Method of detecting and separating Pb<2+> and Cu<2+> in water quickly and simultaneously based on magnetic sensing
A magnetic sensing and fast technology, applied in chemical instruments and methods, centrifugal separation of water/sewage treatment, analysis by nuclear magnetic resonance, etc., can solve problems that cannot fully meet the needs of use, small detection range, complicated procedures, etc., to achieve Good practicability, no secondary pollution, high recovery effect
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Embodiment 1
[0037] Synthesis of functionalized magnetic quercetin nanoparticles (QMNPs) with a roadmap as shown in figure 1 As shown, the specific process is: add FeCl to 250mL ultrapure water 3 ·6H 2 O (10.85g) and FeCl 2 ·6H 2 O (3.99g), stirred and heated to 100°C until the solids were completely dissolved. Then add NH 3 ·H 2 O (5 mL, 28%), resulting in a black precipitate. Separation of magnetic Fe by centrifugation 3 o 4 nanoparticles and washed three times with water and ethanol. 1mg Fe 3 o 4 The powder was added into 100mL of ultrapure water, and dispersed by ultrasonic (40KHz, 30°C) for 1h. Then a certain amount of quercetin (10 -5 mol L -1 ) into the suspension system, let it and Fe 3 o 4 React for 1 h under ultrasonic (40KHz, 30°C) dispersion conditions. Then, the functionalized magnetic quercetin nanoparticles (QMNPs) were separated by centrifugation (15min, 15000rmp). Finally, rinse the product several times with clean water and disperse it in deionized water ...
Embodiment 2
[0042] In order to compare the two samples QMNPs and Fe 3 o 4 The state of nanoparticles in water, the T of the two samples were determined 2 : Put the sample solution into a 5 mm glass tube, T 2 Measured by a 0.55T nuclear magnetic resonance instrument (TE=1000s, TR=1500ms). T 2 The measurement interval is 5 min, and each sample is scanned 3 times.
[0043] The resulting figure is shown in Figure 5, Fe 3 o 4 the T 2 Significantly increased within 22 min, indicating that under magnetic field conditions Fe 3 o 4 The nanoparticles aggregate into clusters in water. Although only minor changes occurred in the QMNPs, this suggests that the quercetin-coated Fe 3 o 4 Can be dispersed in water. In the structure of quercetin, 5 hydroxyl groups can be combined with Fe 3 o 4 form hydrogen bonds, making Fe 3 o 4 Nanoparticles disperse better in water. However, the content of quercetin can affect the stability of QMNPs. In 100mL Fe 3 o 4 Four kinds of quercetin (0.5mg, ...
Embodiment 3
[0044] Embodiment 3QMNPs recognition of metal ions
[0045] In order to detect the T of the QMNPs system for different metal ions 2 , 1mL of QMNPs solution and 10μL of different metal ions (Co 2+ , K + , Zn 2+ , Na + , Ni 2+ , Cd 2+ , Li + , Fe 3+ , Fe 2+ , Mn 2+ , Mg 2+ , La 2+ , Cu 2+ , Pb 2+ ) of acetic acid / nitrate standard solution (1×10 -3 mol L -1 ) mixed, and then put the sample solution into a 5 mm glass tube, T 2 Measured by a 0.55T nuclear magnetic resonance instrument (TE=1000s, TR=1500ms).
[0046] Add each metal ion to the prepared detection system, record T 2 relaxation time. The result is as Figure 7 As shown, the results show that only Pb 2+ and Cu 2+ Make T 2 The relaxation time changes significantly.
[0047] When Pb 2 + or Cu 2+ When added to QMNPs solution, QMNPs and Pb 2+ or Cu 2+ A coordination reaction occurs between them, resulting in the dispersion of QMNPs into clusters, as shown in Figure 8. Larger nanoparticles alter th...
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