Page:NIOSH Manual of Analytical Methods - 5017.pdf/1

 DIBUTYL PHOSPHATE

(C4H9O2)(OH)P=O

MW: 210.21

METHOD: 5017, Issue 2

5017

CAS: 107-66-4

RTECS: TB9605000

EVALUATION: PARTIAL

OSHA : 1 ppm NIOSH: 1 ppm; STEL 2 ppm ACGIH: 1 ppm; STEL 2 ppm (1 ppm = 8.59 mg/m 3 @ NTP)

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

PROPERTIES:

liquid; d 1.06 g/mL; decomposes @ 100 °C; VP unknown

SYNONYMS: phosphoric acid dibutyl ester

SAMPLING

MEASUREMENT

SAMPLER:

FILTER (1.0-µm PTFE)

TECHNIQUE:

GAS CHROMATOGRAPHY, PHOSPHORUS FPD

FLOW RATE:

1 to 3 L/min

ANALYTE:

dibutyl trimethylsilyl phosphate

VOL-MIN: -MAX:

50 L @ 1 ppm 250 L

DESORPTION:

acetonitrile

DERIVATIZATION: SHIPMENT:

routine

N,O-bis(trimethylsilyl)tri fluoroacetamide (BSTFA)

SAMPLE STABILITY:

at least 7 days at room temperature [1]

BLANKS:

2 to 10 field blanks per set

INJECTION VOLUME: 1 µL CARRIER GAS:

He, 30 mL/min

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN: ACCURACY RANGE STUDIED:

BIAS:

2.3 to 10 mg/m 3 [1] (180-L samples)

220 °C 210 °C 155 °C

COLUMN:

glass; 1.2 m x 6-mm OD; 3% OV-101 on 100/120 mesh Chromosorb WHP

CALIBRATION:

dibutyl phosphate in CH 3CN with internal standard

RANGE:

0.4 to 2 mg per sample

not determined

ˆ ): 0.057 [1] OVERALL PRECISION (S rT ESTIMATED LOD: 0.07 mg per sample [1] ACCURACY:

not determined PRECISION (Sr):

0.017 [1]

APPLICABILITY: The working range is 0.2 to 1.2 ppm (2 to 10 mg/m 3) for a 200-L air sample.

INTERFERENCES: None identified.

OTHER METHODS: This method revises P&CAM 297 [2].

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