Page:NIOSH Manual of Analytical Methods - 2017.pdf/1

 	ANILINE, o-TOLUIDINE, AND NITROBENZENE Aniline C6H7N o-Toluidine C7H9N Nitrobenzene C6H5NO2 METHOD: 2017, Issue 1

MW: 93.13 MW: 107.2 MW: 123.1

CAS: 62-53-3 CAS: 95-53-4 CAS: 98-95-3

RTECS: BW6650000 RTECS: XU2975000 RTECS: DA6475000

EVALUATION: PARTIAL

OSHA:	 Table 1 NIOSH:	Table 1 ACGIH:	 Table 1

2017

Issue 1: 15 January 1998

PROPERTIES: Table 1

SYNONYMS:	 Aniline: aminobenzene, benzenamine, phenylamine o-Toluidine: o-aminotoluene, 2-aminotoluene, 1-methyl-2-aminobenzene, o-methylaniline, 2-methylaniline Nitrobenzene:	 nitrobenzol, oil of mirbane SAMPLING

MEASUREMENT

SAMPLER:	 FILTER + SOLID SORBENT (glass fiber filter, sulfuric acid treated + silica gel sorbent tube, 520/260 mg) Alternate samplers: gauze wipes, 4 x 4 in.; dermal badge sampler (1 g silica gel in cotton pouch)

TECHNIQUE:

GAS CHROMATOGRAPHY, FID

ANALYTES:

aniline, o-toluidine, nitrobenzene

DESORPTION:

2 mL ethanol

FLOW RATE:	 0.2 L/min [1]

INJECTION VOLUME:

1 µL

VOL-MIN: -MAX:

5L 50 L

TEMPERATURE-INJECTION:	250 °C -DETECTOR:	300 °C -COLUMN:	35 °C to 150 °C (8 °C/min)

SHIPMENT:	 routine SAMPLE STABILITY:	 aniline and o-toluidine 7 days @ 5 °C [2]; nitrobenzene 60 days [1] BLANKS:

CARRIER GAS:

helium, 2.4 mL/min

COLUMN:

capillary column, 30 m, 0.32-mm ID,1-µm film, (Rtx-5, or equivalent) [1]

CALIBRATION:

solutions of analytes in ethanol

RANGE:

Table 2 [1]

2 to 10 field blanks per set ACCURACY

RANGE STUDIED:

Table 2

BIAS:

not determined

ESTIMATED LOD:	 Table 2 [1] OVERALL PRECISION :	not determined ACCURACY:

PRECISION :

Table 2 [1]

not determined

APPLICABILITY: Under the GC parameters stated in the method, aniline, o-toluidine, and nitrobenzene can be identified based upon retention time and quantified. Analyte recovery was optimized under conditions of moderate relative humidity (< 53%), low sampling rates (0.2 L/min), and sample volumes < 50 L [1]. Sulfuric acid-treated glass fiber filters were used to collect aniline and o-toluidine, while nitrobenzene was collected on the silica gel sorbent [1]. Nitrobenzene collection on silica gel tubes was significantly reduced under conditions of high relative humidity [1]. Dermal badge samplers (cotton pouch with 1 g silica gel) and gauze wipes were developed to estimate exposures via splashes, spills, and passive collection of aerosol vapors. INTERFERENCES: No specific interferences were identified. However, any compound with a similar retention time may interfere. OTHER METHODS: This method revises and combines methods 2002 (aniline and o-toluidine) [3], and 2005 (nitrobenzene) [4].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition