Improved sample treatment for the determination of insoluble soap in sewage sludge samples by liquid chromatography with fluorescence detection.
Summary of "Improved sample treatment for the determination of insoluble soap in sewage sludge samples by liquid chromatography with fluorescence detection."
A new selective and sensitive method for the determination of insoluble fatty acid salts (soap) in sewage sludge samples is proposed. The method involves a clean up of sample with petroleum ether, the conversion of calcium and magnesium insoluble salts into soluble potassium salts, potassium salts extraction with methanol, and a derivatization procedure previous to the liquid chromatography with fluorescence detection (LC-FLD) analysis. Three different extraction techniques (Soxhlet, microwave-assisted extraction and ultrasounds) were compared and microwave-assisted extraction (MAE) was selected as appropriate for our purpose. This allowed to reduce the extraction time and solvent waste (50 mL of methanol in contrast with 250 mL for Soxhlet procedure). The absence of matrix effect was demonstrated with two standards (C(13:0) and C(17:0)) that are not commercials and neither of them has been detected in sewage sludge samples. Therefore, it was possible to evaluate the matrix effect since both standards have similar environmental behaviour (adsorption and precipitation) to commercial soaps (C(10:0)-C(18:0)). The method was successfully applied to samples from different sources and consequently, with different composition.
Affiliation
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
Journal Details
This article was published in the following journal.
Name: Talanta
ISSN: 1873-3573
Pages: 1548-55
Links
- PubMed Source: http://www.ncbi.nlm.nih.gov/pubmed/20801371
- DOI: http://dx.doi.org/10.1016/j.talanta.2010.07.044
Medical and Biotech [MESH] Definitions
Moorella
A genus of gram positive, acetogenic, thermophilic bacteria in the family Thermoanaerobacteraceae. Known habitats include HOT SPRINGS, horse manure, emu droppings, and sewage SLUDGE.
Methanospirillum
The sole genus in the family Methanospirillaceae whose organisms are progressively motile by means of polar, tufted flagella. They have been isolated from sewage-sludge and pear waste digesters as well as marine and non-marine habitats.
Medical Futility
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A type of scanning probe microscopy in which a very sharp conducting needle is swept just a few angstroms above the surface of a sample. The tiny tunneling current that flows between the sample and the needle tip is measured, and from this are produced three-dimensional topographs. Due to the poor electron conductivity of most biological samples, thin metal coatings are deposited on the sample.
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