Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material
A chitosan nanometer and application method technology, applied in the field of analytical chemistry, can solve the problems of long operation time, poor selectivity, slow column passing, etc., and achieve the effect of large adsorption capacity, fast adsorption rate and wide application range
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Embodiment 1
[0026] (1) Synthesis of magnetic chitosan nanoparticles: Dissolve chitosan with acetic acid, prepare 500mL1g / L chitosan acetic acid solution, add 0.25gFeCl 3 ·6H 2 O, 0.25gFeSO 4 ·7H 2 A mixed aqueous solution of O, sonicated at 80 °C and N 2 Add chitosan acetic acid solution under protection and stirring, quickly add 6.67mL NH 3 ·H 2 0, continue to stir 30min, get nanometer iron ferric oxide chitosan solution;
[0027] (2) Preparation of nickel ion-imprinted magnetic chitosan nanomaterials: Add ferric iron tetroxide chitosan solution to 3 ) 2 ·6H 2 In the aqueous solution of O, adjust the volume to 150mL with ultra-pure water; shake at 200rpm and 25°C for 15min, separate with a magnet, wash the separated solid with water three times, add it to 50mL of 5% sodium tripolyphosphate solution, and store at 60°C Ultrasound, N 2 Stir for 10 minutes under protection, add 25mL of 2% epichlorohydrin that has been pre-opened (under alkaline conditions and 60°C, 500W microwave ra...
Embodiment 2
[0029] Carry out every index experiment to embodiment 1 gained material:
[0030] 50mg of the material obtained in Example 1 was added to 100mL of different pH values containing 1mg / LNi 2+ In the solution, examine the pH value of Ni 2+ The influence of adsorption effect; the results show that the recovery rate is close to 100% between pH 4-7, so other adsorption experiments are carried out under neutral conditions.
[0031] 50mg of the material obtained in Example 1 was added to 100mL of pH=7 containing 1mg / LNi 2+ In the solution, the effect of adsorption time on Ni 2+ The influence of adsorption effect; the results show that after 10min, the adsorption equilibrium is reached.
[0032] 50mg of the material obtained in Example 1 was added to different initial Ni 2+ Concentration of the solution, in a constant temperature oscillator at 25 ° C for 2 hours, the adsorption amount of the research material varies with Ni 2+ The change of initial concentration, through the fitt...
Embodiment 3
[0036] Embodiment 1 gained material is used for trace Ni in the solution 2+ Magnetic solid phase extraction separation and enrichment:
[0037] Add 50mg of material to 200mL containing a certain concentration of Ni 2+ In the solution (environmental water sample, beverage sample or other water-based samples), adjust the pH value to 7, shake at 200rpm for 10min, and use a magnet to absorb Ni 2+ The material is separated from the solution, then add 1mL 5% EDTA-Na solution, shake and desorb at 400rpm for 2min, a total of 2 times, mix the 2 eluents evenly, and measure Ni in the eluent by flame atomic absorption spectrometry 2+ content, Ni 2+ The recovery rate is between 94.4%-114.3%, and the relative standard deviation between the results of parallel determination (n=5) is less than 3.2%;
[0038] 5000 times the K that coexists in solution + , 2500 times Na + , 4000 times Ca 2+ , 2500 times Mg 2+ , 800 times Cd 2+ , 2500 times Al 3+ , 800 times Cu 2+ , 600 times Pb 2+ , ...
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