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6716294 
Journal Article 
Synthesis and characterisation of poly(sodium 4-styrenesulfonate) combs 
Fernyhough, CM; Young, RN; Ryan, AJ; Hutchings, LR; , 
2006 
1 
Polymer
ISSN: 0032-3861 
ELSEVIER SCI LTD 
OXFORD 
3455-3463 
WOS:000237859400020 
A series of poly(sodium 4-styrenesulfonate) (NaPSS) combs has been synthesized. Architecturally and molecularly well-defined polystyrene combs were initially produced with the branch molecular mass fixed at 30,000 g/mol, the average number of branches being the major variable. Conditions were established whereby linear polystyrene (PS) synthesized via anionic polymerization was chloromethylated using zinc (11) chloride, side-reactions such as Friedel-Crafts alkylation being suppressed. An excess of diphenylethylene-capped polystyryllithium (PSLi) was then reacted with the functionalized backbone to yield materials having long chain branches. The polystyrene combs were then reacted with sulfuric acid to yield water-soluble poly (styrenesulfonic acid) combs and subsequently neutralized with sodium hydroxide to give the corresponding sodium 4-styrene sulfonate species. The extent of sulfonation was determined via titration and nuclear magnetic resonance spectroscopy (NMR). Aqueous triple-detector size exclusion chromatography (SEC) was used to characterize the sulfonated combs. Although the SEC traces were monomodal and the M-n values agreed well with the expected values, an increase in the polydispersity index compared to the polystyrene combs may reflect the susceptibility of the sulfonation reaction to cross-linking. (c) 2006 Elsevier Ltd. All rights reserved.