Simultaneous DSC-FTIR spectroscopy : comparison of cross-linking kinetics of an epoxy/amine resin system

Surya D. Pandita; Liwei Wang; Ramani S. Mahendran; Venkata R. Machavaram; Muhammad S. Irfan; Dee Harris; Gerard F. Fernando

doi:10.1016/j.tca.2012.04.024

Simultaneous DSC-FTIR spectroscopy : comparison of cross-linking kinetics of an epoxy/amine resin system

Surya D. Pandita
, Liwei Wang
, Ramani S. Mahendran
, Venkata R. Machavaram
, Muhammad S. Irfan
, Dee Harris
, Gerard F. Fernando

Metallurgy and Materials

Research output: Contribution to journal › Article › peer-review

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594 Downloads (Pure)

Abstract

The top-cover of a conventional differential scanning calorimeter (DSC) was modified to accommodate two custom-made fibre-optic probes. The function of the probes was to illuminate the sample and reference compartments of the DSC and to return the reflected light from the DSC pans to a fibre-coupled Fourier transform near-infrared (FTIR) spectrometer. The cross-linking kinetics of a commercially available epoxy/amine resin system were studied using the conventional and modified DSC along with conventional transmission FTIR spectroscopy. The cross-linking kinetics and the activation energies for the epoxy/amine resin system obtained via the conventional DSC and simultaneous DSC/FTIR were similar (60.22–60.97 kJ mol−1). However, the activation energy obtained for the cuvette-based conventional transmission FTIR experiments was found to be lower (54.66 kJ mol−1). This may be attributed to the temperature-control attained within the cuvette holder. The feasibility of using a simple fibre-optic probe to link the DSC to the FTIR spectrometer was demonstrated.

Original language	English
Pages (from-to)	9-17
Journal	Thermochimica Acta
Volume	543
DOIs	https://doi.org/10.1016/j.tca.2012.04.024
Publication status	Published - 10 Sept 2012

Keywords

DSC
FTIR spectroscopy
Thermoset
Cross-linking instrumentation

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10.1016/j.tca.2012.04.024

Pandita_Simultaneous_DSC_Thermochimica_Acta_2012
Elsevier Retrospective Gold article. This version is published in Thermochimica Acta, Acta 543 (2012) 9– 17. DOI: http://dx.doi.org/10.1016/j.tca.2012.04.024. This article is licensed under a CC-BY licence. The funders were EPSRC (TS/G000387/1) and the Technology Strategy Board, Projects AB134K, AB135A and BD072K. Eligibility for repository : checked 03/03/2014
Final published version, 1.12 MBLicence: Creative Commons: Attribution (CC BY)

TSB/EPSRC - Environmentally friendly and energy efficient pultrusion
Fernando, G. (Principal Investigator)
TECHNOLOGY STRATEGY BOARD, Engineering & Physical Science Research Council
18/08/08 → 31/07/12
Project: Research

Cite this

@article{04bcf080e4804dbdabbbc12205827249,

title = "Simultaneous DSC-FTIR spectroscopy : comparison of cross-linking kinetics of an epoxy/amine resin system",

abstract = "The top-cover of a conventional differential scanning calorimeter (DSC) was modified to accommodate two custom-made fibre-optic probes. The function of the probes was to illuminate the sample and reference compartments of the DSC and to return the reflected light from the DSC pans to a fibre-coupled Fourier transform near-infrared (FTIR) spectrometer. The cross-linking kinetics of a commercially available epoxy/amine resin system were studied using the conventional and modified DSC along with conventional transmission FTIR spectroscopy. The cross-linking kinetics and the activation energies for the epoxy/amine resin system obtained via the conventional DSC and simultaneous DSC/FTIR were similar (60.22–60.97 kJ mol−1). However, the activation energy obtained for the cuvette-based conventional transmission FTIR experiments was found to be lower (54.66 kJ mol−1). This may be attributed to the temperature-control attained within the cuvette holder. The feasibility of using a simple fibre-optic probe to link the DSC to the FTIR spectrometer was demonstrated.",

keywords = "DSC , FTIR spectroscopy, Thermoset, Cross-linking instrumentation",

author = "Pandita, \{Surya D.\} and Liwei Wang and Mahendran, \{Ramani S.\} and Machavaram, \{Venkata R.\} and Irfan, \{Muhammad S.\} and Dee Harris and Fernando, \{Gerard F.\}",

year = "2012",

month = sep,

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doi = "10.1016/j.tca.2012.04.024",

language = "English",

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journal = "Thermochimica Acta",

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T1 - Simultaneous DSC-FTIR spectroscopy : comparison of cross-linking kinetics of an epoxy/amine resin system

AU - Pandita, Surya D.

AU - Wang, Liwei

AU - Mahendran, Ramani S.

AU - Machavaram, Venkata R.

AU - Irfan, Muhammad S.

AU - Harris, Dee

AU - Fernando, Gerard F.

PY - 2012/9/10

Y1 - 2012/9/10

N2 - The top-cover of a conventional differential scanning calorimeter (DSC) was modified to accommodate two custom-made fibre-optic probes. The function of the probes was to illuminate the sample and reference compartments of the DSC and to return the reflected light from the DSC pans to a fibre-coupled Fourier transform near-infrared (FTIR) spectrometer. The cross-linking kinetics of a commercially available epoxy/amine resin system were studied using the conventional and modified DSC along with conventional transmission FTIR spectroscopy. The cross-linking kinetics and the activation energies for the epoxy/amine resin system obtained via the conventional DSC and simultaneous DSC/FTIR were similar (60.22–60.97 kJ mol−1). However, the activation energy obtained for the cuvette-based conventional transmission FTIR experiments was found to be lower (54.66 kJ mol−1). This may be attributed to the temperature-control attained within the cuvette holder. The feasibility of using a simple fibre-optic probe to link the DSC to the FTIR spectrometer was demonstrated.

AB - The top-cover of a conventional differential scanning calorimeter (DSC) was modified to accommodate two custom-made fibre-optic probes. The function of the probes was to illuminate the sample and reference compartments of the DSC and to return the reflected light from the DSC pans to a fibre-coupled Fourier transform near-infrared (FTIR) spectrometer. The cross-linking kinetics of a commercially available epoxy/amine resin system were studied using the conventional and modified DSC along with conventional transmission FTIR spectroscopy. The cross-linking kinetics and the activation energies for the epoxy/amine resin system obtained via the conventional DSC and simultaneous DSC/FTIR were similar (60.22–60.97 kJ mol−1). However, the activation energy obtained for the cuvette-based conventional transmission FTIR experiments was found to be lower (54.66 kJ mol−1). This may be attributed to the temperature-control attained within the cuvette holder. The feasibility of using a simple fibre-optic probe to link the DSC to the FTIR spectrometer was demonstrated.

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KW - FTIR spectroscopy

KW - Thermoset

KW - Cross-linking instrumentation

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VL - 543

SP - 9

EP - 17

JO - Thermochimica Acta

JF - Thermochimica Acta

ER -

Simultaneous DSC-FTIR spectroscopy : comparison of cross-linking kinetics of an epoxy/amine resin system

Abstract

Keywords

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TSB/EPSRC - Environmentally friendly and energy efficient pultrusion

Cite this