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Optimization of SPE/GC/HPLC Analytical Procedure for Determination of Phenol, Quinones, and Carboxylic Acids in Water Samples

DOI: 10.5402/2012/680929

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Abstract:

Chromatographic techniques are among the most useful analytical methods. Gas and liquid chromatography were used in the analysis of some organic compounds: phenol, hydroquinone, benzoquinone, and maleic and fumaric acids. The analytical way for the determination of these compounds in water samples was investigated. Solid-phase extraction (SPE) technique was used on the sample preparation step, different divinylbenzene-based sorbents were applied. Calibration curves of given compounds were linear over the ranges: 50–500?μg/mL for phenol and its acetic derivatives, 50–1500?μg/mL for benzoquinone in GC analysis, and 50–250?μg/mL for phenol, 40–1000?μg/mL for hydroquinone, and 4–4500?μg/mL for carboxylic acids in HPLC analysis. The LOD and LOQ of proposed analytical procedure were in the ranges of LOD: 0.042–23.83?μg/mL; LOQ: 0.138–78.64?μg/mL. 1. Introduction Phenol is a toxic compound, which very often appears in the industrial and municipal wastes. That is serious problem for the environment. There are many investigations striving for the scavenging, neutralization, and degradation of phenolic wastes and pollutants. Among the degradation techniques, the most popular are oxidation processes. There are catalytic oxidation, photodegradation, electrochemical oxidation, and degradation procedures using sonoelectrochemistry. These processes are widely described in the literature [1–11]. The main reaction route of the phenol oxidation is as follows: phenol → hydroquinone → benzoquinone → maleic acid and fumaric acid. The most desirable reaction way is the complete mineralization of phenol in which the endproducts are H2O and CO2. The oxidation can be stopped on different steps, so it is necessary to determine all products and byproducts of the reaction. There are many analytical techniques used in the determination of phenol oxidation products and byproducts [10, 12–20]. Chromatographic techniques are the most popular among analytical and separation methods. High performance liquid chromatography (HPLC) is very useful as water samples can be analyzed directly by this technique. However, not all compounds formed during oxidation of phenol and its derivatives can be precisely detected. The other technique useful in determination of phenol and its derivatives is gas chromatography (GC). In this technique the sample preparation step is considered essential, especially when water, medical, or environmental samples are analyzed. On these step extraction techniques, especially solid-phase extraction (SPE or SPME), is used, which is simple, relatively nonexpensive, and

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