METHYL ETHYL KETONE PEROXIDE
C8H16 O4
MW: 176.21
METHOD: 3508, Issue 2
CAS: 1338-23-4
RTECS: EL9450000; 21837
EVALUATION: PARTIAL
OSHA : no PEL NIOSH: C 0.2 ppm/15 min ACGIH: C 0.2 ppm (1 ppm = 7.2 mg/m 3 @ NTP)
3508
PROPERTIES:
Issue 1: 15 August 1987 Issue 2: 15 August 1994
liquid; d 1.170 g/mL @ 20 °C; flash point (open cup) 82 °C
SYNONYMS: MEKP; MEK peroxide; 2-butanone peroxide
SAMPLING
MEASUREMENT
SAMPLER:
IMPINGER (15 mL dimethyl phthalate)
TECHNIQUE:
VISIBLE ABSORPTION SPECTROPHOTOMETRY
FLOW RATE:
0.5 to 2 L/min
ANALYTE:
diphenylcarbazide oxidation product
VOL-MIN: -MAX:
52 L @ 0.2 ppm 520 L
SAMPLE PREPARATION:
SHIPMENT:
transfer to silanized, foil-wrapped vials; ship in dry ice
SAMPLE STABILITY:
90% recovery after 21 days @ -4 °C [2]
BLANKS:
2 to 10 field blanks per set
ACCURACY RANGE STUDIED:
not studied for generated samples
BIAS:
not determined
OVERALL ˆ ): PRECISION (S rT
not determined
ACCCURACY:
not determined
note liquid volume; remove 5 mL aliquot; add 5 mL diphenylcarbazide color reagent; heat at 85 ± 5 °C for 15 min; cool in room temperature water bath exactly 5 min
ANALYSIS:
color development; absorbance @ 565 nm
CALIBRATION:
standard solutions of methyl ethyl ketone peroxide in dimethyl phthalate
RANGE:
75 to 750 µg per sample [1]
ESTIMATED LOD: 75 µg per sample [1] PRECISION (Sr):
0.052 [2]
APPLICABILITY: The working range is 0.11 to 1.1 ppm (0.75 to 7.5 mg/m 3) for a 100-L air sample [1]. This method has not been tested with aerosol generation or field samples. Special care must be taken in the conditioning of the glassware and in the storage of the samples.
INTERFERENCES: The diphenylcarbazide color reaction is relatively non-specific. Most ketones, except acetone, will exhibit positive interference at high levels. Other peroxides or any strong oxidant could also interfere with this procedure. Su bstances which catalyze the decomposition of peroxide may cause a significant decrease in the measurement; in particular, the pre sence of metal ions adsorbed on the glassware.
OTHER METHODS: This revises P&CAM 331 [1].
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94