Recovery is a term that is often associated with the circular economy model. It is implemented in the company Premifab Ltd. that recovers waste organic solvents from various industries with the aim of prolonging product value. Recovery is carried out by batch distillation, after which distillation sludge of various chemical composition remains unused what leads to its disposal at company’s own expense. To give value to distillation sludge, it is necessary to determine its chemical composition. The aim of this work was to develop and validate a chromatographic method for the determination of residual organic solvents in distillation sludge obtained by batch distillation of waste organic solvents. The method was developed on a gas chromatograph with an FID detector and headspace sampling. After the method was developed, validation was performed to confirm the suitability of the method for its purpose. The validation results showed that the method is suitable for the determination of methanol, ethanol, acetone, isopropanol, methyl-ethyl-ketone, ethyl-acetate, cyclohexane, isooctane, and toluene in distillation sludge. For the determination of other organic solvents, methoxy-2-propanol, butanol, methyl-isobutyl-ketone, ethoxy-2-propanol, butyl-acetate, ethylbenzene and xylene isomers, further optimization of the method is required. After validation, a real sample of distillation sludge obtained by distilling a mixture of waste solvents methyl-ethyl-ketone and ethyl-acetate originating from the flexible packaging industry was analyzed. By applying the method of internal standard and relative response factor, quantification of the examined sample of production sludge was successfully performed.