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Monocrystalline TiO2 nanometer rod-based polychlorinated biphenyl photoelectrochemistry analysis method

A technology of polychlorinated biphenyls and nanorods, applied in the direction of material electrochemical variables, etc., can solve the problem of non-existence of selectivity, and achieve the effect of simple method, improved sensitivity and high sensitivity

Inactive Publication Date: 2017-01-11
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although photocatalytic technology has high catalytic efficiency, it has a significant disadvantage, that is, there is no selectivity for various substrates in the catalytic system.

Method used

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  • Monocrystalline TiO2 nanometer rod-based polychlorinated biphenyl photoelectrochemistry analysis method

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Experimental program
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Embodiment 1

[0039] A single-crystal TiO 2 Nanorod-based photoelectrochemical analysis of polychlorinated biphenyls, whose working electrode (SC,MI)-TiO 2 The NRs photoanode was obtained by the following steps:

[0040] Growth of a layer of TiO on FTO substrate by sol-gel method 2 Seed. Then, 7.5 mL of deionized water and 7.5 mL of concentrated hydrochloric acid (38 wt%) were mixed and stirred, and then 0.35 mL of tetrabutyl titanate was added dropwise. At the same time, PCB101 was added as a template molecule at a concentration of 3 μM. Stir vigorously for 30 min until the mixture is clarified. Put the pretreated FTO into a 25mL polytetrafluoroethylene-lined autoclave, pour the above solution, seal and react at 150°C for 4h. The obtained electrode was washed several times with distilled water, dried at 60°C, and then calcined at 500°C for 0.5h in a muffle furnace to obtain (SC,MI)-TiO 2 NRs photoanodes, such as figure 1 As shown, (SC,MI)-TiO 2 The NRs photoanode is a square nanoro...

Embodiment 2

[0042] Using continuous measurement in the containing 1 × 10 -10 mol / L 0.1mol / L Na in PCB101 2 SO 4 Photocurrent method in solution for (SC,MI)-TiO 2 The stability of NRs photoanodes was investigated. Under light conditions, (SC,MI)-TiO 2 The NRs photoanode can rapidly exhibit a photocurrent response and maintain a stable photocurrent under continuous 50s illumination. At the same time, in the process of continuously investigating the photocurrent response by using the method of applying and not applying the light source at intervals, it is found that in 15 consecutive scans, the photocurrent response value basically does not change, as shown in figure 2 shown. The results show that the constructed PCB101 photoelectrochemical sensor has high stability.

Embodiment 3

[0044] A single-crystal TiO 2 Nanorod polychlorinated biphenyl photoelectrochemical analysis method, using I-t curve method, 0.6V potential and ultraviolet lamp irradiation, in 0.1M Na 2 SO 4 solution, measure the photocurrent of the background solution, and then sequentially use a micro sample injector to Na 2 SO 4 A series of concentrations of 1×10 were added to the solution -4 mol / L~1×10 -10 mol / L PCB101 standard solution, and measure its photocurrent respectively. During the experiment, it was found that with the increase of PCB101 concentration, (SC,MI)-TiO 2 The photocurrent response detected by the NRs photoanode increases gradually, as image 3 shown.

[0045] Figure 4 Among them, the linear fitting equation ΔI / I detected by PCB101 blank =0.862+0.059logC, correlation coefficient R 2 = 0.99787, the detection range is 1.0×10 -14 ~1.0×10 -7 mol / L, the detection limit is 1.0×10 -14 mol / L.

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Abstract

The invention relates to a monocrystalline TiO2 nanometer rod-based polychlorinated biphenyl photoelectrochemistry analysis method. The method comprises 1, preparing a series of tested PCB101 standard solutions with different concentrations, fully stirring the solutions and standing the mixture, 2, determining photocurrent response of a (SC, MI)-TiO2NRs photo anode in the tested PCB101 standard solutions with different concentrations under ultraviolet irradiation and bias voltage through a current-time curve method and drawing a work curve, 3, preparing a practical sample, fully stirring the sample and standing the sample, and 4, determining photocurrent response of the (SC, MI)-TiO2NRs photo anode under ultraviolet irradiation and bias voltage, calculating a practical sample concentration according to the work curve and carrying out conversion to obtain a concentration of a substance PCB101 to be detected. Compared with the prior art, the method introduces a molecular imprinting locus to the surface of the monocrystalline photo anode in situ, has good selectivity to the substance to be detected, has simple and easy processes, high sensitivity, a detection limit of 10<-14>mol / L, utilizes a stable electrode and has good reappearance.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, photoelectrochemical analysis and environmental monitoring, and relates to a single crystal TiO 2 Nanorod-based photoelectrochemical analysis of polychlorinated biphenyls, especially involving a molecularly imprinted single-crystal TiO 2 A method for the photoelectrochemical analysis of polychlorinated biphenyls with nanorod photoanodes. Background technique [0002] Polychlorinated biphenyls (PCBs) are a class of chlorinated aromatic hydrocarbons with extremely stable chemical properties, and are one of the persistent organic pollutants that are widely concerned in the world. PCBs have strong carcinogenic and teratogenic toxicity, and can eventually cause long-lasting poison to the human body through the amplification effect of the food chain. The possible hazards are of great importance. PCBs have 209 homologues, and the biochemical and toxicological reactions caused by each PCBs homol...

Claims

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Application Information

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IPC IPC(8): G01N27/26G01N27/28
Inventor 史慧杰赵金芝赵国华
Owner TONGJI UNIV
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