3,3'-DICHLOROBENZIDINE (See Method 5509, BENZIDINE, for procedure)
(C6H3ClNH2)2
MW: 253.13
METHOD: 5509, Issue 2
CAS: 91-94-1
RTECS: DD0525000
EVALUATION: FULL
OSHA : carcinogen (29 CFR 1910.1010) NIOSH: carcinogen (29 CFR 1910.1010) ACGIH: carcinogen (skin)
5509
Issue 1: 15 May 1989 Issue 2: 15 August 1994
PROPERTIES: solid; MP 132 °C
SYNONYMS: 3,3'-dichloro[1,1'-biphenyl]-4,4'-diamine.
SAMPLING SAMPLER:
FILTER (13-mm glass fiber)
MEASUREMENT TECHNIQUE:
HPLC, UV DETECTION
ANALYTE:
3,3'-dichlorobenzidine
DESORPTION:
0.5 mL 0.17% (v/v) triethylamine in methanol; stand 60 min
FLOW RATE: 0.2 L/min VOL-MIN: -MAX:
20 L @ 10 µg/m 3 100 L
SHIPMENT:
ship benzidine samples in dry ice
SAMPLE STABILITY:
12 days @ 23 °C [1]
BLANKS:
2 to 10 field blanks per set
INJECTION VOLUME:
15 µL
MOBILE PHASE:
70% acetonitrile/30% water
FLOW RATE:
1.5 mL/min; ambient temperature
COLUMN:
µBondapak C 18, 10-µm particles, 30 cm x 4-mm
DETECTOR:
UV, 254 nm
CALIBRATION:
solutions eluent
RANGE:
0.2 to 7 µg per sample
ACCURACY RANGE STUDIED:
20 to 130 µg/m 3 [1]
BIAS:
- 4.0%
of
3,3-dichlorobenzidine
ˆ ): 0.07 [1] OVERALL PRECISION (S rT
ESTIMATED LOD: 0.05 µg per sample [1]
ACCURACY:
PRECISION (Sr):
± 15.2%
in
≤0.07 [1]
APPLICABILITY: The working range is 4 to 200 mg/m 3 for a 50-L air sample. Benzidinium sulfate and 3,3'-dichlorobenzidine dihydrochloride will be collected and converted to benzidine and 3,3'-dichlorobenzidine, respectively, during sample pre paration.
INTERFERENCES: Aniline interferes in the determination of benzidine but may be resolved [2]. 4,4'-Methylenebis(2-chloroaniline) interferes in the determination of 3,3'-dichlorobenzidine [1]. A number of compounds were shown not to interfere [1,2] (see NOTE 2, step 12).
OTHER METHODS: This combines and replaces P&CAM 243 and P&CAM 246 [3].
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
