In cooperation with the Iranian Nuclear Society

Document Type : Research Paper

Author

Nuclear Fuel Cycle Research School, Nuclear Science and Technology Research Institute, AEOI, P.O.Box: 11365-8486, Tehran - Iran

Abstract

In this study, an online homogenous sedimentation method was utilized for the in situ production of micro particles to be used as an adsorbent for solid-phase extraction of molybdenum. The process involved the dissolution of yellow cake and the conversion of molybdenum (VI) into a hydrophobic complex, followed by the addition of n-dodecyltrimethylammonium bromide as a precursor to the sample solution. A precipitant reagent, sodium hexafluoride, was then introduced into the solution through a T connection in a flow system. Micro particles were produced as a result of the interaction between the precursor and the precipitant reagent, which then adsorbed the molybdenum complex. After filtration, a desorption reagent was passed over the filter to release the adsorbed molybdenum, which was subsequently measured using ICP-OES. The method yielded a linear range of 0.2-200 µg/L, with a limit of detection of 0.05 µg/g. The repeatability of the method (RSD) was found to be 8.1% and 4.3% for concentrations of 10 and 100 µg/g, respectively. Overall, this method demonstrates potential for the precise and accurate determination of molybdenum in yellow cake samples.

Highlights

  1. Weiss N. Mineral Processing Handbook. American Institute of Mining Metallurgical and Petroleum Engineering Inc. Kings Port Press. USA 1985.

 

  1. IAEA, Uranium extraction technology. Technical Reports Series. 1993;359.

 

  1. Korkisch J, Gross H. Determination of vanadium and molybdenum by atomic-absorption spectrophotometry. Talanta. 1973;11:1153-1165.

 

  1. Korkisch J, Steffan I. Analysis of nuclear raw materials. II. Spectrophotometric determination of molybdenum in yellow cake samples after prior separation by anion exchange (in German). Mikrochim. Acta. 1973;4:545-557.

 

  1. Liang P, Liu Y, Guo L. Determination of molybdenum in steel samples by ICP-AES after separation and preconcentration using nanometre-sized titanium dioxide. J. Anal. At. Spectrom. 2004;19:1006-1009.

 

  1. Divarova V, Saravanska A, Toncheva G, Milcheva N. Spectrophotometric Determination of Molybdenum(VI) as a Ternary Complex with 4-Nitrocatechol and Benzalkonium Chloride. Molecules. 2022;27(4):1217-1223.

 

  1. Ivanov V.M, Kochelaeva G.A, Prokhorova G.V. Methods for Determining Molybdenum. J. Anal. Chem. 2002;57:758–772.

 

  1. Filik H, Tütem E, Apak R. Use of the molybdenum–thiocyanate–rhodamine 6G ternary complex for spectrophotometric molybdenum determination without extraction. Anal. Chim. Acta. 2004;50:77-82.

 

  1. Pyrzynska K. Determination of molybdenum in environmental samples. Anal. Chim. Acta. 2007;590:40-48.

 

  1. Kara D, Karadaş C. A simple spectrophotometric method for the determination of trace levels of molybdenum using N,N′-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane. Spectrochim. Acta Part A. 2015;147:158–162.

 

  1. Amin A.S, Moustafa I.M, El-Sharjawy A.A. Utilization of Cloud-Point Preconcentration for Spectrophotometric Determination of Trace Amounts of Molybdenum(VI) in Plants and Water Samples. Can. Chem. Trans. 2015;3:486–496.

 

  1. Radhika S, Kumar B.N, Kantam M.L, Reddy B.R. Liquid–liquid extraction and separation possibilities of heavy and light rare-earths from phosphoric acid solutions with acidic organophosphorus reagents. Separation and Purification Technology. 2010;75(3):295-302.

 

  1. Xie F, Zhang T.A, Dreisinger D, Doyle F. A critical review on solvent extraction of rare earths from aqueous solutions. Minerals Engineering. 2014;56:10-28.

 

  1. Khanramaki F, Zahakifar F. Separation of impurities from yellow cake by solvent extraction method with Aliquat 336 as extractant. Journal of Nuclear Science and Technology. 2024;45(3):21-30.

 

  1. Kumar J.R, Kim J.S, Lee J.Y, Yoon H.S. A brief review on solvent extraction of uranium from acidic solutions. Separation & Purification Reviews. 2011;40(2):77-125.

 

  1. Hennion M.-C, Cau-Dit-Coumes C, Pichon V. Trace analysis of polar organic pollutants in aqueous samples: Tools for the rapid prediction and optimisation of the solid-phase extraction parameters. J. Chromatogr. A. 1998;823:147-161.

 

  1. Camel V. Solid phase extraction of trace elements. Spectrochimica Acta Part B: Atomic Spectroscopy. 2003;58:1177-1233.

 

  1. Neil C.D, Marc D.P, James S.F. Principles and applications of colorimetric solid-phase extraction with negligible depletion. Anal. Chim. Acta. 2006;558:230-236.

 

  1. Korkisch J, Gross H. Determination of vanadium and molybdenum by atomic-absorption spectro-photometry. Talanta. 1973;20:1153-I 165.

