Divinylbenzene copolymers with styrene

Divinylbenzene copolymers with styrene are produced extensively as supports for the active sites of ion-exchange resins and in biochemical synthesis. About 1—10 wt % divinylbenzene is used, depending on the required rigidity of the cross-linked gel, and the polymerization is carried out as a suspension of the monomer-phase droplets in water, usually as a batch process. Several studies have been reported on the reaction kinetics (200,201). 

Copolymer with styrene and 1,4-divinylbenzene, 10% alkaloid incorporation, 20% crosslinking. d Copolymer with hydroxyethyl methacrylate and ethylene glycol dimcthacrylate, 10% alkaloid incorporation, 20% crosslinking. 

In order to improve the separation efficiency and speed in biopolymer analysis a variety of new packing materials have been developed. These developments aim at reducing the effect of slow diffusion between mobile and stationary phase, which is important in the analysis of macromolecules due to their slow diffusion properties. Perfusion phases [13] are produced from highly cross-linked styrene-divinylbenzene copolymers with two types of pores through-pores with a diameter of 600-800 mu and diffusion pores of 80-150 nm. Both the internal and the external surface is covered with the chemically bonded stationary phase. The improved efficiency and separation speed result from the fact that the biopolymers do not have to enter the particles by diffusion only, but are transported into the through-pores by mobile-phase flow. 

Tatsuzawa et aq 36,37,45,59 separat.ed cold drugs and neuroleptics by using a styrene-divinyl benzene-methyl methacrylate copolymer as stationary phase. The best results were obtained with methanol - ammonia (99 1) as mobile phase. The effect of the pH and of the composition of the mobile phase on the separation were discussed. Aramaki et al.70 analyzed a series of alkaloids on a macroporous styrene-divinylbenzene copolymer with alkaline acetonitrile - water mixtures as mobile phase (Fig. 7.10). The columns showed excellent stability, and also under the strong basic conditions used for the analysis of the alkaloids. 

The priority phenols (Table 4) in tap and river waters were determined by SPE on line with SEC wi DA-UVD. Tetrabutylammonium bromide was used in the extraction process to increase breakthrough volumes. The mobile phase was CO2 at 40 °C, modified by a gradient of MeOH. LOD was 0.4 to 2 tig L , for 20 mL samples, with good repeatability and reproducibility between days (n = 3) for real samples spiked with 10 [xgL . Seven pollutant phenols, 107a-f and pentachlorophenol, were determined by lEC with a basic SAX resin (styrene-divinylbenzene copolymer with quaternary ammonium groups) and single channel UVD. Resolution of overlapping peaks was carried out by inverse least-squares multivariate calibration. LOD was 0.6 to 6.6 ng, with better than 90% recovery from spiked pure water and 83% from river water. No extensive clean-up was necessary . ... 

Next, condition either the silica-based bonded phases or the styrene-divinylbenzene copolymers with methanol to wet and activate the sorbent for good mass transfer when the sample is passed through the sorbent. Rinse the methanol from the sorbent with deionized water. Several bed volumes should be sufficient to displace the majority of methanol and is comparable to that used in reversed-phase SPE. 

A 12-cm column was packed with XAD-2 (styrene-divinylbenzene copolymer) with methanol and rinsed clean of methanol with distilled water. A 20-mL sample was applied to the column and washed with 50 mL of water to rid the column of carbohydrates. 

Chelex-100 is a well-known resin based on styrene-divinylbenzene copolymer with iminodiacetate groups. It has found many applications in preconcentration of traces of heavy metals such as Cu, Cd, Zn, Ni, Co, Mn, Fe, Pb, and Hg [169-172]. 

J. R. Millar, Interpenetrating Polymer Networks—Styrene-Divinylbenzene Copolymers with Two and Three Interpenetrating Networks, and Their Sulphonates, J. Chem. Soc., 1311 (1960). Synthesis of IPNs. Swelling Behavior of IPNs. vs. crosslink density. 

S2 Styrene-divinylbenzene copolymer with nominal surface area of <50 m /g and an average pore diameter of 0.3-0.4 pm... 

