Page:NIOSH Manual of Analytical Methods - 5034.pdf/1

 TRIBUTYL PHOSPHATE

(C4H9O)3P=O

MW: 266.32

METHOD: 5034, Issue 1

CAS: 126-73-8

5034

RTECS: TC7700000

EVALUATION: PARTIAL

OSHA : 0.5 ppm NIOSH: 0.2 ppm ACGIH: 0.2 ppm (1 ppm = 10.9 mg/m 3 @ NTP)

Issue 1: 15 August 1994

PROPERTIES: liquid; boiling point 293 C; density 0.98 g/mL @ 20 C; VP very low @ 20 C; vapor density 9.2 (air=1); flash point 166 C (closed cup)

SYNONYMS: phosphoric acid, tributyl ester; tri-n-butyl phosphate; TBP; Celluphos 4

SAMPLING SAMPLER:

FILTER (0.8-µm mixed cellulose ester membrane); above 23 C, use two filter cassettes in series

MEASUREMENT TECHNIQUE:

GC, FPD with a phosphorus filter

ANALYTE:

tributyl phosphate

FLOW RATE: 1 to 3 L/min

EXTRACTION:

10 mL diethyl ether

VOL-MIN: -MAX:

2 L @ 0.5 ppm 100 L

INJECTION VOLUME:

5 µL

SHIPMENT:

separate front and backup cassettes if two were used; seal cassettes firmly with plugs

DETECTOR:

H 2, 70 mL/min; Air 150 mL/min

SAMPLE STABILITY:

not determined

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

BLANKS:

2 to 10 field blanks per set

CARRIER GAS:

2.7 to 12.6 mg/m 3 [1] (100-L samples)

BIAS:

- 0.3%

N 2, 50 mL/min

COLUMN:

6-ft x -in ID stainless steel, with 3% OV-101 on 100/120 mesh Supelcoport

CALIBRATION:

standard solutions of tributyl phosphate in diethyl ether

ACCURACY RANGE STUDIED:

240 C 240 °C 150 °C

RANGE:

6 to 1500 µg per sample

ˆ ): 0.076 [1] OVERALL PRECISION (S rT ACCURACY:

± 16.8%

ESTIMATED LOD:

2 µg per sample [1]

PRECISION (Sr):

0.0146 @ 234 to 973 µg per sample [1]

APPLICABILITY: The working range is 0.006 to 1.4 ppm (0.06 to 15 mg/m 3) for a 100-L air sample. This method may be adapted to other phosphates of relatively low volatility with appropriate changes in chromatographic conditions.

INTERFERENCES: Any phosphorus-containing compound that has the same retention time as the analyte is an interference. A non-polar capillary column may be used for better resolution.

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