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A fast off-line method for the determination of active species on insoluble photocatalytic materials
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A photocatalytic material and rapid determination technology, which is applied in the preparation of test samples and analysis by electron paramagnetic resonance, etc., can solve the problems of high surface activity, inability to absorb capillary tubes, and inability to meet experimental requirements, etc.
Inactive Publication Date: 2018-08-07
DALIAN UNIV OF TECH
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Problems solved by technology
There are mainly three reasons: (1) Due to the high surface activity, it is easy to adhere to the container wall after being crushed, and cannot be absorbed into the capillary for online EPR detection (2) Some photocatalytic materials with specific forms (such as gold) Porous materials and photocatalytic membranes) cannot be dissolved in water to form a uniform solution because they cannot be mechanically ground (to prevent damage to specific structures). (3) Many photocatalytic materials are only used in specific reaction systems (such as hydrogen and or oxygen). High catalytic performance, the online EPR experiment cannot meet the experimental requirements
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Embodiment 1
[0029] 1. First, set the stirring-offline light excitation induction reaction system, the specific steps are as follows;
[0030] 1) Turn on the light source to preheat for 20 minutes;
[0031] 2) Weigh 20mg of photocatalytic material and place it in a beaker, add 1ml (40mmol / l) DMPO solution for the determination of hydroxyl;
[0032] 3) After adding magnets into the reaction vessel, put it on the stirring device, adjust the rotating speed to shake the solution;
[0033] 4) After 10 minutes of light exposure, take a sample with a capillary tube, encapsulate it with plasticine, and conduct an EPR test. The EPR test conditions are: center magnetic field: 3360G; sweep field width: 100G; receiving gain: 1×10 4 ;Modulation frequency: 100KHz; Modulation amplitude: 2G; Scanning time: 40.96s; Time constant: 163.84s; Resolution: 1024, illumination time: 3min
[0034] 2. Quantitative characterization of hydroxyl radicals, the specific steps are as follows:
[0035] The concentratio...
Embodiment 2
[0039] Quantitative analysis of photogenerated electrons on gold nanoporous nanomaterials by spin trapping
[0040] 1. First, set the stirring-offline light excitation induction reaction system, the specific steps are as follows;
[0041] 1) Turn on the light source to preheat for 20 minutes;
[0042] 2) Weigh 20mg of photocatalytic material and place it in a beaker, add 1ml (0.05mmol / l) TEMPO solution and use electronic measurement;
[0043] 3) After adding magnets into the reaction vessel, put it on the stirring device, adjust the rotating speed to shake the solution;
[0044] 4) After 10 minutes of light exposure, take a sample with a capillary tube, encapsulate it with plasticine, and conduct an EPR test. The EPR test conditions are: center magnetic field: 3360G; sweep field width: 100G; receiving gain: 1×10 4 ; Modulation frequency: 100KHz; Modulation amplitude: 2G; Scan time: 40.96s; Time constant: 163.84s; Resolution: 1024, illumination time: 4min
[0045] 2. Quantita...
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Abstract
The invention discloses a method for quickly determining active species on an insoluble photocatalytic material offline and belongs to the field of environment-oriented analysis. The active species are important intermediate species in a photocatalytic degradation process, and are important indexes of evaluating the catalytic performance of the material. The method capable of determining active species generated in excitation of the insoluble photocatalytic material offline is built; the disadvantages of the method for detecting the active species online are compensated, and a detection method capable of simulating the active species in a reality reaction system is provided. The reaction system is induced through coupled agitation-offline illumination excitation, a proper spin trapping agent is selected for trapping the active species on the photocatalytic material, a proper internal standard substance is selected for quantitative analysis and the method has important practical significance in deep understanding of the photocatalytic material.
Description
technical field [0001] The invention relates to a method for off-line rapid determination of photoactive active species, which belongs to the technical field of environmental analysis, in particular to an off-line rapid determination of active species on insoluble photocatalytic materials. Background technique [0002] Photocatalytic degradation of pollutants is an energy-saving, high-efficiency green and environmentally friendly new technology developed in recent years. With the wide application of photocatalytic technology, various photocatalytic materials have emerged. Active species are important intermediate substances in the process of photocatalytic degradation, and are also important indicators for evaluating the catalytic performance of materials. The active species produced by the photocatalytic process generally include hydroxyl radicals, superoxide anion radicals, singlet oxygen and hydrated electrons, etc. The very short lifetimes (microseconds or nanoseconds)...
Claims
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