Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
38, Number 9, September 000, pp. 393-408
Quantitation
of a Metal Deactivator Additive by Derivatization and Gas Chromatography–Mass
SpectrometryR.C. Striebich*, B. Grinstead, and
S. Zabarnick
University of Dayton Research Institute, 300 College Park, Dayton, Ohio 45469-0140
The quantitative
analysis of phenolic and amine-containing petroleum additives can be challenging.
One such compound—N,N'-disalicylidene-1,2-propanediamine, a common metal
deactivator additive (MDA)—is thought to inhibit fuel oxidation catalyzed
by metals both in the fuel and on surfaces. The ability to measure the concentration
of MDA in storage stability tests, thermal-stressing studies, and field samples
is important. Quantitating low concentrations of MDA can be difficult because
of surface adsorptivity due to the phenol and amine functional groups. This
paper describes the shortcomings of direct-injection gas chromatography–mass
spectrometry to quantitate MDA as well as a solution to the analytical problem
using the common silylation agent BSA to derivatize the MDA. Results demonstrate
that the silylation technique is suitable for the determination of MDA concentrations
in aviation fuel samples and suggests that the MDA may be readily determined
in other petroleum products with a lower detection limit for MDA of 0.5 mg/L.
Measurements conducted in heated batch reactors indicate that MDA concentration
is reduced as hydrocarbon fuels are stressed. In addition, only free or available
MDA is measured by this technique, not MDA that is complexed with metals.
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