CN1975400B - A photoelectric synergistic catalysis device for measuring chemical oxygen demand - Google Patents
A photoelectric synergistic catalysis device for measuring chemical oxygen demand Download PDFInfo
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Abstract
一种光电协同催化测定化学需氧量的装置，属于环境分析化学传感器的技术领域。该装置是传统的电催化水体化学需氧量分析仪的改进产品，改进部分计有：分析检测装置上配置有紫外光源和石英窗；用具有光电协同催化活性的金属氧化物修饰电极作工作电极；工作电极和辅助电极分别依附在上盖板的下表面的中部的两边，是进行光电协同催化测定水体的化学需氧量所必不可少的仪器，确保水样中的有机物能高效地降解和水体化学需氧量能快速、精确地测出。
The invention relates to a device for measuring chemical oxygen demand by photoelectric synergistic catalysis, which belongs to the technical field of environmental analysis chemical sensors. The device is an improved product of the traditional electrocatalytic water chemical oxygen demand analyzer. The improved parts include: the analysis and detection device is equipped with an ultraviolet light source and a quartz window; the metal oxide modified electrode with photoelectric synergistic catalytic activity is used as the working electrode The working electrode and the auxiliary electrode are respectively attached to the two sides of the middle part of the lower surface of the upper cover plate, which is an indispensable instrument for photoelectric synergistic catalysis to determine the chemical oxygen demand of the water body, so as to ensure that the organic matter in the water sample can be efficiently degraded and The chemical oxygen demand of water can be measured quickly and accurately.
Description
Technical field
The present invention relates to a kind of device of measuring chemical oxygen requirement by photoelectric concerted catalysis, definitely say, relate to a kind of device that will contain the analysis and detection device of photoelectric-synergetic catalytically active metal oxides modified electrode, belong to the technical field of Environmental Analytical Chemistry sensor in conjunction with Flow Injection Analysis mensuration chemical oxygen demand (COD).
Background technology
Chemical oxygen demand (COD) (COD) is to measure in the water body to be subject to strong oxidizer, as Cr
2O
7 2-, MnO
4 -Equivalent Deng the organism of oxidation required oxygen when the oxidation.What at present domestic and international COD assay method adopted at most is standard circumfluence method, standard circumfluence method comprises permanganate index method and potassium dichromate oxidation, the former is mainly used in the analysis of the surface water of underground water and slight pollution, and the latter is used for the analysis of industrial waste water and sanitary wastewater more.Adopt said method to detect COD and will consume a large amount of concentrated sulphuric acids and expensive silver sulfate except analytic process, and in order to eliminate the interference of chlorion, outside the mercuric sulfate of need adding severe toxicity is sheltered, also need heating even high temperature to clear up, therefore return time is long, operating process is loaded down with trivial details, and minute reaches 2～4 hours, is easy to generate secondary pollution.
In recent years, a kind of method of utilizing the electro-catalysis technology to measure chemical oxygen demand of water body (CN02111970.8 and CN200510023445.2) has appearred.This method needs to implement in electro-catalysis chemical oxygen demand of water body analyser.Electro-catalysis chemical oxygen demand of water body analyser is made up of three parts: flow injection sampling system, analysis and detection device and data handling system.The flow injection sampling system comprises constant current peristaltic pump and microsyringe, the constant current peristaltic pump is that model is the digital display constant current peristaltic pump of D100B/C type, may command current-carrying flow velocity 2～6000mL/h, purchase instrument plant in Shanghai City Hu Xi, microsyringe is that model is the microsyringe of 7520 types, purchase Rheodyne company, utilize this sampling system can realize the current-carrying system and continuous, the accurate sample introduction of constant flow rate in the U.S..Analysis and detection device comprises working electrode 1, auxiliary electrode 2, contrast electrode 3, induction pipe 4, outlet 5, upper cover plate 6, lower cover 7 and poly tetrafluoroethylene 8, working electrode 1 is the nano-oxide modified electrode, auxiliary electrode 2 is a gold electrode, contrast electrode 3 is saturated calomel electrode or Ag/AgCl electrode, upper cover plate 6 and lower cover 7 are polyfluortetraethylene plate, the middle part of poly tetrafluoroethylene 8 has breach, induction pipe 4 and outlet 5 place the both sides of upper cover plate 6 respectively, contrast electrode 3 places in the outlet 5, poly tetrafluoroethylene 8 is clipped between upper cover plate 6 and the lower cover 7, its middle part breach is a detection cell 11, working electrode 1 is positioned at the middle part of lower cover 7, auxiliary electrode 2 is positioned at the middle part of upper cover plate 6, upper cover plate 6, poly tetrafluoroethylene 8 and lower cover 7 are fixed into one by screw or rivet.Data handling system is made of CHI electrochemical workstation and computing machine, and the CHI electrochemical workstation is purchased in Shanghai occasion China instrument company, and the CHI electrochemical workstation is connected with computing machine by cable.Induction pipe 4 is communicated with the moving phase storage pool by microsyringe and constant current peristaltic pump, outlet 5 is communicated with waste liquid pool, and the electrical signal of working electrode 1, auxiliary electrode 2 and contrast electrode 3 is connected by the electric signal input end of cable with the CHI electrochemical workstation.Water sample flows through working electrode 1, auxiliary electrode 2 and contrast electrode 3 under the driving of constant current peristaltic pump, the electric signal of working electrode 1, auxiliary electrode 2 and contrast electrode 3 outputs, after being gathered by the CHI electrochemical workstation and amplifying, be input to computing machine, handle and analyze by computer data, directly obtain chemical oxygen demand (COD) (COD) value of water sample.
The advantage of above-mentioned electro-catalysis chemical oxygen demand of water body analyser is that the electro-catalytic process of implementing in this analyser is simple to operate short with analysis time, to be this analyser still remain to be improved to the organic degradation efficiency of the water sample in it shortcoming, when the water sample of some difficult degradations is analyzed, be easy to generate than mistake, and sensitivity also remains to be improved.
Summary of the invention
The purpose of this invention is to provide a kind of device that does not have the measuring chemical oxygen requirement by photoelectric concerted catalysis of electro-catalysis chemical oxygen demand of water body analyser shortcoming.
For realizing above purpose, the present invention adopts following technical scheme.This device is the improvement product of traditional electro-catalysis chemical oxygen demand of water body analyser, improvement part in respect of: dispose ultraviolet source and quartz window on the analysis and detection device; Make the work electrode with metal oxide modified electrode with photoelectric-synergetic catalytic activity; Working electrode and auxiliary electrode are attached to the both sides at middle part of the lower surface of upper cover plate respectively.
Now describe technical scheme of the present invention in detail.A kind of device of measuring chemical oxygen requirement by photoelectric concerted catalysis, by the flow injection sampling system, analysis and detection device and data handling system three parts are formed, the flow injection sampling system comprises the moving phase storage pool, constant current peristaltic pump and microsyringe, analysis and detection device comprises auxiliary electrode 2, contrast electrode 3, induction pipe 4, outlet 5, upper cover plate 6, lower cover 7 and poly tetrafluoroethylene 8, auxiliary electrode 2 is a gold electrode, contrast electrode 3 is saturated calomel electrode or Ag/AgCl electrode, upper cover plate 6 and lower cover 7 are polyfluortetraethylene plate, the middle part of poly tetrafluoroethylene 8 has breach, induction pipe 4 and outlet 5 place the both sides of upper cover plate 6 respectively, contrast electrode 3 places in the outlet 5, poly tetrafluoroethylene 8 is clipped between upper cover plate 6 and the lower cover 7, its middle part breach is a detection cell 11, upper cover plate 6, poly tetrafluoroethylene 8 and lower cover 7 are fixed into one by screw or rivet, data handling system is made of CHI electrochemical workstation and computing machine, induction pipe 4 is communicated with the moving phase storage pool by microsyringe and constant current peristaltic pump, outlet 5 is communicated with waste liquid pool, the electrical signal of auxiliary electrode 2 and contrast electrode 3 is connected by the electric signal input end of cable with the CHI electrochemical workstation, the CHI electrochemical workstation is connected with computing machine by cable, it is characterized in that, described analysis and detection device also comprises working electrode 1, quartz window 9 and ultraviolet source 10, working electrode 1 is the metal oxide modified electrode with photoelectric-synergetic catalytic activity, working electrode 1 and auxiliary electrode 2 are attached to the both sides at middle part of the lower surface of upper cover plate 6 respectively, the electrical signal of working electrode 1 is connected by the electric signal input end of cable with the CHI electrochemical workstation, quartz window 9 is opened on lower cover 7 position over against working electrode 1, ultraviolet source 10 place quartz window 9 under.
Device of the present invention is further characterized in that described constant current peristaltic pump is that model is the digital display constant current peristaltic pump of D100B/C type.
Device of the present invention is further characterized in that described CHI electrochemical workstation is the product of Shanghai occasion China instrument company.
Device of the present invention is further characterized in that working electrode 1 is that substrate is TiO
2PbO
2Electrode.
Device of the present invention is further characterized in that the centre wavelength of ultraviolet source 10 and power are respectively 253nm and 11～35W.
Device of the present invention is further characterized in that, described constant current peristaltic pump is that model is the digital display constant current peristaltic pump of D100B/C type, described CHI electrochemical workstation is the product of Shanghai occasion China instrument company, working electrode 1 is that substrate is the PbO2 electrode of TiO2, and the centre wavelength of ultraviolet source 10 and power are respectively 253nm and 11～35W.
The principle of work of device of the present invention.
The work of device of the present invention is the basis based on the photoelectric-synergetic catalytic theory of metal oxide.See Fig. 4.The working electrode 1 that device of the present invention adopted is that substrate is TiO
2PbO
2Electrode, MO among Fig. 4
xRepresentative is attached to the lip-deep metal oxide with light or electro catalytic activity of working electrode 1.
Open ultraviolet source 10 (253nm, 11～35W) irradiation working electrodes 1 and on this electrode, apply less positive voltage (less than+05V) time, working electrode 1 lip-deep metal oxide with photocatalytic activity can absorb ultraviolet ray and generate photohole (h
+) and light induced electron (e
-), photohole (h
+) can will be adsorbed in photocatalyst surface avtive spot (MO
x[]) on hydrone be oxidized to hydroxyl radical free radical (OH), the organism of hydroxyl radical free radical (OH) in can oxidize water, light-catalyzed reaction mechanism reaction equation described as follows (1) is shown in (2) and (4); Only on this working electrode, apply voltage and be+1.1～+ during the operating potential of 1.5V, hydrone can be adsorbed in electrode active surface site (MO
x[]) on, and decompose generating hydroxyl radical free radical (OH), hydroxyl radical free radical (OH) is the organism in the oxidize water further, and this belongs to electrocatalytic reaction mechanism, and detailed process reaction equation described as follows (3) is shown in (4).
Device of the present invention is being opened ultraviolet source 10 (253nm, on this electrode, apply voltage in the time of 11～35W) irradiation working electrodes 1 and be+1.1～+ operating potential of 1.5V, under this experiment condition, light, electrocatalytic reaction will take place in surface at working electrode 1 simultaneously, the photoelectric-synergetic catalytic reaction promptly takes place, and two kinds of catalytic process can be mutually promoted: at first, on this electrode, apply+1.1～+ operating potential of 1.5V will promote photohole (h
+) and light induced electron (e
-) separation, improve photocatalysis efficiency; Secondly, take place in the time of two kinds of catalytic process to make electrode surface generate more avtive spot, two kinds of catalytic process are all had facilitation.Because the mutually promoting of two kinds of catalytic process realized organic photoelectric-synergetic catalytic oxidation in this electrode pair water body, can be than simple electro-catalysis degrade more efficiently organism in the mineralising water body of the degree of depth and then the sensitivity that improves analysis water-like.
MO
x+hv→h
++e
- (1)
MO
x[]+h
++H
2O→MO
x[·OH]+H
+ (2)
MO
x[]+H
2O→MO
x[·OH]+H
++e
- (3)
MO
x[·OH]+R→MO
x[]+R
·+H
++e
- (4)
In the formula, R represents organism, R
Represent the oxidized oxidation product that obtains of organism.
Compare with electro-catalysis chemical oxygen demand of water body analyser, device of the present invention has following advantage:
Device of the present invention is to carry out the requisite instrument of chemical oxygen demand (COD) that water body is measured in photoelectric-synergetic catalysis, guarantees that organism in the water sample can be degraded efficiently and chemical oxygen demand of water body can be measured quickly and accurately.
