Page:NIOSH Manual of Analytical Methods - 5510.pdf/2

 CHLORDANE: METHOD 5510, Issue 2, dated 15 August 1994 - Page 2 of 4 REAGENTS:

EQUIPMENT:

1. 2. 3. 4.

Toluene, distilled in glass. Hexane, distilled in glass. Chlordane, 95%.* Calibration stock solution, ca. 6 mg/mL. Dissolve 10 mg Chlordane in 1 mL toluene. NOTE: Since Chlordane is available only as a mixture, standardize the solution as follows: a. Dilute 10 µL calibration stock solution to 10 mL. b. Analyze by steps 11-13. c. Divide combined area of Chlordane peaks (Fig. 1) by total area of all peaks to determine fraction Chlordane, f. 5. Internal standard, p,p'-DDT, 98%.* 6. 95% Argon/5% methane mixture, purified.



See SPECIAL PRECAUTIONS.

1. Sampler: 37-mm, 0.8-µm pore size cellulose ester membrane filter supported by a stainless steel screen in a two-piece filter cassette holder plus a 10 cm x 8-mm OD x 6-mm ID, 20/40 Chromosorb 102 tube (front = 100 mg; back = 50 mg), separated by 3-mm silanized glass wool plug, flame sealed ends with plastic caps. Pressure drop across the tube at 1 L/min must not exceed 2.5 mm Hg. Filters and tubes are commercially available. 2. Personal sampling pump, 0.5 to 1 L/min, with flexible connecting tubing. 3. Gas chromatograph, electron capture detector, integrator and column (page 5510-1). 4. Vials, scintillation, 20-mL, PTFE-lined caps. 5. Syringe, 10-µL, readable to 0.1 µL. 6. Flasks, volumetric 10-mL. 7. Bottles, 60 mL, 40-mm ID, straight-sided with a PTFE-lined cap for extracting filter holder and screen. 8. Stopwatch. 9. Manometer. 10. Pipets, 1- and 10-mL an other convenient sizes for preparing standards. 11. Tweezers.

SPECIAL PRECAUTIONS: Chlordane and p,p'DDT are toxic and rapidly absorbed through the skin [4]. Use gloves and eyeglasses to avoid direct contact with these compounds. Handle these chemicals and organic solvents with care in the laboratory hood. Chlordane is a potential human carcinogen [5].

SAMPLING: 1.

Calibrate each personal sampling pump with a representative sampler in line. 2. Assemble the sampler and connect the sorbent tube (ends broken just before the connection) to the sampling pump with backup section nearest the sampling pump. Keep the sampler in a vertical position during sampling. 3. Sample at an accurately known flow rate between 0.5 and 1 L/min for a total sample size of 10 to 200 L. 4. Remove the sorbent tube from the outlet of the cassette and connect it to the inlet side of the cassette. Cap the open end of the sorbent tube and plug the outlet of the cassette. Ship sampler with appropriate blanks to laboratory. 5. In separate package, ship bulk sample of the suspected material. SAMPLE PREPARATION: 6.

7.

Separate the sampler components for extraction as follows: a. Into a bottle, transfer the filter, front sorbent section and glass wool plugs. Add 10.0 mL toluene. After desorption is complete, dilute a 1-mL aliquot to 10 mL for analysis. b. Into a second bottle, transfer the stainless steel screen. Using a 10-mL volumetric pipet, rinse the inner surfaces of the cassette into the bottle with hexane. c. Into a scintillation vial, transfer the back sorbent section. Add 10.0 mL toluene. Cap each container and allow to stand 30 min. with occasional swirling. NOTE: A suitable internal standard such as p,p'-DDT may be added, at 0.4 µg/mL, at this point.

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