Chromatography molecular-weight

Molecular weight chromatography (mass chromatography EGA (16) Gives molecular masses, absolute quantities, and GC retention times... 

Kiran, E. and Gillham, J. (1976) Pyrolysis-molecular weight chromatography A new on-line system for analysis of polymers. II. Thermal decomposition of polyolefins Polyethylene, polypropylene, polyisoprene J. Appl. Polym. Sci. 20, 2045-2068. 

Apparatus and experimental techniques have been discussed in several papers. The techniques include thermal volatilization analysis," pyrolysis-gas chromatography, pyrolysis-molecular weight chromatography-i.r. spectrophotometry, and pyrolysis-mass spectrometry. Methods have also been described for collecting and separating pyrolysis products. - ... 

Kiran, E. and GillheWi, J.K., Pyrolysis-Molecular Weight-Chromatography-Vapour Phase Infra Red Spectrophotometry An On Line System for Analysis of Polymers. In Developments in Polymer Degradation 2j. Grassle, N. (Ed), Appl. Sci. Publ. London (1979). 

A series of polyvinylpyridine standards of different molecular weight were analyzed by size-exclusion chromatography, yielding the following results. 

For mixture.s the picture is different. Unless the mixture is to be examined by MS/MS methods, usually it will be necessary to separate it into its individual components. This separation is most often done by gas or liquid chromatography. In the latter, small quantities of emerging mixture components dissolved in elution solvent would be laborious to deal with if each component had to be first isolated by evaporation of solvent before its introduction into the mass spectrometer. In such circumstances, the direct introduction, removal of solvent, and ionization provided by electrospray is a boon and puts LC/MS on a level with GC/MS for mixture analysis. Further, GC is normally concerned with volatile, relatively low-molecular-weight compounds and is of little or no use for the many polar, water soluble, high-molecular-mass substances such as the peptides, proteins, carbohydrates, nucleotides, and similar substances found in biological systems. LC/MS with an electrospray interface is frequently used in biochemical research and medical analysis. 

At first glance, the contents of Chap. 9 read like a catchall for unrelated topics. In it we examine the intrinsic viscosity of polymer solutions, the diffusion coefficient, the sedimentation coefficient, sedimentation equilibrium, and gel permeation chromatography. While all of these techniques can be related in one way or another to the molecular weight of the polymer, the more fundamental unifying principle which connects these topics is their common dependence on the spatial extension of the molecules. The radius of gyration is the parameter of interest in this context, and the intrinsic viscosity in particular can be interpreted to give a value for this important quantity. The experimental techniques discussed in Chap. 9 have been used extensively in the study of biopolymers. 

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. 

Whereas recombinant proteins produced as inclusion bodies in bacterial fermentations may be amenable to reversed-phase chromatography (42), the use of reversed-phase process chromatography does not appear to be widespread for higher molecular weight proteins. 

Solution Polymers. Acryflc solution polymers are usually characterized by their composition, solids content, viscosity, molecular weight, glass-transition temperature, and solvent. The compositions of acryflc polymers are most readily determined by physicochemical methods such as spectroscopy, pyrolytic gas—liquid chromatography, and refractive index measurements (97,158). The solids content of acryflc polymers is determined by dilution followed by solvent evaporation to constant weight. Viscosities are most conveniently determined with a Brookfield viscometer, molecular weight by intrinsic viscosity (158), and glass-transition temperature by calorimetry. 

The molecular weight of SAN can be easily determined by either intrinsic viscosity or size-exclusion chromatography (sec). Relationships for both multipoint and single point viscosity methods are available (18,19). Two intrinsic viscosity and molecular weight relationships for azeotropic copolymers have been given (20,21) ... 

The separation of the polysaccharide components utilizes their different solubUities, polar groups, extents of branching, molecular weights, and molecular flexibUities and may be accompUshed batchwise or with easUy automated column techniques such as column or high performance Uquid chromatography. These procedures have been summarized in several reviews (3,141—143). 

Cyclic Peroxides. CycHc diperoxides (4) and triperoxides (5) are soHds and the low molecular weight compounds are shock-sensitive and explosive (151). The melting points of some characteristic compounds of this type are given in Table 5. They can be reduced to carbonyl compounds and alcohols with zinc and alkaH, zinc and acetic acid, aluminum amalgam, Grignard reagents, and warm acidified iodides (44,122). They are more difficult to analyze by titration with acidified iodides than the acycHc peroxides and have been sucessfuUy analyzed by gas chromatography (112). 

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