300 mm columns and a flow rate of
10.0 mL/min, an approximate ten-fold scale-up over the analytical separation. The flow rate from the columns was split
into two lines, about 0.5 mL/min went to a UV detector, the
remainder of the flow to a waste/fraction collector. The epoxy
resin sample was injected at a concentration of 1.0% (w/v).
Conditions - Analytical
Samples
min
Analytical separation of Epikote 828 on Agilent OligoPore columns
indicates that a 2.0% w/v concentration is appropriate for preparative analysis.
2
Figure 3 shows a chromatogram of Epikote 828 obtained on
the preparative columns indicating the resolution. The sample
was re-run and the two oligomers n = 0 and n = 1 were collected. The fractions were then analyzed on two Agilent
OligoPore analytical columns.
Figure 4 shows the original analytical chromatogram of Epikote
828 run at a concentration of 2.0% (w/v) and an overlay of
analytical chromatograms of the n = 0 and n = 1 oligomers
collected from the Agilent OligoPore preparative GPC columns.
Conditions - Preparative
Samples
Epikote 828, 1.0% (w/v)
Columns
2 × Agilent OligoPore, 25 × 300 mm
(p/n PL1213-6520)
Eluent
THF
Flow rate
10.0 mL/min, about 9.5 mL/min collected;
0.5 mL/min to the detector
Inj vol
2 mL
Detector
UV
System
PL-GPC 50
10
Figure 4.
min
18
Epikote 828 analytical chromatogram from Figure 1 run at
2.0% (w/v) compared to overlaid analytical chromatograms of the
n = 0 and n = 1 oligomers collected from the Agilent preparative
GPC system.
Conclusions
Low pore size preparative GPC columns from Agilent can be
used to isolate individual oligomers from complex samples
after method development with an equivalent analytical-scale
column.
For More Information
10
Figure 3.
min
These data represent typical results. For more information on
our products and services, visit our Web site at
www.agilent.com/chem.
20
Epikote 828 separated on an Agilent OligoPore two-column set.
3
www.agilent.com/chem
Agilent shall not be liable for errors contained herein or for incidental or consequential
damages in connection with the furnishing, performance, or use of this material.
Information, descriptions, and specifications in this publication are subject to change
without notice.
© Agilent Technologies, Inc., 2015
Printed in the USA
April 30, 2015
5990-8606EN
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