Polymer HPLC mobile phase

For polymer/additive analysis complete dissolution is not a prerequisite. Rather, the solvent should at least swell the polymer by diffusion, which allows the physically blended additives to dissolve. True dissolution occurs predominantly when polymer chain lengths are small, on the order of 5000-10 000 Da. Solvent choice for dissolution or extraction should take into account restrictions imposed by further analysis steps (compatibility with chromatographic and/or spectroscopic requirements). When microwave extraction of additives from a polymer is followed by HPLC analysis, the solvent must be compatible with the HPLC mobile phase so that solvent exchange is not required before analysis. 

Ion exchange is another form of HPLC that nses a stationary phase consisting of a cross-linked synthetic organic polymer, often called a resin, with —SO3H or — NH2 groups attached to phenyl or other aromatic rings on the polymer backbone. Mobile phases are nsnally water or... 

The hydrophilic surface characteristics and the chemical nature of the polymer backbone in Toyopearl HW resins are the same as for packings in TSK-GEL PW HPLC columns. Consequently, Toyopearl HW packings are ideal scaleup resins for analytical separation methods developed with TSK-GEL HPLC columns. Eigure 4.44 shows a protein mixture first analyzed on TSK-GEL G3000 SWxl and TSK-GEL G3000 PWxl columns, then purified with the same mobile-phase conditions in a preparative Toyopearl HW-55 column. The elution profile and resolution remained similar from the analytical separation on the TSK-GEL G3000 PWxl column to the process-scale Toyopearl column. Scaleup from TSK-GEL PW columns can be direct and more predictable with Toyopearl HW resins. 

For acrylate polymers with higher levels of carboxylic acids, THF can be modified by the addition of acids such as acetic, phosphoric, or trifluoroacetic. Levels as high as 10% acetic acid are considered acceptable by most manufacturers for their styrene/DVB columns. If such a modified mobile phase is used, it may need to be premixed rather than generated using a dynamic mixing HPLC pump because on-line mixing often leads to much noisier baselines, particularly when using a refractive index detector. 

Lord and Pawliszyn" developed a related technique called in-tube SPME in which analytes partition into a polymer coated on the inside of a fused-silica capillary. In automated SPME/HPLC the sample is injected directly into the SPME tube and the analyte is selectively eluted with either the mobile phase or a desorption solution of choice. A mixture of six phenylurea pesticides and eight carbamate pesticides was analyzed using this technique. Lee etal. utilized a novel technique of diazomethane gas-phase methylation post-SPE for the determination of acidic herbicides in water, and Nilsson et al. used SPME post-derivatization to extract benzyl ester herbicides. The successful analysis of volatile analytes indicates a potential for the analysis of fumigant pesticides such as formaldehyde, methyl bromide and phosphine. 

BHA, BHT, PG, TBHQ and tocopherols) a variety of stationary phases, mobile phases and detectors can be used [711]. Common antibacterials such as carba-dox, thiamphenicol, furazolidone, oxolinic acid, sul-fadimethoxine, sulfaquinoxaline, nalidixic and piromidic acid can be analysed by GE-RPLC-UV (at 254 nm). Collaborative studies have been reported for the HPLC determination of the antimicrobial sodium benzoate in aqueous solutions [712], Plastics devices used for field collection of water samples may contain polymer additives (such as resorcinol monobenzoate, 2,4-dihydroxybenzophenone or bisphenol A) or cyanobac-terial microcystins [713],... 

In SEC analysis of additive extracts from polymers, the effect of the extraction solvent on the mobile phase is less critical than in HPLC analysis. The extraction solvents typically employed generally do not interfere with the SEC mobile phases. Moreover, the same solvents are often used both as extraction solvent and as mobile phase. Therefore, there is no need to evaporate the extract to dryness prior to analysis and then to redissolve it in a suitable solvent. Typical extraction procedures often produce extracts that generally contain a small amount of wax. Frequently, removal of such oligomers from an extract is necessary, e.g. by means of precipitation, centrifuging, precolumn filtration or protection (use of a reversed-phase guard column). In SEC separations the presence of polyolefin wax does not usually disturb provided that the MW of the wax is higher than that of the analysed compounds. 

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