Page:NIOSH Manual of Analytical Methods - 5037.pdf/1

 TRIORTHOCRESYL PHOSPHATE

(C6H4(CH3)O)3P=O

MW: 368.37

METHOD: 5037, Issue 1

CAS: 78-30-8

RTECS: TD0350000

EVALUATION: PARTIAL

OSHA : 0.1 mg/m 3 NIOSH: 0.1 mg/m 3 (skin) ACGIH: 0.1 mg/m 3 (skin)

PROPERTIES:

5037

Issue 1: 15 August 1994

liquid; melting point 11 °C; boiling point 410 °C 1.20 g/mL; VP very low at 20 °C; vapor density 12.7 (air=1); flash point 210 °C (closed cup)

SYNONYMS: phosphoric acid, tri- o-cresyl ester; phosphoric acid, tri- o-tolyl ester; phosphoric acid, tri(2-tolyl) ester; phosphoric acid, tris(2-methylphenyl) ester; o-cresyl phosphate; o-tolyl phosphate; tricresyl phosphate; tris( o-cresyl)phosphate; tris(o-tolyl)phosphate; tris( o-methylphenyl)phosphate; TOCP; TOTP; Phosflex 179-C SAMPLING SAMPLER:

FILTER (0.8-µm MIXED CELLULOSE ESTER MEMBRANE)

MEASUREMENT TECHNIQUE:

GC, FPD in phosphorus mode

ANALYTE:

triorthocresyl phosphate

EXTRACTION:

10 mL diethyl ether

FLOW RATE: 1 to 3 L/min VOL-MIN: -MAX:

2 L @ 0.1 mg/m 3 100 L

INJECTION VOLUME:

SHIPMENT:

routine

CARRIER GAS:

N 2, 50 mL/min

SAMPLE STABILITY:

DETECTOR: not determined

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

BLANKS:

2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

29 to 170 µg/m 3 (100-L samples) [1]

BIAS:

- 1.0%

ˆ rT): 0.086 [1] OVERALL PRECISION (S ACCURACY:

± 16.9%

TEMPERATURES-INJECTION: -DETECTOR: -COLUMN:

5 µL

250 °C 250 °C 220 °C

COLUMN:

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

CALIBRATION:

standard solutions of triorthocresyl phosphate in diethyl ether

RANGE:

0.15 to 24 µg per sample

ESTIMATED LOD:

0.05 µg per sample [1]

PRECISION (Sr):

0.0236 [1]

3

APPLICABILITY: The working range of this method is 0.002 to 2 mg/m 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. Triorthocresyl phosphate may be a minor component in a product containing numerous isomeric tricresyl phosphates. When dealing with such products, it must be verified that the chromatographic parameters employed result in separation of the triorthocresyl phosphate isomer from the other tricresyl phosphate isomers. A non-polar capillary column may be used for better resolution.

OTHER METHODS: This revises Method S209 [2]. The separation of aryl phosphate isomers by capillary-column GC has been investigated [3,4]. A GC/FID method has been reported that determines triorthocresyl phosphate (TOCP) in the presence of other isomeric tricresyl phosphates (TCPs) in edible oils [5]. GC/MS has been used to determine total TCP in water [6]. Revers edphase (RP) LC/UV [7], RPLC/MS [8], and RPLC/TID (thermionic detection) [9] have been shown to be useful analytical metho ds for TOCP, but all were evaluated in the absence of other TCP isomers. Normal-phase (NP) LC/UV has been used to determine total TCP in edible oils [10]. NPLC has been used to quantify low levels of TOCP in commercial TCP products [11].

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