NICOTINE: METHOD 2544, Issue 2, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1. 2. 3.
4. 5. 6.
EQUIPMENT:
Nicotine, reagent grade.* Ethyl acetate, chromatographic quality. Calibration solution, 5 mg/mL: Add 5 mg (5 µL) of nicotine to a 1.0 mL volumetric flask. Dilute to the mark with ethyl acetate. Nitrogen, purified. Hydrogen, pre-purified. Air, filtered.
See SPECIAL PRECAUTIONS.
1. Sampler: Glass tube, 7 cm long, 6-mm OD, 4-mm ID; two sections of 20/50 mesh preextracted XAD-2 (front = 100 mg, back = 50 mg separated by a plug of silylated glass wool and held in place with plugs of silylated glass wool, flame-sealed with plastic caps. The pressure drop across the tube should be 0.133 kPa at ≤1.0 L/min. Tubes are commercially available. 2. Personal sampling pump, 1.0 L/min with flexible connecting tubing. 3. Gas chromatograph, NPD, integrator, and column (p-2544-1). 4. Vials, glass, 2-mL, PTFE-lined crimp caps. 5. Syringes, 10-µL and 25-µL, readable to 0.1 µL. 6. Volumetric flasks, 1.0-mL. 7. Pipets, delivery-type, 1.0-mL. 8. File.
SPECIAL PRECAUTIONS: Nicotine is a SAMPLING: vasoconstrictor. Perform all work with these chemicals in a hood. 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Before sampling, score the ends of each sampling tube with a file, and break open. Attach the sampler to personal sampling pump with flexible tubing. 3. Sample at 1.0 L/min to obtain the recommended sample volume of 60 to 400 L. 4. Cap the tubes with plastic (not rubber) caps immediately following sampling and pack securely for shipment.
SAMPLE PREPARATION: 5.
6. 7.
Transfer the front (larger) section of XAD-2 with glass wool plug to a 2-mL vial. Transfer the backup sorbent section along with the separating section of glass wool to another vial. Discard the back glass wool plug. Pipet 1.0 mL of ethyl acetate into each vial. Seal the vials with a teflon-lined crimp-cap. Allow to stand 30 minutes with occasional agitation.
CALIBRATION AND QUALITY CONTROL: 8.
Calibrate daily with at least six working standards covering the analytical range 0.005 to 0.13 mg nicotine per sample. a. Add 1 to 25 µL or other convenient aliquots of the calibration solution to 1.0 mL of ethyl acetate in separate vials. Correct the volume of ethyl acetate in each vial to account for volume of the aliquot of calibration solution added. Seal the vials with septum-lined crimpcaps. b. Analyze the standards together with the samples (steps 11 through 13). c. Prepare a calibration graph of peak area vs. mg of analyte.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
