Oxidative losses of anthracene, acenaphthylene, and benzo(a)pyrene during Florisil and silica gel cleanup using diethyl ether containing peroxides

Journal Article · Sat Dec 01 04:00:00 EST 1984 · Anal. Chem.; (United States)

DOI:https://doi.org/10.1021/ac00278a085· OSTI ID:5677135

Ligocki, M E; Pankow, J F

In the analysis of samples for nonpolar trace organic compounds, a cleanup procedure is often required to remove interfering compounds. Columns of Florisil (magnesium silicate) and silica gel (silicic acid, SiO/sub 2/ x H/sub 2/O) are frequently used for this purpose. Occasionally, the occurrence of unexpected and undesired processes may be detected and eliminated before the modification is incorporated into ongoing analytical protocols. This paper describes such an experience involving acenaphthylene, benzo(a)pyrene, anthracene, and anthracene-d/sub 10/. The last compound has been recommended for use as an internal standard (IS) compound. Toward the goal of the development of a cleanup method which would allow the recovery of a range of neutral compounds following the extraction of filters used to sample ambient air, Florisil column chromatography was tested using solvent mixes of pentane and diethyl ether. Hexane:diethyl ether has been recommended for use in the cleanup of pesticide-containing extracts. Pentane was substituted here for hexane because of its greater volatility. It was hoped that the pentane:diethyl ether solvent mix ratio could be adjusted to allow the simultaneous recovery of the PAH compounds in the same eluant fraction. Recovery studies were carried out using a standard solution of pesticides and PAHs.

• Research Organization: Oregon Graduate Center, Beaverton
• OSTI ID: 5677135
• Journal Information: Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 56:14; ISSN ANCHA
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400105* -- Separation Procedures
ACENAPHTHENE
ADSORBENTS
ADSORPTION
ALKALINE EARTH METAL COMPOUNDS
ANTHRACENE
AROMATICS
CHEMICAL REACTIONS
CHROMATOGRAPHY
CONDENSED AROMATICS
DATA
ETHERS
ETHYL ETHER
EXPERIMENTAL DATA
GAS CHROMATOGRAPHY
HYDROCARBONS
INFORMATION
LIQUID COLUMN CHROMATOGRAPHY
MAGNESIUM COMPOUNDS
MAGNESIUM SILICATES
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
OXIDATION
OXYGEN COMPOUNDS
PEROXIDES
PYRENE
SEPARATION PROCESSES
SILICA GEL
SILICATES
SILICON COMPOUNDS
SORPTION