Sampling and analytical procedures for use in monitoring worker exposure to dichloroethyl-ether (111444), isophorone (78591), toluene (108883), diisobutyl-ketone (108838), and isopropyl-ether (108203) are presented. Methods described are validated under the NIOSH/OSHA Standards Completion Program for Set-V compounds. Validated methods are suitable for determining compliance with standards or need for control, research, or when measurements of airborne concentrations in the workplace are required. Parameters utilized in each analytical sequence include principle of method, range and sensitivity, interferences, precision and accuracy, advantages and disadvantages, apparatus, reagents, procedures, calibration and standards, calculations, and references cited. Procedures described are applicable for each compound and include adsorption on charcoal, desorption with carbon disulfide, and gas chromatography.