Preconcentration of with magnetic solid phase extraction and determination by ICP-OES

In recent years, magnetic nanoparticles have been used frequently in the SPE method. A new method for SPE, magnetic solid phase extraction (MSPE), was using these nanoparticles. As magnetic nanoparticles are used magnetic sorbents or modified magnetic sorbents. In this method, magnetic sorbents are used for the extraction of target analytes. In the first step, the analytes are adsorbed, and then these particles are separated from the sample solution using an external magnetic field and after this analyzed. Magnetic sorbents have many advantages over traditional sorbents. This method, which is easier and gives faster results, can be preferred over SPE. Other advantages of the widespread use of MSPE can be listed as follows: use of less organic solvents, less waste generation, higher enrichment factor nanoparticles with suitable materials is necessary in order to avoid these negative situations. The thesis is the synthesis of the Fe3O4 nanoparticle modified with APTES and TX-114, respectively, as adsorbent, and then determining these nanoparticles by magnetic solid phase extraction technique, by enriching them with Co(II) and Cd(II) heavy metal cations. Using FESEM, EDX, FT-IR, and TGA devices, the characterization of magnetic nanoparticles synthesized to determine heavy metals was performed. After this stage, all the determinations were made with the ICP-OES device. In was used as a standard internal substance in all of the experiments. All chemicals used for the experiment were of analytical purity, therefore they were used directly. The most powerful of elemental analysis laboratories, ICP OES, is widely used in routine analysis with its robustness, precise, accurate procedures and technique that will benefit greatly from fast. It is capable of simultaneous determination for up to 70 elements. ICP-OES has the least interference of all analytical atomic spectrometry techniques. The study performed all sets separately for Co (II) and Cd (II) ions. The effects of pH value, adsorbent amount, and contact time on the enrichment study were investigated, and thus optimal conditions for enrichment were determined. In addition, the effects of adsorption isotherms, adsorption kinetics, desorption, and foreign ion studies on the recovery of Co(II) and Cd(II) heavy metal cations were investigated. Na+, K+, Ca2+, Mg2+, Fe3+, Cu2+, Ni2+, Zn2+, Al3+, NH4+, NO3-, SO42-, CH3COO- ions were used in foreign ion study. The method was compatible with both Langmuir and Freundlich isotherm models. The analytical performance of the developed method was evaluated by finding the analytical values RSD (relative standard deviation), LOD (limit of detection), LOQ (limit of quantification), and EF (enrichment factor). The adsorbent material enriched with Co(II) and Cd(II) heavy metal cations is easily separated from the solution by applying an external magnetic field without additional processing. The study determined optimal conditions as pH = 7, adsorbent amount 10 mg, and contact time 180 minutes. The heavy metal cations Co(II) and Cd(II) from the aqueous solution were initiated in these conditions. In isotherm studies, the effects of Co(II) and Cd(II) concentration on adsorption were examined by applying different values between 1 mg/L and 50 mg/L in separate experiments, and the Langmuir model for Co (R2 > 0.99) was found for Freundlich model (R2 > 0.97); the Langmuir model for Cd (R2 > 0.98) was found for Freundlich model (R2 > 0.96). In adsorption kinetics studies, so-called first-degree and so-called second-degree equations were studied. As a result of the value of the so-called second-order equation (R2 > 0.99) for the Co(II) ion, it was observed that the so-called first-order equation (R2 < 0.74) is more compatible than the so-called second-order equation (R2 > 0.99). The so-called second-order equation (R2 < 0.73) for the Cd(II) ion is more compatible than the so-called first-order equation. The effect of Co(II) and Cd(II) ions on displaying was studied at four different concentrations in acidic and basic environments, ranging from 0.25 mol/L to 1.5 mol/L. It was found that HCl achieves maximum recovery for both Co(II) and Cd(II) at a concentration of 1.5 mol/L. NaOH's desorption study did not achieve significant recovery for both heavy metals. The joint ion study examined the effect of recovery of many cations and anions at different concentrations. In the presence of these ions at specific concentrations, the Co(II) and Cd(II) heavy metal cations were experimentally recovered over 95%. In order of relative standard deviation values (RSD), limit of quantification (LOQ), limit of detection (LOD) and enrichment factor (EF) were calculated as for Co2+ 3.05%, 1.88 μg/L, 0.564 μg/L, 109.41; for Cd2+ 1.40%, 2.963 μg/L, 0.889 μg/L, 20.99.