Page:NIOSH Manual of Analytical Methods - 6402.pdf/1

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PHOSPHORUS TRICHLORIDE

PCl3

MW: 137.33

METHOD: 6402, Issue 2

RTECS: TH3675000

EVALUATION: PARTIAL

OSHA : 0.5 ppm NIOSH: 0.2 ppm; STEL 0.5 ppm ACGIH: 0.2 ppm; STEL 0.5 ppm (1 ppm = 5.61 mg/m 3 @ NTP)

SYNONYMS:

CAS: 7719-12-2

6402

PROPERTIES:

Issue 1: 15 May 1985 Issue 2: 15 August 1994

liquid; d 1.574 g/mL @ 21 °C; BP 76 °C; MP -112 °C; VP 13 kPa (100 mm Hg; 13% v/v) @ 21 °C

phosporous chloride.

SAMPLING

MEASUREMENT

SAMPLER:

BUBBLER (15 mL H 2O)

METHOD:

FLOW RATE:

0.05 to 0.2 L/min

ANALYTE:

molybdenum blue

VOL-MIN: -MAX:

11 L @ 0.5 ppm 100 L

COLOR DEVELOPMENT:

3 mL Br 2 water + 5 mL Na 2MoO 4 + 2 mL hydrazine sulfate → molybdenum blue

SHIPMENT:

ship in sealed bubblers

SAMPLE STABILITY:

unknown

FIELD BLANKS:

2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

ca. 3.1 mg/m 3 [1]

BIAS:

not significant [1]

ˆ ): OVERALL PRECISION (S rT

unknown

ACCURACY:

not determined

VISIBLE SPECTROPHOTOMETRY

WAVELENGTH:

830 nm

CALIBRATION:

KH 2PO 4 solutions

RANGE:

0.03 to 0.5 mg PCl 3 per sample

ESTIMATED LOD: 3 µg PCl 3 per sample

PRECISION (Sr):

0.06 @ 0.03 to 0.14 mg PCl 3 per sample [1]

APPLICABILITY: The working range is 0.2 to 14 ppm (1.2 to 80 mg/m 3) for a 25-L air sample.

INTERFERENCES: Phosphorus (V) compounds do not interfere. The sample solutions are stable to oxidation by air during sampling [1].

OTHER METHODS: This revises P&CAM 305 [2].

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