Page:NIOSH Manual of Analytical Methods - 5036.pdf/1

 TRIMELLITIC ANHYDRIDE

C9H4O 5

MW: 192.13

METHOD: 5036, Issue 1

CAS: 552-30-7

5036

RTECS: DC2050000

EVALUATION: PARTIAL

OSHA : No PEL NIOSH: 0.005 ppm/10 h ACGIH: 0.005 ppm (1 ppm = 7.86 mg/m 3 @ NTP)

PROPERTIES:

Issue 1: 15 August 1994

solid; MP 161 to 163 °C; VP 5.3 x 10 -4 Pa (4 x 10 -6 mm Hg) @ 20 °C

SYNONYMS: anhydrotrimellitic acid; 1,3-dioxo-phthalancarboxylic acid; 1,3-dihydro-1,3-dioxo-5-isobenzofurancarboxylic acid; 1,2,4-benzenetricarboxylic acid anhydride; 1,2,4-benzenetricarboxylic acid cyclic-1,2-anhydride. SAMPLING

MEASUREMENT

SAMPLER:

FILTER (0.8-µm PVC-copolymer)

TECHNIQUE:

GAS CHROMATOGRAPHY, FID

FLOW RATE:

1.5 to 2.0 L/min

EXTRACTION:

methanol, 3 mL

VOL-MIN: -MAX:

400 L not specified

DERIVATIZATION:

SHIPMENT:

routine

SAMPLE STABILITY:

unknown

BLANKS:

2 to 10 field blanks per set

INJECTION VOLUME:

boron trifluoride/methanol

5 µL

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

315 325 250 310

°C °C °C, 2 min; 16 °C/min; °C, 4 min

COLUMN:

stainless steel, tenax 60/80 mesh, (9 ft x 2-mm)

CARRIER GAS:

Helium, 35 mL/min

CALIBRATION:

standard solutions of trimethyl trimellitate (derivative) in a mixture of pyridine, diethyl ether, and pentane

RANGE:

19 to 96 µg per sample

ACCURACY RANGE STUDIED:

0.048 to 0.24 mg/m 3 [1] (400-L samples)

BIAS:

not significant

ˆ ): not determined OVERALL PRECISION (S rT

ESTIMATED LOD: 2 µg per sample

ACCURACY:

PRECISION (Sr):

not determined

0.087 @ 19.2 to 96 µg per sample

APPLICABILITY: The working range is 0.048 to 0.24 mg/m 3 for a 400-L air sample. The method was used for analysis of bulk samples and air (field samples) [2,3]. This method will not differentiate between trimellitic anhydride and trimellitic acid [1].

INTERFERENCES: Any compound with the same retention time is an interference. The interference may be eliminated by changing the temperature program or carrier gas flow rate.

OTHER METHODS: This revises Method P&CAM 322 [1], which was based on a procedure by Biondi and Cagnosso [4].

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