Matrix-assisted laser desorption/ionization time-of-flight (MALDI/TOF)
mass spectrometry has been used for the analysis of poly(butyl methac
rylate) synthesized by group-transfer polymerization, and the absolute
molecular weight distributions have been determined for polymers up t
o 100 000. For lower molecular weight poly(butyl methacrylate) we obta
ined structural information confirming composition and end groups. The
compounds were desorbed from trans-3-indoleacrylic acid and detected
as positive ions showing molecular weight and several multiply charged
distributions from submilligram amounts of sample. The results provid
ed answers to ambiguities which two separate GPC measurements had crea
ted. MALDI results were supported by light scattering measurements.