Determination of lead ions in fish and oyster samples using a nano-adsorbent of functionalized magnetic graphene oxide nanosheets-humic acid and the flame atomic absorption technique.

This study aims at the functionalization of magnetic graphene oxide nanosheets and the binding of humic acid as a lead complex ligand. Graphene oxide nanosheets possess a large surface area and various carboxylic acid groups which can be activated easily by activating agents. Therefore, they are suitable to be used for the extraction of heavy metals. To have a better process of extracting lead ions, magnetic graphene oxide was used in this research. Humic acid, as a lead metal complex agent, has an amine functional group which can be bound to modified graphene oxide from one side. The process of constructing the nano-adsorbent proposed for the preconcentration of lead ions as well as its characterization was studied by infrared spectroscopy (IR), ultraviolet-visible spectroscopy (UV-visible), field emission scanning electron microscopy (FESEM), and vibrating sample magnetometry (VSM). The designed nano-adsorbent was tested to measure lead ions in simulated and real samples of sea water, fish, and oysters. The detection limit obtained in the simulated samples was 0.07 µg/L, and the linear range was 0.2-12 µg/L. The apparatus used to measure the ions was a flame atomic absorption device. In the analysis of the real samples, the values obtained through flame atomic absorption were compared with those obtained through furnace atomic absorption. The proposed technique is advantageous due to being cheap, precise, and sensitive for the trace measurement of lead ions.

The extraction and measurement of nickel metal ion in crab, shellfish and rice samples using magnetic silk fibroin - EDTA ligand and furnace atomic absorption spectrometry.

The main aim of the present study was the measurement of nickel metal ion in the real samples of crab, oyster and rice by the designed magnetic nano adsorbent silk fibroin-EDTA ligand (SF-Fe3O4-EDTA). Due to the structure of silk fibroin (possessing lots of functional groups which are suitable for attachment of ligands and high surface area), it was used in the structure of fabricated nano-adsorbent. To follow the fabrication processes of the magnetic nano-adsorbent, different techniques of fourier-transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-Visible), vibrating sample magnetometer (VSM), and field emission scanning electron microscopy (FE-SEM) were used. The optimization processes were performed with the chemometric method of response surface modeling with sufficient accuracy and precision. Using this chemometric method, the optimum values of pH, absorption time, the concentration of nano-adsorbent and temperature were calculated to be 6, 21 min, 4 mg L-1 and 28 °C, respectively. Due to the magnetic nature of the constructed nano-adsorbent, a magnet bar was used to separate the nano-adsorbent from the solution and then inject to the furnace atomic absorption device. Using the magnetic nano-adsorbent of silk fibroin-EDTA ligand and furnace atomic absorption a detection limit of 0.0017 µg L-1 and a linear range of 0.0030-5.0 µg L-1 for determination of nickel metal ion were obtained. The determination of nickel metal ion in the crab tissue, oyster tissue and rice samples were performed and the obtained results revealed the successful applicability of the designed method for determination of nickel metal ion in the real samples.