Page:NIOSH Manual of Analytical Methods - 1619.pdf/2

 PHENYL GLYCIDYL ETHER: METHOD 1619, Issue 1, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1. 2. 3. 4. 5.

EQUIPMENT:

Carbon disulfide* (CS 2), chromatographic quality. Phenyl glycidyl ether*, reagent grade. Nitrogen, purified. Hydrogen, purified. Air, compressed, filtered.



See SPECIAL PRECAUTIONS.

1. Sampler: borosilicate tubes, 7.0 cm long, 6mm 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 1 L/min, with flexible connecting tubing. 3. Gas chromatograph, FID, integrator, and column (page 1619-1). 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, with bulb.

SPECIAL PRECAUTIONS: Both phenyl glycidyl ether and CS 2 are toxic [3]. In addition, CS 2 is a serious fire and explosion hazard (flash point = -30 °C). All work with these compounds must be done in a hood.

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 1 L/min for a total sample size of 80 to 150 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 0.5 mL CS 2 to each vial. Cap each vial. 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 0.01 to 6 mg phenyl glycidyl ether per sample. a. Add a known amount of phenyl glycidyl ether to CS 2 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). NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94