Polymer Testing 31 (2012) 716–721

Contents lists available at SciVerse ScienceDirect

Polymer Testing
journal homepage: www.elsevier.com/locate/polytest

Analysis method

Determination of epoxy equivalent weight of glycidyl ether based

epoxides via near infrared spectroscopy
Monoj Pramanik, Sharathkumar K. Mendon, James W. Rawlins*
School of Polymers and High Performance Materials, The University of Southern Mississippi, 118 College Drive #5217, Hattiesburg, MS 39406-0001, USA

a r t i c l e i n f o a b s t r a c t

Article history: A method to quantify the epoxy equivalent weights (EEW) of glycidyl ether-based epoxides
Received 1 March 2012 using near infrared spectroscopy (NIR) in combination with the Lambert–Beer law has
Accepted 10 April 2012 been developed and validated by NMR and titration studies (ASTM D 1652). EEWs of
a series of commercial aromatic epoxy prepolymers based on diglycidyl ether of bisphenol-
Keywords: A (DGEBA) and aliphatic epoxy prepolymers based on polypropylene glycol were deter-
Near infrared spectroscopy
mined via NIR. For instance, the commercial epoxide, Epon 828, was determined to possess
Epoxy equivalent weight
an EEW of 186.44
0.15 and 185.43
2.55 via titration and NIR, respectively. Furthermore,
Lambert–Beer’s law
Molar absorptivity the method was also validated to be applicable to determining EEW of rubber toughened
Glycidyl ether based epoxide epoxy prepolymers for two commercial materials. The results were supported and
consistent with the EEW reported by the suppliers. NIR technique has been confirmed to
be an excellent and rapid method to characterize epoxides as it is non-destructive and
does not require the use of solvents or other chemicals.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction characterize epoxides [1–6]. Titration is a convenient

technique but requires chemicals such as perchloric acid
Epoxides are widely used in coatings, adhesives, or hydrobromic acid. 1H NMR (based on epoxy ring
composites, electrical systems, electronics, and marine and protons) has been reported to be a useful technique for
aerospace applications. Its wide range of availability (low to determining EEWs. Cure kinetics of epoxy prepolymers via
high molecular weights, liquids to solids), simple reaction mid-IR spectroscopy has been reported [7,8], however,
with various crosslinking agents such as amines, hydroxyls, the presence of overlapping bands often complicates
carboxyls, etc., and its ability to provide flexible or rigid quantification of component reactions. Near IR (NIR)
materials depending on the crosslinking agent enable spectroscopy has been used to characterize distinct bands
epoxides to be employed in a broad range of applications. for epoxide, primary amine, phenyl, combined primary-
Most epoxides for use as prepolymers are the reaction secondary amine and hydroxyl groups of epoxy-amine
products of epichlorohydrin and phenols or alcohols. systems, and to study cure kinetics for the reaction
Proper utilization of epoxy precursors require them to be between epoxy prepolymers and primary amines [9–18].
formulated in stoichiometric proportions with various Peck et al. determined the epoxy content of commercial
crosslinking agents. Consequently, the epoxy content or bisphenol-A-based epoxy prepolymers via NIR spectros-
epoxy equivalent weight (EEW) of each epoxy material is copy after dissolving the prepolymers in chloroform [6].
a critical value that each formulator needs to know accu- With higher molecular weight materials, chloroform is not
rately. Titration, nuclear magnetic resonance (NMR) spec- always appropriate as a solvent choice thus the use of
troscopy and infrared spectroscopy (NIR) have been used to solvents is restrictive in that it involves an extra step of
determining a solvent in which the epoxy prepolymer is
* Corresponding author. Tel.: þ1 601 266 4781; fax: þ1 601 266 5880. completely soluble. Moreover, epoxy prepolymers (espe-
E-mail address: james.rawlins@usm.edu (J.W. Rawlins). cially those employed in composite applications) are often

