Page:NIOSH Manual of Analytical Methods - 1302.pdf/1

 N-METHYL-2-PYRROLIDINONE C5H9NO

MW: 99.13

METHOD: 1302, Issue 1

CAS: 872-50-4

1302 RTECS: UY5790000

EVALUATION: PARTIAL

OSHA: None NIOSH: None ACGIH: None (1 ppm = 4.05 mg/m3 @ NTP)

Issue 1: 15 January 1998

PROPERTIES:

Clear liquid, amine-like odor; d = 1.027 g/mL@ 25 C; BP = 202 C @ 760 mm Hg; FP = -24.4 C; VP = 0.29 mm Hg (0.039 kPa) @ 20 C; explosive limits = 1.3% to 9.5% (v/v).

SYNONYMS: 1-methyl-2-pyrrolidone, N-methyl- -pyrrolidone, N-methyl- -butyrolactone, NMP, 1-methylazacyclopentan-2-one, MP, M-Pyrol SAMPLING SAMPLER:

SOLID SORBENT TUBE (Coconut shell charcoal, 100/50 mg)

FLOW RATE:

0.05 to 0.2 L/min

MEASUREMENT TECHNIQUE: GAS CHROMATOGRAPHY, NPD or FID ANALYTE:

N-methyl-2-pyrrolidinone (NMP)

DESORPTION: 1 mL methylene chloride/methanol (95:5) VOL-MIN: -MAX:

0.5 L 125 L

SHIPMENT:

INJECTION VOLUME:

1 µL

Keep cold. Protect from prolonged exposure to light.

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

SAMPLE STABILITY:

14 days at 5 C [1]

CARRIER GAS:

Helium, 2.4 mL/min

BLANKS:

2 to 10 field blanks per set

COLUMN:

amine capillary, 30 m, 0.32-mm ID, 1-µm film, crossbonded® 5% diphenyl-95% dimethyl polysiloxane

CALIBRATION:

solutions of NMP in solvent

RANGE:

0.063 to 25.8 µg/sample (NPD) [1] 0.662 to 2066 µg/sample (FID) [1]

250 C 300 C 60 to 200 C (10 C/min)

ACCURACY RANGE STUDIED:

not determined

BIAS:

not determined

OVERALL PRECISION ( ACCURACY:

rT

): not determined not determined

ESTIMATED LOD: 0.02 µg/sample (NPD) [1] 0.3 µg/sample (FID) [1] PRECISION ( r):

0.05 (NPD) [1] 0.01 (FID) [1]

APPLICABILITY: Under the GC parameters given in the method N-methyl-2-pyrrolidinone can be identified based upon retention time and quantified. INTERFERENCES:No specific interferences were identified. However, any compound with a similar retention time may interfere.

OTHER METHODS:This method represents an improvement over an OSHA In-House method for N-methyl-2-pyrrolidone [2]. Method 1302 employs a shorter capillary column, improved sensitivity and recovery at lower sample levels, and a choice of two detection systems.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition