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 NICKEL CARBONYL: METHOD 6007, Issue 2, dated 15 August 1994 - Page 4 of 4 NOTE 2:

If peak height is above the linear range of the working standards, dilute an aliquot of the desorbed liquid with 3% HNO 3, reanalyze and apply the appropriate dilution factor in calculations.

CALCULATIONS: 14.

15.

Determine the mass, µg (corrected for DE) of Ni found in the sample front (W f) and back (W b) sorbent sections, and in the average media blank front (B f) and back (B b) sorbent sections. NOTE: If W b > W f/10, report breakthrough and possible sample loss. Calculate concentration, C, of nickel carbonyl in the air volume sampled, V (L):

where: 2.91 = stoichiometric conversion factor from Ni to Ni(CO)

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EVALUATION OF METHOD: Method P&CAM 344 was issued on August 31, 1981 [2], and evaluated with generated atmospheres of Ni(CO) 4 containing 6 to 300 ppm added carbon monoxide. Mean recovery was 93% (24 samples) in the range 5 to 121 µg/m 3 (0.0007 to 0.017 ppm). Breakthrough (effluent = 5% of test concentration) did not occur after sampling for 240 min at 0.475 L/min from an atmosphere containing 34 µg/m 3 (0.005 ppm) Ni(CO) 4 in air at 22 °C and 19% RH. Desorption efficiency for eighteen samples containing 0.08 to 0.5 µg Ni (nickel nitrate standard solution added to 120 mg charcoal) averaged 0.934 with S r = 0.029. Nickel carbonyl was observed to pass quantitatively through 0.8-µm cellulose ester membrane filters in these experiments.

REFERENCES: [1] [2] [3]

Eller, P. M. "Determination of Nickel Carbonyl by Charcoal Tube Collection and Furnace Atomic Absorption," Appl. Ind. Hyg. 1:115-118 (1986). NIOSH Manual of Analytical Methods, 2nd ed., Vol. 7, P&CAM 344, U.S. Department of Health and Human Services, Publ. (NIOSH) 82-100 (1982). Special Occupational Hazard Review and Control Recommendations for Nickel Carbonyl, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-184 (1977).

METHOD WRITTEN BY: Peter M. Eller, Ph.D., NIOSH/DPSE.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94