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