LEAD by Flame AAS
Pb
MW:
7082
207.19 (Pb) CAS: 7439-92-1 (Pb) RTECS: 223.19 (PbO) 1317-36-8 (PbO)
METHOD: 7082, Issue 2
EVALUATION: FULL
OSHA : 0.05 mg/m3 NIOSH: <0.1 mg/m3; blood Pb 60 µg/100 g ACGIH: 0.05 mg/m3
OF7525000 (Pb) OG1750000 (PbO) Issue 1: 15 February 1984 Issue 2: 15 August 1994
PROPERTIES: soft metal; d 11.3 g/cm3; MP 327.5 C valences +2, +4 in salts
SYNONYMS: elemental lead and lead compounds except alkyl lead
SAMPLING
MEASUREMENT
SAMPLER:
FILTER (0.8-µm cellulose ester membrane)
TECHNIQUE:
ATOMIC ABSORPTION SPECTROPHOTOMETER, FLAME
FLOW RATE:
1 to 4 L/min
ANALYTE:
lead
VOL-MIN: -MAX:
200 L @ 0.05 mg/m3 1500 L
ASHING:
SHIPMENT:
routine
FINAL SOLUTION:
10% HNO3, 10 mL
SAMPLE STABILITY:
FLAME:
air-acetylene, oxidizing
stable WAVELENGTH:
283.3 nm
BLANKS:
2 to 10 field blanks per set BACKGROUND CORRECTION:
D2 or H2 lamp, or Zeeman
CALIBRATION:
Pb2+ in 10% HNO3
RANGE
10 to 200 µg per sample [2,3]
ESTIMATED LOD:
2.6 µg per sample [4]
PRECISION ( r):
0.03 [1]
ACCURACY RANGE STUDIED:
BIAS: OVERALL PRECISION(
ACCURACY:
0.13 to 0.4 mg/m3 [1]; 0.15 to 1.7 mg/m3 (fume) [2] 3.1% rT): 0.072 [1]; 0.068 (fume) [2]
conc. HNO3, 6 mL + 30% H2O2, 1 mL; 140 C
± 17.6%
APPLICABILITY: The working range is 0.05 to >1 mg/m3 for a 200-L air sample. The method is applicable to elemental lead, including Pb fume, and all other aerosols containing lead. This is an elemental analysis, not compound specific. Aliquots of the samples can be analyzed separately for additional elements.
INTERFERENCES: Use D2 or H2 continuum or Zeeman background correction to control flame or molecular absorption. High concentrations of calcium, sulfate, carbonate, phosphate, iodide, fluoride, or acetate can be corrected.
OTHER METHODS: This method combines and replaces P&CAM 173 [3] and S341 [4,5] for lead. Method 7300 (ICP-AES) and 7105 (AAS/GF) are alternate analytical methods. Method 7505 is specific for lead sulfide. The following have not been revised: the dithizone method, which appears in P&CAM 102 [5] and the lead criteria document [6]; and P&CAM 191 (ASV) [7].
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
