Degradation of unstabilised polypropylene and a propene- 1-pentene copolymer

e-Polymers ◽  
2004 ◽  
Vol 4 (1) ◽  
Author(s):  
Stefan de Goede ◽  
Robert Brüll ◽  
Harald Pasch ◽  
Niall Marshall
Keyword(s):  
Chemical Composition ◽  
Mass Distribution ◽  
Molar Mass ◽  
Degradation Process ◽  
Size Exclusion ◽  
Molar Mass Distribution ◽  
Low Molecular Weight ◽  
Composition Distribution ◽  
Chemical Composition Distribution ◽  
Exclusion Chromatography

Abstract The degradation of polypropylene (PP) and a propene-1-pentene copolymer (P2) have been monitored with regard to chemical composition, molar mass distribution and chemical composition distribution. The increase in the carbonyl index can be monitored by IR and a decrease in molar mass can be observed from size-exclusion chromatography (SEC). CRYSTAF shows that the chemical heterogeneity of the samples broadens with continuing degradation. SEC-FTIR reveals that the degraded species are mainly found in the low-molecular-weight end of the molar mass distribution. Spatial heterogeneity of the degradation process has been proven by the analysis of abrased layers. It was found that the P2 copolymer degrades at a higher rate compared to PP.

High-throughput screening of the chemical composition distribution of random styrene-butyl acrylate copolymers

e-Polymers ◽  
2005 ◽  
Vol 5 (1) ◽  
Author(s):  
Iván García Romero ◽  
Harald Pasch
Keyword(s):  
Chemical Composition ◽  
High Throughput ◽  
Butyl Acrylate ◽  
High Throughput Screening ◽  
Size Exclusion ◽  
Chemical Compositions ◽  
Composition Distribution ◽  
Chemical Composition Distribution ◽  
Exclusion Chromatography ◽  
Liquid Chromatographic

AbstractThe development of high-throughput liquid chromatographic techniques for the analysis of styrene-butyl acrylate (SBA) copolymers is discussed. The analysis time in size-exclusion chromatography (SEC) can be reduced to about 3 min per sample when high-throughput SEC columns and high flow rates are used. In gradient HPLC, small columns with improved separation efficiencies can be applied. The time requirements can be decreased to less than 2 min per sample. Using the high-throughput HPLC technique, the chemical composition distribution of high-conversion SBA copolymers can be analyzed in a fast and efficient way. The calibration of HPLC separation is conducted by coupling the HPLC system with FTIR through the LC-transform interface. A comparison of the chemical compositions of the copolymers obtained by 1H NMR, off-line FTIR and coupled HPLCFTIR verifies the accuracy of the high-throughput copolymer analysis approach.

High-temperature gradient HPLC and LC-NMR for the analysis of complex polyolefins

2008 ◽  
Vol 80 (8) ◽  
pp. 1747-1762 ◽  
Author(s):  
Harald Pasch ◽  
Lars-Christian Heinz ◽  
Tibor Macko ◽  
Wolf Hiller
Keyword(s):  
High Temperature ◽  
Chemical Composition ◽  
Temperature Gradient ◽  
Molar Mass ◽  
Size Exclusion ◽  
Copolymer Composition ◽  
Composition Distribution ◽  
High Temperature Gradient ◽  
Chemical Composition Distribution ◽  
On Line

The synthesis and characterization of polyolefins continues to be one of the most important areas for academic and industrial polymer research. One consequence of the development of new "tailor-made" polyolefins is the need for new and improved analytical techniques for the analysis of polyolefins with respect to molar mass and chemical composition distribution. The present article briefly reviews different new and relevant techniques for polyolefin analysis. Crystallization analysis fractionation is a powerful new technique for the analysis of short-chain branching in linear low-density polyethylene (LLDPE) and the analysis of polyolefin blends and copolymers regarding chemical composition. For the fast analysis of the chemical composition distribution, a new high-temperature gradient high-performance liquid chromatography (HPLC) system has been developed. The efficiency of this system for the separation of various olefin copolymers is demonstrated. The correlation between molar mass and chemical composition can be accessed by on-line coupling of high-temperature size exclusion chromatography (HT-SEC) and 1H NMR spectroscopy. It is shown that the on-line NMR analysis of chromatographic fractions yields information on microstructure and tacticity in addition to molar mass and copolymer composition.

scholarly journals Size-exclusion chromatography of cellulose: observations on the low-molar-mass fraction

Cellulose ◽  
2020 ◽  
Vol 27 (16) ◽  
pp. 9217-9225
Author(s):  
Leena Pitkänen ◽  
Herbert Sixta
Keyword(s):  
Mass Distribution ◽  
Size Exclusion Chromatography ◽  
Mass Fraction ◽  
Molar Mass ◽  
Accurate Determination ◽  
Size Exclusion ◽  
Molar Mass Distribution ◽  
Universal Method ◽  
Exclusion Chromatography

AbstractAccurate determination of molar mass distribution for disperse cellulose samples has proved to be a challenging task. While size-exclusion chromatography coupled to multi-angle light scattering (MALS) and differential refractive index (DRI) detectors has become the most commonly used method for molar mass determination of celluloses, this technique suffers low sensitivity at the low-molar mass range. As discussed here, the universal method for accurate molar mass distribution analysis of cellulose samples not exists and thus thorough understanding on the differences of the various methodological approaches is important. In this study, the focus is in the accurate determination of the low-molar mass fraction. The results obtained by combining the two calibration strategies, MALS/DRI for polymeric region of a cellulose sample and conventional calibration for oligomeric region, was compared to the results obtained using only MALS/DRI (with extrapolation of the curve where signal-to-noise of MALS is low). For birch pulp sample, the results from the two approaches were comparable; it should be highlighted, however, that MALS/DRI slightly overestimates the molar masses at the low-molar-mass region.

Influence of the Molar Mass Distribution on the Elongational Behaviour of Polymer Solutions in Capillary Breakup

2005 ◽  
Vol 15 (1) ◽  
pp. 28-37 ◽  
Author(s):  
J. P. Plog ◽  
W.-M. Kulicke ◽  
C. Clasen
Keyword(s):  
Mass Distribution ◽  
Molar Mass ◽  
Relaxation Times ◽  
Size Exclusion ◽  
Molar Mass Distribution ◽  
Mean Values ◽  
Capillary Breakup ◽  
Mass Distributions ◽  
Uniaxial Elongation ◽  
Exclusion Chromatography

AbstractCommercially available, blended methylhydroxyethyl celluloses with similar weight-average molar masses but varying molar mass distributions were characterized by different techniques like steady shear flow and uniaxial elongation in capillary breakup experiments. The determined relaxation times t were then correlated with the absolute molar mass distribution acquired via SEC/MALLS/DRI (combined methods of size-exclusion-chromatography, multi angle laser light scattering and differential refractometer). In order to describe the longest relaxation time of the polymers in uniaxial elongation via integral mean values of the molar mass distribution, defined blends of polystyrene standards with varying molar mass distributions were characterized. The obtained data was scaled via different moments of the molecular weight distribution and could be correlated with the results obtained for the methylhydroxyethyl celluloses.

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