Page:NIOSH Manual of Analytical Methods - 2560.pdf/1

 1-NITROPYRENE IN DIESEL PARTICULATES C16 H9 NO2

MW: 247.26

METHOD: 2560, Issue 1

CAS: 5522-43-0

RTECS: UR2480000

EVALUATION: PARTIAL

OSHA : no PEL NIOSH: no REL ACGIH: no TLV

PROPERTIES:

2560

Issue 1: 15 March 2003

solid; d 1.246 g/cc @ 20 °C; MP 154157 °C; BP 231 °C

SYNONYMS: None

SAMPLING

MEASUREMENT

SAMPLER:

FILTER (Glass Fiber, 37-mm)

TECHNIQUE:

GAS CHROMATOGRAPHY, NITROGEN CHEMILUMINESCENCE DETECTOR

FLOW RATE:

1.0 to 2.0 L/min

ANALYTE:

1-Nitropyrene

VOL-MIN: -MAX:

480 L 960 L

DESORPTION:

1 mL toluene; place on a rotary shaker for minimum of 12 hours.

SHIPMENT:

Ship in container at ambient temperature.

INJECTION VOLUME:

SAMPLE STABILITY:

At least 28 days @ 25 °C

BLANKS:

2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

Generated atmospheres not studied

BIAS:

Not determined

TEMPERATURE -INJECTION: -DETECTOR: -COLUMN:

Not determined

250 °C Furnace: 850 °C Initial: 100 °C, ramp at 7.5 °C/min to 305 °C

CARRIER GAS:

Helium @ 10.0 mL/min (splitless)

COLUMN:

Capillary, fused silica, 30m x 0.53-mm ID; 1.5 µm film 5% diphenyl-95% dimethyl polysiloxane.

CALIBRATION:

Liquid standard solutions of 1-nitropyrene in toluene.

RANGE:

0.020 to 50 µg per sample

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

20 µL

ESTIMATED LOD: 0.010 µg per sample (see Evaluation of Method) PRECISION ( þ r ):

0.02 @ 1 to 50 µg per sample

APPLICABILITY: The working range is 0.021 to 104 µg/m3 for a 500 L sample. An appropriate range of calibration standards should be used to bracket the expected analyte concentration range. Because of sensitivity and accuracy considerations, a single calibration curve will not be appropriate for the entire working range. This method was developed to analyze 1nitropyrene in a diesel particulate matrix (see Figure 2). 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 capillary column. Identification can also be confirmed by mass spectrometry. OTHER METHODS: None identified.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition