Page:NIOSH Manual of Analytical Methods - 3518.pdf/1

 PHENYLHYDRAZINE

C6H5NHNH2

MW: 108.14

METHOD: 3518, Issue 1

CAS: 100-63-0

3518

RTECS: MV8925000

EVALUATION:

OSHA : 5 ppm (skin) NIOSH: C 0.14 ppm/120 min (skin) ACGIH: 5 ppm, STEL 10 ppm, suspect carcinogen (1 ppm = 4.42 mg/m 3 @ NTP)

PROPERTIES:

Issue 1: 15 August 1994

solid; MP 19.5 °C; d 1.098 g/mL @ 20 °C; VP 5 Pa (0.04 mm Hg; 50 ppm) @ 25 °C

SYNONYMS: hydrazinobenzene, hydrazine-benzene

SAMPLING SAMPLER:

GLASS MIDGET BUBBLER (containing 15 mL 0.1 M hydrochloric acid)

FLOW RATE:

0.2 to 1 L/min

VOL-MIN: -MAX:

25 L @ 5 ppm 120 L

SHIPMENT:

hand delivery or use of bubbler shipping cases

SAMPLE STABILITY: BLANKS:

MEASUREMENT TECHNIQUE:

VISIBLE ABSORPTION SPECTROPHOTOMETRY

ANALYTE:

phenylhydrazine hydrochloride/ phosphomolybdic acid complex

SAMPLE WORKUP:

transfer bubbler solution, two 5-mL rinses, and 10 mL phosphomolybdic acid to 50-mL volumetric flask

DILUTION:

3-mL aliquot diluted to 10 mL

at least 5 days at room temperature [1]

COLORIMETRY:

absorbance @ 730 nm

2 to 10 field blanks per set

CALIBRATION:

phenylhydrazine hydrochloride in 0.1 M hydrochloric acid

RANGE:

0.5 to 4.4 mg per sample [1]

ACCURACY RANGE STUDIED:

10.4 to 44.8 mg/m 3 [1] (100-L samples)

BIAS:

4.8%

ESTIMATED LOD: 0.2 mg per sample [2] PRECISION (Sr):

0.023 [1]

ˆ ): 0.060 [1] OVERALL PRECISION (S rT ACCURACY:

± 16.6%

APPLICABILITY: The working range is 1.1 to 11 ppm (5 to 45 mg/m 3) for a 100-L air sample.

INTERFERENCES: Other hydrazines may interfere in the analysis; reducing agents such as ferrous salts may interfere also [2].

OTHER METHODS: This is Method S160 [2] in a revised format. Feinsilver et al. [3] provided the basis for this method. Murty et al. [4] used photometry and photometric titrations with cacotheline as a reagent to determine phenylhydrazine i n the range of 0.1 to 2 mg. Hasan [5] determined phenylhydrazine spectrophotometrically over a range of 0.1 to 3.0 mg using copper (II) nitrate.

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