Page:NIOSH Manual of Analytical Methods - 2513.pdf/2

 ETHYLENE CHLOROHYDRIN: METHOD 2513, Issue 2, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1.

2. 3. 4. 5. 6.

EQUIPMENT:

Eluent: carbon disulfide,* (chromatographic grade), containing 5% (v/v) 2-propanol (reagent grade) and 0.1% (v/v) n-pentadecane as internal standard. Ethylene chlorohydrin (reagent grade).* Calibration stock solution, 50 mg/mL. Nitrogen, purified. Hydrogen, prepurified. Air, filtered.



See SPECIAL PRECAUTIONS.

1. Sampler: glass tube, 7 cm long, 6-mm OD, 4mm ID, flame-sealed ends with plastic caps, containing two sections of petroleum-derived activated 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 at 0.2 L/min airflow must be less than 3.4 kPa. Tubes are commercially available. 2. Personal sampling pump, 0.01 to 0.2 L/min, with flexible connecting tubing. 3. Gas chromatograph, flame ionization detector, integrator and column (page 2513-1). 4. Vials, 2-mL, PTFE-lined caps. 5. Syringes, 10-µL, readable to 0.1 µL, and 100-µL, readable to 1 µL. 6. Volumetric flasks, 10-mL. 7. Pipet, 1-mL.

SPECIAL PRECAUTIONS: Carbon disulfide is toxic and extremely flammable (flash point = -30 °C); work with it only in a hood. Ethylene chlorohydrin is highly toxic, has poor warning properties, and as a liquid, is readily absorbed through the skin and penetrates rubber [3]. Toxic effects may be cumulative. Wash liquid from skin immediately if contacted. SAMPLING: 1. 2. 3. 4.

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 2 to 35 L. Cap the samplers. Pack securely for shipment.

SAMPLE PREPARATION: 5. 6. 7.

Place the front and back sorbent sections of the sampler tube in separate vials. Discard the glass wool and foam plugs. Add 1.0 mL eluent to each vial. Attach cap to each vial. Allow to stand 30 min with occasional agitation.

CALIBRATION AND QUALITY CONTROL: 8.

Calibrate daily with at least six working standards covering the range 3 to 1000 µg ethylene chlorohydrin per sample. a. Add known amounts of calibration stock solution to eluent in 10-mL volumetric flasks and dilute to the mark. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94