13C NMR, GPC, and DSC Study on a Propylene-ethylene-1-butene Terpolymer Fractionated by Temperature Rising Elution Fractionation

Zhang, Yudong; Gou, Qing Qiang; Wang, Jun; Wu, Chang Jiang; Qiao, Jin Liang

doi:10.1295/polymj.35.551

Cited by 8 publications

(8 citation statements)

References 25 publications

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“…The 13 C NMR spectra were obtained with Bruker Advance DPX 400 NMR spectrometer at 120 °C using a 5 mm broadband QNP probe, with a 9.57 µs 90 ° pulse, 17 kHz spectral width, 10,240 transients, 1 s acquisition time. The spectra were obtained with WALTZ-16 proton decoupling.…”

Section: Acquisition Of 1d 13 C Nmr Spectramentioning

confidence: 99%

“…The quantitative 13 C NMR spectra were obtained with a 9.57 µs 90 ° pulse, 17 kHz spectral width, 2048 transients, 35s acquisition times. To eliminate NOE, spectra were obtained with an inverted gated WALTZ-16 proton decoupling.…”

Section: Acquisition Of 1d Quantitative 13 C Nmr Spectramentioning

confidence: 99%

“…If two or more monomers are copolymerized in a statistically random manner, many possible monomer sequences can be formed. The 1 H and 13 C NMR spectra can be extremely complex due to the overlap of the resonances. The spectra are sensitive to the variations of the comonomer sequences.…”

Section: Introductionmentioning

confidence: 99%

“…Although there are extensive reports on the 13 C NMR determination of copolymers such as poly(ethyleneco-propylene) [1][2][3][4] , poly(ethylene-co-butene) [5][6][7] , and poly(propylene-co-butene) [8,9] , only few 13 C NMR studies of poly(ethylene-co-propylene-co-butene) terpolymer were investigated [10][11][12][13] .…”

Section: Introductionmentioning

confidence: 99%

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Microstructural Analysis of Poly(ethylene-co-propylene-co-1-butene) terpolymers by Multidimensional NMR Spectroscopy

Nuamthanom,

Sandee

2022

bull appl sci

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Physical, rheological and optical properties of polymer depend on its molecular microstructure. Specifically, the monomer content and sequence distribution of polymer significantly affect the mechanical performance of the final product. To this base, Nuclear Magnetic Resonance Spectroscopy (NMR) has been introduced as a very powerful technique to study the microstructure of polymer. The purpose of this study was to develop a methodology to investigate the microstructure of poly(ethylene-co-propylene-co-butene) terpolymer by using multidimensional NMR spectroscopy, including pulsed-field-gradient (PFG) 1H-13C heteronuclear single quantum coherence (GHSQC), heteronuclear multiple bond coherence (gHMBC), and heteronuclear single quantum coherence-total correlation spectroscopy (GHSQC-TOCSY). The combination of 1D and 2D NMR experiments, permit the characterization of the complex structure of poly(ethylene-co-propylene-co-butene) terpolymer. The completed 13C NMR assignments provided in this work allow more accurate quantitative determination of the microstructure in these polymers.

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Section: Acquisition Of 1d 13 C Nmr Spectramentioning

confidence: 99%

Section: Acquisition Of 1d Quantitative 13 C Nmr Spectramentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Microstructural Analysis of Poly(ethylene-co-propylene-co-1-butene) terpolymers by Multidimensional NMR Spectroscopy

Nuamthanom,

Sandee

2022

bull appl sci

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“…Thus, this method is more labor-intensive compared to other analytical methods. [4][5][6][7][8] Liquid chromatography (LC) method was also reported for separating PP/PE blend. [9][10][11][12] Similar to 13 C NMR, LC also involves dissolving the blend in a high-temperature solvent.…”

Section: Introductionmentioning

confidence: 99%

Determination of mass fractions in polypropylene/polyethylene blends using fast scanning calorimetry

Furushima

Hirota

Nakada

et al. 2023

J of Applied Polymer Sci

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Fast scanning calorimetry (FSC) enables rapid sample cooling from the melt at rates of several thousand Kelvin per second. A perfect amorphous state for polypropylene (PP) can be achieved by fast cooling at rates of 5000 K s−1. In comparison, polyethylene (PE) crystallizes during cooling, even at cooling rates accessible with FSC. Thus, in this study, a novel method was proposed for determining the PP/PE mixing ratio with a standard deviation of 1.4 mass% that combines FSC and differential scanning calorimetry. The proposed method considers the above thermal behavior of the components of polyolefin blends. In addition, the proposed method is expected to provide a convenient way to analyze the composition of recycled polyolefins from the market or industrial processes without the need for high‐temperature solvents that are typically used in nuclear magnetic resonance or for calibration curves in Fourier transform infrared spectrophotometry.

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Carbon‐13 NMR, GPC, and DSC study on a propylene‐1‐butene copolymer fractionated by temperature rising elution fractionation

Zhang

2005

J of Applied Polymer Sci

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A random copolymer of propylene with small amounts of 1‐butene comonomer, synthesized with a Ziegler–Natta catalyst, was fractionated by temperature rising elution fractionation (TREF) to systemically investigate the fraction samples' molecular microstructure, as well as their relationship to the melting and crystallization behavior. First, TREF was employed to fractionate the sample, and then crystallization analysis fractionation (Crystaf) was used to check the effect of the TREF experiment. In the characterization of the molecular microstructure, carbon‐13 NMR spectroscopy (13C NMR) and gel permeation chromatography (GPC) experiments gave the following results: the fraction samples have relatively uniform molecular microstructure; with an increase in elution temperature, the 1‐butene content in the fraction samples decreases, but the molecular weight (Mn) and number average sequence length of propylene (n̄P) increase. In the study on melting and crystallization behavior, differential scanning calorimetry (DSC) experimental results show that the melting temperature increasingly decreases with an increase in 1‐butene content; however, dependence of the melting temperature on molecular weight becomes weaker and weaker with an increase in the number average molecular weight in the range of number average molecular weight below 1.82 × 105 g/mol. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 845–851, 2006

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13C NMR, GPC, and DSC Study on a Propylene-ethylene-1-butene Terpolymer Fractionated by Temperature Rising Elution Fractionation

Cited by 8 publications

References 25 publications

Microstructural Analysis of Poly(ethylene-co-propylene-co-1-butene) terpolymers by Multidimensional NMR Spectroscopy

Microstructural Analysis of Poly(ethylene-co-propylene-co-1-butene) terpolymers by Multidimensional NMR Spectroscopy

Determination of mass fractions in polypropylene/polyethylene blends using fast scanning calorimetry

Carbon‐13 NMR, GPC, and DSC study on a propylene‐1‐butene copolymer fractionated by temperature rising elution fractionation

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