The use of 15% ethyl ether/hexane as the extracting solvent for BIS(2‐chloro‐)ethers in aqueous samples is evaluated using the p‐value approach to liquid‐liquid extraction. The evaluation supports the choice of solvent and largely accounts for diminished recovery of the BIS(2‐chloro‐)ethers in terms of losses that occur during solvent enrichment, particularly as affected by nitrogen blow‐down from 8 ml to 1 ml.