A method for the sampling and analysis of nickel (7440020) metal, stainless steel, and nickel-oxide (1313991) in the air of the workplace environment was tested for NIOSH validation. Samples were on a 37 millimeter 0.8 micron Type AA Millipore cellulose ester filter, acid digested, and analyzed by graphite furnace atomic absorption spectrophotometry. The protocol for establishing NIOSH validation of the method was to analyze spiked samples and samples from dynamically generated test atmospheres, test the storage stability of spiked and generated filters, and test the breakthrough capacity of a cellulose ester filter. The aerosol generation and sampling system was presented. The absolute total error for sampling and analysis was less than 25 percent at the NIOSH recommended standard 95 percent of the time. The authors conclude this method satisfies NIOSH criteria for validation.