RT Conference Proceedings T1 Optimization of the synthesis of functionalized magnetic nanoparticles and their characterization A1 Siles-Cordero, María Teresa A1 López-Guerrero, María del Mar A1 Vereda-Alonso, Elisa Isabel A1 García-de-Torres, Amparo A1 Cano-Pavón, José Manuel K1 Nanopartículas AB Magnetic nanoparticles (MNPs), a new kind of nanometer-sized material, are widely used in the fields ofbiotechnology and biomedicine. These particles are superparamagnetic, which means that they are attracted to amagnetic field, but retain no residual magnetism after the field is removed. In recent years, MNPs have beenstudied because of their potential applications as magnetic carries for various biomedical uses such as cell andDNA separation, drug delivery system, magnetic resonance imaging, bio separation, and preconcentration ofvarious anions and cations.16 Magnetite, Fe3O4 is the magnetic material most used in biomedical application due toits several interesting properties such as great chemical stability, low toxicity, high saturation magnetization toallow its manipulation with an external field, ability to bond with different molecules to surface functionalized,biocompatibility and the heating ability in presence of a field, which made it an candidate for hyperthermiatreatment.17 The quality of the MNPs is extremely sensitive to synthesis conditions, such as reaction time,temperature, reagent concentration, quality of solvent, etc. In order to optimize the synthesis to obtain a high yieldwith the smallest size of these nanoparticles, a factorial design 24 (16 experiments) was developed. Two levelfactorial designs have many advantages, for example they are more efficient than studying one factor at a time. Afactorial design allows the effect of several factors and even interactions between them to be determined with thesame number of trials as are necessary to determine any one of the effects by itself with the same degree ofaccuracy. The selected factors and their corresponding ranges were determined after preliminary experiments.These factors were the reaction time, volume and concentration of NH3. The lower and upper values given to eachfactor are shown in Table 1.Table 1. Factor levels in the screeningVariable Lower UpperReaction time (min) 15 60NH3 volume (mL) 10 40NH3 concentration (%) 10 30In order to quantify the synthesis yields a new method by Fourier transform infrared spectrometry (FTIR) hasbeen developed for the direct determination of Fe-O by absorbance measurements in KBr pellets. The procedure isbased on the use of the ratio between the absorbance of the characteristic band of iron oxide and threecharacteristics bands of a nitrate internal standard added to samples.Simple linear regression (SLR) and multiple linear regression (MLR) were proved with each of the three arearatios chosen between the analyte and the internal standard, obtaining the best results with the MLR method.For validation purposes the different yields of the synthesis were analysed by the proposed IR method and HR CSETAAS using solid samples auto sampler. The results obtained were satisfactorily compared. At the same time,the size of the MNPs obtained was determined by Scanning Electron Microscopy (SEM).Keywords: MNPs, coprecipitation synthesis, experiments designAcknowledgements The authors thank the Spanish Ministerio de Ciencia y Tecnología (MCyT project no.CTQ2013-44791-P) for supporting this study and also FEDER funds. And Universidad de Málaga, Plan Propio.16 M.H. Mashhadizadeh, Z. Karami, J. Hazard. Mat., 190 (2011) 1023-1029.17 P.E. García Casillas, C.A. Rodríguez González, C. A. Martínez Pérez, Infrared Spectroscopy of Functionalized Magnetic Nanoparticles, in: InfraredSpectroscopy – Materials Science, Engineering and Technology, Ed by Prof. T. Theophile (2012) ISBN 978-953-51-0537-4. YR 2015 FD 2015-12-21 LK http://hdl.handle.net/10630/10857 UL http://hdl.handle.net/10630/10857 LA eng NO Universidad de Málaga. Campus de Excelencia Internacional Andalucía Tech DS RIUMA. Repositorio Institucional de la Universidad de Málaga RD 21 ene 2026