Poly(p-lithiostyrene), a highly reactive polymer prepared from iodinated polystyrene and lithium, yielded a copolymer containing 62 mol-% p-mercaptostyrene when sulfur was added 61). Similarly, treatment of styrene-divinylbenzene copolymers with sulfur and aluminum chloride yielded sulfur-containing polymers in which 21 % of the incorporated sulfur is present in the form of mercaptan groups (62). 

Fig. . Pore size distribution for synthetic carbons prepared from styrene-divinylbenzene copolymers with various cross-iinKage and pore -former content (a) 10/60X (b) 30/130X (c) 30/160X (d) 40/180X.

This type of analysis requires several chromatographic columns and detectors. Hydrocarbons are measured with the aid of a flame ionization detector FID, while the other gases are analyzed using a katharometer. A large number of combinations of columns is possible considering the commutations between columns and, potentially, backflushing of the carrier gas. As an example, the hydrocarbons can be separated by a column packed with silicone or alumina while O2, N2 and CO will require a molecular sieve column. H2S is a special case because this gas is fixed irreversibly on a number of chromatographic supports. Its separation can be achieved on certain kinds of supports such as Porapak which are styrene-divinylbenzene copolymers. This type of phase is also used to analyze CO2 and water. 

To illustrate the specific operations involved, the scheme below shows the first steps and the final detachment reaction of a peptide synthesis starting from the carboxyl terminal. N-Boc-glycine is attached to chloromethylated styrene-divinylbenzene copolymer resin. This polymer swells in organic solvents but is completely insoluble. ) Treatment with HCl in acetic acid removes the fert-butoxycarbonyl (Boc) group as isobutene and carbon dioxide. The resulting amine hydrochloride is neutralized with triethylamine in DMF. 

The first, and still widely used, polymer-supported ester is formed from an amino acid and a chloromethylated copolymer of styrene-divinylbenzene. Originally it was cleaved by basic hydrolysis (2 N NaOH, FtOH, 25°, 1 h). Subsequently, it has been cleaved by hydrogenolysis (H2/Pd-C, DMF, 40°, 60 psi, 24 h, 71% yield), and by HF, which concurrently removes many amine protective groups. Monoesterification of a symmetrical dicarboxylic acid chloride can be effected by reaction with a hydroxymethyl copolymer of styrene-divinylbenzene to give an ester a mono salt of a diacid was converted into a dibenzyl polymer. ... 

Modern SEC columns are packed with material other than polystyrene gels, such as porous silica particles or highly cross-linked styrene-divinylbenzene copolymers. Because of improvements in speed and resolution, the term SEC is sometimes replaced by the term high-performance size-exclusion chromatography (HPSEC). 

Shodex has a wide variety of columns for organic GPC using organic solvents. The columns are packed with porous styrene-divinylbenzene copolymer gels especially developed for GPC use. Five types of standard-size GPC columns packed with different solvents are available. Downsized GPC columns are also available. 

The Shodex GPC KF-600 series is packed with 3- im styrene-divinylbenzene copolymer gels in a column having a volume of about one-third compared to standard-types of columns, which are best suited for reducing the organie solvents eonsumption, shortening the analysis time, and lowering the detection limit (Table 6.5). 

Monoesterification of a symmetrical dicarboxylic acid chloride can be effected by reaction with a hydroxymethyl copolymer of styrene-divinylbenzene to give an ester a mono salt of a diacid was converted into a dibenzyl polymer." ... 

These small columns,(usually 10 mm X 1-4.6 mm i.d.) are normally packed with 10-40 p.m sorbents such as Cig-bonded silica, Cg-bonded silica or styrene-divinylbenzene copolymer. These sorbents are not very selective and more selective sorbents, such as the immunosorbent (94), have also been used with good results. Coupling of SPE-gas chromatography is in fact the one most often used in environmental analysis because it reaches a high level of trace enrichment, eliminates water and elutes retained compounds easily with an organic solvent that can be injected into the gas chromatograph. 

A research group in Lehigh University has extensively studied the synthesis and characterization of uniform macroporous styrene-divinylbenzene copolymer particles [125,126]. In their studies, uniform porous polymer particles were prepared via seeded emulsion polymerization in which linear polymer (polystyrene seed) or a mixture of linear polymer and solvent were used as inert diluents [125]. The average pore diameter was on the order of 1000 A with pore volumes up to... 

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