We performed WAXS procedures immediately upon completion of the SAXS procedures using the same 30 silk samples at the end station of beamline BL01C2 at NSRRC, Hsinchu, Taiwan. We used the same samples because we were interested in measuring a combination of nanostructural properties within the crystalline, amorphous and lamella regions of the same silk threads. We thus first performed a series of pre-tests to establish that the short exposure time (10–60 s) of the SAXS procedures was unlikely to damage the silk nanostructures and affect the WAXS measurements.