CN106990152A - A kind of sensitive portable light electro-catalysis COD sensor - Google Patents
A kind of sensitive portable light electro-catalysis COD sensor Download PDFInfo
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- CN106990152A CN106990152A CN201710219525.8A CN201710219525A CN106990152A CN 106990152 A CN106990152 A CN 106990152A CN 201710219525 A CN201710219525 A CN 201710219525A CN 106990152 A CN106990152 A CN 106990152A
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- light source
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
Abstract
The invention belongs to environment monitoring device technical field, a kind of sensitive portable light electro-catalysis COD sensor is disclosed.The sensor is made up of light source sleeve pipe, three electrodes suit and volume for the 0.1~1L part of reaction tank three, and light source sleeve pipe and three electrodes suit are inserted vertically into reaction tank；LED uviol lamps are set in the light source sleeve pipe and set transparent window to be used for printing opacity in side；Three ducts are set to insert reference electrode, the TiO to electrode and hydrogenation respectively in the three electrodes suit2Nano-array thin film working electrode, the duct side of working electrode opens up reacting hole, and reacting hole is just right with the transparent window on light source sleeve pipe.TiO of the present invention to hydrogenate2Nano-array is light source as photochemical catalyst, built-in LED uviol lamps, has the advantages that photoelectric respone is strong, photo-generated carrier recombination rate is low and transfer velocity is fast.And built-in ultraviolet source small volume, it is easy to carry, it is to avoid damage of the ultraviolet source to operator.
Description
Technical field
The invention belongs to environment monitoring device technical field, and in particular to a kind of sensitive portable light electro-catalysis chemistry is needed
Oxygen amount sensor.
Background technology
Water resource is the indispensable part of nature, is the origin of life of all species of world and the weight depended on for existence
Will basis.China is one of country of water resource famine on the earth, although fresh water is abundant, but occupancy volume per person is less than
The a quarter of world average level.Since 20th century, due to the continuous growth and urbanization, industrialized fast of China human mortality
Exhibition is hailed, constantly having sanitary sewage and industrial wastewater to be drained into, river is marine, and substantial amounts of nutrient and organic pollution cause
Planktonic organism drastically breeds in water body, causes water quality severe contamination and deterioration, so as to cause ecological balanced system to destroy.Particularly
Pearl River Delta and Yangtze River Delta Area, the density of population is big, industrial development is rapid, so as to cause water resource pollution especially serious, has given people
Once serious warning, obtain unprecedented concern the problem of water quality monitoring.COD (COD) is to use chemical oxidation
Method determines the amount of reducing substances in water sample.The amount for the oxidant that every liter of water sample is consumed is converted to the quality of the oxygen of needs,
In units of mg/L, water body degree polluted by organic matter can be reflected, be an important water quality index in wastewater treatment, be water
The project of most conventional determining in analysis is surveyed in quality supervision.Fortune in river pollution and industrial wastewater Quality Research and waste water treatment plant
In row management, it is a physical quantity that is important and can comparatively fast determining.Current conventional determining COD method mainly has height
Potassium manganate method or potassium dichromate method.But it is numerous that these above-mentioned methods generally require substantial amounts of experimental drug, process in operation
It is trivial, it is time-consuming and be also possible to cause secondary pollution to environment.In recent years, to solve the above problems, there has been proposed many COD measure
New method, such as chemiluminescence, Flow Injection Technique, Ozonation, electrochemical process, photocatalytic method and photoelectrocatalysioxidization oxidization
Method etc..Because photocatalysis can be carried out at normal temperatures and pressures, secondary pollution is not produced, and equipment is simple, catalyst can be returned
Receive and reuse.At present, photocatalytic method is always the focus of water process research.
Organic substance in water is while photocatalyst surface is aoxidized by hydroxyl radical free radical, some reactants in reaction system
The concentration of (electronics capturing agent) or product will change, and according to the change of these material concentrations, just can measure COD in water
Content.Based on this principle, develop some new photochemical catalytic oxidation systems to determine COD.Zhang Shanqing et al.
