Determination of nickel carbonyl by charcoal tube collection and furnace atomic absorption spectrophotometry.
Appl Ind Hyg 1986 Sep; 1(3):115-118
An analytical procedure was developed for the determination of the toxic gas, nickel-carbonyl (13463393), which is used in the Mond process for the production of nickel and in the synthesis of methyl- acrylate and ethyl-acrylate monomers. A test atmosphere was generated by the injection of several microliters of nickel-carbonyl liquid into 10 percent carbon-monoxide and 90 percent nitrogen and pressurizing to 40 pounds per square inch gauge (psig); carbon- monoxide stabilized the nickel-carbonyl. The pressure vessel contained 6 parts per million of nickel-carbonyl and served as a reservoir from which the desired atmospheres were produced by combining samples with humidified air and 10 percent carbon-monoxide in nitrogen. The nickel-carbonyl concentration in the test atmosphere was determined by atomic absorption spectrophotometry after sampling in midget impingers containing 5 percent iodine in isopropanol. The new sampling method used a Calgon coconut based charcoal sorbent which was washed in nitric-acid before use. After sample adsorption, the sorbent was eluted with 3 percent nitric-acid in an ultrasonic water bath and aliquots analyzed by graphite furnace atomic absorption spectrophotometry. The desorption efficiency was 0.934 for nickel-nitrate at the concentration range carbonyl in air ranged between 90.8 and 95.0 percent. The author concludes that the sensitivity of the method makes it possible to determine nickel-carbonyl concentrations of 2 to 50 micrograms per cubic meter of air corresponding to 0.4 to 7 parts per billion in a 20 liter sample.
NIOSH-Author; Analytical-chemistry; Sampling-methods; Chemical-analysis; Air-sampling; Nickel-compounds; Toxic-gases; Adsorbents; Atomic-absorption-spectrometry
Applied Industrial Hygiene