Efficient Quantification by X-ray Photoelectron Spectroscopy and Thermogravimetric Analyses of the One-Pot Grafting of Two Molecules on the Surface of Iron Oxide Nanoparticles

In this study, Superparamagnetic iron oxide nanoparticles (SPION) were functionalized in one pot with two organic molecules. Firstly, polyethylene glycol (PEG) was mixed for 46 hours to improve steric stability and then, two hours before the end of the reaction, dimercaptosuccinic acid (DMSA) was added to provide negative charges and thiol groups for post-functionalization. Three different molecular weights of PEG were used (550, 2000 and 5000 g mol -1 ). The main goal of this study was to characterize and quantify accurately the surface of SPION functionalized with two organic molecules. We demonstrated the advantages of coupling thermogravimetric and X-ray photoelectron spectrometry analyses to distinguish accurately the covering of SPION's surface. Thanks to the combination of these two techniques we were able to distinguish the amount of DMSA and PEG on SPION regarding the length of the polymer. We also showed that the length of the PEG influenced the quantity of DMSA adsorbed. With the smallest PEG (550 g mol -1 ) the presence of DMSA is almost ten times higher than with the two other PEG used proving that long polymers prevent the adsorption of small molecules on the surface of SPION.