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