Page:NIOSH Manual of Analytical Methods - 6002.pdf/1

 PHOSPHINE PH3

MW: 34.00

METHOD: 6002, Issue 2

OSHA : NIOSH: ACGIH:

6002

CAS: 7803-51-2

RTECS: SY7525000

EVALUATION: FULL

0.3 ppm 0.3 ppm; 1 ppm STEL 0.3 ppm; 1 ppm STEL (1 ppm = 1.39 mg/m3 @ NTP)

PROPERTIES:

Issue 1: 15 August 1994 Issue 2: 15 January 1998

gas, BP 87.8 C; vapor density 1.17 (air = 1); spontaneously flammable in air if P2H4 is present

SYNONYMS: hydrogen phosphide; phosphorous hydride; phosphorated hydrogen; phosphorous trihydride

SAMPLING SAMPLER:

MEASUREMENT

SORBENT TUBE (Hg(CN)2-coated silica gel, 300 mg/150 mg)

TECHNIQUE:

UV-VIS SPECTROMETER

ANALYTE:

phosphate

EXTRACTION:

10 mL hot (65-70 C) acidic permanganatereagent solution

DETECTOR:

UV @ 625 nm

CALIBRATION:

standard solutions of potassium dihydrogen phosphate (KH2PO4) (1.00 mL = 49.94 µg PH3)

RANGE:

0.3 to 10 µg per sample [2]

FLOW RATE: 0.01 - 0.2 L/min VOL-MIN: 1 L @ 0.3 ppm -MAX: 16 L SHIPMENT:

routine

SAMPLE STABILITY:

7 days @ 25 C

BLANKS:

2 to 10 field blanks per set

ESTIMATED LOD: 0.1 µg per sample [1] PRECISION ( r):

0.074 @ 2.6 to 17.4 µg per sample [2]

ACCURACY 0.195 to 0.877 mg/m3 [1] (16-L samples)

RANGE STUDIED:

0.4%

BIAS: OVERALL PRECISION ( ACCURACY:

rT):

0.091 @ 2.64 to 17.41 µg per sample [2] ± 17.6%

APPLICABILITY: The working range is 0.013 to 0.6 ppm (0.02 to 0.9 mg/m3) for a 16-L air sample. The sampler is not commercially available.

INTERFERENCES: The colorimetric determination of phosphate is subject to interference by any species that also forms a molybdate complex under these condition; possible interfering species include PCl3 and PCl5 vapors and organic phosphorous compounds.

OTHER METHODS: This revises Method S332 [2]. OSHA Method ID-180, "Phosphine in Workplace Atmospheres", [3] employing potassium hydroxide-impregnated carbon media may be used as an alternative method.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition