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Sensitive Potentiometric Method for Determination of Micromolar Level of Polyethoxylated Nonionic Surfactants in Effluents

  • M. Sak-Bosnar , D. Madunic-Cacic , R. Matesic-Puac and Z. Grabaric
Published/Copyright: April 2, 2013
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Abstract

The Metrohm NIO surfactant electrode has been used as end-point indicator for potentiometric titration of low concentration level of polyethoxylated nonionic surfactants. This can be achieved by using of a diluted titrant concentration, thus reducing the amount of precipitate formed during titration and preventing the electrode deterioration. The solutions of low levels (down to 10−6 mol/L) of selected nonionic surfactants containing 5 to 23 EO groups were successfully titrated with diluted (as low as 10−4 mol/L) sodium tetraphenylborate as standard anionic titrant, increasing up to 20 times the sensitivity of the method. The low surfactant concentration has been determined in synthetic formulations of widely used detergent products and industrial waste waters. The titration end-point has been determined by applying extended Savitzky-Golay least-squares regression. The accuracy and precision has been evaluated by using the standard addition method. Relative standard deviation within results was between 3.4 and 12.8 % depending on the sample complexity and the surfactant concentration level.

Kurzfassung

Eine Metrohm NIO-Tensidelektrode wurde bei der potentiometrischen Titration polyethoxylierter nichtionischer Tenside in niedriger Konzentration zur Endpunktbestimmung verwendet. Das kann mit Hilfe einer verdünnten Titrant-Konzentration erreicht werden, wodurch die während der Titration gebildete Niederschlagsmenge reduziert und eine Elektrodenschädigung verhindert wird. Die Lösungen mit geringem Gehalt (bis zu 10−6 mol/L) an ausgewählten nichtionischen Tensiden, die 5 bis 23 EO-Gruppen enthalten, wurden mit verdünntem (bis zu 10−4 mol/L) Natriumtetraphenylborat als anionischer Standard-Titrant erfolgreich titriert. Die Empfindlichkeit der Methode wurde dadurch bis zu 20 mal erhöht. Die niedrige Tensidkonzentration wurde in synthetischen Formulierungen weit verbreiteter Wasch- und Reinigungsmitteln und in industriellen Abwässern bestimmt. Der Titrationsendpunkt wurde mittels einer erweiterten Savitzky-Golay-Regressionsanalyse bestimmt. Die Genauigkeit und Präzision wurde durch Verwendung der Standard-Additions-Methode bewertet. Die relative Standardabweichung innerhalb der Ergebnisse lag je nach Probenkomplexität und Tensidekonzentration zwischen 3,4 und 12,8 %.


Dr. Milan Sak-Bosnar, Department of Chemistry, Josip Juraj Strossmayer University of Osijek, F. Kuhaca 20, HR-31000 Osijek, Croatia. E-mail:

Milan Sak-Bosnar obtained his Ph.D. in 1982. His main research areas are surfactant analyses, electroanalytical methods and chemical sensors. At present he is employed at the Department of Chemistry, Josip Juraj Strossmayer University of Osijek.

Dubravka Madunic-Cacic obtained her B.Sc. at the Faculty of Food Technology, Josip Juraj Strossmayer University of Osijek. Since 1995 she is employed in Saponia Chemical Industry, Osijek, at the Department for Analytical Methods Development (electrochemical and enzymatic methods). Her main research interests are development and application of chemical and electrochemical sensors for surfactant and enzyme based products analysis.

Ruzica Matesic-Puac received her diploma in food technology from Faculty of Food Technology, Josip Juraj Strossmayer University of Osijek, M.Sc. degree from Faculty of Science and her Ph.D. from University of Zagreb. Currently she is assistant lecturer in analytical chemistry at the Faculty of Food Technology, Josip Juraj Strossmayer University of Osijek. Her main research areas are ion-selective electrodes, surfactants and electroanalytical methods.

Prof. Dr. Zorana Grabaric is a full professor of chemistry at the Faculty of Food Technology and Biotechnology, University of Zagreb, teaching General and Inorganic Chemistry and Instrumental analysis (electrochemistry). Her main research interests are development and application of chemometric methods for resolution of analytical signals and development of chemical sensors and biosensors for application in food analyses and biomedicine.


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Received: 2006-10-07
Published Online: 2013-04-02
Published in Print: 2007-02-01

© 2007, Carl Hanser Publisher, Munich

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