National Institute for Occupational Safety and Health

“ Use of an internal standard is recommended to minimize errors caused by sample solvent evaporation and FPD response variations. c. Prepare a calibration graph of area vs. μg of tributyl phosphate per 10 mL of sample. Determine recovery in the concentration range of interest for each lot of filters used for sampling. Prepare three filters at each of five levels plus three media blanks. a. Spike aliquot of calibration solution onto each filter. b. After air-drying, extract filters with 10 mL diethyl ether (steps 5 through 7) . c. Analyze together with working standards (steps 11 and 12) . ”

“ Do not leave container open. Diethyl ether can oxidize in air to form explosive peroxides, a reaction accelerated by light. Distillation and evaporation can concentrate unstable peroxides in the residue, a potentially explosive condition [10] . Avoid inhalation of tributyl phosphate vapors and contact with eyes, skin, and clothing [11,12] . Handle only in a hood.
SAMPLING: 1. 2.
3. 4.
Calibrate each personal sampling pump with the representative filter cassettes in line. Remove cassette plugs and connect cassette filter to the personal sampling pump with flexible tubing. ”

“ Any phosphorus-containing compound that has the same retention time as the analyte is an interference. A non-polar capillary column may be used for better resolution.
NIOSH Manual of Analytical Methods (NMAM) , Fourth Edition, 8/15/94 OTHER METHODS: This revises Method S208 [2] . Analytical methods for tributyl phosphate (TBP) have been reviewed [3] . ”