We have developed a method of measuring the distribution of polymer se
gments at a liquid/liquid interface using neutron reflection. The meth
od consists of forming a stable (1-4 mu m) hexane layer on top of an a
queous sub-phase so that two interfaces contribute to the measured ref
lectivity. This has been done by condensing vapour onto the surface in
an accurately temperature-controlled environment. The neutron reflect
ivity was measured at four angles of incidence on the SURF reflectomet
er. The attenuation of the reflectivity from the lowest angle is used
to determine the thickness of the hexane layer. A series of poly(ethyl
ene oxide) poly(propylene oxide) ABA block copolymers adsorbed at the
hexane/water interface have been investigated. Since the polymers were
hydrogenous, measurements were made with D2O as the aqueous phase and
with either null reflecting hexane or 60% D-hexane as the oil phase i
n order to obtain adequate contrast. The polymer volume fraction profi
le has been determined by simultaneous fits to the data from these com
binations of solvent contrasts. It was found that there was a good cor
relation between the molar mass of the poly(ethylene oxide) block and
the thickness of the polymer layer in the aqueous phase and that the c
hains were stretched beyond their radii of gyration expected for bulk
solution. (C) 1998 Elsevier Science B.V. All rights reserved.