Liquid chromatographic determination of benzo(a)pyrene at part-per-billion concentrations in highly-refined coal- and petroleum-derived fuels
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
Similar Records
The determination of chlorophenoxy acid herbicides by liquid chromatography using carbon-14 tracers
Liquid chromatography/electrochemistry for coal analysis: Quarterly progress report for period of December 16, 1986-March 15, 1987
Related Subjects
BENZOPYRENE
ENRICHMENT
LIQUID COLUMN CHROMATOGRAPHY
RECOVERY
COAL LIQUIDS
SMOKES
LUBRICATING OILS
PETROLEUM
SHALE OIL
TOBACCO PRODUCTS
CARBON 14
CARCINOGENS
CHEMICAL ANALYSIS
EXPERIMENTAL DATA
TRACER TECHNIQUES
AEROSOLS
AROMATICS
BETA DECAY RADIOISOTOPES
BETA-MINUS DECAY RADIOISOTOPES
CARBON ISOTOPES
CHROMATOGRAPHY
COLLOIDS
CONDENSED AROMATICS
DATA
DISPERSIONS
ENERGY SOURCES
EVEN-EVEN NUCLEI
FLUIDS
FOSSIL FUELS
FUELS
HYDROCARBONS
INFORMATION
ISOTOPE APPLICATIONS
ISOTOPES
LIGHT NUCLEI
LIQUIDS
LUBRICANTS
MINERAL OILS
NUCLEI
NUMERICAL DATA
OILS
ORGANIC COMPOUNDS
OTHER ORGANIC COMPOUNDS
PETROLEUM PRODUCTS
RADIOISOTOPES
RESIDUES
SEPARATION PROCESSES
SOLS
YEARS LIVING RADIOISOTOPES
010600* - Coal
Lignite
& Peat- Properties & Composition