Description of drawings
Fig. 1 is the structural representation of electro-catalysis chemical oxygen demand (COD) analyser.
Fig. 2 is the structural representation of analysis and detection device in the electro-catalysis chemical oxygen demand (COD) analyser, among the figure, and the 1st, working electrode, the 2nd, auxiliary electrode, the 3rd, contrast electrode, the 4th, induction pipe, the 5th, outlet, the 6th, upper cover plate, the 7th, lower cover and 8 is poly tetrafluoroethylenes.
Fig. 3 is the structural representation of analysis and detection device in the device of measuring chemical oxygen requirement by photoelectric concerted catalysis, among the figure, and the 9th, quartz window and 10 is ultraviolet sources.
Fig. 4 is photoelectric-synergetic mechanism of catalytic reaction figure.
Embodiment
The device of embodiment 1 measuring chemical oxygen requirement by photoelectric concerted catalysis
Present embodiment is by the flow injection sampling system, analysis and detection device and data handling system three parts are formed, the flow injection sampling system comprises the moving phase storage pool, constant current peristaltic pump and microsyringe, analysis and detection device comprises auxiliary electrode 2, contrast electrode 3, induction pipe 4, outlet 5, upper cover plate 6, lower cover 7 and poly tetrafluoroethylene 8, auxiliary electrode 2 is a gold electrode, contrast electrode 3 is saturated calomel electrode or Ag/AgCl electrode, upper cover plate 6 and lower cover 7 are polyfluortetraethylene plate, the middle part of poly tetrafluoroethylene 8 has breach, induction pipe 4 and outlet 5 place the both sides of upper cover plate 6 respectively, contrast electrode 3 places in the outlet 5, poly tetrafluoroethylene 8 is clipped between upper cover plate 6 and the lower cover 7, its middle part breach is a detection cell 11, upper cover plate 6, poly tetrafluoroethylene 8 and lower cover 7 are fixed into one by screw or rivet, data handling system is made of CHI electrochemical workstation and computing machine, induction pipe 4 is communicated with the moving phase storage pool by microsyringe and constant current peristaltic pump, outlet 5 is communicated with waste liquid pool, the electrical signal of auxiliary electrode 2 and contrast electrode 3 is connected by the electric signal input end of cable with the CHI electrochemical workstation, the CHI electrochemical workstation is connected with computing machine by cable, it is characterized in that, described analysis and detection device also comprises working electrode 1, quartz window 9 and ultraviolet source 10, working electrode 1 is the metal oxide modified electrode with photoelectric-synergetic catalytic activity, working electrode 1 and auxiliary electrode 2 are attached to the both sides at middle part of the lower surface of upper cover plate 6 respectively, the electrical signal of working electrode 1 is connected by the electric signal input end of cable with the CHI electrochemical workstation, quartz window 9 is opened on lower cover 7 position over against working electrode 1, ultraviolet source 10 place quartz window 9 under, wherein: described constant current peristaltic pump is that model is the digital display constant current peristaltic pump of D100B/C type; Described CHI electrochemical workstation is the product of Shanghai occasion China instrument company, and working electrode 1 is that substrate is the PbO2 electrode of TiO2.
Below three devices with embodiment 1 are the embodiment that measure chemical oxygen demand (COD) (COD) value of sewage water sample.
Measure chemical oxygen demand (COD) (COD) value of Shanghai sanitary sewage water sample, measure with international standard IS06066-(E) method, its COD value is 256mg/L.The result who helps photocatalytic method to measure above-mentioned water sample COD value with galvanochemistry and electricity is respectively 235mg/L (replicate determination 7 times, RSD=5.1%) and 241mg/L (replicate determination 7 times, RSD=6.2%), the result who records with international standard IS06066-(E) method compares, and deviation is respectively-8.2% and-5.8%.
When measuring the COD value of above-mentioned water sample with the device of embodiment 1, working electrode 1 is that substrate is TiO
2PbO
2Electrode, the flow velocity of moving phase is 0.5mL/min, the centre wavelength of ultraviolet source 10 and power are respectively 253nm and 11W, apply the operating potential of voltage by the computer starting electrochemical workstation to working electrode 1 for+1.1V, the each sample size of microsyringe is 10 μ L, the linear fit equation of working curve is: Y=0.0198X+1.052, linearly dependent coefficient (R) is 0.9981, and 10 μ L water sample to be measured is injected the Flow Injection Analysis system.
