POLYNUCLEAR AROMATIC HYDROCARBONS by HPLC: METHOD 5506, Issue 3, dated 15 January 1998 - Page 2 of 9
REAGENTS:
EQUIPMENT:
1. Water, distilled, deionized, degassed. 2. Acetonitrile, HPLC grade, degassed. 3. PAH test mixture,* a liquid standard containing the PAHs except benzo[e]pyrene (EPA 610 Polynuclear Aromatic Hydrocarbons,Supelco, Cat. No. 4-8743; or equivalent). 4. Benzo[e]pyrene,* solid (Supelco, Cat. No. 442475; or equivalent).
1. Sampler: a. Filter. 37-mm, 2-µm pore size, PTFE membrane filter laminated to PTFE, (Zefluor, Pall Gelman Sciences, Cat. No. P5PJ037; SKC Inc., Cat. No. 225-17-07; or equivalent filter), cellulose spacer ring, 37-mm OD, 32-mm ID, (SKC Inc., Cat. No. 225-23; or equivalent) in a 37-mm cassette filter holder. NOTE: If sampling is to be done in bright sunlight, use opaque or foil-wrapped cassettes to prevent sample degradation. b. Sorbent tube, washed XAD-2 resin (front = 100 mg; back = 50 mg) (ORBO 43, Supelco, Cat. No. 2-0258; or equivalent), connected to filter with minimum length of PVC tubing. Plastic caps are required after sampling. NOTE: If pressure drop is excessive or pump fails, use a larger diameter sorbent tube with XAD-2 resin (ORBO 42 Large, Supelco, Cat. No. 2-0264U; or equivalent). 2. Personal sampling pump capable of operating for 8 h at 2 L/min, with flexible connecting tubing. 3. Aluminum foil. 4. Refrigerant, bagged. 5. Culture tubes, PTFE-lined screw cap, 13-mm x 100-mm. 6. Forceps. 7. Syringe filters, 0.45-µm, 25-mm, PTFE (Acrodisc-CR, Pall Gelman Sciences, Cat. No. 4219; or equivalent). 8. Pipet, 5-mL. 9. Syringe or micropipets, 1- to 100-µL. 10. Ultrasonic bath. 11. HPLC, with gradient capability, fluorescence (excitation @ 340 nm, emission @ 425 nm) and UV (254 nm) detectors in series, electronic integrator, and a 250 x 4.6-mm C 18 column (Vydac 201TP, The Separations Group, Hesperia, CA, Cat. No. 201TP54; or equivalent). 12. Volumetric flasks, 10- and 100-mL. 13. Recommendation: lighting in laboratory should be incandescent or UV-shielded fluorescent.
- See SPECIAL PRECAUTIONS
SPECIAL PRECAUTIONS: Treat all polynuclear aromatic hydrocarbons as carcinogens. Samples and unused standards are considered toxic waste. Dispose of in an appropriate manner. Counter tops and equipment should be checked regularly with a "black light" for fluorescence as an indicator of contamination by PAHs.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
