PHENYL ETHER-DIPHENYL MIXTURE: METHOD 2013, Issue 1, dated 15 August 1994 - Page 2 of 3 REAGENTS: 1. 2. 3.
4. 5. 6. 7. 8. 9.
EQUIPMENT:
Diphenyl *, reagent grade. Phenyl ether *, reagent grade. Phenyl ether-biphenyl mixture: dissolve 2.65 g solid diphenyl in 7.35 g melted phenyl ether (10 g mixture, liquid eutectic). Benzene *, reagent grade. Hexane, reagent grade. Calibration stock solution, analyte mixture in hexane, 17.5 mg/mL. Hydrogen, prepurified. Air filtered, compressed. Nitrogen, purified.
See Special Precautions
1. Sampler: glass tube, 7 cm long, 6-mm OD, 4mm ID; with plastic caps; containing two sections of 20/40 mesh silica gel separated by a 2-mm portion of urethane foam (front = 150 mg; back = 75 mg). A silylated glass wool plug proceeds the front section and a 3-mm urethane foam plug follows the back section. Pressure drop across the tube at 1 L/min airflow must be less than 3.4 kPa. Tubes are commercially available. 2. Personal sampling pump, 0.01 to 0.20 L/min, with flexible polyethylene or PTFE tubing. 3. PTFE plugs and/or tubing. 4. Vials, glass, 1-mL with PTFE-lined crimp caps. 5. Gas chromatograph, flame ionization detector, recorder, integrator and column (page 2013-1). 6. Tweezers. 7. File. 8. Syringes, 5-, 50- and 100-µL, other sizes if needed. 9. Volumetric flasks, 10-mL. 10. Pipets, 0.5-, and 1.0-mL glass, delivery, graduated in 0.1-mL increments, with pipet bulb. 11. Graduated cylinders, glass, 10-mL.
SPECIAL PRECAUTIONS: Benzene is a carcinogen, toxic and is flammable. Phenyl ether is toxic by inhalation. Diphenyl is toxic. Work in a fume hood.
SAMPLING: 1. 2.
3. 4. 5.
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 at an accurately known flow rate between 0.01 and 0.2 L/min for a total sample volume of 1 to 40 L. After the sample is collected, 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: 6. 7. 8.
Place front and back sorbent sections of the sampler tube in separate vials. Discard the glass wood and foam plugs. Add 0.5 mL benzene to each sample vial and attach the crimp cap. Allow to stand for 30 min with occasional agitation.
CALIBRATION AND QUALITY CONTROL: 9.
Calibrate daily with at least six working standards. a. Add known amounts of calibration stock solution to 0.5 mL benzene. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
