A superparamagnetic fe 3 o 4 @void @tio 2 Photoelectrochemical detection method for in situ construction of silver ions
A photoelectrochemical and detection method technology, applied in the field of analytical chemistry, can solve the problems of photobleaching, poor solubility, organic synthesis and purification process, sensitivity can not meet the requirements of trace analysis, etc. Matching, easy-to-operate effects
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Embodiment 1
[0029] A superparamagnetic Fe-based 3 o 4 @void @TiO 2 In-situ construction of a photoelectrochemical detection method for silver ions, said method comprising the steps of:
[0030] S1, preparation of Fe 3 o 4 Nanoclusters: Dissolve 50mmol of NaOH in 20mL of DEG, heat the mixture at 120°C for 1h under nitrogen protection, cool the resulting NaOH / DEG solution and keep it at 60°C; add 4mmol of PAA, 0.4mmol of FeCl 3 Heat the mixture with 17mL DEG to 220°C, stir vigorously in a nitrogen atmosphere for 45min, then quickly inject 1.8mL of NaOH / DEG solution, the reaction solution slowly turns from light yellow to black, continue heating for 1h, and dilute the obtained product with ethanol and ultrapure water were washed three times to obtain Fe 3 o 4 nanoclusters and redisperse them in 3 mL of ultrapure water;
[0031] S2, preparation of Fe 3 o 4 @SiO 2 Microspheres: Add 3 mL of Fe to a mixture of 20 mL of ethanol and 1 mL of ammonia 3 o 4 Suspension, vigorously stirred ...
experiment example 1
[0042] In S4, the Fe 3 o 4 @void @TiO 2 -Na + The suspension was mixed with 0, 1, 2, 4, 6, 8, 10, 20, 40, 60, 80, 100, 200, 400, 1000, 2000, 4000, 6000, 8000 and 10000pmol / L silver ion solution reaction, to the final Fe 3 o 4 @void @TiO 2 -The ITO electrode modified by Ag microspheres was tested for photocurrent response; the test conditions were: 0.1mol / L PBS buffer solution (pH 7.0), and the bias potential was 0.1V; the test results were as follows Figure 8 (A), Figure 8 (B) is the corresponding linear calibration curve, given by Figure 8 It can be seen that the photocurrent gradually amplifies with the increase of silver ion concentration, Figure 8 (B) shows the quantitative relationship between the increase in photocurrent and the increase in silver ions; its dynamic linear range is 1-6000 pmol / L, and the detection limit is 0.5 pmol / L, and the high sensitivity benefits from the in situ generated Ag nano Particle-generated hot electron injection into amorphous ...
experiment example 2
[0044] In 0.1mol / L PBS (pH is 7.0), for the Fe 3 o 4 @void @TiO 2 -Na + Microsphere-modified electrode for photocurrent interference test, interference substances include: 50 times Fe(NO 3 ) 3 , 50 times HAuCl 4 , 100 times Ni(NO 3 ) 2 , 500 times Zn(NO 3 ) 2 , 500 times MgSO 4 , 500 times Co(NO 3 ) 2 , 500 times CuSO 4 , 500 times CdSO 4 、500 times KNO 3 and 50 times the mixture of the above substances; the test results are as follows Figure 9 shown by Figure 9 It can be seen that the maximum interference of the common ions mentioned above to the sensor does not exceed 7.6%, which proves that the sensor has good selectivity. It benefits from the common metal ion or acid group (AuCl 4 - , which are negatively charged and cannot undergo normal cation exchange) cannot be reduced to metal nanoparticles with plasmon resonance.
[0045] In this example, first, prepare superparamagnetic Fe 3 o 4 nanoparticles, which are then sequentially coated with silicon di...
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