Methods for polynuclear aromatic hydrocarbon determination in air samples using polar-bonded phase HPLC and GC-MS with application to oil refinery samples

Thesis/Dissertation · Tue Jan 01 00:00:00 EST 1985

OSTI ID:7013322

Karlesky, K L

Particle samples were collected using high volume air samplers fitted with glass fiber filters or with a cascade impactor containing paper filters. They were then cleaned using either extraction with dimethylsulfoxide and pentane or utilizing a small cartridge containing a diamine polar-bonded phase material, the second method being more effective. Vapor phase PAH were sampled using an apparatus designed in the laboratory. After collection, the resins were desorbed with solvent and the PAH content was determined. The suitability of the resins decrease in the following order: Amberlite XAD-2, Chromosorb 105, Tenax GC, coconut charcoal, and Ambesorb XE-348. High performance liquid chromatography (HPLC) was used to determine the behavior of PAH in the normal and reversed phase on polar-bonded phases containing amine, diamine, and pyrrolidone substrates. Results support the proposed mechanism in the normal phase and indicate that both a partitioning and liquid-solid adsorption mechanism takes place in the reversed phase depending upon the mobile phase. Occasionally, these polar-bonded phases can be deactivated by the formation of amine-carbonyl complexes from polar aldehydes or ketones in the solvent or sample. Deactivation can be reversed by flushing with water to hydrolyze the Schiff's base imine back to the amine. Gas chromatography-mass spectroscopy (GC-MS) was used to analyze air samples from oil refineries in Port Arthur, collected over a period of three years. The analytical procedures are applied to the collected samples to determine if they contain detectable amounts of PAH. The GC-MS analysis was adequate for this study but the use of SIM detection is preferred because of the greater sensitivity for PAH.

• Research Organization: Texas A and M Univ., College Station (USA)
• OSTI ID: 7013322
• Resource Relation: Other Information: Thesis (Ph. D.)
• Country of Publication: United States
• Language: English

Related Subjects

02 PETROLEUM
54 ENVIRONMENTAL SCIENCES
GAS CHROMATOGRAPHY
TECHNOLOGY ASSESSMENT
LIQUID COLUMN CHROMATOGRAPHY
MASS SPECTROSCOPY
POLYCYCLIC AROMATIC HYDROCARBONS
AIR POLLUTION MONITORING
CHEMICAL ANALYSIS
AIR SAMPLERS
MEASURING INSTRUMENTS
PERFORMANCE
PETROLEUM REFINERIES
RESINS
SAMPLE PREPARATION
AROMATICS
CHROMATOGRAPHY
EQUIPMENT
HYDROCARBONS
INDUSTRIAL PLANTS
ORGANIC COMPOUNDS
ORGANIC POLYMERS
PETROCHEMICALS
PETROLEUM PRODUCTS
POLYMERS
SAMPLERS
SEPARATION PROCESSES
SPECTROSCOPY
023000* - Petroleum- Properties & Composition
020900 - Petroleum- Environmental Aspects
500200 - Environment
Atmospheric- Chemicals Monitoring & Transport- (-1989)