Page:NIOSH Manual of Analytical Methods - 1008.pdf/1

 ETHYLENE DIBROMIDE

BrH2CCH2Br

MW: 187.88

METHOD: 1008, Issue 2

1008

CAS: 106-93-4

RTECS: KH9275000

EVALUATION: PARTIAL

OSHA : 20 ppm; C 30 ppm; PEAK 50 ppm/5 min NIOSH: 0.045 ppm; C 0.13 ppm/15 min; Group I Pesticide ACGIH: carcinogen (skin) (1 ppm = 7.68 mg/m 3 @ NTP)

Issue 1: 15 February 1984 Issue 2: 15 August 1994

PROPERTIES: liquid; d 2.169 g/mL @ 25 °C; BP 131 °C; MP 10 °C; VP 1.5 kPa (11 mm Hg; 1.4% v/v) @ 25 °C

SYNONYMS: EDB, 1,2-dibromoethane

SAMPLING SAMPLER:

SOLID SORBENT TUBE (coconut shell charcoal, 100 mg/50 mg)

FLOW RATE:

0.02 to 0.2 L/min

VOL-MIN: -MAX:

0.1 L @ 0.1 ppm 25 L

SHIPMENT:

insulated container, dry ice

MEASUREMENT 63

TECHNIQUE:

GAS CHROMATOGRAPHY,

ANALYTE:

ethylene dibromide

DESORPTION:

10 mL 99:1 benzene:methanol (v/v); stand 1h

INJECTION VOLUME:

5 µL 175 °C 315 °C 50 °C

Ni ECD

SAMPLE STABILITY:

2 weeks at -25 °C or below [1,2].

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

FIELD BLANKS:

2 to 10 field blanks per set

CARRIER GAS:

N 2, 35 mL/min

COLUMN:

1.8 m x 4-mm ID, borosilicate glass packed with 3% OV-210 on 80/100 Gas Chrom Q

CALIBRATION:

ethylene dibromide in 99:1 benzene:methanol (v/v) with internal standard

RANGE:

0.1 to 0.5 µg per sample [1]

ACCURACY RANGE STUDIED: BIAS:

see EVALUATION OF METHOD [1] not significant

ˆ ): not determined OVERALL PRECISION (S rT ACCURACY:

not determined

ESTIMATED LOD: 0.01 µg per sample [1,2] PRECISION (Sr):

0.044 [3]

APPLICABILITY: The working range is 0.0003 to 1 ppm (0.002 to 8 mg/m 3) for a 25-L air sample. The range of an ECD most useful for quantitation depends on the type of detector and chromatograph used. For reliable quantitation, the ECD must be optimized for the smallest possible amount of analyte.

INTERFERENCES: None identified. The chromatographic column or separation conditions may be changed to circumvent interference problems. An alternate chromatographic column packing is GP 20% SP-2100/0.1% Carbowax 1500 on 100/120 Chromosorb WHP [2].

OTHER METHODS: This revises P&CAM 260 [1] and Method 1008 (dated 2/15/84). Method S104 [4], which has not been revised, can also be used but uses the less sensitive flame ionization detector.

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