Page:NIOSH Manual of Analytical Methods - 1604.pdf/1

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ACRYLONITRILE

CH2=CHCN

MW : 53.06

METHOD: 1604, Issue 2

CAS: 107-13-1

1604

RTECS: AT5250000

EVALUATION: FULL

OSHA : 2 ppm; C 10 ppm (skin) NIOSH: carcinogen; 1 ppm; C 10 ppm/15 min; Group I Pesticide (skin) ACGIH: carcinogen; 2 ppm (skin) (1 ppm = 2.17 mg/m 3 @ NTP)

Issue 1: 15 February 1984 Issue 2: 15 August 1994

PROPERTIES: liquid; d 0.806 g/mL @ 20 °C; BP 77.2 °C; VP 11 kPa (83 mm Hg 11% v/v) @ 20 °C; explosive range 3 to 17% v/v in air

SYNONYMS: 2-propenenitrile; vinyl cyanide; AN.

SAMPLING SAMPLER:

SOLID SORBENT TUBE (coconut shell charcoal, 100 mg/50 mg)

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, FID

ANALYTE:

acrylonitrile

DESORPTION:

1 mL 2% (v/v) acetone in CS 2; stand 30 min

FLOW RATE: 0.01 to 0.2 L/min VOL-MIN: -MAX:

3.5 L @ 2 ppm 20 L

SHIPMENT:

routine

INJECTION VOLUME: 2 µL

SAMPLE STABILITY:

at least 7 days @ 25 °C [1,2]

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

BLANKS:

2 to 10 field blanks per set

CARRIER GAS:

N 2 or He, 25 mL/min

COLUMN:

3-m x 3-mm stainless steel, 20% SP-1000 on 80/100 Chromosorb WHP

CALIBRATION:

standard solutions of distilled acrylonitrile in hexane

RANGE:

15 to 1000 µg per sample [1]

ACCURACY RANGE STUDIED: BIAS:

1 to 100 mg/m 3 [1,2] (20-L samples) - 4.8%

200 °C 200 °C 85 °C

ESTIMATED LOD: 1 µg per sample [1]

ˆ ): 0.06 [1,2] OVERALL PRECISION (S rT ACCURACY:

± 14.1%

PRECISION (Sr):

0.06 @ 16 µg per sample [1]

APPLICABILITY: The working range is 0.7 to 46 ppm (1.5 to 100 mg/m 3) for a 10-L air sample. This method is applicable to 15-minute ceiling measurements. NIOSH has sampled for acrylonitrile at acrylic and electric plants.

INTERFERENCES: None known. An alternate chromatographic column is a fused silica capillary, 30 m x 0.32-mm, coated with 0.5 µm DB-WAX or 1 µm DB-5.

OTHER METHODS: This revises NIOSH Method S156 [1,3] and Method 1604 (dated 2/15/84). P&CAM 202 has been dropped because of poor sensitivity (LOD 0.1 mg per sample) [4]. Marano et al. [5] have shown that the use of a nitrogen selecti ve detector (NPD) increases the sensitivity and specificity of the analysis.

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