Gel Permeation Chromatography GPC

For this technique to be successful the sample must be readily soluble in an organic solvent. It has a wide application in the analysis of plastic samples. It is possible to obtain molecular weight data on both amorphous plastics and semi-crystalline plastics. In the amorphous case (e.g., polystyrene), the system used is set around ambient temperature (30 °C) and solvents such as THF, chloroform and toluene are used. With semi-crystalline plastics (e.g., polyolefins), more aggressive solvents such as ortho-dichlorobenzene and meta-ctesol are used at elevated (140 °C) temperatures. 

In the case of some complex plastic systems (e.g., blends), the development of interfaces such as the Lab Connections LC Transform, have proved very useful in increasing the amount of information that can be obtained in a GPC analysis by enabling IR data to be recorded on the resultant chromatogram. Hence, with the correct choice of separating column, polymer blends can be separated and identified as well as plasticisers. 

TLC is a relatively simple technique that can be used for both the separation and identification of additives such as antioxidants and UV stabilisers. A number of approaches are possible using different developing solvents and spraying agents. 

It is also the case that TLC can be used in a preparative way for the isolation of san le fractions for subsequent chromatographic or spectroscopic analysis. 

TLC does have the image of being somewhat old fashioned and it is to be expected that the market penetration of LC-MS systems will further erode the standing of this technique in the modern analytical laboratory. 

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This chapter contains one of the more diverse assortments of topics of any chapter in the volume. In it we discuss the viscosity of polymer solutions, especially the intrinsic viscosity the diffusion and sedimentation behavior of polymers, including the equilibrium between the two and the analysis of polymers by gel permeation chromatography (GPC). At first glance these seem to be rather unrelated topics, but features they all share are a dependence on the spatial extension of the molecules in solution and applicability to molecular weight determination. 

Gel permeation chromatography (GPC) is the term found most widely in the polymer literature. In this context it is used most widely as an analytical... 

Among the techniques employed to estimate the average molecular weight distribution of polymers are end-group analysis, dilute solution viscosity, reduction in vapor pressure, ebuUiometry, cryoscopy, vapor pressure osmometry, fractionation, hplc, phase distribution chromatography, field flow fractionation, and gel-permeation chromatography (gpc). For routine analysis of SBR polymers, gpc is widely accepted. Table 1 lists a number of physical properties of SBR (random) compared to natural mbber, solution polybutadiene, and SB block copolymer. 

In Table 1 some of the properties of raw synthetic hj -l,4-polyisoprene (Goodyear s Natsyn) and natural mbber (Hevea) are presented along with references that contain additional thermal, optical, electrical, and mechanical property data. Some properties of synthetic /n j -l,4-polyisoprene (Kuraray TP-301) are also given. Molecular weights and mol wt distribution are determined by gel-permeation chromatography (gpc) (11). 

In the preparation of commercial DGEBPA, an excess of epichl orohydrin is used in order to minimize polymeriza tion of the reactants to higher molecular-weight species. Nevertheless, the typical viscous final product usually contains ca 80% by weight of the monomeric (n = 0) DGEBPA as deterrnined by gel-permeation chromatography (gpc). The manufacture of Hquid epoxy resins in a batch process has been described in some detail (9). 

TSK-GEL H type columns are for gel-permeation chromatography (GPC) in organic solvents. They are packed with porous poly(styrene-divinylbenzene) resins that have a high degree of cross-linking. 

The selection of the right gel-permeation chromatography (GPC) column or column combination for a special task is a multistage procedure. First, a decision about the type of column has to be made according to the polymer samples in question ... 

ASTM D-3536-91, Standard Test Method for Molecular Weight Averages and Molecular Weight Distribution by Liquid Exclusion Chromatography (Gel Permeation Chromatography-GPC), ASTM Annual Books of ASTM Standards, Vol. 08.02, P. 349—359. This method was deleted in the 1997 edition of the ASTM book. 

This chapter makes no distinction between gel-permeation chromatography (GPC) and size exclusion chromatography (SEC). We make mention of specific analysis conditions wherever possible. We have attempted to include a variety of conditions but by no means should this chapter be considered a comprehensive review of conditions for analyzing polyacrylates. We have drawn extensively from our own experience in selecting examples. 

The enantioselective determination of 2,2, 3,3, 4,6 -hexachlorobiphenyl in milk was performed by Glausch et al. (21). These authors used an achiral column for an initial separation, followed by separation of the eluent fraction on a chiral column. Fat was separated from the milk by centrifugation, mixed with sodium sulfate, washed with petroleum ether and filtered. The solvent was evaporated and the sample was purified by gel permeation chromatography (GPC) and silica gel adsorption chromatography. Achiral GC was performed on DB-5 and OV-1701 columns, while the chiral GC was performed on immobilized Chirasil-Dex. 

We have prepared a copolymer-bearing amino side group and used it either alone or in combination with BP to initiate the photopolymerization of MM A [89]. The gel permeation chromatography (GPC) plot of PMMA initiated by the former system showed a bimodal distribution of molecular weight because both the radicals produced initiate polymerization as follows ... 

Nonionic surfactants, including EO-PO block copolymers, may be readily separated from anionic surfactants by a simple batch ion exchange method [21] analytical separation of EO-PO copolymers from other nonionic surfactants is possible by thin-layer chromatography (TLC) [22,23] and paper chromatography [24], and EO-PO copolymers may themselves be separated into narrow molecular weight fractions on a preparative scale by gel permeation chromatography (GPC) [25]. 

The molecular weights and molecular weight distributions (MWD) of phenolic oligomers have been evaluated using gel permeation chromatography (GPC),23,24 NMR spectroscopy,25 vapor pressure osmometry (VPO),26 intrinsic viscosity,27 and more recently matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS).28... 

ADMET polymers are easily characterized using common analysis techniques, including nuclear magnetic resonance ( H and 13C NMR), infrared (IR) spectra, elemental analysis, gel permeation chromatography (GPC), vapor pressure osmometry (VPO), membrane osmometry (MO), thermal gravimetric analysis (TGA), and differential scanning calorimetry (DSC). The preparation of poly(l-octenylene) (10) via the metathesis of 1,9-decadiene (9) is an excellent model polymerization to study ADMET, since the monomer is readily available and the polymer is well known.21 The NMR characterization data (Fig. 8.9) for the hydrogenated versions of poly(l-octenylene) illustrate the clean and selective nature of ADMET. 

Gel permeation chromatography (GPC) or size exclusion chromatography (SEC) has been routinely used to estimate die molecular weight of die polymers. The molecular weight measured by GPC is relative to a polymer standard, typically polystyrene GPC is dius a relative method rather than an absolute one. For those polymers whose structure is very different from polystyrene, GPC molecular weight values could significantly differ from the real ones. In those cases, GPC values should only be regarded as a reference. 

Hie hydrolytic depolymerization of nylon-6 was followed by gel permeation chromatography (GPC), viscometry, and gravimetry. GPC determinations were performed on a Waters 150C chromatography system using benzyl alcohol as die eluant, two Plgel 10-p.m crosslinked polystyrene columns, and a differential refractometer detector. The flow rate was 1 mL/min. The concentration of the polymer solutions was 0.5 wt% and dissolution was accomplished at 130°C. 

Gellation catalysts, 224, 227-236 Gel permeation chromatography (GPC), 385-386, 490 Gels, urethane, 205 Glass-fiber-filled polyamides, 136 Glass transition temperature (7)), 3, 266, 267... 

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