Page:NIOSH Manual of Analytical Methods - 2534.pdf/1
TETRAMETHYL LEAD (as Pb)
Pb(CH3)4
MW: 267.34
METHOD: 2534, Issue 2
CAS: 75-74-1
2534
RTECS: TP4725000
EVALUATION: FULL
OSHA : 0.075 mg/m 3 (as Pb; skin) NIOSH: 0.075 mg/m 3 (as Pb; skin) ACGIH: 0.15 mg/m 3 (as Pb; skin) (1 ppm = 8.47 mg/m 3 as Pb)
Issue 1: 15 August 1987 Issue 2: 15 August 1994
PROPERTIES: liquid; d 1.995 g/mL @ 20 °C; BP 110 °C; MP -27.5 °C; VP 2.9 kPa (22 mm Hg; 245 g/m 3 as Pb) @ 20 °C; lower explosive limit 1.8% v/v in air
SYNONYMS: TML; lead tetramethyl; tetra methyl plumbane
SAMPLING
MEASUREMENT
SAMPLER:
SOLID SORBENT TUBE (XAD-2 resin, 400 mg/200 mg)
TECHNIQUE:
GAS CHROMATOGRAPHY, PHOTOIONIZATION DETECTOR
FLOW RATE:
0.01 to 0.2 L/min
ANALYTE:
tetramethyl lead
VOL-MIN: -MAX:
15 L 100 L
DESORPTION:
2 mL pentane; stand 30 min
SHIPMENT:
routine
INJECTION VOLUME:
5 µL
SAMPLE STABILITY:
98% recovered after 7 days @ 25 °C [1]
BLANKS:
2 to 10 field blanks per set
TEMPERATURE-INJECTOR: -MANIFOLD: -PID: -COLUMN: CARRIER GAS:
N 2, 17 mL/min
COLUMN:
6 m x 3-mm OD stainless steel packed with 10% Carbowax 20M on 80/100 mesh Chromosorb WHP
CALIBRATION:
standard solution of tetramethyl lead in pentane
RANGE:
1 to 10 µg (as Pb) per sample
ACCURACY
0.04 to 0.18 mg/m 3 (as Pb) (24-L samples) [1]
RANGE STUDIED: BIAS:
- 0.27%
ˆ ): OVERALL PRECISION (S rT
0.112
ACCURACY:
± 22.2%
185 °C 200 °C 210 °C 75 °C
ESTIMATED LOD: 0.4 µg (as Pb) per sample [2] PRECISION (Sr):
0.0763 @ 0.9 to 3.6 µg (as Pb) per sample [1]
APPLICABILITY: The working range is 0.04 to 0.4 mg/m 3 (as Pb) for a 24-L air sample.
INTERFERENCES: None identified. The chromatographic column or separation conditions may be changed to circumvent interference problems.
OTHER METHODS: This revises Method S384 [2].
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94