The paper presents two sample preparation procedures for the determination of aldehydes in wet deposition. In both cases the 2,4-dinitrophenylhydrazine derivatization and solid phase extraction were applied. The derivatization in method A was applied before the extraction, the extraction in method B was carried out with simultaneous derivatisation. Accuracy of both methods was evaluated on the basis of the analysis of aqueous solutions of selected carbonyl compounds. Both methods were characterized by good recovery, however, due to the precision of the method expressed as RSD for testing of environmental samples the method B was used. The analysis of environmental samples showed significant differences in the concentrations of aldehydes in wet deposition, depending on the location of the sampling point. In the case of samples taken from agricultural areas the predominant aldehydes were formaldehyde and acetaldehyde. Formaldehyde was from 31% to 47% of the determined compounds. While in samples collected near a traffic source, in the deposition acrolein was determined at the levels from 62% to 64% of the identified compounds.