0142-9418/$ – see front matter Ó 2012 Elsevier Ltd. All rights reserved.
doi:10.1016/j.polymertesting.2012.04.004
 M. Pramanik et al. / Polymer Testing 31 (2012) 716–721 717

modified with tougheners such as core-shell rubber parti- via the integrating sphere in combination with the OMNIC
cles or silica nanoparticles to enhance fracture toughness. version 7.3 software.
Therefore, a non-destructive NIR method that is applicable
to epoxy materials as supplied would be advantageous in 2.3. Epoxy titration
determining the epoxy content of commercial epoxy
prepolymers. The commercial epoxides were titrated as per ASTM D
The goal of this work was to examine the applicability of 1652 to determine their respective EEW values. 100 g of
NIR spectroscopy in conjunction with the Lambert–Beer tetraethylammonium bromide was dissolved in 400 mL
law to quantify epoxy content (EEW) of epoxide materials glacial acetic acid. 0.5318 g of Epon 825 was dissolved in
as supplied. The epoxy prepolymers that were evaluated 10 mL methylene chloride in a 150 mL flask. 10 mL of the
include those based on bisphenol-A and polypropylene above tetraethylammonium bromide solution was then
glycol as well as those containing dispersed tougheners, added to the flask containing Epon 825. Seven drops of
and the results were compared directly with the values crystal violet indicator were added to the same flask, stirred
obtained via titration (ASTM D 1652), NMR, and those well and titrated against 0.1 N perchloric acid solution to an
reported in suppliers’ data sheets. end point transition from sharp blue to green. The other
epoxy prepolymers were also titrated.
2. Materials and methods
2.4. Proton NMR spectroscopy
2.1. Materials
Proton NMR spectra were obtained using a Varian
Diglycidyl ether of bisphenol-A (DGEBA) based epoxy mercury NMR spectrometer operating at a frequency of
prepolymers (EponÒ825, Epon 828, Epon 1001F, Epon 300.13 MHz. Typical 1H NMR acquisition parameters were
1002F, Epon 1004F, Epon 1007F and Epon 1009F) were as follows: recycle delay of 1 s, 7.1 ms pulse width corre-
donated by Hexion (Momentive). Epon 825 and Epon 828 sponding to a 45 flip angle, and acquisition time of 2 s. All
are liquid materials while the other epoxy prepolymers are chemical shifts (indicated as d ppm) were referenced either
solid polyepoxides at ambient temperature. The basic automatically by the software (VNMR 6.1C) or manually
structure of the DGEBA-based epoxy prepolymers, i.e., using the resonance frequency of the deuterated solvent
Epon 825 – Epon1009F is shown in Fig. 1. D.E.R.Ô 732, (CDCl3).
a polypropylene glycol-based (aliphatic) liquid epoxy pre-
polymer, was supplied by Dow Chemicals. Kane AceÒMX- 3. Results and discussion
125, a 25 wt% core-shell rubber dispersed within a liquid
epoxy prepolymer was donated by Kaneka Texas Corpora- 3.1. Near infrared spectra of diglycidyl ether of bisphenol-A
tion. PolydisÒ 3604, a 40 wt% rubber dispersed liquid epoxy based epoxides
prepolymer, was supplied by Struktol Company of America.
Chemicals for titration and NMR characterization, i.e., Fig. 2 displays the NIR spectra obtained for the epoxides.
perchloric acid (0.1 N), tetraethylammonium bromide and Weak absorption at 7001 cm1 is attributed to the 1st
chloroform-d were purchased from Ricca Chemical overtone of –OH stretching (z2  3507) [19]. The bands
Company, EMD Chemicals and Acros Organics, respectively. observed at 6071 and 4530 cm1 are ascribed to the 1st
Glacial acetic acid, methylene chloride and Crystal Violet overtone of terminal –CH2– stretching (z2  3056) and
indicator were procured from Fisher Scientific. combination between the epoxy –CH2– stretching and the
epoxy –CH2– deformation (z3056 þ 1456 cm1), respec-
tively [19–21]. The bands detected at 5989–5656 cm1 are
2.2. Near infrared (NIR) spectroscopy due to overtones of aromatic C–H (z2  3037) and
aliphatic C–H (z2  2968, 2  2931, 2  2874, 2  2834)
NIR spectra were obtained using an Antaris II, FT-NIR stretching [19,20]. The two bands at 4681 and 4622 cm1
analyzer from Thermo Scientific. Liquid epoxy prepolymer result from the combination of the aromatic C–H and C]C
was sandwiched between two glass micro slides using stretching (z3037 þ 1607, z3037 þ 1509) [19,21].
a specific microscope cover glass designed to act as a spacer
to achieve a standard sample thickness of 0.16 mm. The 3.2. Near infrared spectroscopy in combination with the
solid epoxy prepolymers were melted and sandwiched in Lambert–Beer law to determine epoxy content of glycidyl
a similar fashion. A 0.04 mm thick aluminum strip was used ether based epoxide
as the spacer for low viscosity epoxide, D.E.R 732.
Absorption spectra were recorded in the near infrared It was observed that all of the DGEBA-based epoxy
region of 4000–8000 cm1 (32 scans, resolution 4 cm1) prepolymers exhibited an epoxide band at 4530 cm1

O CH3 OH CH3 O
H2C C CH2 O O CH2 CH CH2 O O CH2 C CH2
H CH3 n CH3 H

Fig. 1. Chemical structure of DGEBA-based epoxy prepolymer.

718 M. Pramanik et al. / Polymer Testing 31 (2012) 716–721

Fig. 2. Near IR spectra of Epon 825, Epon 828, Epon 1001, Epon 1002, Epon 1004, Epon 1007 and Epon 1009.

between the epoxy –CH2– stretching and the epoxy –CH2– specimen preparation. Consequently, if c1 is known, c2 can
deformation. Epoxy concentrations were calculated using be calculated from Eq. (3).
the integrated area under the epoxy peak at 4530 cm1 Concentration is expressed as mol$kg1 in EEW calcu-
using the Lambert–Beer law [19], which is normally lations instead of mol$litre1 in the above equations. For
expressed as: further protocol development, a standard DGEBA-based
epoxy prepolymer was needed with a known concentra-
 
I0 tion expressed in mol$kg1. For this, the EEW of Epon 825
A ¼ log10 ¼ 3 bc (1) was determined via titration. Using it as the standard, the
It
corresponding c values for the other Epon prepolymers
where A, I0, It, 3 , b and c refer to absorbance, intensity were determined from their respective NIR spectra
of incident radiation, intensity of transmitted radiation, applying Eq. (3) (shown in Table 1). From the c (mol/kg)
molar extinction coefficient or molar absorptivity values, EEW can be calculated as:
(litre$mol1$cm1), path length of radiation passed
through the sample and molar concentration (mol$litre1), 1000
EEW ¼ (4)
respectively. Molar extinction coefficient is a unique c
property of each material/functional group at a particular
For validation, the EEWs of the various Epon resins were
frequency and is widely used for quantitative determina-
determined via the standard titration method (Table 1).
tion. Specifically measuring the epoxy is expected to be
Before applying Eq. (3), the condition 3 1 ¼ 32 was veri-
very challenging because of the shifting of the physical
fied by plotting the absorbances of the various Epon resins
state of epoxides from liquid epoxy to crystalline solid
as a function of ct (mol$kg1) using values obtained via
depending their molecular weight and structural backbone.
titration. The linear relationship shown in Fig. 3 was
If two DGEBA-based epoxy prepolymers exhibit absor-
expected as molecular weight increases from Epon 825 to
bances A1 and A2 for their epoxide moiety at 4530 cm1, Eq.
Epon 1009F and confirms the validity of our assumption.
(1) can be reorganized as:
The protocol resulted in quantified EEWs of the various
Epon resins as determined via NIR spectroscopy that cor-
A1 3 1 b1 c1 responded closely to the EEW values obtained via titration.
¼ (2)
A2 3 2 b2 c2 Therefore, the molar extinction coefficient of NIR band at
where 3 1, b1 and c1 are molar extinction coefficient, sample 4530 cm1 due to combination of terminal CH2 stretching
thickness and molar concentration of epoxide, respectively, and deformation is indeed a unique property of DGEBA-
of the first epoxy prepolymer, while 3 2, b2 and c2 are the based epoxy prepolymers, and Eqs. (3) and (4) can be
corresponding values for the second epoxy prepolymer. As employed to determine the EEW of DGEBA-based epoxy
both the epoxy prepolymers are glycidyl ether based, 31 ¼ 32 prepolymer.
for the epoxide band at 4530 cm1 and Eq. (2) becomes:
3.3. 1H NMR spectroscopy to determine epoxy content
A1 b1 c1
¼ (3) of glycidyl ether based epoxide
A2 b2 c2
A1 and A2 are obtained from their respective NIR spectra. The EEWs of the various Epon resins were also
Sample thicknesses b1 and b2 must be recorded during NIR compared with the corresponding EEWs obtained via 1H
 M. Pramanik et al. / Polymer Testing 31 (2012) 716–721 719

Table 1
EEWs, concentration (c, mol$kg1), and absorbances (A) of Epon resins.

Epoxy EEW (titration) Ct (mol/kg) A (NIR) c (mol/kg) using EEW (NIR) using
prepolymera titration Eq. (3) Eq. (4)
E 825 175.89
0.19 5.6851
0.0062 6.9200
0.080 – –
E 828 186.44
0.15 5.3636
0.0043 6.5440
0.076 5.3935
0.0626 185.43
2.55
E 1001F 524.42
1.34 1.9069
0.0048 2.2970
0.047 1.8932
0.0387 528.41
10.81
E 1002F 659.43
0.15 1.5165
0.0004 1.8625
0.026 1.5351
0.0218 651.55
9.27
E 1004F 858.24
2.18 1.1652
0.0029 1.3980
0.016 1.1522
0.0131 867.97
9.93
E 1007F 2083.5
5.50 0.4800
0.0012 0.5820
0.003 0.4797
0.0025 2084.70
10.75
E 1009F 3007.32
8.20 0.3325
0.0009 0.4020
0.003 0.3313
0.0024 3018.23
22.52
a
Epon resins have been coded as E in some places in the text, table and figures.

The specific structural base for a DGEBA prepolymer

whose molecular weight is 340, i.e., one mole of bisphenol-
A reacted with two moles of epichlorohydrin, results in six
protons from two epoxide rings and eight protons from two
benzene rings. Thus, the ratio Rt ¼ (8/6) ¼ 1.33 while the
ratio Rp is expressed as:

I2
Rp ¼ (6)
I1
where I1 and I2 correspond to the intensity of epoxide ring
Fig. 3. NIR absorbance versus concentration (ct) in mol$kg1 (determined protons and aromatic ring protons, respectively. Once the
via titration) with error bars included within each sphere. value of n is known, the value of EEW and molecular weight
Mn can be calculated as shown in Eqs. (7) and (8) [2]:
NMR spectroscopy and technical data provided by the
epoxy prepolymer suppliers. EEW values of the Epon EEW ¼ 142n þ 170 (7)
resins were determined by integrating the glycidyl ether
group protons following the procedure developed by Gra-
cia and Soares [2]. The degree of polymerization (n) of the
Mn ¼ 284n þ 340 (8)
DGEBA-based Epon resins can be calculated using Eqs. (5)
1
and (6) [2]: The H NMR spectra of the various Epon resins are shown

in Fig. 4 while the EEWs derived from the NMR data and
Rp  R t mentioned in the suppliers’ data sheets are shown in Table
n ¼ (5)
Rt 2. It was observed that EEWs of Epon resins obtained via

Fig. 4. 1H NMR spectra of DGEBA-based epoxy prepolymers, Epon 825 – Epon 1009F.
720 M. Pramanik et al. / Polymer Testing 31 (2012) 716–721

Table 2
EEWs, concentrations (c, mol$kg1), absorbances (A) of DER 723, Polydis 3604 and ACE MX 125 epoxy materials.

Epoxy material EEW (titration) A (NIR) c (mol/kg) using Eqs. (2),a or (3) EEW (NIR) EEW (supplier)
DER 732 322.54
3.10 0.9935
0.008 3.2754
0.0280 305.32
2.61 310–330
Polydish 3604 335.06
1.79 3.2950
0.145 2.7158
0.1195 368.92
16.23 w330
ACEMX 125 248.17
0.04 4.7975
0.034 3.9542
0.0284 252.91
1.82 243
11
a
NIR spectrum for DER 732 was recorded at 0.04 mm path length and hence Eq. (2) was applied instead of Eq. (3). DER 732 had very low viscosity and
because the material flowed out when a 0.16 mm spacer was used.

0.50
E825
DER 732
0.45
Polydis 3604
ACE MX 125
0.40

Epoxy
0.35

0.30

Absorbance
0.25

Phenyl
0.20

0.15
Epoxy

0.10

0.05

0.00
8000 7500 7000 6500 6000 5500 5000 4500 4000
Wavenumber (cm-1)

Fig. 5. Near IR spectra of Epon 825, DER 732, Polydis 3604 and ACE MX 125.

