Page:NIOSH Manual of Analytical Methods - 7082.pdf/1

 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