Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation
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Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation
Chinese Journal of Polymer ScienceVol. 33, Issue 7, Pages: 1000-1008(2015)
Affiliations:
a.State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
b.University of Chinese Academy of Sciences, Beijing 100049, China
Yan-hu Xue, Shu-qin Bo, Xiang-ling Ji. Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation[J]. Chinese Journal of Polymer Science, 2015, 33(7): 1000-1008.
DOI:
Yan-hu Xue, Shu-qin Bo, Xiang-ling Ji. Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation[J]. Chinese Journal of Polymer Science, 2015, 33(7): 1000-1008.DOI: 10.1007/s10118-015-1648-5.
Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation
A series of copolymers of ethylene with 1-hexene synthesized using a metallocene catalyst are selected and mixed. The blend is fractionated
via
preparative temperature rising elution fractionation (P-TREF). All fractions are characterized via high-temperature gel permeation chromatography (GPC)
13
C nuclear magnetic resonance spectroscopy (
13
C-NMR)
and differential scanning calorimetry (DSC). The changes in the DSC melting peak temperatures of the fractions from P-TREF as a function of elution temperature are almost linear
thereby providing a reference through which the elution temperature of TREF experiments could be selected. Moreover
the standard calibration curve (ethylene/1-hexene) of P-TREF is established
which relates to the degree of short-chain branching of the fractions. The standard calibration curve of P-TREF is beneficial to study on the complicated branching structure of polyethylene. A convenient method for selecting the fractionation temperature for TREF experiments is elaborated. The polyethylene sample is fractionated
via
successive self-nucleation and annealing (SSA) thermal fractionation. A multiple-melting endotherm is obtained through the final DSC heating scan for the sample after SSA thermal fractionation. A series of fractionation temperatures are then selected through the relationship between the DSC melting peak temperature and TREF elution temperature.
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Related Author
Yan-hu Xue
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Related Institution
School of Applied Chemistry and Engineering, University of Science and Technology of China
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