a b s t r a c tSolid-phase extraction (SPE) followed by derivatization and gas chromatography-atomic emission detection (GC-AED) was evaluated for the determination of five chlorophenols (CPs) in water samples. The derivatization was based on the esterification of phenolic compounds with ferrocenecarboxylic acid. The determination of the derivatized phenols was performed by GC-AED in the iron selective detection mode at 302 nm. The described method was tested on spiked water samples.The overall method gave detection limits of 1.6-3.7 ng L −1 and recoveries of 90.9-104.5% for the examined mono-to trichlorophenols in 10 mL water samples. The CPs extracted from a 10 mL water sample with SPE were concentrated into 100 L of organic solvent, a preconcentration factor of 100. The method was applied to lake and tap water samples, and CP contents between 6 and 51 ng L −1 in lake water and between below the detection limit and 8 ng L −1 in tap water were found for different CPs. The method is quick, simple and gives excellent recoveries, limits of detection and standard deviations.
In this work, a simple and sensitive method for the analysis of the pesticide o-phenylphenol (OPP) on citrus fruits was developed. OPP is extracted with dichloromethane by ultrasonication and derivatized with ferrocenecarboxylic acid chloride. Using ferrocene as a label, residues of OPP are determined by gas chromatography with atomic emission detection in the iron selective mode or with mass spectrometric detection. Sample cleanup is simple and rapid and merely involves a removal of excess reagent on an alumina minicolumn. The method detection limit is 2 ng of OPP/g of fruit, and recoveries from lemon samples fortified at levels of 35 and 140 ng/g are 101 and 106%, respectively. The citrus fruits analyzed (oranges, grapefruits, lemons) contained between 60 ng/g and 0.37 microg/g OPP (RSD = 8-13%), and the results were in good agreement with results obtained when OPP was analyzed using an established HPLC-FLD method. Several alcohols could also be identified in the fruit peel.
Performance characteristics of fuels, such as storage stability and lubricity, are determined mainly by the polar species of the fuel, among them the alkylated phenols. Here, we analyze gas oil and diesel samples, which have been successively desulfurized with different methods, and compare the phenol content and the phenol alkylation pattern of these materials. Because phenols occur in the low parts per million range in the fuel, very sensitive and selective analytical methods are needed for their determination. A derivatization of phenols to ferrocene esters followed by analysis by gas chromatography with both atomic emission detection (iron emission) and mass spectrometric detection is used in this work. Individual concentrations of smaller phenols with up to three substituent carbon atoms and sum parameters were determined. The classical hydrodesulfurization was found to lower the phenol content more drastically than the adsorptive desulfurization. Especially the larger alkylphenols are removed nearly completely during hydrodesulfurization, while they are almost unaffected by adsorptive desulfurization on a Ni/NiO sorbent.
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