The characterization of branched polymers is available utilizing the techniques
listed below. Other analyses may be appropriate, dependent on the polymer structure
and area of interest.
13C Nuclear Magnetic Resonance (NMR) Spectroscopy Provides a sensitive measurement
of the magnetic environment for every carbon atom in the polymer. Symmetrical polymers
with equivalent terminal groups typically have a balanced magnetic environment,
providing a spectrum that is easily interpreted for even the higher molecular weight
materials.
Mass Spectrometry (MS) The electrospray ionization technique used in this analysis strips away
the solvent, leaving gas-phase ions that are introduced into a conventional quadrapole mass
spectrometer. Formation of the ions from solutions at room temperature results in low energy
ionization that minimizes fragmentation. Spectra of the molecular ions, as they exist in solution,
are produced and direct calculations of the molecular weight distributions of the sample are made.
Size Exclusion Chromatography (SEC) Separates polymer molecules by hydrodynamic volume with smaller
molecules retained longer on the column. Increases in polymer size correspond to increases in molecular
weight; therefore, SEC is used to measure the distribution of molecular weights in a sample. Refractive
index detectors determine relative molecular weight values based on a series of known standards. Light
scattering detection is used to determine the absolute molar masses and sizes of polymers in solution as
well as detect aggregations. Light scattering is used independently or in combination with size
exclusion chromatography.
Gel Electrophoresis/High Performance Capillary Electrophoresis (HPCE) Hyperbranched polymers resemble
globular proteins in their size and morphology. As a result, polyacrylamide gel electrophoresis (PAGE)
is valuable as a tool to separate monomers and oligomers by drawing analytes through increasingly smaller
gel pores. Capillary electrophoresis has a high number of theoretical plates, which are particularly
useful in separating hyperbranched polymers based on the electrophoretic mobility of the molecule.