Page:NIOSH Manual of Analytical Methods - 2515.pdf/1

 DIAZOMETHANE CH2=N+N-

MW: 42.04

METHOD: 2515, Issue 2

2515

CAS: 334-88-3

RTECS: PA7000000

EVALUATION: PARTIAL

OSHA : 0.2 ppm NIOSH: 0.2 ppm ACGIH: 0.2 ppm; suspect carcinogen (1 ppm = 1.719 mg/m 3 @ NTP)

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

PROPERTIES: yellow gas; MP -145 °C; BP -23 °C; pure material explodes above 150 °C; impure material explodes at lower temp.

SYNONYMS: azimethylene; diazirine

SAMPLING SAMPLER:

MEASUREMENT

SOLID SORBENT TUBE (octanoic acid-coated XAD-2 resin, 100 mg/50 mg)

TECHNIQUE:

GAS CHROMATOGRAPHY, FID

ANALYTE:

methyl octanoate

FLOW RATE:

0.2 L/min

DESORPTION:

1 mL carbon disulfide; stand 30 min

VOL-MIN: -MAX:

6L 30 L

INJECTION VOLUME:

SHIPMENT:

routine

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

SAMPLE STABILITY:

not determined

CARRIER GAS:

N 2, 30 mL/min

BLANKS:

2 to 10 field blanks per set

COLUMN:

stainless steel, 3 m x 3-mm OD, 5% SP-1000 on 100/120 mesh Chromosorb WHP preceded by a 15 cm x 3-mm OD stainless steel precolumn packed with 10% Carbowax 20M and 1.2% NaOH on 80/100 mesh Gas Chrom Q

CALIBRATION:

methyl octanoate in carbon disulfide with internal standard

RANGE:

2 to 8 µg diazomethane (8 to 32 µg methyl octanoate) per sample

ACCURACY RANGE STUDIED:

BIAS:

0.17 to 0.80 mg/m 3 [1] (10-L samples) -30% at 0.17 mg/m 3 [1]; -10% at 0.36 to 0.75 mg/m 3 [1]

ˆ ): 0.084 [1] OVERALL PRECISION (S rT ACCURACY:

22.5% at 0.36 to 0.75 mg/m 3

5 µL 225 °C 250 °C 95 °C

ESTIMATED LOD: not determined PRECISION (Sr):

0.024 [1]

APPLICABILITY: The working range is 0.1 to 0.6 ppm (0.2 to 1 mg/m 3) diazomethane for a 10-L air sample.

INTERFERENCES: None reported.

OTHER METHODS: This revises S137 [2].

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