Page:NIOSH Manual of Analytical Methods - 2537.pdf/1

 METHYL AND ETHYL METHACRYLATE (1) H2 C=C(CH3 )COOCH3 (2) H2 C=C(CH3 )COOC2 H5 METHOD: 2537, Issue 3

MW: 100.12 CAS: 80-62-6 114.15 97-63-2

(1) 1 ppm = 4.10 mg/m (2) 1 ppm = 4.68 mg/m3 3

SYNONYMS:

Issue 1: 15 August 1990 Issue 3: 15 March 2003

PROPERTIES: (1) liquid; d = 0.944 g/mL @ 20°C; BP = 100°C; VP = 4.7 kPa (35 mm Hg) @ 20°C; explosive range 1.7 to 8.2% v/v in air. (2) liquid; d = 0.917 g/mL @ 20°C; BP = 119°C; flash point = 21.1°C; index of refraction = 1.4116 (25°C).

(1) Methyl ester of methacrylic acid, methyl-2-methyl-2-propenoate (2) Ethyl ester of methacrylic acid; ethyl-2-methyl-2-propenoate

SAMPLING SAMPLER:

SOLID SORBENT TUBE (XAD-2, 400/200 mg)

FLOW RATE:

0.01 to 0.05 L/min

VOL-MIN: -MAX:

1 L @ 100 ppm 8L

SHIPMENT:

In dry ice

SAMPLE STABILITY: BLANKS:

7 days @ 25°C; 31 days @ 5°C [1]

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, FID

ANALYTE:

Methyl and ethyl methacrylate

DESORPTION:

2 mL CS2 with sonication for 30 minutes

INJECTION VOLUME:

1 µL

TEMPERATURE -INJECTION: 250°C -DETECTOR: 300°C -COLUMN: 50°C (3 min) to 150°C (8°C/min)

2 - 10 samples per set ACCURACY

CARRIER GAS:

Helium, 5.0 mL/min

COLUMN:

Capillary, fused silica, 30-m x 0.53-mm ID, 3-:m film crossbonded® 35% diphenyl-65% dimethyl polysiloxane or equivalent

CALIBRATION:

Solutions of analytes in CS 2

RANGE:

(1) 0.9 to 8240 µg [1,2] (2) 1.5 to 275 µg [1]

RANGE STUDIED: (1) 193 to 725 mg/m3 (3-L samples) [3] (2) Not studied BIAS:

OVERALL PRECISION ( Ö r T ): ACCURACY:

RTECS: OZ5075000 OZ4550000

EVALUATION: (1) FULL (2) PARTIAL

OSHA : (1) 100 ppm; (2) None NIOSH: (1) 100 ppm; (2) None ACGIH: (1) 100 ppm; (2) None

2537

(1) 2.55% [3] (2) Not determined

(1) 0.063 [3] (2) Not determined (1) +/- 12.6% [3] (2) Not determined

ESTIMATED LOD: (1) 0.4 µg/sample (Instrumental)[1] (2) 0.5 µg/sample (Instrumental)[1] PRECISION ( þ r ):

(1) 0.009 (2) 0.025 [1]

APPLICABILITY: The working range for methyl methacrylate is 0.07 to 670 ppm (0.30 to 2747 mg/m3 ) and for ethyl methacrylate is 0.11 to 19.7 ppm (0.50 to 91.7 mg/m3 ) for a 3-L air sample.

INTERFERENCES: None identified. Chromatographic conditions may be modified to resolve any interferences.

OTHER METHODS: This method updates NMAM 2537, Issue 2 (4 th ed.) [4] which previously revised NIOSH method S43 [5]. Improvements include the evaluation and addition of ethyl methacrylate to the method, higher desorption efficiency (DE) recoveries at lower study levels for both analytes, lowered LOD values, the incorporation of capillary column chromatography for analyte resolution, and the completion of a 30 day storage stability study.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition