National Institute for Occupational Safety and Health

“ Calibrate daily with at least six working standards over the range 2 to 20 μg antimony per sample. a. Add known amounts of antimony stock solution and conc. HCl to cover the antimony concentration of 2 to 20 μg Sb per 15 mL and a reagent blank. b. Proceed as in steps 10 through 15 and 18 and 19. c. Prepare a calibration graph (absorbance vs. μg antimony/15 mL) . Analyze three quality control spikes to ensure that the calibration graph is in control. ”

“ Attach sampler to personal sampling pump with flexible tubing. NOTE: Use a cellulose ester membrane prefilter if particulate antimony compounds may be present. Sample at an accurately known flow rate between 0.01 and 0.2 L/min for a total sample size of 4 to 50 L. Cap the sampler and pack securely for shipment.
SAMPLE PREPARATION: 5. 6. 7. 8. 9. 10.
Place front and back sorbent sections of the sampler tube in separate 50-mL beakers. Discard the glass wool. Add 15.0 mL conc. HCl to each beaker. Mildly agitate (swirl) the beaker contents every 10 min for a total desorption time of 30 min. ”

“ Pressure drop across the tube at 1 L/min airflow must be less than 3.4 kPa. Tubes are commercially available. 2. Personal sampling pump, 0.01 to 0.2 L/min, with flexible connecting tubing. 3. Visible spectrophotometer capable of measuring absorbance at 552 nm, with two matched 1-cm silica absorbance cells with tight-fitting PTFE caps.* 4. Separatory funnels, 125-mL.* 5. Beakers, Griffin, 50-mL. 6. Volumetric flasks, 25-, 50-, 250-, and 500-mL. 7. Pipets, 4-, 15-, and 20-mL.* 8. Graduated cylinders, 10- and 25-mL.* 9. ”