Page:NIOSH Manual of Analytical Methods - 2559.pdf/1

 DECABROMODIPHENYL OXIDE

C12 Br10 O

MW: 959.12

METHOD: 2559, Issue 1

CAS: 1163-19-5

RTECS: KN3525000

EVALUATION: PARTIAL

OSHA : no PEL NIOSH: no REL ACGIH: WEEL: 5.0 mg/m3

PROPERTIES:

2559

Issue 1: 15 March 2003

solid, white powder; MP 300 °C; sp gr 3.0; decomposes @ ca. 425 °C

SYNONYMS: DBDPO; Pentabromophenyl ether; bis(pentabromophenyl)ether; decabromodiphenyl ether; decabromobiphenyl ether.

SAMPLING SAMPLER:

Filter (Quartz fiber filter, 37-mm)

FLOW RATE:

2.0 L/min

VOL-MIN: -MAX:

48 L 960 L

SHIPMENT:

Ship at ambient temperature.

SAMPLE STABILITY:

At least 30 days @ room temp.

BLANKS:

2 to 10 field blanks per set.

MEASUREMENT TECHNIQUE:

HPLC, UV DETECTION

ANALYTE:

Decabromodiphenyl oxide (DBDPO)

DESORPTION:

1.5 mL DMSO; place on a rotary shaker for minimum of 2 hours.

INJECTION VOLUME:

5 µL

MOBILE PHASE:

98% methanol/2% pH 7 buffer of KH2 PO4 and Na2 HPO4 @ 0.225 mL/min; ambient temperature.

COLUMN:

C-18, 5 µm, 150 cm x 2.1 mm ID or equivalent.

ACCURACY DETECTOR:

UV absorption @ 228 nm.

RANGE STUDIED:

Generated atmospheres not studied.

CALIBRATION:

DBDPO dissolved in DMSO.

BIAS:

Not determined

RANGE:

2 to 240 µg per sample.

OVERALL PRECISION (Ö r T ): Not determined ACCURACY:

Not determined

ESTIMATED LOD: 1.0 µg per sample. PRECISION ( þ r ):

0.038 @ 2.6 to 240 µg per sample. [1]

APPLICABILITY: The working range is 0.002 to 5.0 mg/m3. An appropriate range of calibration standards should be used to bracket the expected analyte concentration range. To prevent the need to switch detector sensitivity settings for field samples with higher levels of DBDPO, a calibration curve made from standards containing greater levels of DBDPO may be appropriate. This method was developed to analyze DBDPO in an air sample.

INTERFERENCES: None identified - however, compounds with a similar retention time may interfere. Positive identification may be confirmed by dual column chromatography using an appropriate alternative LC column. Identification can also be confirmed by mass spectrometry.

OTHER METHODS: None identified.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition