Page:NIOSH Manual of Analytical Methods - 2551.pdf/1
NICOTINE
C10H14N2
MW: 162.2
METHOD: 2551, Issue 1
OSHA : NIOSH: ACGIH:
CAS: 54-11-5
2551
RTECS: QS5250000
EVALUATION: PARTIAL
0.5 mg/m3 0.5 mg/m3, group I pesticide 0.5 mg/m3 (1 ppm = 6.74 mg/m3 @ NTP)
PROPERTIES:
Issue 1: 15 January 1998
liquid; d = 1.009 g/mL @ 20 C; BP = 245.5 C; VP = 0.08 mm Hg; FP = -29 C; range of explosive limits: 0.7 to 4.0% in air.
SYNONYMS: 3-(1-methyl-2-pyrrolidyl)-pyridine
SAMPLING SAMPLER:
SORBENT TUBE (XAD-4, 80/40 mg)
FLOW RATE:
0.1 to 1.0 L/min [1-3]
VOL-MIN: -MAX:
0.5 L 600 L
SHIPMENT:
MEASUREMENT TECHNIQUE:
GAS CHROMATOGRAPHY, NPD
ANALYTE:
nicotine
DESORPTION:
1 mL ethyl acetate with 0.01% triethylamine
INJECTION VOLUME:
Keep cold. Protect from prolonged exposure to light.
SAMPLE STABILITY :
14 days at 5 C in dark [4]
BLANKS:
2 to 10 field blanks per set
TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:
not determined.
BIAS:
not determined.
OVERALL PRECISION ( ACCURACY:
rT):
not determined. not determined.
200 C 300 C 60 to 200 C (20 C/min); hold @ 200 C for 3 min
CARRIER GAS:
helium, 2.4 mL/min
COLUMN:
capillary column, 30 m, x 0.32-mm ID, 1.0-µm film, crossbond® 5% diphenyl 95% dimethyl polysiloxane, Rtx-5® or equivalent
CALIBRATION:
solutions of nicotine in desorbing solution
RANGE:
0.050 to 20 µg/sample [4]
ACCURACY RANGE STUDIED:
1 µL
ESTIMATED LOD: 0.013 µg/sample (instrumental) [4] PRECISION ( r):
0.024
APPLICABILITY: Under the GC parameters stated in the method, nicotine can be identified based upon retention time. Nicotine is quantified using quinoline as an internal standard [1]. At high sample concentration, XAD-4 sorbent tube capacity (300 µg) may be exceeded and breakthrough may occur [1]. INTERFERENCES:No specific interferences were identified. However, any compound with a similar retention time may interfere. Positive identification can be confirmed by dual column chromatography with an appropriate alternative capillary column. In this method development a Rtx-1 capillary column was used. Mass spectrometry also may be used as a confirmation aid. OTHER METHODS: Other methods for nicotine are NMAM 2544 (August 15,1994) [2] and Method S293 [5] on which it was based. This method replaces the XAD-2 sorbent with XAD-4, and uses a capillary column in place of a packed GC column. The ethyl acetate desorption solvent was modified to improve nicotine recovery from sides of glass sorbent tube, and to improve recoveries for the lower DE levels.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition