Page:NIOSH Manual of Analytical Methods - 5013.pdf/1

 DYES, BENZIDINE-, o-TOLIDINE-, o-DIANISIDINE-

Table 1

MW: Table 1

METHOD: 5013, Issue 2

CAS: Table 1

RTECS: Table 1

EVALUATION: PARTIAL

OSHA : no PEL NIOSH: lowest feasible; carcinogen ACGIH: carcinogen

PROPERTIES:

5013

Issue 1: 15 May 1989 Issue 2: 15 August 1994

colored powders; water soluble; VP not significant

SYNONYMS: Table 1.

SAMPLING SAMPLER:

FILTER (5-µm PTFE membrane)

MEASUREMENT TECHNIQUE:

HPLC, UV DETECTION

ANALYTE:

benzidine, o-tolidine, o-dianisidine

DESORPTION:

2 mL H 2O; ultrasonic

REACTION:

reductive cleavage of dye to free amine with sodium hydrosulfite

FLOW RATE: 1 to 3 L/min VOL-MIN: -MAX:

150 L @ 0.1 mg/m 3 500 L

SHIPMENT:

keep samples dry and cool; protect from light

SAMPLE STABILITY: FIELD BLANKS: BULK SAMPLE:

INJECTION VOLUME:

10 µL

at least 7 days @ 25 °C in the dark MOBILE PHASE:

60% methanol/40% phosphate buffer; ambient temperature

COLUMN:

10 cm x 8-mm ID, Waters Radial Pak C 18, 10-µm particles, with Radial Compression Module or equivalent

DETECTOR:

UV detector @ 280 nm

CALIBRATION:

solutions of benzidine, o-tolidine and odianisidine in methanol

RANGE:

ca. 15 to 250 µg per sample (Table 1)

2 to 10 field blanks per set

include 1 bulk sample for each dye present on the filter ACCURACY

RANGE STUDIED:

not studied

BIAS:

none identified

ˆ ): not evaluated OVERALL PRECISION (S rT ACCURACY:

not determined

ESTIMATED LOD: 3 µg benzidine per sample [1] PRECISION (Sr):

0.04 to 0.08 [2,3]

APPLICABILITY: The working range is ca. 0.06 to 8 mg/m 3 for a 250-L air sample. This method determines benzidine, o-tolidine or o-dianisidine from dyes based on these amines, but will not distinguish different dyes based on the same amine. The metho d will not distinguish benzidine obtained from reduction of the dyes and free benzidine in the dye formulation.

INTERFERENCES: Aniline, azobenzene, p-aminophenol, p-phenylenediamine or p-nitroaniline do not interfere in the measurement when present in equimolar amounts.

OTHER METHODS: This revises P&CAM 325 [2,3]. P&CAM 234 [4,5], a general colorimetric method for diazonium salts and azo dyes, has not been revised.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94