Journal of Chromatography A, 1368 (2014) 199–203
Contents lists available at ScienceDirect
Journal of Chromatography A
j o ur na l ho me page: www.elsevier.com/locate/chroma
Application of inverse gas chromatography in physicochemical
characterization of phenolic resin adhesives
Beata Strzemiecka, Adam Voelkel
∗
, Mateusz Hinz, Mateusz Rogozik
Pozna´ n University of Technology, Institute of Chemical Technology and Engineering, pl. M. Sklodowskiej-Curie 2, 60-965 Pozna´ n, Poland
a r t i c l e i n f o
Article history:
Received 29 July 2014
Received in revised form
24 September 2014
Accepted 25 September 2014
Available online 2 October 2014
Keywords:
Phenolic resins
Degree of hardening
Work of adhesion
Inverse gas chromatography
FTIR
a b s t r a c t
One of the most important stages during production of abrasive tools is their hardening. The degree of
hardening is very important and influence toughness of the final product. During hardening process the
cross-linking of the phenolic resins, used as a binder, occurs. Nowadays, there is no standard, accurate and
simple method for the estimation of the hardening degree of abrasive tools. The procedure of the deter-
mination of hardening degree of the binder (phenolic resins) by means of inverse gas chromatography
(IGC) was presented in this paper. Results obtained by use of IGC derived method was verified by Soxhlet
extraction and by FTIR method. Good agreement was found for results from IGC and Soxhlet extraction
whereas those from FTIR were much lower. FTIR method supplies data concerning bulk properties not
the surface as in case of IGC and Soxhlet methods. These results indicate that resins are more cross-linked
on the surface than inside the material.
© 2014 Elsevier B.V. All rights reserved.
1. Introduction
The production of the abrasive materials includes the fol-
lowing stages: covering of abrasive materials by wetting agent,
addition of the filler with the binding material, mixing of the
components, stabilization of the composition and the hardening.
The most important processes influencing the properties of the
final product are the coverage of the abrasive materials, mixing
and proper hardening [1,2]. The homogeneity of the mixture of
semi-product increases the quality of the final product. The effec-
tiveness of the hardening process depends also on the applied
temperature programme. Although the determination of wettabil-
ity of abrasive materials is relatively simple, the controlling of the
hardening process is much more complicated. There is no easy
standard industry method for controlling the hardening degree
of such complex composites [3]. Brinell test is the most com-
monly used test for assessment of hardness of abrasive tools. This
method suffers from several disadvantages. The main disadvan-
tage of this standard method is its very low repeatability and
accuracy in case of such composites as abrasive tools. The results
depend strongly on the place of ball pressing. Moreover, only final
hardness of abrasive tool can be assessed. It is not possible to
∗
Corresponding author.
E-mail addresses: Adam.Voelkel@put.poznan.pl, adamvoelkel@wp.pl
(A. Voelkel).
monitor the hardening process on-line. Viscoelastic parameters
can be also applied for estimation of the degree of hardening. This
method needs to use expensive equipment for dynamic rheolo-
gical measurements. Moreover, it can be applied only for resins
without additives or with nano/microfillers. The presence of filler
nano/microparticles in resins can influence the rheological param-
eters significantly.
Inverse gas chromatography is an extension of classic gas chro-
matography [4–8]. The word “inverse” means that the examined
material is placed in the chromatographic column and its proper-
ties are determined based on the retention behaviour of carefully
selected test compounds. Inverse gas chromatography method is
widely used for characterization of polymers and polymer blends
[8], surfactants [9,10], biopolymers, solid food and petroleum
pitches [1]. Inverse gas chromatography can be divided into inverse
gas liquid and inverse gas solid chromatography. The obvious cri-
terion of such discrimination is the state of the examined material
placed in the column. The dominating retention mechanism is
related to the temperature of IGC experiment. Polymeric materials
might be characterized by using both surface parameters (surface
free energy, surface acid/base properties and bulk parameters).
The pertinence of IGC measurements to surface or bulk properties
clearly depends on whether or not the probe molecules can diffuse
into the bulk during the experiment. Retention volume measured
at the temperature of IGC experiment higher than T
g
of the exam-
ined polymer (or blend) results from the sum of surface and bulk
sorption. Below T
g
mainly from the adsorption of probe molecules
http://dx.doi.org/10.1016/j.chroma.2014.09.069
0021-9673/© 2014 Elsevier B.V. All rights reserved.