Amphiphilic block copolymers are used in a variety of applications, for example, as stabilizers for emulsions and dispersions or as compatibilizers in polymer blends. Amphiphilic diblock copolymer composed of methoxypoly(ethylene glycol) and polystyrene (MPEG-b-PS) was synthesized using atom transfer radical polymerization (ATRP) and nitroxide-mediated radical polymerization (NMRP). In order to synthesize MPEG-b-PS diblock copolymer using ATRP, monofunctional MPEG macroinitiator (chloroacetylated MPEG [MPEG-Cl]) was prepared from monohydroxyfunctional poly(ethylene glycol) and initiated end group on the basis of chloroacetyl chloride. ATRP was carried out in bulk using MPEG-Cl as the macroinitiator, copper chloride (CuCl)/2,2 0 -bipyridine (bipy) as the catalyst ([MPEG-Cl]/[CuCl]/[bipy] ¼ 1:1:3), and styrene as the monomer. For preparation of MPEG-b-PS by means of NMRP, firstly, 1-hydroxy-2,2,6,6-tetramethylpiperidine (TEMPO-OH) was obtained by reduction of 2,2,6,6-tetramethyl-piperidinyl-1oxy (TEMPO) with sodium ascorbat. Then, TEMPO-OH was coupled with chloroacetylated MPEG (MPEG-Cl) to yield the macroinitiator MPEG terminated with a TEMPO unit
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