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Title: Liquid chromatographic determination of benzo(a)pyrene at part-per-billion concentrations in highly-refined coal- and petroleum-derived fuels

Conference ·
OSTI ID:5723254

Benzo(a)pyrene (BaP), a well-known carcinogen, is frequently measured as an ''indicator'' of the potential dermal tumorigenicity of a sample. The present sequential HPLC/HPLC method overcomes problems in trace-level sample enrichment and recovery correction encountered earlier. Five g of naphtha or fuel oil are diluted to 10 mL with methylene chloride and spiked with a small quantity (Ca. 0.25 ..mu..g) of carbon-14 labeled BaP tracer. A BaP-enriched fraction is obtained from a 1 mL aliquot of this simple using a semipreparative-scale Partisil PAC 10 column (10% methylene chloride/hexane eluent), and concentrated to exactly 0.3, 0.5, or 1.0 mL (acetonitrile solvent). Quantitation is performed using a reverse-phase Vydac 201 TP 5415 column (75/25 v/v acetonitrile/water eluent) and a Waters Model 420 E/420 AC fluorescence detector employing an excitation/emission filter pair of 360/425 nm. The recovery of the radiolabeled tracer is evaluated by combusting 50 ..mu..L of the final isolate in pure oxygen, collecting the liberated carbon-14 CO/sub 2/ in an alkaline desorber and liquid scintillation spectroscopy. The recovery of BaP normally exceeds 90%; however, values as low as ca. 50% are occasionally observed. Potential matrix interferences in the recovery determination are eliminated via sample combustion. The nominal precision of the overall method is approximately +- 30% relative standard deviation at a BaP concentration of 30 ppb. The nominal analysis time for a single sample is approximately 4 hr. 7 refs., 2 figs., 1 tab.

Research Organization:
Oak Ridge National Lab., TN (USA)
DOE Contract Number:
AC05-84OR21400
OSTI ID:
5723254
Report Number(s):
CONF-8605132-1; ON: DE86011059
Resource Relation:
Conference: 10. international symposium on column liquid chromatography, San Francisco, CA, USA, 18 May 1986
Country of Publication:
United States
Language:
English