The result who measures above-mentioned water sample COD value with the device of embodiment 1 be 251mg/L (replicate determination 7 times, RSD=3.8%), the result who records with international standard IS06066-(E) method compares, deviation is-2.7%.
Measure chemical oxygen demand (COD) (COD) value of Shanghai brewery sewage water sample, measure with international standard IS06066-(E) method, its COD value is 115mg/L.The result who helps photocatalytic method to measure above-mentioned water sample COD value with galvanochemistry and electricity is respectively 101mg/L (replicate determination 7 times, RSD=3.9%) and 104mg/L (replicate determination 7 times, RSD=5.1%), the result who records with GB IS06066-(E) method compares, and deviation is respectively-11.8% and-9.7%.
Measure the COD value of above-mentioned water sample with the device of embodiment 1, the flow velocity of moving phase is 3.5mL/min, the centre wavelength of ultraviolet source 10 and power are respectively 253nm and 18W, apply the operating potential of voltage by the computer starting electrochemical workstation to working electrode 1 for+1.35V, the each sample size of microsyringe is 35 μ L, the linear fit equation of working curve is: Y=0.0535X+1.896, linearly dependent coefficient (R) is 0.9992, and 35 μ L water sample to be measured is injected the Flow Injection Analysis system.
The result who measures above-mentioned water sample COD value with the device of embodiment 1 be 109mg/L (replicate determination 7 times, RSD=1.8%), the result who records with international standard IS06066-(E) method compares, deviation is-5.2%.
Measure chemical oxygen demand (COD) (COD) value of Shanghai pharmaceutical factory sewage water sample, measure with international standard IS06066-(E) method, its COD value is respectively 495mg/L (replicate determination 7 times for 522mg/L. with the result that galvanochemistry and electricity help photocatalytic method to measure above-mentioned water sample COD value, RSD=4.2%) and 501mg/L (replicate determination 7 times, RSD=3.8%), the result who records with GB IS06066-(E) method compares, deviation be respectively-5.2% and-4.0%.
Measure the COD value of above-mentioned water sample with the device of embodiment 1, the flow velocity of moving phase is 5.0mL/min, the centre wavelength of ultraviolet source 10 and power are respectively 253nm and 35W, apply the operating potential of voltage by the computer starting electrochemical workstation to working electrode 1 for+1.5V, the each sample size of microsyringe is 50 μ L, the linear fit equation of working curve is: Y=0.0629X+1.235, linearly dependent coefficient (R) is 0.9967, and 50 μ L water sample to be measured is injected the Flow Injection Analysis system.
The result who measures above-mentioned water sample COD value with the device of embodiment 1 be 531mg/L (replicate determination 7 times, RSD=2.2%), the result who records with international standard IS06066-(E) method compares, deviation is+1.7%.
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| CN101551351B (en) * | 2009-05-07 | 2012-06-20 | 郑俊褒 | VOCs detection system and detection method based on photocatalysis technology and self-cleaning method thereof |
| CN103674936B (en) * | 2013-12-11 | 2016-05-04 | 常熟理工学院 | A kind of based on electrochemical luminescence COD method for quick and device |
| CN103954671B (en) * | 2014-05-07 | 2016-03-23 | 北京化工大学 | Chemical oxygen demand online monitoring device |
| CN104316581B (en) * | 2014-10-23 | 2016-08-17 | 华南理工大学 | A kind of COD sensor based on visible ray photoelectrocatalysis and its preparation method and application |
| CN105021673B (en) * | 2015-07-02 | 2017-06-27 | 北京师范大学 | A high-throughput electrocatalytic electrode screening and evaluation device |
| CN109052581B (en) * | 2018-09-29 | 2024-02-02 | 四川捷途环保服务有限公司 | Graphene-based small-drainage-basin electrocatalytic degradation system |
| CN113721635A (en) * | 2021-09-14 | 2021-11-30 | 江苏理工学院 | Photoelectrochemistry chlorine salt removing underwater robot |
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