A technique for quantitative analysis of 3-aminopropylsilane on the surface of chemically modifi ed Fe 3 O 4 magnetic nanoparticles in the concentration range 0.32-3.03 mmol/g was developed using attenuated total refl ection infrared spectroscopy. The technique was based on the ratios of band areas corresponding to Fe-O vibrations of the nanoparticles and Si-O vibrations of the coating as a function of the Si mass fraction in the nanocomposite that was determined by inductively coupled plasma atomic-emission spectroscopy.Introduction. Magnetic nanoparticles (MNP), including those based on iron and its oxides (γ-Fe 2 O 3 and Fe 3 O 4 ), are currently being investigated for medical applications (targeted drug delivery, improved contrast in magnetic-resonance imaging, and hyperthermal treatment of tumors [1-3]). Magnetic materials are used routinely, e.g., in biology for magnetic separation of biomolecules and cells [4] or in chemistry for development of magnetic separation of catalysts [5]. A promising method for modifying iron-oxide nanoparticles (NP) consists of depositing an organic layer on MNP using functionalized alkoxysilanes, in particular, 3-aminopropyltrialkoxysilanes [6-18] that form an organosilicon layer with functional groups on the surface. This enables the NP to be modifi ed further. The ability to conjugate MNP to biomolecules or organic catalysts depends essentially on the surface concentration of functional groups. IR spectroscopy is most often employed for a qualitative assessment of the degree of functionalization. As a rule, elemental analysis, inductively coupled plasma atomic-emission spectroscopy (AES), or thermogravimetric analysis (TGA) is used for a quantitative determination of the number of organic molecules on the MNP surface [6-8, 10-14].The number of molecules immobilized on the MNP can be determined indirectly using sorption (desorption) or covalent binding of various organic chromophores to the surface groups. Fluorescence or UV/vis spectrometry can determine the number of free molecules remaining in solution [6][7][8][9][15][16][17]. For example, MNP with surface 3-aminopropylsilane (APS) groups were modifi ed covalently with rhodamine B [15], N-difl uorenylmethoxycarbonyl-L-lysine [6], or S-naproxene [7] (production of amide derivatives) or p-nitrobenzaldehyde (Schiff base formation) [16,17] in order to determine the concentration of surface amines. The degree of functionalization of the starting MNP was determined from the difference between the amounts of reagent added to the reaction mixture and unreacted reagent. Conductometric titration with HCl was used to determine the concentration of amines on the MNP surface [18]. The conductivity of the suspension began to rise rapidly after all amines were neutralized. The amount of consumed HCl and; therefore, the amount of amines could be calculated from this.The goal of the present work was to develop a technique for measuring the amount of APS from 0.320 to 3.06 mmol/g of MNP on the surface of chemically modifi ed Fe 3 O 4 MNP us...