Special electrode for in-vivo voltammetry analysis and preparation method thereof
A micro-electrode and potential technology, which is used in the analysis of materials, material analysis by electromagnetic means, and electrochemical variables of materials, etc., to achieve good stability, low detection limit, and easy reproducibility.
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Embodiment 1
[0027] Example 1. Preparation of carbon fibers covered with carbon nanomaterials
[0028] Carbon fiber (T650-35, 7 μm diameter) (Fabric Development Inc.). The carbon fiber is placed in a high temperature furnace of 1100 ° C, and the SiCl 4 The mixed gas flow of 300mL / min argon and 40mL / min hydrogen was injected into the high temperature furnace containing atmospheric oxygen for 20min. 4 Reaction with carbon fiber to generate SiO on the surface of carbon fiber 2 thin layer. The prepared carbon fibers and 0.1-0.3 g of iron phthalocyanine (FeC 32 N 8 H 16 ) were placed in the same quartz glass tube, in Ar / H 2 (The volume ratio is 1:1~1:2, and the flow rate is 20~40cm 3 / min), different heat treatments were performed for carbon fibers and iron phthalocyanine. For the heat treatment of carbon fibers, the temperature is 800-1100°C for 2-15 minutes, and for the heat treatment of iron phthalocyanine, the temperature is 500-600°C for 2-15 minutes. Then, the temperature of both...
Embodiment 2
[0029] Example 2. Preparation of carbon fiber microelectrodes covered with carbon nanomaterials
[0030] Micro-adhere the 1-2cm carbon fiber covered with carbon nanomaterials on the surface of Example 1 to 5-10cm copper wire with conductive glue, and insert it into the drawn glass capillary with both ends open (inner diameter is 1.5 cm). mm, the length is 10cm), the inner diameter of the thin end opening is 30-50μm, and the length of the carbon fiber exposed at this end is about 1mm. The thick end of the glass tube exposes the copper wire. After the openings at both ends of the glass tube were sealed with insulating glue, the prepared electrodes were dried at 100° C. for 1 h to obtain carbon fiber microelectrodes covered with carbon nanomaterials on the surface.
Embodiment 3
[0031] Embodiment 3. Preparation method one of special electrodes for in vivo voltammetry analysis of physiologically active substances
[0032] 1) The carbon fiber electrodes with carbon nanomaterials on the surface prepared in Example 2 were prepared in acetone, ethanol, and 1.0-3.0M HNO in sequence. 3 , 1.0~2.0M KOH solution and ultrasonic in secondary water. Ultrasonic intensity is 20W / cm 2 , the ultrasonic frequency is 50kHz, the ultrasonic action mode is 20s of ultrasonic work every 15s, and the ultrasonic time is 2 to 5min;
[0033] 2) Electrochemically activate the carbon fiber electrode in step 1) in a 0.5M sulfuric acid solution, that is, firstly apply a potential polarization of +2.0V to the electrode for 30-50s, and then apply a potential polarization of -1.0V for 10-30s. The obtained electrode is then subjected to 0.05-0.2Vs -1 The scanning speed is cyclically scanned in the potential range of 0.0-1.0V until a stable cyclic voltammogram is obtained. The schema...
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