Page:NIOSH Manual of Analytical Methods - 5515.pdf/2

 POLYNUCLEAR AROMATIC HYDROCARBONS by GC: METHOD 5515, Issue 2, dated 15 August 1994 - Page 2 of 7

REAGENTS: 1.

2. 3. 4. 5.

6. 7. 8.

EQUIPMENT:

Filter extraction solvent: acetonitrile, benzene,* cyclohexane, methylene chloride,* or other appropriate solvents, pesticide grade (step 7). Toluene, pesticide grade. Water, distilled, deionized. PAH reference standards,* appropriate to the PAH-containing matrix sampled. Calibration stock solution, 0.25 mg/mL.* Check purity of each PAH reference standard by GC/FID, HPLC/fluorescence and/or melting point. Purify, if necessary, by recrystallization. Weigh 25 mg of each PAH into a 100-mL volumetric flask; dilute to volume with toluene. Stable six months if refrigerated and protected from light. Helium, prepurified. Hydrogen, dry. Air, filtered.



See SPECIAL PRECAUTIONS.

1. Sampler: a. Filter. PTFE-laminated membrane filter, 2-µm pore size, 37-mm diameter (Gelman Zefluor, Membrana, Pleasantown, CA, or equivalent), backed by a spacer (37-mm OD, 32-mm ID) cut from a cellulose support pad or SKC #225-23, in cassette filter holder. NOTE 1: If sampling is to be done in bright sunlight, use opaque or foil-wrapped cassettes to prevent sample degradation. NOTE 2: Take filters to be preweighed from the filter package and allow to equilibrate 24 h with laboratory atmosphere before taring. b. Sorbent tube, connected to filter with minimum length PVC tubing. Plastic caps are required after sampling. Washed XAD-2 resin (front = 100 mg; back = 50 mg) (Supelco ORBO 43 or equivalent). Pressure drop at 2 L/min airflow 1.6 to 2 kPa (15 to 20 cm H 2O). 2. Personal sampling pump capable of operating for 8 h at 2 L/min, with flexible connecting tubing. 3. Aluminum foil. 4. Vial, scintillation, 20-mL, glass, PTFE-lined cap. 5. Refrigerant, bagged. 6. Culture tubes, PTFE-lined screw cap, 13-mm x 100-mm. 7. Forceps. 8. Filters, 0.45-µm, PTFE (for filtering sample solutions). 9. Pipet, 5-mL. 10. Syringes or micropipets, 1- to 100-µL. 11. Ultrasonic bath. 12. Gas chromatograph with FID, electronic integrator, and capillary column (page 5515-1). 13. Volumetric flasks, 10- and 100-mL. 14. Lighting in laboratory: incandescent or UVshielded fluorescent.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94