NIR spectroscopy are within the data range mentioned by Hence, the epoxy band at 4530 cm1 was employed to
the supplier and very close to the data obtained via 1H NMR apply the Lambert–Beer law in the form of Eqs. (2)–(4) to
spectroscopy. determine the EEWs of DER 732, Polydis 3604 and ACE MX
The NIR spectroscopy methodology was further applied 125 which are compared with the EEW values from the
to a broader range of epoxy containing epoxy precursors, suppliers’ data sheets as well as data obtained via titration
i.e., aliphatic polypropylene glycol-based epoxy prepol- (Table 3). It was noted that the EEWs of DER 732, Polydis
ymer (D.E.R. 732) and two toughener dispersed glycidyl 3604 and ACE MX 125 were very close to values obtained
ether-based epoxy prepolymers, ACE MX-125 and Polydis via titration and data supplied by suppliers. Consequently,
3604. Fig. 5 shows the NIR spectra of DER 732, Polydis 3604 NIR spectroscopy in combination with the Lambert–Beer
and ACE MX 125. The NIR spectra of Polydis 3604 and ACE law can be a viable means of determining the EEWs of
MX 125 were similar in that an epoxy band was noted at glycidyl ether-based epoxy prepolymers, regardless of
w4530 cm1 and phenyl bands were detected at 4681 and backbone chemistry basis, as long as the prepolymer being
4622 cm1 (as was observed with the aromatic based Epon characterized exhibits an epoxy NIR band at 4530 cm1.
prepolymers). The NIR spectrum of D.E.R. 732 did not reveal
any band at 4681 and 4622 cm1 as it lacks the phenyl
4. Conclusions
moiety, but the epoxy band was still noted at 4530 cm1.

DGEBA-based epoxy prepolymers (Epon 828, Epon

1001F, Epon 1002F, Epon 1004F, Epon 1007F, Epon 1009F),
Table 3
EEWs of DGEBA-based epoxy prepolymers determined via NMR and
polypropylene glycol-based epoxy prepolymer (DER 732),
provided by supplier’s data sheet (Hexion or Momentive). rubber dispersed epoxy prepolymer (Polydis 3604) and
core-shell particles dispersed epoxy prepolymer (ACE MX
Epoxy EEW EEW
prepolymer (provided by suppliers) (determined by 1H NMR)
125) exhibited an NIR absorbance band at 4530 cm1 that
was attributed to their glycidyl ether group. Epoxy pre-
Epon 825 175–180 182.30
Epon 828 185–192 194.11 polymers containing a common glycidyl/oxirane band at
Epon 1001F 525–550 574.57 4530 cm1 were characterized on a solid basis and vali-
Epon 1002F 600–700 716.76 dated to possess the same molar extinction coefficient.
Epon 1004 800–950 936.26 Based on this assumption, the EEWs of glycidyl ether-based
Epon 1007 1700–2300 2340.80
Epon 1009 2300–3800 3173.13
epoxy prepolymers were determined directly via NIR
spectroscopy and confirmed to be in good agreement with
 M. Pramanik et al. / Polymer Testing 31 (2012) 716–721 721

