Article

1998 ◽  
Vol 76 (11) ◽  
pp. 1699-1706 ◽  
Author(s):  
Jonathan Z Knaul ◽  
Mohammad R Kasaai ◽  
V Tam Bui ◽  
Katherine AM Creber

Starting from a chitosan sample with a degree of deacetylation of 71%, three separate sample sets were generated by successive deacetylation and reacetylation processes. The degree of deacetylation of samples was determined by UV spectrometry supported by thermogravimetric analysis. The molecular weight of chitosan samples was determined in a solvent system of 0.25 M CH3COOH/0.25 M CH3COONa, using viscometry and gel permeation chromatography (GPC) with a TSK-gel column. The first set of samples had a similar degree of deacetylation (DDA) but differing molecular weights. The second set of samples had a similar molecular weight but differing degrees of deacetylation. The Mark-Houwink-Sakurada constants used for the determination of viscosity average molecular weight and the universal calibration of the GPC system were K = 1.40 × 10-4 dL/g and a = 0.83. Results showed that molecular weights determined from both techniques are in good accord only at lower degrees of deacetylation. This may be attributed to the fact that the chemical structure of chitosan samples could have been largely altered with increasing or decreasing degree of deacetylation. Nevertheless, the trend with which the molecular weights vary with the deacetylation time is consistent over a limited DDA range. A literature review of molecular weight analysis of chitosan is included.Key words: chitosan, degree of deacetylation, gel permeation chromatography, molecular weight, viscometry.

TAPPI Journal ◽  
2021 ◽  
Vol 20 (6) ◽  
pp. 381-391
Author(s):  
JULIANA M. JARDIM ◽  
PETER W. HART ◽  
LUCIAN LUCIA ◽  
HASAN JAMEEL

The present investigation undertook a systematic investigation of the molecular weight (MW) of kraft lignins throughout the pulping process to establish a correlation between MW and lignin recovery at different extents of the kraft pulping process. The evaluation of MW is crucial for lignin characterization and utilization, since it is known to influence the kinetics of lignin reactivity and its resultant physicochemical properties. Sweetgum and pine lignins precipitated from black liquor at different pHs (9.5 and 2.5) and different extents of kraft pulping (30–150 min) were the subject of this effort. Gel permeation chromatography (GPC) was used to deter- mine the number average molecular weight (Mn), mass average molecular weight (Mw), and polydispersity of the lignin samples. It was shown that the MW of lignins from both feedstocks follow gel degradation theory; that is, at the onset of the kraft pulping process low molecular weightlignins were obtained, and as pulping progressed, the molecular weight peaked and subsequently decreased. An important finding was that acetobromination was shown to be a more effective derivatization technique for carbohydrates containing lignins than acetylation, the technique typically used for derivatization of lignin.


1976 ◽  
Vol 49 (5) ◽  
pp. 1290-1304
Author(s):  
M. Kurata ◽  
H. Okamoto ◽  
M. Iwama ◽  
M. Abe ◽  
T. Homma

Abstract An iterative computer method was proposed for estimating the degree of branching and molecular weight distribution simultaneously from a pair of measurements on intrinsic viscosity and gel-permeation chromatography. The validity of the method as applied to randomly branched polymers was tested by using both fractionated and unfractionated samples of branched polystyrenes. It was experimentally concluded that the average number of branch points per unit molecular weight, λ, can be determined by this method with an accuracy of about 15%, and the weight-average molecular weight with accuracy of about 10%.


1987 ◽  
Vol 65 (8) ◽  
pp. 1804-1809 ◽  
Author(s):  
C. Aitken ◽  
J. F. Harrod ◽  
U. S. Gill

The structures of some poly(organosilylenes), [Formula: see text] (R = Ph, p-tolyl, n-hexyl, and benzyl), produced by catalytic dehydrogenative coupling of primary silanes have been studied by infrared, nuclear magnetic resonance, and mass spectroscopies. These results, combined with data on molecular weights and molecular weight distributions from vapour pressure osmometry and gel permeation chromatography, lead to the conclusion that the polymers are linear and have SiH2R end groups. The polymers all have degrees of polymerization of ca. 10 and very narrow molecular weight dipersions. Some possible features of the mechanism that gives rise to this behaviour are discussed.


2011 ◽  
Vol 179-180 ◽  
pp. 1203-1207
Author(s):  
Zheng Zai Cheng ◽  
Yu Jing Nie ◽  
Xiao Chao Yan ◽  
Rui Lei ◽  
Su Su Lin

Novel titanium complex [2-O-(5- NO2)C6H3CH=N[(C6H4) –2-O ]]2TiCl2 (1) has been prepared by treatment of the ligand complex 1a with TiCl4•2THF in dichloromethane solution. The complex 1a and 1 were characterized by 1H-NMR . Activated by MAO, Complex 1 displayed very high activity for methyl methacrylate polymerization and the viscosity-average molecular weight of PMMA is more than 35×104 at 60°C.The molecular-weight distribution of PMMA measured by gel permeation chromatography (GPC) is narrow.


1973 ◽  
Vol 46 (1) ◽  
pp. 115-126
Author(s):  
M. R. Ambler ◽  
R. D. Mate

Abstract Data are presented which show that when a polymer contains an appreciable amount of low molecular weight species below the diffusion limit of the osmometer membrane, the osmotic molecular weight, Mn, is generally higher than the Mn calculated from gel-permeation chromatography (GPC). Experiments were performed on samples of poly(vinylchloride) (PVC) and high-cis poly (butadiene) polymers. Osmotic data were obtained in the usual manner, while GPC data were obtained using the universal calibration approach. It was found that when all polymer species below approximately 10,000 molecular weight were excluded from the calculation of Mn by GPC, agreement in Mn was obtained between membrane osmometry and GPC. The data obtained suggest that the choice of Mn as measured by membrane osmometry in the calibration of the GPC should not be done casually, as the measured Mn may not reflect the “true” value of that sample, especially when the polymer sample contains an appreciable amount of low molecular weight material.


