Concepts for the characterization of composite latex particles by adva
nced solid-state NMR methods are discussed. The techniques are based o
n H-1 spin-diffusion experiments usually applied to detect heterogenei
ties in polymers and polymer blends. In latexes, they allow one to cha
racterize the morphology, including substructures in the interphase be
tween core and shell. Motional heterogeneities within the phases are a
lso detected. The techniques are used to characterize an extended seri
es of core-shell particles composed of poly(n-butyl acrylate) (PBuA) a
nd poly(methyl methacrylate) (PMMA) synthesized in semicontinuous two-
step emulsion polymerization processes. The influence of process param
eters such as synthesis temperature, crosslinking density in the core,
shell content, particle size, and annealing are investigated.