Simultaneous determination of phenolic antioxidants in dicyclopentadiene
Abstract
Polydicyclopentadiene is generally a highly crosslinked polymer of high toughness formed by a
ring-opening metathesis polymerization (ROMP) with ruthenium-based catalysts (Grubbs’ catalysts) of its
precursor dicyclopentadiene (DCPD). During operation, storage or transportation the DCPD is exposed to air
oxidation, photo-oxidation, thermal influence. DCPD oxides are a poison for ruthenium catalyst and in the
big amounts can deactivate it. Antioxidants are incorporated into monomers to prevent oxidation, to prevent
degradation of polymers by ultraviolet light, heat, and oxygen; to aid in the processing of polymers; and to
save the physical properties of polymers. Study was carried out to develop a simple, rapid and effective
method for quantitative analysis of phenolic antioxidants in the DCPD and composite monomer based on it.
To estimate system suitability, different solvents in various ratios were tested and it was found that
using water, acetonitrile and isopropanol as a mobile phase is optimal and provides effective separation. The
separation was performed on a column ZORBAX Eclipce XDB-C18 (150×4.5 mm, 5.0 µm) at a flow-rate
1.0 mL/min. The determination was performed with a UV-Vis detector at 276 nm. The volume of the injected
sample was 20 µL. The method is linear for all compounds over the concentration range tested, and shows
good precision and accuracy. Recovery studies showed good results for all substances (96–104%). A new
method for simultaneous determination including BHT, Irganox-3114, Irganox-1010, Irgafos-168-F, Irganox1076
and Irgafos-168 in the DCPD of antioxidants was developed using reverse-phase high performance
liquid chromatography. The method was validated with respect to system suitability, accuracy, precision,
linearity and repeatabilities within day and between days and satisfactory results were obtained. The
proposed method can be recommended to apply for the routine determination of these compounds both in
scientific and commercial laboratories.
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