Optimization of run parameters of temperature-rising elution fractionation with the aid of a factorial design experiment

Aust, Nicolai; Gahleitner, Markus; Reichelt, Kristin; Raninger, Bettina

doi:10.1016/j.polymertesting.2006.05.008

Cited by 17 publications

(10 citation statements)

References 8 publications

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“…Melting temperatures decreased with increasing 1-butene content in the copolymers. Aust et al [23] proposed an experimental design plan for optimization of the TREF process taking ethylene/ propylene copolymers (EPC) as an example. It was shown that the separation quality can be remarkably improved by the aid of factoral design experiments.…”

Section: Temperature Rising Elution Fractionationmentioning

confidence: 99%

Recent Advances in High-Temperature Fractionation of Polyolefins

Pasch

Malik

Macko³

2012

Advances in Polymer Science

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Section: Temperature Rising Elution Fractionationmentioning

confidence: 99%

Recent Advances in High-Temperature Fractionation of Polyolefins

Pasch

Malik

Macko³

2012

Advances in Polymer Science

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“…According to recent literature a significant operation parameter influencing CRYSTAF is the cooling rate 23, 24. Optimization analysis of TREF showed a dependency of the separation process on stabilization start temperature 29. In TREF the dissolved polymer is separated in a column.…”

Section: Experimental Partmentioning

confidence: 99%

Mathematical Modeling and Optimization of Run Parameters of Crystallization Analysis Fractionation (CRYSTAF)

Fischlschweiger

Aust

Oberaigner

et al. 2010

Macro Chemistry & Physics

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Blends of a random poly(propylene) copolymer with different types of polyethylene were used to develop a sample independent statistic mathematical model which describes the quality of phase separation of polymer blends obtained by CRYSTAF. By coupling the abstract model with experimental data, process parameters influencing the non‐equilibrium CRYSTAF separation process can be determined. It could be shown that the stirring speed applied during the fractionation process strongly influences the resolution of the derived CRYSTAF profile and thus the quality of fractionation. Nonlinear optimization of the models' response function leads to optimized run parameters for the CRYSTAF process which results in CRYSTAF profiles of high resolution and thus to a high quality in fractionation.magnified image

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“…Solution crystallization‐based techniques like temperature rising elution fractionation (TREF) have been largely utilized for the analysis of CCD of many polyolefin systems . Preparative TREF (being tedious and time consuming) separates and concentrates minor constituents within the bulk sample.…”

Section: Introductionmentioning

confidence: 99%

On the Homogeneity of Metallocene Ethylene–Propylene Copolymers as Investigated by Multiple Fractionation Techniques

Phiri

Dimeska²,

Pasch

2015

Macro Chemistry & Physics

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The chemical heterogeneity of ethylene–propylene copolymers by multiple fractionation techniques is addressed. Three metallocene copolymer samples with different ethylene contents, ranging from 30 to 50 mol% are analyzed using bulk methods to confirm their molecular heterogeneity. In a second step, the samples are fractionated by temperature rising elution fractionation (TREF) to obtain fractions at 30, 60, 90, and 130 °C. These fractions are subsequently analyzed regarding their thermal and molecular properties. Differential scanning calorimetry, crystallization analysis fractionation, and high‐temperature high performance liquid chromatography (HT‐HPLC) results reveal that the TREF fractions collected at 130 °C are mainly due to polypropylene homopolymer, which is rather unexpected considering the high ethylene contents of the bulk samples. Most importantly, HT‐HPLC reveals a remarkably high chemical heterogeneity of the fractions and thus the bulk samples. Solution 13C NMR provides the comonomer contents and sequence distributions of the fractions. These indicate that the same TREF fractions from different samples have distinctively different chemical compositions.

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Optimization of run parameters of temperature-rising elution fractionation with the aid of a factorial design experiment

Cited by 17 publications

References 8 publications

Recent Advances in High-Temperature Fractionation of Polyolefins

Recent Advances in High-Temperature Fractionation of Polyolefins

Mathematical Modeling and Optimization of Run Parameters of Crystallization Analysis Fractionation (CRYSTAF)

On the Homogeneity of Metallocene Ethylene–Propylene Copolymers as Investigated by Multiple Fractionation Techniques

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