n-BUTYL GLYCIDYL ETHER: METHOD 1616, Issue 1, dated 15 August 1994 - Page 2 of 3
REAGENTS:
EQUIPMENT:
1. Carbon disulfide* (CS2), chromatographic quality. 2. n-Butyl glycidyl ether*, reagent grade. 3. Nitrogen, purified. 4. Hydrogen, prepurified. 5. Air, compressed, filtered.
- See SPECIAL PRECAUTIONS.
1. Sampler: borosilicate tubes, 7.0 cm long, 6-mm OD, 4-mm ID; flame-sealed ends with plastic caps, containing two sections of 20/40 mesh activated (600 °C) coconut charcoal (front = 100 mg; back = 50 mg) separated by a urethane foam plug. A silanized 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 1.0 L/min air flow 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, FID, integrator, and column (page 1616-1). 4. Vials, 2-mL, with PTFE-lined crimp caps. 5. Microliter syringes, 10-µL and convenient sizes for making dilutions. 6. Flasks, volumetric, 10-mL. 7. Pipets, 0.5-mL.
SPECIAL PRECAUTIONS: Both n-butyl glycidyl ether and CS2 are toxic. In addition, CS2 is a serious fire and explosion hazard (flash point = −30 °C). All work with these compounds must be done in a hood. SAMPLING: 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Break the ends of the sampler immediately before sampling. Attach sampler to personal sampling pump with flexible tubing. 3. Sample at an accurately known flow rate between 0.01 and 0.2 L/min for a total sample size of 15 to 30 L. 4. Cap the samplers. Pack securely for shipment. SAMPLE PREPARATION: 5. Place the front and back sorbent sections of the sampler tube in separate vials. Discard the glass wool and foam plugs. 6. Add 0.5 mL CS2 to each vial. Cap each vial. 7. Allow to stand 30 min with occasional agitation. CALIBRATION AND QUALITY CONTROL: 8. Calibrate daily with at least six working standards over the range of 0.1 to 8 mg n-butyl glycidyl ether per sample. a. Add a known amount of n-butyl glycidyl ether to CS2 in 10-mL volumetric flask and dilute to the mark. Use serial dilutions as needed for smaller concentrations. b. Analyze with samples and blanks (steps 11 and 12). c. Prepare calibration graph (n-butyl glycidyl ether peak area vs. mg n-butyl glycidyl ether). 9. Determine desorption efficiency (DE) at least once for each lot of charcoal used for sampling in the NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
