Preparation method of reduction state graphene and platinum nanometer particle composite material modified molecularly imprinted membrane electrochemical sensor
A technology of molecular imprinting and membrane electrochemistry, which is applied in the field of analysis and detection, can solve problems affecting the sensitivity of electrochemical sensors, etc., and achieve the effects of increasing sensitivity, catalytic efficiency, and improving specificity
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[0040] The preparation method of reduced graphene: take 3.0g of graphite, add 120ml of concentrated sulfuric acid, stir in an ice bath, add a total of 16.0g of potassium permanganate in 3 times. Control the reaction temperature to 35-40°C and stir for 20 hours. After stirring, add 250ml of water in batches, heat in a water bath and stir at a temperature of 80°C, and react for 2 hours, and the reactant gradually turns bright yellow. After cooling, 40ml of hydrogen peroxide was added and stirred overnight to obtain graphene (GO) in an oxidized state. Then it was washed with acid and water until the pH was close to 6. Sonicate GO for 1-2 hours. Take 60mg of GO and add 600mg of polystyrene sodium sulfonate (PSS) to sonicate for 30min, and stir at 50°C for 24h. After cooling, add 4ml each of ammonia water and hydrazine hydrate, and keep stirring at 95-100°C for 24h. After water washing and ultrasonic dispersion, the reduced graphene (PSS-RGO) was obtained.
[0041] The prepara...
Embodiment 1
[0043] a) Electrode pretreatment: Glassy carbon electrode (Φ=3mm) is treated with 0.05μm Al 2 o 3 After the suspension was polished, put into Piranha solution (30% H 2 o 2 : Concentrated H 2 SO 4 =3:7, V / V) for 2 minutes, and then ultrasonically cleaned with absolute ethanol and deionized water for 2 minutes;
[0044] b) Electrochemical deposition of platinum nanoparticles: place the cleaned glassy carbon electrode in a solution containing 0.5 mol L -1 Sulfuric acid and 5mmol·L -1 In the mixed aqueous solution of hexachloroplatinic acid, within the potential range of -0.2 ~ 0.6V, at 30mV s -1 The scan rate is cyclically scanned for 3 minutes; then rinsed with absolute ethanol and deionized water in sequence, dried with nitrogen, soaked in Piranha solution for 2 minutes, rinsed with deionized water, and dried with nitrogen to obtain platinum nanoparticles Modified electrode;
[0045] c) Assembly of reduced graphene and platinum nanoparticles: Sonicate 5 μL of 0.5 mg / mL ...
Embodiment 2
[0049] a) Electrode pretreatment: Glassy carbon electrode (Φ=3mm) is treated with 0.05μm Al 2 o 3 After the suspension was polished, put into Piranha solution (30% H 2 o 2 : Concentrated H 2 SO 4 =3:7, V / V) for 2 minutes, and then ultrasonically cleaned with absolute ethanol and deionized water for 2 minutes;
[0050] b) Electrochemical deposition of platinum nanoparticles: place the cleaned glassy carbon electrode in a solution containing 0.5 mol L -1 Sulfuric acid and 5mmol·L -1 In the mixed aqueous solution of hexachloroplatinic acid, within the potential range of -0.2 ~ 0.6V, at 50mV s -1 The scan rate is cyclically scanned for 10 minutes; then rinsed with absolute ethanol and deionized water in sequence, dried with nitrogen, soaked in Piranha solution for 2 minutes, rinsed with deionized water, and dried with nitrogen to obtain platinum nanoparticles Modified electrode;
[0051] c) Assembly of reduced graphene and platinum nanoparticles: 10 μL of 0.5 mg / mL reduced...
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