Page:NIOSH Manual of Analytical Methods - 5506.pdf/1

 POLYNUCLEAR AROMATIC HYDROCARBONS by HPLC

Formulae: Table 1

MW: Table 1

METHOD: 5506, Issue 3

RTECS: Table 2

EVALUATION: PARTIAL

OSHA : Table 3 NIOSH: Table 3 ACGIH: Table 3 Compounds

CAS: Table 2

PROPERTIES:

acenaphthene acenaphthylene anthracene benz[a]anthracene benzo[b]fluoranthene benzo[k]fluoranthene

5506

Issue 1: 15 May 1985 Issue 3: 15 January 1998 Table 1

benzo[ghi]perylene benzo[a]pyrene benzo[e]pyrene chrysene dibenz[a,h]anthracene fluoranthene

fluorene indeno[1,2,3-cd]pyrene naphthalene phenanthrene pyrene

NAMES & SYNONYMS: Polycyclic aromatic hydrocarbons, PAHs; also see Table 2.

SAMPLING SAMPLER: FILTER + SORBENT TUBE (37-mm, 2-µm, PTFE + washed XAD-2, 100 mg/50 mg) FLOW RATE:

2 L/min

VOL-MIN: -MAX:

200 L 1000 L

SHIPMENT:

transfer filters to culture tubes; wrap sorbent and culture tubes in Al foil; ship @ 0 C

MEASUREMENT TECHNIQUE:

HPLC, FLUORESCENCE/UV DETECTION

ANALYTE:

compounds listed above

EXTRACTION:

5 mL acetonitrile; ultrasonic bath, 30 to 60 minutes

INJECTION VOLUME:

SAMPLE STABILITY:

unknown; protect from heat and UV light

FIELD BLANKS: MEDIA BLANKS:

3 to 10 field blanks per set 6 to 10 media blanks per set

10 to 50 µL

MOBILE PHASE:

acetonitrile/water gradient @ ambient temperature, 1 mL/min

COLUMN:

250 x 4.6-mm, reversed-phase, 5-µm C18

DETECTOR:

UV @ 254 nm; fluorescence @ 340 nm (excitation), 425 nm (emission)

CALIBRATION:

standards in acetonitrile

RANGE:

see EVALUATION OF METHOD

ACCURACY RANGE STUDIED: not determined BIAS: OVERALL PRECISION ( ACCURACY:

not determined

rT

):

not determined

ESTIMATED LOD: see EVALUATION OF METHOD PRECISION ( r):

see EVALUATION OF METHOD

not determined

APPLICABILITY: This method is applicable to samples that can be extracted with acetonitrile. This method is not applicable to samples that require a different extraction solvent or contain large amounts of highly adsorptive particulate matter, e.g., fly ash or diesel soot; also, this method is not applicable to asphalt fume samples.

INTERFERENCES: Any compound that elutes at the same HPLC retention time may interfere. Heat, ozone, NO2, or UV light may cause sample degradation.

OTHER METHODS: This revises P&CAM 206 and 251 [1]. Method 5515 uses the same sampling technique, with gas chromatographic measurement [2]. Method 5800 uses the same sampling technique, and a flow-injection method to determine total polycyclic aromatic compounds at two different sets of fluorescent wavelengths [3].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition