Combination of ultrasonic extraction and stripping analysis: an effective and reliable way for the determination of Cu and Pb in lubricating oils.

The determination of metals in lubricating oil has been used as an important way to prevent components failures, to provide environmental information and in some cases, to identify adulteration. In this work, an effective and simple procedure is proposed for Cu and Pb determination in lubricating oils. An ultrasonic bath was employed for extraction of these elements from oil samples in a mixture 1:1 (v/v) of concentrated HCl and H(2)O(2). A very efficient extraction of Cu and Pb (approximately 100%) was attained after 30 min of ultrasound, allowing the simultaneous determination of both metals using square-wave anodic stripping voltammetry at thin-film gold electrodes. The extraction procedure was performed in 4 mL polypropylene closed vessels and dozens of samples could be treated simultaneously in the same ultrasonic bath. The regions of the ultrasonic bath, where the maximum efficiency of extraction was attained were evaluated. Over the optimized region, 30 samples can be treated simultaneously. Used lubricating oils from automotive engines were analyzed by using the optimized extraction procedure.

[1]  Richard G. Compton,et al.  Sono-Electroanalysis: Application to the Detection of Lead in Petrol , 2000 .

[2]  R. Muñoz,et al.  Amperometric determination of dipyrone in pharmaceutical formulations with a flow cell containing gold electrodes from recordable compact discs. , 2001, Journal of pharmaceutical sciences.

[3]  E. Richter,et al.  Square-Wave Quantification of Lead in Rainwater with Disposable Gold Electrodes Without Removal of Dissolved Oxygen , 2003 .

[4]  J. Fortune,et al.  Sonochemical stripping voltammetry , 1995 .

[5]  R A Muñoz,et al.  Gold electrodes from compact discs modified with platinum for amperometric determination of ascorbic acid in pharmaceutical formulations. , 2001, Talanta.

[6]  L. Ceccon,et al.  Determination of lead in oil products by derivative potentiometric stripping analysis , 1999 .

[7]  A. Krejčová,et al.  Determination of metals in lubricating oils by X-ray fluorescence spectrometry. , 2001, Talanta.

[8]  M. Arruda,et al.  Ultrasound-assisted extraction of Ca, K and Mg from in vitro citrus culture , 2003 .

[9]  R. Muñoz,et al.  Simultaneous determination of copper and lead in ethanol fuel by anodic stripping voltammetry , 2004 .

[10]  M. Al-Masri,et al.  Cold ultrasonic acid extraction of copper, lead and zinc from soil samples , 2002 .

[11]  E. Richter,et al.  Gold electrodes from recordable CDs , 2000, Analytical chemistry.

[12]  Lúcio Angnes,et al.  Compact Disks, a New Source for Gold Electrodes. Application to the Quantification of Copper by PSA , 2001 .

[13]  E. J. Ekanem,et al.  The determination of wear metals in used lubricating oils by flame atomic absorption spectrometry using sulphanilic acid as ashing agent. , 1997, Talanta.

[14]  L. Danielsson,et al.  Computerized potentiometric stripping analysis for the determination of cadmium, lead, copper and zinc in biological materials , 1981 .

[15]  J. Capelo,et al.  Comparison of ultrasound-assisted extraction and microwave-assisted digestion for determination of magnesium, manganese and zinc in plant samples by flame atomic absorption spectrometry. , 2000, Talanta.

[16]  L. Ciraolo,et al.  Determination of cadmium(II) and zinc(II) in olive oils by derivative potentiometric stripping analysis , 2003 .

[17]  C. Banks,et al.  Electroanalytical detection of zinc in whole blood , 2004 .

[18]  F. Marken,et al.  Sono-electroanalysis: Application to the detection of lead in wine , 1998 .

[19]  M. D. Luque de Castro,et al.  Continuous ultrasound-assisted extraction of hexavalent chromium from soil with or without on-line preconcentration prior to photometric monitoring. , 2002, The Analyst.

[20]  J Ziȩba–Palus Examination of used motor oils by flame AAS for criminalistic purposes: a diagnostic study , 1998 .

[21]  M. Guardia,et al.  Multi-elemental analysis of mussel samples by atomic absorption spectrometry after room temperature sonication , 1998 .

[22]  D. Giuffrida,et al.  Determination of Cd(II), Cu(II), Pb(II), and Zn(II) content in commercial vegetable oils using derivative potentiometric stripping analysis , 2004 .

[23]  M. D. L. Castro,et al.  New methods for acceleration of meat sample preparation prior to determination of the metal content by atomic absorption spectrometry , 2003, Analytical and bioanalytical chemistry.

[24]  R. Compton,et al.  Sonoelectroanalysis: Anodic Stripping Voltammetric Determination of Cadmium in Whole Human Blood , 2004 .

[25]  C. Brett,et al.  Ultrasound-Enhanced Anodic Stripping Voltammetry Using Perfluorosulfonated Ionomer-Coated Mercury Thin-Film Electrodes , 1997 .

[26]  R. Compton,et al.  The Electroanalytical Detection and Determination of Copper in Blood: Ultrasonically Enhanced Solvent Extraction Coupled with Electrochemical Detection by Sono‐Square‐Wave Stripping Voltammetry Analysis , 2002 .

[27]  R. Compton,et al.  Anodic stripping voltammetry of copper at insonated glassy carbon-based electrodes: application to the determination of copper in beer , 1999 .

[28]  M. Murillo,et al.  Determination of metals in used lubricating oils by AAS using emulsified samples. , 1998, Talanta.

[29]  F. Barbosa,et al.  Comparison of ultrasound-assisted extraction, slurry sampling and microwave-assisted digestion for cadmium, copper and lead determination in biological and sediment samples by electrothermal atomic absorption spectrometry , 2000 .

[30]  C. Barbas,et al.  DEVELOPMENT AND VALIDATION OF EXTRACTION METHODS FOR DETERMINATION OF ZINC AND ARSENIC SPECIATION IN SOILS USING FOCUSED ULTRASOUND: APPLICATION TO HEAVY METAL STUDY IN MUD AND SOILS , 2001 .

[31]  C. Cámara,et al.  Determination of Cd in sonicate slurries and leachates of biological and environmental materials by FI-CV-AAS. , 2000, Talanta.

[32]  J. Capelo,et al.  Solid-liquid extraction of copper from slurried samples using high intensity probe sonication for electrothermal atomic absorption spectrometry. , 1999, Talanta.

[33]  M. D. Luque de Castro,et al.  Dynamic ultrasound-assisted extraction of cadmium and lead from plants prior to electrothermal atomic absorption spectrometry , 2003 .

[34]  I. Lavilla,et al.  Ultrasonic extraction combined with fast furnace analysis as an improved methodology for total selenium determination in seafood by electrothermal-atomic absorption spectrometry , 2002 .

[35]  Marco Aurélio Zezzi Arruda,et al.  Use of ultrasonic baths for analytical applications: a new approach for optimisation conditions , 2001 .

[36]  C. Banks,et al.  Ultrasound: promoting electroanalysis in difficult real world media. , 2004, The Analyst.

[37]  R. Compton,et al.  Sonoelectroanalysis – an overview , 2000, Fresenius' journal of analytical chemistry.

[38]  M. Arruda,et al.  A fast ultrasound-assisted extraction of Ca, Mg, Mn and Zn from vegetables , 2001 .

[39]  J. Capelo,et al.  Ultrasound-assisted extraction of lead from solid samples: a new perspective on the slurry-based sample preparation methods for electrothermal atomic absorption spectrometry , 1999 .

[40]  R. Muñoz,et al.  Potentiometric Stripping Analysis for Simultaneous Determination of Copper and Lead in Lubricating Oils After Total Digestion in a Focused Microwave-Assisted Oven , 2005 .