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Clickable poly(ethylene glycol) (PEG) derivatives are used with two sequential aqueous two‐phase systems to produce microsphere‐based scaffolds for cell encapsulation. In the first step, sodium sulfate causes phase separation of the clickable PEG precursors and is followed by rapid geleation to form microspheres in the absence of organic solvent or surfactant. The microspheres are washed and then...