Exploratory synthetic strategies may yield limited quantities of sample. Characterization of such limited-quantity samples is facilitated by the use of sensitive analytical methods and smart sample preparation. Polymers may be analyzed by mass spectrometry for molecular weight distributions, structural information (such as endgroups), and impurities. However, polymer research using mass spectrometry has not focused on detection limits; in some work the amount of polymer used is not even mentioned. Studies to determine detection limits of polymers and studies that characterize sample preparation techniques can provide valuable information.

Examination of the sample surface on a probe tip, generated by the use of an aerospray technique for sample deposition, was accomplished by scanning electron microscopy (SEM). Aerospraying the polymer and matrix solutions allowed signal averaging of mass spectra from up to 400 shots on the same sample spot. SEM images showed the surface of the probe to have a fairly uniform coating of the sample and matrix.