Electrochemical sensing analysis method of environmental hormone p-nitrophenol
An environmental hormone and analysis method technology, applied in the field of electrochemical sensing and analysis of environmental hormone p-nitrophenol, can solve the problems of lack of surface active sites, serious carrier recombination, small specific surface area, etc., to improve electrocatalysis Speed, low cost, easy to synthesize effects
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Embodiment 1
[0029] WO 2.9 / g -C 3 N 4 Preparation of stepped heterojunction:
[0030] Weigh 2-10g of melamine into a ceramic crucible, heat and stir evenly, put it into a muffle furnace for heating, the heating rate is 3-12°C / min, the heating temperature is 500-600°C, the constant temperature is 3-10h, and it is ready after cooling Pale yellow g-C 3 N 4 powder. Then g-C 3 N 4 Put it in a cell wall breaker for ultrasound, the ultrasound power is 800-1500W, the ultrasound start: stop time ratio is 10:2, and the ultrasound time is 2-4h. Take 2-10mL of supernatant and dilute to 0.5-1.5L, sonicate at 80-140W for 1-4h, and let it rest overnight to obtain a thin layer of g-C 3 N 4 Dispersion liquid; 0.05~0.20g of WCl 6 Put it in 20-50mL of absolute ethanol, and ultrasonically dissolve it completely. The ultrasonic power is 80-140W, and the ultrasonic time is 3-10min. In the still, seal and heat to 150-200°C for 10-15h. After the reaction is over, cool down to room temperature naturall...
Embodiment 2
[0035] Equipped with 0.04 ~ 100μM environmental hormone 4-NP sample of known concentration, the WO 2.9 / g -C 3 N 4 The modified electrode performs DPV scanning in the environmental hormone 4-NP, and calculates the linear equation according to the magnitude of the oxidation peak current and the corresponding environmental hormone 4-NP concentration: I p =0.0491c+0.0908(R 2 =0.9985); c is the concentration (μmol / L) of environmental hormone 4-NP, I p is the oxidation peak current (μA). According to this equation, the unknown concentration of environmental hormone 4-NP can be quantitatively detected.
Embodiment 3
[0037] With reference to example 1, prepare WO 2.9 / g -C 3 N 4 Modify the electrode, put the modified electrode into the sodium acetate-acetate buffer solution containing the analyte at a pH of 3 to 7 for DPV scanning, and measure the current intensity corresponding to the electrocatalytic oxidation peak of the environmental hormone 4-NP to determine the environmental hormone 4 - NP content. Its optimal pH value is 5, and the peak current is the largest. According to the relationship between pH and voltage, the number of electrons and protons transferred is analyzed, and E is obtained by linear regression analysis of pH value and voltage. pa (V)=-0.06019pH+1.376 (R 2 =0.993), according to the formula: d Epc / d pH =0.059m / n, where m is the number of protons, n is the number of electrons, and dE pc / d pH =0.06019, close to 0.059, so it can be concluded that m / n=1, that is, in WO 2.9 / g -C 3 N 4 On the electrode, the number of electrons transferred during the electroca...
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