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Original Articles

Statistical tools for the optimization of a highly reproducible method for the analysis of polycyclic aromatic hydrocarbons in sludge samples

Pages 995-1008 | Received 26 Jan 2004, Accepted 15 Jul 2004, Published online: 25 Jan 2007
 

Abstract

The aim of this study is to develop and optimize an analytical method for the determination of 14 priority PAHs in sludge samples based on Accelerated Solvent Extraction (ASE) coupled to RP-HPLC/fluorescence detection. Statistical tools were used to demonstrate the influence of the parameters during the optimization steps. The final parameters were selected to provide analytical errors statistically as low as possible. First, couples of excitation/emission detection wavelengths were tested, and some were finally selected to provide errors lower than 2%. It was then demonstrated that PAH extraction efficiencies are not statistically influenced by the ASE parameters. It was also found that the ASE extraction from sludge samples provides statistically similar results to those obtained with traditional Soxhlet extraction, but with a lower reproducibility error. After optimization, the accuracy of the method was validated with a certified sludge. In conclusion, an optimized analytical procedure has been proposed to monitor PAHs during lab-scale experiments requiring highly repeatable and accurate results from a low sample volume contaminated by PAHs at trace levels.

Acknowledgements

The Agence de l’Environnement et de la Maîtrise de l’Energie (ADEME, Angers, France) is especially thanked for the grant to Eric Trably.

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