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PENTACHLOROETHANE: METHOD 2517, Issue 2, dated 15 August 1994 - Page 2 of 4
REAGENTS:
- Hexane, distilled in glass.*
- Pentachloroethane, 96% pure.*
- Mixture of 5% methane, 95% argon.
- Calibration stock solution, 2 mg/mL. Dissolve 0.2 g pentachloroethane in hexane to make 100 mL solution. Stable indefinitely at room temperature.
*See SPECIAL PRECAUTIONS.
EQUIPMENT:
- Sampler: borosilicate tubes, 7 cm long, 6-mm OD, 4-mm ID, flame-sealed ends with plastic caps, containing two sections of 50/80 mesh Porapak R (front = 70 mg; back = 35 mg) separated by a urethane foam plug. A glass wool plug held in place with a metal spring precedes the front section and a urethane foam plug follows the back section. Pressure drop across the tube at 0.2 L/min airflow must be less than 1.2 kPa (5 inches H2O). Tubes are commercially available, e.g., SKC, Inc. ST226-59-04.
- Personal sampling pump, 0.01 to 0.2 L/min, with flexible connecting tubing.
- Gas chromatograph, 63Ni ECD, integrator, and column (page 2517-1).
- Vials, 2-mL, with PTFE-lined crimp caps.
- Microliter syringes, 10-µL and convenient sizes for making dilutions.
- Ultrasonic bath.
- Pipets, 2-mL.
- Volumetric flasks, 10-mL.
SPECIAL PRECAUTIONS:
Hexane is flammable (flash point = -21 °C) and toxic; all work with it must be done in a hood.
Pentachlorothenae causes CNS effects, with possible liver and kidney effects [3]. Technical grade pentachloroethane (containing 4.2% hexachloroethane, a known carcinogen in mice) was carcinogenic for B6C3F1 mice, causing hepatocellular carcinomas in males and females, and adenomas in females [4].
SAMPLING:
- Calibrate each personal sampling pump with a representative sampler in line.
- Break the ends of the sampler immediately before sampling. 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 1 to 10 L.
- Cap the samplers with PTFE tape and plastic caps. Pack securely for shipment.
SAMPLE PREPARATION:
- Refrigerate the samples upon receipt.
- Place the front and back sorbent sections of the sampler tube in separate vials. Add the glass wool plug to the front sorbent section and the foam plugs to the back sorbent section.
- Add 2.0 mL hexane to each vial. Attach crimp cap to each vial.
- Allow to stand 30 min in an ultrasonic bath.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
