Page:NIOSH Manual of Analytical Methods - 2545.pdf/2
ALLYL GLYCIDYL ETHER: METHOD 2545, Issue 1, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1. 2.
3. 4. 5. 6.
EQUIPMENT:
Allyl glycidyl ether*, reagent grade. Diethyl ether*, anhydrous, containing approximately 0.1 mg/mL isoamyl alcohol or other suitable internal standard. Hexane. Nitrogen, purified. Hydrogen, prepurified. Air, compressed, filtered.
See SPECIAL PRECAUTIONS.
1. Sampler: borosilicate tubes, 10 cm long, 8-mm OD, 6-mm ID; flame-sealed ends with plastic caps, containing two sections of 35/60 mesh Tenax GC (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 2545-1). 4. Vials, 5-mL, with PTFE-lined crimp caps. 5. Microliter syringes, 10-µL and convenient sizes for making dilutions. 6. Flasks, volumetric, 10-mL. 7. Pipets, 2-mL.
SPECIAL PRECAUTIONS: Allyl glycidyl ether is flammable (flash point = 57 °C) and a moderate skin and severe eye irritant [3]. Diethyl ether is a serious fire and explosion hazard (flash point = -45 °C) and may form explosive peroxides during storage. 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 0.02 and 0.2 L/min for a total sample size of 1.5 to 8 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 2.0 mL diethyl ether 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 10 to 800 µg allyl glycidyl ether per sample. a. Add a known amount of allyl glycidyl ether to diethyl ether in 10-mL volumetric flask and dilute to the mark. Use serial dilutions as needed for smaller concentrations.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94