Page:NIOSH Manual of Analytical Methods - 3516.pdf/1

 CROTONALDEHYDE CH3CH=CHCHO

MW: 70.09

METHOD: 3516, Issue 1

3516

CAS: 4170-30-3

RTECS: GP9499000

EVALUATION: FULL

OSHA : 2 ppm NIOSH: 2 ppm ACGIH: 2 ppm; suspect carcinogen (1 ppm = 2.87 mg/m 3 @ NTP)

Issue 1: 15 August 1994

PROPERTIES: liquid; pungent odor; BP 104 °C; d 0.85 g/mL @ 20 °C; VP 2.7 kPa (20 mm Hg, 2.6% v/v) @ 20 °C; explosive range 2.1 to 15.5% v/v in air

SYNONYMS: crotonic aldehyde; trans-2-butenal, crotonal

SAMPLING SAMPLER:

TECHNIQUE:

D I F F E R E N T I A L POLAROGRAPHY

FLOW RATE: 0.1 to 0.2 L/min

ANALYTE:

crotonaldehyde oxime

VOL-MIN: -MAX:

1 L @ 2 ppm 49 L

DROP TIME:

1s

SCAN RATE:

5 mV/s

SHIPMENT:

refrigerate bubblers at 8 °C during shipment if samples cannot be analyzed within 4 h

SCAN RANGE:

-0.6 to -1.2 V (vs. SCE)

CALIBRATION:

standard solutions of crotonaldehyde in hydroxylamine/formate buffer solution

RANGE:

35 to 139 µg per sample

SAMPLE STABILITY:

BLANKS:

MIDGET BUBBLER (hydroxylamine/formate buffer solution)

MEASUREMENT

4 h maximum @ 25 °C, 7 days minimum at 8 °C

P U L S E

2 to 10 field blanks per set ESTIMATED LOD: not determined PRECISION (Sr):

0.024 [1]

ACCURACY RANGE STUDIED:

2.9 to 23.4 mg/m 3 (12-L samples)

BIAS:

-2.8%

ˆ rT): 0.061 (2.9 to 11.6 mg/m 3) [1] OVERALL PRECISION (S ACCURACY:

±14.8%

APPLICABILITY: The working range is 1 to 10 ppm (2.9 to 29 mg/m 3) for a 12-L air sample. The upper limit of the method is dependent on the concentration of hydroxylamine, which should be maintained at 50-fold molar excess over total amount of crotonaldehyde sampled. Collection efficiency outside the method range has not been evaluated.

INTERFERENCES: Other volatile aldehydes (e.g., acrolein, formaldehyde, benzaldehyde).

OTHER METHODS: This is Method P&CAM 285 [2] in a revised format. An aldehyde screening method [3] and a method for priority pollutants [4], both of which include crotonaldehyde, have been described.

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