the corresponding values obtained via titration and those [8] M. Ghaemy, H.A. Shahriari, S.M.A. Nasab, Study of the cure kinetics
and water absorption of the DGEBA/ODA resin, Iran. Polym. J. 16
reported in the respective technical data sheets provided
(2007) 829–838.
by the suppliers. Additionally, the method is very simple [9] L. Xu, J.H. Fu, J.R. Schlup, In situ near-infrared spectroscopic inves-
and does not require additional chemicals or dissolving the tigation of the kinetics and mechanisms of reactions between
epoxides in solvents. Thus, NIR spectroscopy in combina- phenyl glycidyl ether (PGE) and multifunctional aromatic amines,
Ind. Eng. Chem. Res. 35 (1996) 963–972.
tion with the Lambert–Beer law was confirmed to be [10] C.J. de Bakker, N.A. St John, G.A. George, Simultaneous differential
a viable and simple technique to determine the EEW of scanning calorimetry and near-infrared analysis of the curing of
a variety of glycidyl ether-based epoxy materials. tetraglycidyldiaminodiphenylmethane with diaminodiphenyl
sulfone, Polymer 34 (1993) 716–725.
[11] N.A. St John, G.A. George, Cure kinetics and mechanisms of a tet-
raglycidyl-4,40 -diaminodiphenylmethane/diaminodiphenyl sulfone
Acknowledgement epoxy resin using near IR spectroscopy, Polymer 33 (1992) 2679–
2688.
The authors acknowledge the Office of Naval Research [12] D.J.T. Hill, G.A. George, D.G. Rogers, A systematic study of the
microwave and thermal cure kinetics of the DGEBA/DDS and
for their financial support via Award No. N00014-07-1- DGEBA/DDM epoxy-amine resin systems, Polym. Adv. Technol. 13
1057 and Northrop Grumman Shipbuilding, Inc., Gulfport, (2002) 353–362.
Mississippi for their material donation and support. [13] G. Ragosta, P. Musto, M. Abbate, G. Scarinzi, Reactivity, viscoelastic
behavior and mechanical performances of hybrid systems based on
epoxy resins and reactive polyhedral oligosilsesquioxanes, Polymer
50 (2009) 5518–5532.
References [14] M. Pramanik, J.A. Scott, S.K. Mendon, J.W. Rawlins, Epoxy Matrix
Architecture and Connectivity Characterization, SAMPE, Salt Lake
[1] S.A. Garea, A.C. Corbu, C. Deleanu, H. Iovu, Determination of the City, UT, USA, October 11–14, 2010.
epoxide equivalent weight (EEW) of epoxy resins with different [15] E.W. Fowler, M. Pramanik, J.W. Rawlins, Cure Kinetics of DGEBA-
chemical structure and functionality using GPC and 1H-NMR, Polym. based Epoxy Prepolymer with Various Crosslinkers, SAMPE, Fort
Test. 25 (2006) 107–113. Worth, TX, USA, October 17–20, 2011.
[2] F.G. Garcia, B.G. Soares, Determination of the epoxide equivalent [16] J. Mijovic, S. Andjelic, A study of reaction kinetics by near-infrared
weight of epoxy resins based on diglycidyl ether of bisphenol A spectroscopy. 1. Comprehensive analysis of a model epoxy/amine
(DGEBA) by proton nuclear magnetic resonance, Polym. Test. 22 system, Macromolcules 28 (1995) 2787–2796.
(2003) 51–56. [17] V.I. Raman, G.R. Palmese, Influence of tetrahydrofuran on epoxy-
[3] H. Lee, K. Neville, Handbook of Epoxy Resins, McGrawHill, New amine polymerization, Macromolcules 38 (2005) 6923–6930.
York, 1967. [18] L. Xu, J.H. Fu, J.R. Schlup, In situ near-infrared spectroscopic inves-
[4] B. Dobinson, W. Hofmann, B.P. Stark, The Determination of Epoxide tigation of epoxy resin-aromatic amine cure mechanisms, J. Am.
Groups, Pergamon Press, Oxford, 1969. Chem. Soc. 116 (1994) 2821–2826.
[5] J.G. Dorsey, G.F. Dorsey, A.C. Rutenberg, L.A. Green, Determination of [19] B.G. Min, Z.H. Stachurski, J.H. Hodgkin, G.R. Heath, Quantitative
the epoxide equivalent weight of glycidyl ethers by proton magnetic analysis of the cure reaction of DGEBA/diaminodiphenyl sulfone
resonance spectrometry, Anal. Chem. 49 (1977) 1144–1145. epoxy resins without and with thermoplastic polysulfone modifier
[6] M.C. Paputa Peck, R.O. Carter III, S.B.A. Qaderi, Near-infrared measure- using near infrared spectroscopy, Polymer 34 (1993) 3620–3629.
ments of terminal epoxides in polymer resin systems. I. Analytical [20] C. Billaud, M. Vandeuren, R. Legras, V. Carlier, Quantitative analysis
considerations, J. Appl. Polym. Sci. 33 (1987) 77–86. of epoxy resin cure reaction: a study by near-infrared spectroscopy,
[7] P. Musto, E. Martuscelli, G. Ragosta, P. Russo, P. Villano, Tetrafunc- Appl. Spectrosc. 56 (2002) 1413–1421.
tional epoxy resins: modeling the curing kinetics based on FTIR [21] H.W. Siesler, Y. Ozaki, H. Kawata, H.M. Heise, Near-infrared Spec-
spectroscopy data, J. Appl. Polym. Sci. 74 (1999) 532–540. troscopy, Wiley-VCH, Weinheim, Germany, 2004.