Page:NIOSH Manual of Analytical Methods - 6007.pdf/1

 NICKEL CARBONYL

Ni(CO)4

MW: 170.73

METHOD: 6007, Issue 2

CAS: 13463-39-3

6007

RTECS: QR6300000

EVALUATION: PARTIAL

OSHA : 0.001 ppm (as Ni) NIOSH: 0.001 ppm; carcinogen ACGIH: 0.05 ppm (as Ni) (1 ppm = 6.98 mg/m 3 @ NTP)

Issue 1: 15 August 1987 Issue 2: 15 August 1994

PROPERTIES: liquid; d 1.318 g/mL @ 20 °C; BP 43 °C; MP -25 °C; VP 43 kPa (321 mm Hg; 42% v/v) @ 20 °C; lower explosive limit 2% v/v in air

SYNONYMS: nickel tetracarbonyl

SAMPLING SAMPLER:

PREFILTER + SOLID SORBENT TUBE (low-Ni charcoal, 120 mg/60 mg; 0.8-µm cellulose ester membrane)

MEASUREMENT TECHNIQUE:

ATOMIC ABSORPTION, GRAPHITE FURNACE

ANALYTE:

nickel

DESORPTION:

1 mL 3% HNO 3; 30 min ultrasonic bath

INJECTION VOLUME:

20 µL

FLOW RATE: 0.05 to 0.2 L/min VOL-MIN: -MAX:

7 L @ 0.001 ppm 80 L

SHIPMENT:

routine

SAMPLE STABILITY:

BLANKS:

GRAPHITE FURNACE: 95% recovered after 17 days @ room temperature [1]

110 °C dry 30 sec; 800 °C char 15 sec; ≥ 2700 °C atomize 10 sec

WAVELENGTH:

232 nm, with background correction

CALIBRATION:

standard solution of Ni 2+ in 3% (w/v) HNO 3

RANGE:

0.05 to 0.6 µg Ni per sample [1]

2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

0.0007 to 0.017 ppm [1] (3- to 40-L air samples)

BIAS:

- 7% [1]

ESTIMATED LOD: 0.01 µg Ni per sample [1] PRECISION (Sr):

0.028 @ 0.08 to 0.5 µg Ni per sample

ˆ ): 0.099 [1] OVERALL PRECISION (S rT ACCURACY:

± 26.4%

APPLICABILITY: The working range is 0.00036 to 0.007 ppm (0.0025 to 0.05 mg/m 3) nickel carbonyl for a 20-L air sample.

INTERFERENCES: Particulate nickel compounds will give a positive interference unless a prefilter is used during sampling.

OTHER METHODS: This revises P&CAM 344 [2]. A colorimetric method has also been recommended [3].

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