Page:NIOSH Manual of Analytical Methods - 1617.pdf/2

 PHENYL ETHER: METHOD 1617, Issue 1, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1. 2. 3. 4. 5. 6. 7.

EQUIPMENT:

Phenyl ether *, ACS reagent grade. Carbon disulfide *, ACS reagent grade. Hexane, distilled in glass. Calibration stock solution, 17.3 mg/mL, of phenyl ether in hexane. Prepurified nitrogen. Prepurified hydrogen. Filtered compressed air.



See SPECIAL PRECAUTIONS.

1. Sampler: glass tubes, 7 cm long, 6-mm OD, 4-mm ID, flame-sealed ends with plastic caps, containing two sections of activated (600 °C) coconut shell charcoal (front = 100 mg, back = 50 mg)separated by a 2-mm urethane foam plug. A silylated glass wool plug precedes the front section and a 3-mm urethane foam plug follows the back section. Pressure drop across the tube a 1 L/min airflow must be less than 4.3 kPa. Tubes are commercially available. 2. Personal sampling pump, 0.01 to 0.2 L/min, with flexible polyethylene or PTFE tubing. 3. PTFE plugs and/or tubing. 4. Vials, glass, 1-mL with PTFE-lined caps. 5. Gas chromatograph with a flame ionization detector, recorder, integrator and column (page 1617-1). 6. Tweezers. 7. Syringes, 5-, 10- and 100-µL; other sizes as needed. 8. Volumetric flasks, 10- and 25-mL. 9. Pipets, 0.5-, 1-, and 10-mL glass, delivery, with pipet bulb, graduated to 0.1-mL increments. 10. Graduated cylinders, glass, 25-mL. 11. File.

SPECIAL PRECAUTIONS: Phenyl ether is toxic by inhalation. All work with carbon disulfide should be performed in a hood because of its high toxicity and flammability (flash point = -30 °C).

SAMPLING: 1. 2.

3. 4. 5. 6.

Calibrate each personal sampling pump with a representative sampler in line. Immediately before sampling, break the ends of the tube to provide an opening at least one-half the internal diameter of the tube (2 mm). Attach sampler to personal sampling pump with flexible tubing. Sample 1 to 50 L of air at an accurately known flow rate between 0.01 and 0.2 L/min. Record the humidity temperature, and pressure of the atmosphere being sampled, if pressure reading is not available, record the elevation. Cap each tube with plastic plugs and pack securely for shipment. Collect a bulk sample (ca. 1 g) in a glass vial and ship it separately.

SAMPLE PREPARATION: 7. 8. 9.

Place front and back sections of the sampler in separate 1-mL vials. Discard the glass wool and foam plugs. Add 0.5 mL carbon disulfide to each sample vial and attach the crimp cap. Allow to stand 30 min with occasional agitation. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94