A group from the University of Nottingham working with a Nottingham company, Molecular Profiles, have developed a method for quantifying the amount of amorphous material in a substance by H/D exchange.  As yet this was demonstrated only for lactose, but surely extensions will follow (P T Whiteside et al, Pharm Res., 2008), DOI 10.1007/s 11D95-008-9682-4.

The samples are exposed to a flow of D₂O vapour followed by FT Ramon spectroscopy monitoring the OD wavelength.  A linear response if the integral of the OD band with amorphous content was obtained.  The limit of detection is approx 1-7%.