(Sensors and Actuators:B Chemical,2009,141(2):634) TiO is grown on ITO2Film is urged as light
Polarizing electrode, this portable, electrode material with low cost and environmentally friendly can be used for COD detections, with quick, efficiently
And it is accurate the characteristics of.TiO2Electrode is the key factor that photoelectrocatalysioxidization oxidization method determines COD.Etc., which is protected, with the Later Zhou Dynasty, one of the Five Dynasties has invented one kind
Short TiO2The preparation method (CN101509886A) of nano-tube array photoelectrocatalysis COD sensor, due to nanotube with
The adhesion of substrate is strong, and photogenerated charge is combined low, and transmission is fast, be conducive to improving the stability of titanium-based nano pipe sensor array,
Working life and PhotoelectrocatalytiPerformance Performance, thus be conducive to improving the stability and reappearance of assay method.Due to TiO2Only in purple
There is response under outer light, ultraviolet light has certain radiation injury to human body as excitation source, in operation ultraviolet light.Zhang Sheng
It is gloomy etc. to disclose a kind of TiO of hydrogenation2Nanometer stick array is applied to the preparation of visible ray photoelectrocatalysis COD sensor
Method (ZL201410570773.3), detection COD scope is 0~300mg/L.But the TiO hydrogenated under visible light2To one
The organic matter of a little difficult degradations is unable to permineralization, and the error of generation can be than larger.Current photoelectrocatalysioxidization oxidization method determines COD light
Source is all placed in outside photocell, and the light source of this external is typically necessary large-scale light source generator and provided, such as xenon lamp, this
Sample can cause most luminous energy to be wasted, and the ultraviolet light that xenon lamp is sent in operation has certain radiation to damage to human body
Wound.Moreover, being especially unsuitable for field work by the use of large-scale xenon lamp as light source.
The content of the invention
In place of shortcoming and defect in order to solve above prior art, primary and foremost purpose of the invention is to provide a kind of sensitive
Portable light electro-catalysis COD sensor.
Another object of the present invention is to provide above-mentioned sensitive portable light electro-catalysis COD sensor in water
Application in middle COD detections.
The object of the invention is achieved through the following technical solutions：
A kind of sensitive portable light electro-catalysis COD sensor, by light source sleeve pipe, three electrodes suit and volume
Constituted for the 0.1~1L part of reaction tank three, light source sleeve pipe and three electrodes suit are inserted vertically into reaction tank；The light source sleeve pipe
Interior setting LED uviol lamps, and at LED uviol lamps light source sleeve pipe side set transparent window be used for printing opacity；Three electrode
Three ducts are set to insert Ag/AgCl reference electrodes, Pt respectively to electrode and the TiO of hydrogenation in suit2Nano-array film work
Make electrode, wherein reference electrode and the duct bottom to electrode is not closed, the duct bottom lock of working electrode is simultaneously opened in side
If reacting hole, the reacting hole and the transparent window on light source sleeve pipe of working electrode duct side are just right.
Further, reaction tank lid is set on the reaction tank, and reaction tank covers two openings of setting and inserts light source respectively
Sleeve pipe and three electrodes are set with and fixed.
Preferably, the light source sleeve pipe is prepared using aluminium, and the transparent window material of the light source sleeve pipe side is quartz.
Preferably, the light wave that the LED uviol lamps are sent be 280~400nm, rated voltage be 2~6V, power be 2~
20W。
Preferably, the reacting hole of working electrode duct side is a diameter of 5~15mm circular hole.
Preferably, the transparent window distance on the reacting hole of working electrode duct side and light source sleeve pipe for 5~
15mm。
Preferably, the TiO of the hydrogenation2Nano-array film is by by TiO2Nano-stick array thin film is in hydrogen atmosphere
High temperature hydrogenation is obtained.
Preferably, described hydrogen atmosphere refers to containing the mixed of the hydrogen and inert gas that volume fraction is 10%~50%
Atmosphere is closed, the temperature of the high temperature hydrogenation is 300~700 DEG C.
Preferably, the TiO2Nano-stick array thin film is by the way that substrate to be put into the water containing butyl titanate and hydrochloric acid
In solution, prepared (specific preparation method refers to patent 201410570773.3 or corresponding document) through hydro-thermal reaction；
The substrate is the SnO of doping fluorine2Electro-conductive glass (FTO), indium tin oxide-coated glass (ITO) or metal titanium sheet.
