Page:NIOSH Manual of Analytical Methods - 3508.pdf/1

 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