Page:NIOSH Manual of Analytical Methods - 2524.pdf/1

 DIMETHYL SULFATE

(CH3O)2SO2

MW: 126.13

METHOD: 2524, Issue 2

2524

CAS: 77-78-1

RTECS: WS8225000

EVALUATION: PARTIAL

OSHA : 0.1 ppm (skin) NIOSH: 0.1 ppm/8 hours (skin); carcinogen ACGIH: 0.1 ppm (skin); suspect carcinogen (1 ppm = 5.16 mg/m 3 @ NTP)

Issue 1: 15 May 1985 Issue 2: 15 August 1994

PROPERTIES: liquid; d 1.332 g/mL @ 20 C; BP 188 °C with decomposition; MP -31.8 °C; VP 0.07 kPa (0.5 mm Hg; 700 ppm) @ 20 °C

SYNONYMS: methyl sulfate

SAMPLING SAMPLER:

SOLID SORBENT TUBE (Poropak P, 100 mg/50 mg)

FLOW RATE:

0.01 to 0.2 L/min

VOL-MIN: -MAX:

0.25 L @ 1 ppm 12 L

SAMPLE STABILITY:

at least 1 week @ 25 °C [1]

BLANKS:

2 to 10 field blanks per set

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, ELECTROLYTIC CONDUCTIVITY DETECTOR (SULFUR MODE)

ANALYTE:

dimethyl sulfate

DESORPTION:

1 mL diethyl ether, 30 min

INJECTION VOLUME:

TEMPERATURE-INJECTION: -COLUMN:

1.8 to 24.5 mg/m 3 [1] (1.2-L samples)

BIAS:

see EVALUATION OF METHOD

ˆ ): 0.073 [1] OVERALL PRECISION (S rT ACCURACY:

not determined

180 °C 2 min @ 50 °C; then 30 °C/min to 120 °C; hold

CARRIER GAS:

He, 20 mL/min

COLUMN:

1.8 m x 3.2-mm OD stainless steel, packed with 5% DEGS on 80/100 mesh Chromosorb WHP

CALIBRATION:

dimethyl sulfate in diethyl ether

RANGE:

1 to 120 µg per sample

ACCURACY RANGE STUDIED:

4 µL

ESTIMATED LOD: 0.25 µg per sample [1] PRECISION (Sr):

0.06 @ 1.1 to 39 µg per sample [1]

APPLICABILITY: The working range is 0.03 to 4 ppm (0.17 to 20 mg/m 3) for a 6-L air sample.

INTERFERENCES: None identified.

OTHER METHODS: This revises P&CAM 301 [2].

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