Preferably, the TiO of the hydrogenation2TiO in nano-array film2The length of nano-array is 100~2000nm.
Application of the above-mentioned sensitive portable light electro-catalysis COD sensor in water in COD detections, specifically should
It is with process：Water sample solution is injected in reaction tank, addition inorganic salts are electrolyte, and three electrodes during three electrodes are set with connect
Electrochemical workstation is connect, is biased on the working electrode (s, while opening LED uviol lamps and adjusting its intensity, ultraviolet light
In the TiO of hydrogenation2On nano-array film, by the change of electrochemical signals during organic matter photoelectrocatalysioxidization oxidization, it is determined that
COD value in water sample.
Relative to prior art, the invention has the advantages that and beneficial effect：
(1) TiO of the present invention to hydrogenate2Nano-array is as photochemical catalyst, with unhydrided TiO2Nano-array sensor
Compare, have the advantages that photoelectric respone is strong, photo-generated carrier recombination rate is low and transfer velocity is fast, be conducive to improving TiO2Nanometer battle array
The PhotoelectrocatalytiPerformance Performance and detection range of sensor；
(2) present invention constitutes portable light electrocatalytic chemical oxygen demand (COD) sensor, built-in ultraviolet source body with built-in LED uviol lamps
Small, TiO of the light source relative to hydrogenation of product2The distance of nano-array film catalyst is short, and photoelectric respone is strong, facilitates sensor
Field work, and avoid damage of the ultraviolet source to operator.
Brief description of the drawings
Fig. 1 is the structural representation of the portable light electro-catalysis COD sensor of the embodiment of the present invention.
Fig. 2 regards for the top that three electrodes in the portable light electro-catalysis COD sensor of the embodiment of the present invention are set with
Scheme (A) and bottom view (B).
Fig. 3 inserts work in being set with for the electrode of portable light electro-catalysis COD sensor three of the embodiment of the present invention
The duct cross-sectional view (C) and insertion reference electrode, the duct cross-sectional view (D) to electrode of electrode.
Numbering is described as follows in Fig. 1~3：The electrodes of 1- tri- are set with, 2- reference electrodes, and 3- is to electrode, 4- working electrodes, 5- aluminium
Light source sleeve pipe processed, 6- light source controllers, 7-LED uviol lamps, 8- quartz transparent windows, the circular hole of 9- working electrodes duct side,
10- reaction tank lids, 11- reaction tanks.
Fig. 4 and Fig. 5 are the TiO of hydrogenation prepared by the embodiment of the present invention2The field emission scanning electron microscope figure of nano-array film
(FESEM) front elevation and side view.
Fig. 6 determines the glucose of various concentrations for the portable light electro-catalysis COD sensor of the embodiment of the present invention
The photocurrent response figure of solution.
It is molten that Fig. 7 determines different glucose for the portable light electro-catalysis COD sensor of the embodiment of the present invention
COD relation curve in the photoelectric current value added and solution of liquid.
Fig. 8 is TiO in the embodiment of the present invention2Photocurrent response comparison diagram before and after the hydrogenation of nano-array film.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.
Embodiment
A kind of portable light electro-catalysis COD sensor of the present embodiment, the institute of its structural representation such as Fig. 1~3
Show.The portable light electro-catalysis COD sensor is by aluminum light source sleeve pipe 5, three electrodes suit 1 and reaction tank 11 3
Part is constituted, and the internal diameter of reaction tank size is 44mm, and external diameter is 50mm, a height of 70mm.Set reaction tank lid 10 (interior on reaction tank
Footpath is 50mm, and external diameter is 56mm), reaction tank covers two semicircle orifices of setting, and size can just be adapted to fixed light source sleeve pipe
With three electrodes suit, light source sleeve pipe and three electrodes suit are all two semicircle orifices that are up big and down small, being covered respectively by reaction tank
It is stable to be inserted vertically into reaction tank.LED uviol lamps 7 are set simultaneously to be connected to light source controller 6 in the light source sleeve pipe, available for controlling
Light intensity output processed；Light source sleeve pipe side at LED uviol lamps sets quartzy transparent window 8 to be used for printing opacity；The three electrodes suit
It is made up of polytetrafluoroethylmaterial material, sets three ducts to insert Ag/AgCl reference electrodes 2, