National Institute for Occupational Safety and Health

Summary

National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

Set spectrophotometer according to manufacturer's instructions. Set zero with dimethyl phthalate vs. air. Read sample absorbance at 565 nm vs. air when a stable value is obtained. NOTE: See SPECIAL PRECAUTIONS for procedure for disposal of waste MEKP solutions.
CALCULATIONS: 14. 15.
Determine the mass, μg, of MEKP in the 5-mL aliquot of sample, W, and the average media blank, B, from the calibration graph. Calculate the concentration, C, of MEKP in the air volume sampled, V (L) :
NOTE: Correct for the average media blank, B, only if it exceeds twice the reagent blank (y-intercept) .
Source: Wikisource

National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

Dilute to the mark with DMP. These working standards contain ca. 5, 10, 25, and 50 mg MEKP/mL (25, 50, 125, and 250 μg MEKP per 5-mL aliquot) . b. Process the working standards together with samples, field blanks, media blanks, and reagent blanks (steps 7 through 10 and 12 and 13) during the same time period using the same batch of reagents. c. Prepare calibration graph (absorbance vs. μg MEKP) . Extrapolate to zero concentration (y-intercept) . Any sample whose absorbance is less than twice the "blank" should be reported as less than that level (about 25 μg MEKP per 5-mL aliquot) .
Source: Wikisource

National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

Dilute to 100 mL. NOTE: This solution is light-sensitive. Prepare immediately before using. 9. Color reagent. Mix 30 mL 0.25% DPC solution with 20 mL glacial acetic acid. 10. Methyl ethyl ketone peroxide (MEKP) , 60%, technical grade, in dimethyl phthalate. Standardize as in APPENDIX. 11. Calibration stock solution.* Pipet ca. 10 μL of 60% MEKP into a 50-mL pre-weighed volumetric flask. Accurately weigh the flask plus MEKP; dilute to the mark with dimethyl phthalate. Wrap flask in Al foil. Prepare in duplicate. 12. Sodium thiosulfate solution, 0.1 N, standardized.
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