A protocol is described for measuring and analyzing neutron reflectivity da
ta from a buried oil-water interface. A hexadecane-water interface is consi
dered, and data from the bare interface and from films of polybutadiene-pol
y(ethylene oxide) Linear diblock copolymers with M-w similar to 60 000 g mo
l(-1) and containing similar to 50 mol % poly(ethylene oxide) spread (with
interfacial concentrations of Gamma = 4 and 10 mg m(-2)) at the interface a
re reported. From the analysis, it emerges that the hexadecane-water interf
ace is "rougher" than capillary wave theory based expectations. This could
be attributable to the influence of molecular size and shape on the intrins
ic thickness of the interface. When present, the amphiphilic copolymers seg
regate at the interface with the blocks occupying a concentrated region (si
milar to 20% polymer) with thickness similar to 20 Angstrom and a dilute re
gion (much less than 10% polymer) of thickness similar to 50 Angstrom on ei
ther side of a nominal dividing surface. The amount of copolymer at the int
erface, determined using a Guinier-type analysis, is in line with the sprea
d amount at the interface at a moderate (Gamma = 4 mg m(-2)) interfacial co
ncentration but is consistent with a more expanded configuration at Gamma =
10 mg m(-2).