2011 ◽  
Vol 138-139 ◽  
pp. 1072-1077
Author(s):  
Sheng Hua Lv ◽  
Rui Gong ◽  
Yan Fen Ma

A phenolic copolymer was synthesized from resorcinol (RSC) and 3,5-dihydroxy benzoic acid (DBA) using horseradish peroxidase (HRP)/H2O2 as the radical copolymerization’s initiateor. It was discussed that the effects of monomer composition on the properties of the copolymer. The best molar ratio was 1:1. The structure and properties of the copolymer was characterized by Fourier Transform Infrared spectroscopy (FTIR) and Nuclear Magnetic Resonance (HNMR), Molecular weight (MW) was determined by gel permeation chromatography (GPC). The result shows that the average molecular weight of the copolymer is about 40000. The effect of dosage of HRP on the properties of the copolymer was investigated. And the mechanism of polymerization of RSC and DBA was advanced. The copolymer was used as tanning agent, applied results show that it has excellent retanning properties. It was realized the applicatiom of HRP on the phenols syntan.


1972 ◽  
Vol 45 (1) ◽  
pp. 346-358 ◽  
Author(s):  
A. Subramaniam

Abstract The Waters Model 200 Gel Permeation Chromatograph has been used to study the molecular weight distribution of natural rubber. The cumulative weight distribution curve of synthetic cis-polyisoprene from the GPC method showed fair agreement with the distribution obtained by fractional precipitation. For natural rubber the agreement was not so good. Natural rubber samples from six clones of Hevea Brasiliensis were examined with the GPC. Differences were observed in their distributions. Five clones showed a distinct bimodal distribution. The weight and number average molecular weights from the GPC were found to be too low. Some possible reasons for this have been suggested.


1995 ◽  
Vol 7 (1) ◽  
pp. 55-68 ◽  
Author(s):  
E J Siochi ◽  
S J Havens ◽  
P R Young ◽  
P M Hergenrother

A controlled-molecular-weight LARCr'-CPI 2 poly(amide acid) was synthesized to investigate solution property changes that result from aging'Both dilute and concentrated solutions were aged at five temperatures and periodically analysed over a 33 d period. Various molecular weight parameters were obtained by gel permeation chromatography in combination with differential viscometry. Chemical changes were also followed by Fourier transform infrared spectroscopy. The temperatures used allowed the calculation of the energy of activation associated with changes in weight and number average molecular weights.


2013 ◽  
Vol 812 ◽  
pp. 250-253 ◽  
Author(s):  
Yoga Sugama Salim ◽  
Chin Han Chan ◽  
Kumar Sudesh ◽  
Seng Neon Gan

With blooming interests in the research of biodegradable polyesters produced from microorganisms as well as polymer processing and technology, this study is intended to reveal the influence of thermal treatment on the molecular weight of poly (3-hydroxybutyrate-co-3 mol% 3-hydroxyhexanoate)/P(3HB-co-3 mol% 3HHx), a copolymer of polyhydroxyalkanoates (PHA). P(3HB-co-3 mol% 3HHx) was thermally treated using Differential Scanning Calorimeter and analyzed using Gel Permeation Chromatography and Attenuated Total Reflectance-Fourier transform infrared (ATR-FTIR) spectrometer. Results from gel permeation chromatography suggest a major reduction of molecular weight up to 50 % when P(3HB-co-3 mol% 3HHx) is exposed to 180 °C for 30 mins. The half-time degradation of P(3HB-co-3 mol% 3HHx) treated at 170 °C and 180 °C is 14.1 and 9.9 mins, respectively. FTIR spectroscopy shows an increase absorbance intensity of P(3HB-co-3 mol% 3HHx) after thermal treatment, indicating a formation of more alkenyl and carboxylic end-group in polymer chains due to random chain scissions.


Crystals ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1543
Author(s):  
Juan Li ◽  
Zhaohua Liang ◽  
Chengtao Gao ◽  
Shanshan Luo ◽  
Shaowen Huang ◽  
...  

Two kinds of organic phosphate nucleating agent (NA-11 and NA-21) were used in PP with different molecular weights through the melt extrusion method. The dispersibility of the nucleating agents in PP, and the effect of the nucleating agents on the molecular weight, rheological behavior and crystallization behavior of PP were investigated. SEM and TEM analysis showed that the average radius of the dispersed particles (nucleating agents) was larger in LPP than that in HPP. The good dispersion of NA-21 also created more nucleation embryos for the adsorption of polypropylene molecules than the agglomerated NA-11. The gel permeation chromatography (GPC) analysis showed that the average molecular weight of HPP and LPP both decreased with the addition of a nucleating agent. The rotational rheometer and capillary rheometer analysis showed that the effect of NA-21 on reducing intermolecular entanglement was more significant, whether in HPP or LPP. The addition of NA-21 had less elastic energy storage and better flow stability, and could be processed at a higher speed. Simultaneously, the relaxation time in the blends with LPP was shorter than that with HPP. It was found that the crystallinity and nucleation efficiency of HPP/nucleating agent blends increased remarkably, while there was a barely perceptible increase in LPP/nucleating agent blends.


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