Page:NIOSH Manual of Analytical Methods - 3506.pdf/1
ACETIC ANHYDRIDE
(CH3CO)2O
MW: 102.09
METHOD: 3506, Issue 2
CAS: 108-24-7
EVALUATION: FULL
OSHA : 5 ppm NIOSH: C 5 ppm ACGIH: C 5 ppm (1 ppm = 4.17 mg/m 3 @ NTP)
3506
RTECS: AK1925000 Issue 1: 5 May 1985 Issue 2: 15 August 1994
PROPERTIES: liquid; d 1.080 g/mL @ 15 °C; BP 139 °C; MP -73 °C; VP 4 mm Hg @ 20 °C; explosive range 2.9 to 10.3% v/v in air
SYNONYMS: acetic acid anhydride; acetyl oxide
SAMPLING SAMPLER:
LIQUID IN BUBBLER (mixed bubbler with 10 mL alkaline hydroxylamine)
FLOW RATE:
0.2 to 1.0 L/min
VOL-MIN: -MAX:
25 L 100 L
SHIPMENT:
hand delivery or special bubbler cases
SAMPLE STABILITY:
≥ 4 days @ 25 °C [1]
BLANKS:
2 to 10 field blanks per set
ACCURACY RANGE STUDIED:
9.35 to 37.4 mg/m 3 [1] (100-L samples)
BIAS:
4.9%
MEASUREMENT TECHNIQUE:
VISIBLE ABSORPTION SPECTROPHOTOMETRY
ANALYTE:
acetic anhydride-hydroxylamine-ferric chloride complex
FINAL VOLUME:
50 mL
WAVELENGTH:
540 nm
CALIBRATION:
complexed acetic anhydride standards
RANGE:
0.5 to 4 mg acetic anhydride per sample [2]
ESTIMATED LOD:
0.05 mg acetic anhydride per sample
PRECISION (Sr):
0.021 @ 1 to 4 mg acetic anhydride per sample [1]
ˆ ): 0.060 [1] OVERALL PRECISION (S rT ACCURACY:
± 15.3%
APPLICABILITY: The working range is 1.2 to 10 ppm (5 to 40 mg/m 3) for a 100-L air sample. The upper limit of the range may be extended by diluting the sample with the collection medium prior to color development. The method is sensitive enough for short-term (>5 min) determinations if a 5-cm or longer cuvette is used.
INTERFERENCES: Any substance containing a hydrolyzable carbonyl group, such as esters, acid chlorides, and aldehydes, is an interference. The most likely interference to coexist with acetic anhydride in air is ketene [2,3].
OTHER METHODS: This revises Method S170 [2].
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94