National Institute for Occupational Safety and Health

“ Concentrate the sample to 2.0 mL in a graduated centrifuge tube.
CALIBRATION AND QUALITY CONTROL: 22. 23. 24. 25.
Prepare at least six working standards in the range 5 to 1000 μg/L PCP by dilution of the calibration stock solution with hexane. Prepare a calibration graph (peak area of analyte vs. μg/L PCP) . Maintain standardization by injecting a working standard after each five sample injections. Run a spiked urine every ten samples or if less than ten determinations are required, run at least three spiked urines per run or study. ”

“ Freeze the samples and pack them in an insulated shipper (e.g., styrofoam with dry ice) .
SAMPLE PREPARATION: 4. 5. 6. 7. 8. 9. 10. 11.
Perform a creatinine determination on an aliquot of the urine (e.g., [5] ) . Transfer a 4-mL aliquot of each urine sample to a 16 x 150-mm culture tube. Add 1.0 mL conc. HCl and 100 mg sodium bisulfite to each culture tube. Cap and place the culture tubes in a boiling waterbath for 1 h. Shake gently at 15-min intervals. Cool the culture tubes to room temperature. Add 5 mL benzene to each culture tube. Extract on a rotary mixer at 60 rpm for 1 h. ”

“ NIOSH Manual of Analytical Methods (NMAM) , Fourth Edition, 8/15/94 PENTACHLOROPHENOL in urine: METHOD 8303, Issue 2, dated 15 August 1994 - Page 2 of 4 REAGENTS:
EQUIPMENT:
1. Hexane, acetone, and benzene* (pesticide grade) . 2. 20% benzene in hexane (v/v) . 3. 10% benzene in hexane (v/v) . 4. Hydrochloric acid (conc.) . 5. Sodium bisulfite. 6. Sodium sulfate. 7. Alumina (acid-washed) , Brockman Activity I, 80/200 mesh. 8. Pentachloroanisole (available from EPA Analytical Reference Lab) . 9. Calibration stock solution equivalent to 100 mg/L PCP. Weigh 0.0105 g pentachloroanisole ”