Page:NIOSH Manual of Analytical Methods - 2551.pdf/2

 NICOTINE: METHOD 2551, Issue 1, dated 15 January 1998 - Page 2 of 4 REAGENTS:

EQUIPMENT:

1. Ethyl acetate, chromatographic grade.* 2. Triethylamine, reagent grade.* 3. Desorbing solution (modified ethyl acetate solution). 0.01% triethylamine in ethyl acetate. 4. Nicotine* primary stock solution (1.0 mg/mL). Dilute 100 mg nicotine to 100 mL with desorbing solution. 5. Nicotine* secondary stock solution (10 µg/mL). Dilute 1.0 mL nicotine primary stock solution to 100 mL with desorbing solution. 6. Quinoline* (Internal standard) primary stock solution (1.0 mg/mL). Dilute 100 mg quinoline to 100 mL with desorbing solution. 7. Quinoline* secondary stock solution (100 µg/mL). Dilute 10.0 mL quinoline primary stock solution to 100 mL with desorbing solution. 8. Helium, purified. 9. Hydrogen, prepurified. 10. Air, filtered.

1. Sampler: Glass tube, 70 mm, 7-mm OD, containing two sections of XAD-4 (front = 80 mg, back = 40 mg)separated by a silylated glass wool. A silylated glass wool plug precedes the front section and follows the back section. (Glass wool plugs must be specified when ordering XAD-4 tubes.) Tubes are commercially available (SKC, Inc., Cat. No. 226-93, or equivalent). 2. Personal sampling pump, 0.1 to 1.0 L/min, with flexible connecting tubing. 3. Gas chromatograph, nitrogen-phosphorous detector, integrator, and Rtx-5® capillary column or equivalent (page 2551-1). 4. Ultrasonic bath. 5. Vials, autosampler, with PTFE-lined caps. 6. Microliter syringes, 10-µL and other sizes as needed, readable to 0.1 µL. 7. Flasks, volumetric, various sizes. 8. Pipets, various sizes. 9. Refrigerant packs.

SPECIAL PRECAUTIONS: Nicotine is classified as a neurotoxin and possible teratogen [6]. Avoid inhalation, skin contact, and ingestion. Quinoline is classifiedas moderately toxic, a severe eye irritant, and possible carcinogen [6]. Avoid skin contact (readily adsorbed), inhalation, and ingestion. Ethyl acetate is flammable and a fire hazard. Triethylamine is an eye, skin, and respiratory irritant. Wear appropriate protective clothing and work with these compounds in a well ventilated hood.
 * See SPECIAL PRECAUTIONS

SAMPLING: 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Break ends of tubes immediately before sampling. Attach tubes to personal sampling pump with flexible tubing. 3. Sample at an accurately known flow rate between 0.1 and 1.0 L/min for a total sample size of 0.5 to 600 L. 4. Cap the tubes with plastic caps and pack securely for shipment. Protect from exposure to light. Ship with refrigerant packs to keep samples cold. SAMPLE PREPARATION: 5. Place front (include glass wool plug) and back sorbent sections of the sampler in separate vials. Discard middle and back glass wool plugs. 6. Add 1 mL of desorbing solution (modified ethyl acetate) to each vial. 7. Add aliquots (10 to 50 µL) of the quinoline secondary stock internal standard solution to both the calibration standards and sample vials and attach PTFE-lined crimp caps. NOTE: Determine the approximate level of nicotine that will be in the samples and add a similar amount of quinoline. Environmental tobacco smoke usually has low nicotine levels. Pesticide operations usually have relatively high levels. 8. Place vials in an ultrasonic bath for 30 min to aid desorption. CALIBRATION AND QUALITY CONTROL: NIOSH Manual of Analytical Methods (NMAM), Fourth Edition