A New Technique for Characterizing Comonomer Distribution in Polyolefins: High-Temperature Thermal Gradient Interaction Chromatography (HT-TGIC)

Cong, Rongjuan; deGroot, Willem; Parrott, Al; Yau, Wallace W.; Hazlitt, Lonnie G.; Brown, Ray; Miller, Matt; Zhou, Zhe

doi:10.1021/ma200304e

Cited by 90 publications

(156 citation statements)

References 31 publications

(40 reference statements)

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“…TCB has been used to desorb polyolefins from Hypercarb™ and other carbonaceous sorbents at 140 or 160°C. It is known that temperature can alter the extent of adsorption of synthetic polymers on a solvent/sorbent interface .…”

Section: Resultsmentioning

confidence: 99%

Carbonaceous sorbents for high‐temperature interactive liquid chromatography of polyolefins

Chitta

Macko

Brüll

et al. 2013

J of Separation Science

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The elution behavior of polyethylene (PE) and the three stereoisomers of polypropylene (PP) was studied on porous graphite along with three other carbon-based sorbents, carbon-clad zirconia particles, activated carbon, and exfoliated graphite in a systematic way in this work. Decahydronaphthalene, 1,2,3,4-tetrahydronaphthalene, 1,3,5-trimethylbenzene, tetrachloroethylene, xylene and p-xylene were used as mobile phases. While PE is adsorbed to various extents on all the tested carbonaceous sorbents from the majority of the solvents, PP is fully adsorbed only in selected cases. Testing alcohols (C7-C9) as mobile phase with Hypercarb™ indicates that all stereoisomers of PP are selectively adsorbed and desorbed when a solvent gradient alcohol→1,2,4-trichlorobenzene is used at 160°C. The retention of all stereoisomers of PP increases with the polarity of the alcohol. Linear PE is retained on Hypercarb™ even from 1,2-dichloro- and 1,2,4-trichlorobenzene, when a temperature below 120°C is applied, while it is not retained from these solvents at higher temperatures. All stereoisomeric forms of PP are not adsorbed under the same conditions. Some of the tested new sorbent/solvent systems have potential to be applied in routine analysis of industrially synthesised polyolefins.

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Section: Resultsmentioning

confidence: 99%

Carbonaceous sorbents for high‐temperature interactive liquid chromatography of polyolefins

Chitta

Macko

Brüll

et al. 2013

J of Separation Science

Self Cite

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show abstract

“…These concentrations are significantly lower than the concentrations usually used in 13 C NMR with a conventional probe [131,132]. Cong et al [133] phase NMR measurements were performed. The new cryoprobe enabled one to determine the content of octene in the collected copolymer fractions, thus demonstrating the practical applicability of the excellent improvement of detectability of polyolefins in NMR.…”

Section: Coupled Sec-1 H-nmrmentioning

confidence: 96%

“…This phenomenon has been applied to the separation of synthetic polymers by Lochm€ uller [171] for poly(ethylene glycol) and by Chang [172] for polystyrene. Very recently, Cong et al described experimental conditions which enable one to apply temperature changes to the separation of polyolefins [133]. Separation was achieved by the interaction of the polyolefin with a graphite surface in a thermodynamically good solvent for PE.…”

Section: Temperature Gradient Interaction Chromatographymentioning

confidence: 99%

“…29 Schematic of HT-TGIC experimental setup, the definition of each variable is described in Table 5. (Reprinted from [133] with permission of American Chemical Society) crystallization based techniques. The authors claim that co-crystallization does not play a role in TGIC.…”

Section: Temperature Gradient Interaction Chromatographymentioning

confidence: 99%

“…C; final temperature during cooling process 0 C; final temperature during elution process 175 C; cooling rate during cooling process 6 C/min; heating rate during elution process 3 C/min; flow rate during cooling process 0.03 mL/min; flow rate during elution process 0.5 mL/min. (Reprinted from [133] with permission of American Chemical Society)…”

Section: Two-dimensional Liquid Chromatographymentioning

confidence: 99%

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