Recent Advances in Gel Permeation Chromatography

1981 ◽  
Vol 54 (3) ◽  
pp. 535-575 ◽  
Author(s):  
A. C. Ouano

Abstract Gel permeation chromatography (GPC), sometimes referred to as size-exclusion chromatography (SEC), has progressed at an almost explosive rate since its introduction less than two decades ago. One has only to refer to the open literature or thumb through the list of Chromatographic equipment manufacturers anxious to sell their latest innovation to be fully convinced of this fact. Because of the extensive progress in GPC technique and instrumentation, the author had a very difficult time in deciding the scope of this review. Mindful that he may be criticized of being myopic in his presentation of the most significant and recent contributions and guilty of gross omission of important references, the author has nevertheless decided to narrow the scope to three major areas and a few key references. The three major areas to be covered are: (1) data acquisition and processing, (2) high-pressure chromatography and (3) detectors. Extensive progress has been made in the computerization of both data acquisition and data reduction, the latter allowing molecular weight distribution (MWD) and molecular weight averages to be obtained on the sample in a matter of minutes rather than hours or days. The main beneficiaries of the computerization of data acquisition and processing have been those concerned with polymer quality control, for it has liberated them from the drudgery of the manual digitization, integration, and normalization of the chromatograms required to reduce them to a useful format. The hours of monotonous eye-straining work to obtain MWD and molecular weight averages has been reduced to a few seconds of punching a few keys of the data system console. The development of the high-pressure Chromatograph has added a new dimension to GPC, for, when it is combined with a computerized data system, the MWD can be obtained almost in real time in relation, for example, to a characteristic time of a polymerization reactor. In high-speed Chromatograph y under nearly ideal conditions (low-viscosity mobile phase and molecular weight of no more than a few hundred thousand), the MWD can be obtained in a few minutes. This capability allows the use of GPC as on-line process-control equipment. The Chromatograph can be used as part of a “feed-back” loop to control the polymerization conditions to obtain a product of consistent MWD.

1985 ◽  
Vol 58 (2) ◽  
pp. 295-303 ◽  
Author(s):  
H. K. Gupta ◽  
R. Salovey

Abstract Molar mass and compositional distributions in copolymers of butadiene and acrylonitrile have been analyzed by gel permeation chromatography with multiple detection. In some cases, a third component could not be separated by size-exclusion chromatography and was presumed to be an antioxidant attached to the copolymer chains. The amount of this antioxidant was measured by ultraviolet detection at 280 nm of chromatographic effluents and found to increase in amount with decreasing molar volume. Molar mass and compositional distributions were derived from corrected ultraviolet responses at 254 nm coupled with refractive index detection of BAN solutions separated by GPC. The variation of composition with molecular size depends on the composition of the monomer feed and, presumably, the conversion. For copolymers close the azeotropic composition (36% ACN), the composition was fairly uniform over the entire molecular weight distribution and showed a single Tg by differential scanning calorimetry. Some of the materials showed gel or insoluble fractions which had to be separated from the soluble moieties prior to GPC. Copolymers of composition slightly above azeotropic showed a single Tg but could be separated into sol and gel fractions which differed in composition. Infrared and calorimetric analysis showed that, in these cases, the gel was enriched in acrylonitrile. A sample containing 20% acrylonitrile showed marked deviations from compositional uniformity, and the high molecular weight components were enriched in butadiene. Infrared and calorimetric analysis of the sol and gel fractions showed that they were enriched in acrylonitrile and butadiene, respectively. In fact, the elastomer evidenced two glass transition temperatures. We suggest that gel permeation chromatography with multiple detection, specifically refractive index and ultraviolet absorption at 254 and at 280 nm, permits a fairly complete characterization of BAN elastomers. With computer analysis, a sophisticated raw material quality control is feasible and simple. We plan to reexamine our assumptions using laboratory synthesized BAN copolymers. Moreover, we hope to relate the physical properties of elastomers and rubber compounds with the molecular characterization of BAN copolymers. As an alternative to ultraviolet detection in GPC, it may be possible to get a more complete functional group analysis by infrared spectroscopy.


2012 ◽  
Vol 487 ◽  
pp. 48-52
Author(s):  
Sheng Hua Lv ◽  
Gong Rui ◽  
Di Li

The radical copolymerization of resorcinol (RSC) and 3,5-dihydroxyl benzoic (DHBA) was carried out in water by the initiator of horseradish (HRP)/H2O2. It was discussed that the effects of monomer composition on the properties of the copolymer. The best monomer mass ratio of RSC:DHBA was 60:40 and the shrink temperature can reached to 88.5oC. The tanning result indicated that the copolymer of RSC and DHPA has particularly excellent tanning properties and can be served as leather tannage substitute for chrome tanning materials. And also the mechanism of the HRP initiated copolymerization was proposed. The structure and molecular weight of the copolymer was characterized by Fourier Transform Infrared spectroscopy (FTIR), Nuclear Magnetic Resonance (NMR) and Gel Permeation Chromatography (GPC). The copolymer can be as tannage and retannage in making leather process. The results showed that it has excellent tanning properties and retanning effects.


1975 ◽  
Vol 28 (1) ◽  
pp. 189 ◽  
Author(s):  
RA Shanks

Gel permeation columns of Bio Beads S-X8 have been used to provide separation of oligomers and other small organic molecules. Results show successful separations up to molecular weight c. 600. The retention times of compounds have been correlated with the largest molecular dimension of the molecules and also with molar volumes.


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