Exploring complex transitions between polymorphs on a small scale by coupling AFM, FTIR and DSC: the case of Irganox 1076® antioxidant

Saunier, Johanna; Herry, Jean‐Marie; Yagoubi, Najet; Marlière, C.

doi:10.1039/c6ra25632e

Cited by 8 publications

(16 citation statements)

References 44 publications

(55 reference statements)

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“…Its melting properties found by DSC are the following: T m ¼ 52.0 ± 0.4 C and DH m ¼ 119 ± 1 J g À1 . These values are quite consistent with literature data [41].…”

Section: Dsc Analysissupporting

confidence: 93%

“…According to literature, Irganox 1076® can crystallize under different structures [33,40,41]. Saunier et al [41], for instance, mentioned the existence of four different crystalline structures that they called forms I, II, III, and IV. The commercially available structure, called form I by these authors, is characterized by the highest melting point.…”

Section: Dsc Analysismentioning

confidence: 99%

“…In addition, the exothermic peak observed at 3 C during the cooling ramp at 10 C.min À1 corresponds to the recrystallization of Irganox 1076® into the metastable crystalline form IV. This latter structure is only stable at low temperature and is generally obtained by rapid cooling after melting [41]. Indeed, its melting peak observed at 6 C during the second heating ramp was immediately followed by an exothermic peak of recrystallization into form I.…”

Section: Dsc Analysismentioning

confidence: 99%

“…At the opposite, transformations into forms II and III are more complex and seem to involve enantiotropic transitions. For this reason, they cannot be discriminated using classical DSC experiments [41].…”

Section: Dsc Analysismentioning

confidence: 99%

“…However, Molt and Ihlbrock [40] mentioned the existence of two different crystalline structures of Irganox 1076®, named "alpha" and "beta", which could be distinguished using near infrared spectroscopy. More recently, Saunier et al [33,41] mentioned the existence of four different crystalline structures for Irganox 1076®, among which three of them were obtained and isolated by recrystallization in different solvents.…”

Section: Introductionmentioning

confidence: 99%

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Physico-chemical characterization of the blooming of Irganox 1076® antioxidant onto the surface of a silane-crosslinked polyethylene

Roland

Colin

2020

Polymer Degradation and Stability

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This study aims at investigating the blooming of Irganox 1076® onto the surface of a silane-crosslinked polyethylene. Preliminary studies on the commercial Irganox 1076® powder enabled to identify its crystalline structure and determine its main physico-chemical properties (characteristic IR absorption bands, melting properties, etc.). Then, the behaviour of Irganox 1076® in silane-grafted polyethylene was studied. Several films containing a concentration of Irganox 1076® ranged between 0.1 wt% and 2.1 wt% were characterized with FTIR spectroscopy and DSC. A peculiar attention was paid to the phase separation within the polymer bulk and the blooming of the antioxidant onto the polymer film surface. Then, this methodology was transposed to an industrial silane-crosslinked polyethylene containing at least 1 wt% of Irganox 1076® as in-service protective antioxidant. For this latter, optical microscopy was of great help for monitoring the blooming of Irganox 1076® onto the polymer film surface. In addition, the polymorphism phenomenon of Irganox 1076® was revealed by FTIR spectroscopy and DSC after thermal treatment at 70 C under vacuum.

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“…Its melting properties found by DSC are the following: T m ¼ 52.0 ± 0.4 C and DH m ¼ 119 ± 1 J g À1 . These values are quite consistent with literature data [41].…”

Section: Dsc Analysissupporting

confidence: 93%