Thin layer chromatography with a flame ionization detection (TLC‐FID) technique was applied to the separation and determination of nonionic surfactants containing oxyethylene (OE) chains. The OE adducts with an average number of 4.2, 6.0 and 8.0 oxyethylene units were separated on Chromarod S‐II (Silica gel‐coated rods) with double development using benzene:ethyl acetate (6:4) and ethyl acetate:acetic acid:water (8:1:1). OE adducts of nonionic surfactants were well separated by the TLC‐FID method using simple and standard techniques that eliminate the need for any chemical modification.