The synthesis of various D-labeled perfume ingredients (orris-like, sandalwood-like, musky, and amber-like) is presented. These substances, possessing practically identical H 2 O/solid and solid/gas partition coefficients as their unlabeled analogues, are used as internal standards for the validation of a new analytical GC/MS method for the determination of low residual concentrations in H 2 O after biodegradability tests.