HEXACHLORO-1,3-CYCLOPENTADIENE: METHOD 2518, Issue 2, dated 15 August 1994 - Page 2 of 4 EQUIPMENT:
REAGENTS: 1.
2. 3. 4. 5. 6.
7.
8.
Porapak T (optional if commercial tubes are used), 80/100 mesh (Waters Associates, Inc.), cleaned as follows: a. Soxhlet extract 4 h with 80/20 acetone/methanol (v/v). b. Soxhlet extract 4 h with hexane. c. Dry in vacuo 12 h at 50 to 75 °C. Hexane, spectral quality.* Hexachloro-1,3-cyclopentadiene, 98% or purer. Acetone, spectral quality.* Methanol, spectral quality.* Stock solution, 20 mg/mL. Dissolve 2.00 g hexachloro-1,3-cyclopentadiene in hexane to make 100 mL solution. Store at 0 °C, protect from light and discard after 60 days. Calibration stock solution, 10 µg/mL. Dilute 50 µL stock solution with hexane to make 100 mL solution. Store at 0 °C, protect from light and discard after 14 days. Mixture of 5% methane and 95% argon.
See SPECIAL PRECAUTIONS.
SPECIAL PRECAUTIONS: Hexane, acetone and methanol are flammable. Hexachloro-1,3-cyclopentadiene is highly toxic and can be absorbed through the skin. Wear gloves, avoid inhalation of vapors and protect solvents from sparks and flames.
SAMPLING: 1. 2. 3.
4.
1. Sampler: two glass tubes connected in series with 1.8-cm piece of plastic tubing; each tube, 5 cm long, 6-mm OD, 4-mm ID, contains one section of 80/100 mesh Porapak T held in place with two plugs of silylated glass wool (front tube = 75 mg; back tube = 25 mg) with plastic caps. Pressure drop <2.3 kPa (<17 mm Hg) at flow rate of 0.2 L/min. Samplers are commercially available. 2. Personal sampling pump, 0.01 to 0.2 L/min, with flexible connecting tubing. 3. PTFE tape. 4. Gas chromatograph, 63Ni ECD, integrator and column (page 2518-1). 5. Volumetric flasks, 10- and 100-mL. 6. Vials, 1-mL, with PTFE-lined caps. 7. Syringes, 10-µL, readable to 0.1 µL. 8. Syringes, 100-µL, readable to 1 µL. 9. Syringes, 1-mL, readable to 10 µL. 10. Pipet, 1-mL. 11. Ultrasonic bath.
Calibrate each personal sampling pump with a representative sampler in line. Attach sampler to personal sampling pump with flexible tubing. Sample at an accurately known flow rate between 0.01 and 0.2 L/min for a total sample size of 0.25 to 90 L. Do not sample for longer than 8 h. Separate the two tubes of the sampler. Cap the ends of each tube with PTFE tape and plastic caps. Pack securely for shipment.
SAMPLE PREPARATION:
5. 6. 7.
NOTE: If the tubes have been refrigerated, allow the tubes to stand at room temperature before removal of the caps and tape to prevent condensation of water on the sorbent. Place the front and back sorbent sections with their respective glass wool plugs, in separate vials. Add 1.0 mL hexane to each vial. Attach cap to each vial. Allow to stand 60 min in an ultrasonic bath.
CALIBRATION AND QUALITY CONTROL: 8.
Calibrate daily with at least six working standards over the range 5 to 140 ng hexachloro-1,3-cyclopentadiene per sample.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