 

  1. Zhou Z, Niu Y, Deng H, Zhang Y, Chang X, Cao X, Ye K. Recovery of molybdenum from uranium raffinate solution containing phosphorus. Separation Science and Technology. 2020;56(17):2920-2929.

 

  1. Varga Z, Wallenius M, Mayer K, Meppen M. Analysis of uranium ore concentrates for origin assessment. Proceedings in Radiochemistry. 2011;1:27-30.

 

  1. Yousefi S.R, Shemirani F. Novel method for insitu surfactant-based solid-phase extraction: application to the determination of Co(II) and Ni(II) in aqueous samples. Microchim Acta. 2011;173:4-9.

Keywords

  1. Weiss N. Mineral Processing Handbook. American Institute of Mining Metallurgical and Petroleum Engineering Inc. Kings Port Press. USA 1985.

 

  1. IAEA, Uranium extraction technology. Technical Reports Series. 1993;359.

 

  1. Korkisch J, Gross H. Determination of vanadium and molybdenum by atomic-absorption spectrophotometry. Talanta. 1973;11:1153-1165.

 

  1. Korkisch J, Steffan I. Analysis of nuclear raw materials. II. Spectrophotometric determination of molybdenum in yellow cake samples after prior separation by anion exchange (in German). Mikrochim. Acta. 1973;4:545-557.

 

  1. Liang P, Liu Y, Guo L. Determination of molybdenum in steel samples by ICP-AES after separation and preconcentration using nanometre-sized titanium dioxide. J. Anal. At. Spectrom. 2004;19:1006-1009.

 

  1. Divarova V, Saravanska A, Toncheva G, Milcheva N. Spectrophotometric Determination of Molybdenum(VI) as a Ternary Complex with 4-Nitrocatechol and Benzalkonium Chloride. Molecules. 2022;27(4):1217-1223.

 

  1. Ivanov V.M, Kochelaeva G.A, Prokhorova G.V. Methods for Determining Molybdenum. J. Anal. Chem. 2002;57:758–772.

 

  1. Filik H, Tütem E, Apak R. Use of the molybdenum–thiocyanate–rhodamine 6G ternary complex for spectrophotometric molybdenum determination without extraction. Anal. Chim. Acta. 2004;50:77-82.

 

  1. Pyrzynska K. Determination of molybdenum in environmental samples. Anal. Chim. Acta. 2007;590:40-48.

 

  1. Kara D, Karadaş C. A simple spectrophotometric method for the determination of trace levels of molybdenum using N,N′-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane. Spectrochim. Acta Part A. 2015;147:158–162.

 

  1. Amin A.S, Moustafa I.M, El-Sharjawy A.A. Utilization of Cloud-Point Preconcentration for Spectrophotometric Determination of Trace Amounts of Molybdenum(VI) in Plants and Water Samples. Can. Chem. Trans. 2015;3:486–496.

 

  1. Radhika S, Kumar B.N, Kantam M.L, Reddy B.R. Liquid–liquid extraction and separation possibilities of heavy and light rare-earths from phosphoric acid solutions with acidic organophosphorus reagents. Separation and Purification Technology. 2010;75(3):295-302.

 

  1. Xie F, Zhang T.A, Dreisinger D, Doyle F. A critical review on solvent extraction of rare earths from aqueous solutions. Minerals Engineering. 2014;56:10-28.

 

  1. Khanramaki F, Zahakifar F. Separation of impurities from yellow cake by solvent extraction method with Aliquat 336 as extractant. Journal of Nuclear Science and Technology. 2024;45(3):21-30.

 

  1. Kumar J.R, Kim J.S, Lee J.Y, Yoon H.S. A brief review on solvent extraction of uranium from acidic solutions. Separation & Purification Reviews. 2011;40(2):77-125.

 

  1. Hennion M.-C, Cau-Dit-Coumes C, Pichon V. Trace analysis of polar organic pollutants in aqueous samples: Tools for the rapid prediction and optimisation of the solid-phase extraction parameters. J. Chromatogr. A. 1998;823:147-161.

 

  1. Camel V. Solid phase extraction of trace elements. Spectrochimica Acta Part B: Atomic Spectroscopy. 2003;58:1177-1233.

 

  1. Neil C.D, Marc D.P, James S.F. Principles and applications of colorimetric solid-phase extraction with negligible depletion. Anal. Chim. Acta. 2006;558:230-236.

 

  1. Korkisch J, Gross H. Determination of vanadium and molybdenum by atomic-absorption spectro-photometry. Talanta. 1973;20:1153-I 165.

 

  1. Zhou Z, Niu Y, Deng H, Zhang Y, Chang X, Cao X, Ye K. Recovery of molybdenum from uranium raffinate solution containing phosphorus. Separation Science and Technology. 2020;56(17):2920-2929.

 

  1. Varga Z, Wallenius M, Mayer K, Meppen M. Analysis of uranium ore concentrates for origin assessment. Proceedings in Radiochemistry. 2011;1:27-30.

 

  1. Yousefi S.R, Shemirani F. Novel method for insitu surfactant-based solid-phase extraction: application to the determination of Co(II) and Ni(II) in aqueous samples. Microchim Acta. 2011;173:4-9.