Abstract
Magnetite nanoparticles (Fe3O4), average particle size of 12.9 nm, were synthesized de novo from ferrous and ferric iron salt solutions (total iron salt concentration of 3.8 mM) using steady-state headspace NH3(g), 3.3% v/v, at room temperature and pressure, without mechanical agitation, resulting in >99.9% yield. Nanoparticles size distributions were based on enumeration of TEM images and chemical compositions analyzed by: XRD, EDXRF, and FT-IR; super-paramagnetic properties were analyzed by magnetization saturation (74 emu/g). Studies included varying headspace [NH3(g)] (1.6, 3.3, 8.4% v/v), and total iron concentrations (1.0 mM, 3.8 mM, 10.0 mM, and >>10 mM). An application of the unmodified synthesized magnetite nanoparticles included analyses of tetracycline’s (50, 100, 200, 300, and 400 ppb) in aqueous, which was compared to the same tetracycline concentrations prepared in aqueous synthesis suspension with >97% extraction, analyzed with LC-MS/MS.
Highlights
Magnetite (Fe3O4) nanoparticles (MNP) are of interest to industry and academia with research and applications in: medicine [1,2,3,4,5], technology [6,7], bioremediation, and analytical analysis [8,9,10,11]
We present a simple, high-yield, phase pure approach to MNP synthesis
ResFuigltusraen1dpDreisecuntsssiaondiagram and photograph of the apparatus developed for the synthesis of magnetite nanoparticles (MNP) using NH3(g) headspace and iron salts (Fe2+, Fe3+) solution, in Vessel J. 2T.h1.eAappppaarraattuuss is described in detail in the Section 3.2.4
Summary
Magnetite (Fe3O4) nanoparticles (MNP) are of interest to industry and academia with research and applications in: medicine [1,2,3,4,5], technology [6,7], bioremediation, and analytical analysis [8,9,10,11]. Co-precipitation is one of the simplest techniques for MNP synthesis It is typically carried out in aqueous solutions of ferrous (Fe2+) and ferric (Fe3+), with bulk addition of OH, with heat and/or agitation and/or sonication. These approaches are required to disrupt crystal growth during MNP synthesis [15]. 2. ResFuigltusraen1dpDreisecuntsssiaondiagram and photograph of the apparatus developed for the synthesis of magnetite nanoparticles (MNP) using NH3(g) headspace and iron salts (Fe2+, Fe3+) solution, in Vessel J. In order to minimize the phenomenon observed, researchers have attempted to decrease the droplet size of base titrant [21,22], still with limited success for MNP synthesis yield and mass. Mobile phases for LC-MS/MS analysis were: A: Fisher Optima water with 0.1% v/v formic acid and B: Fisher LC-MS grade methanol with 0.1% v/v formic acid
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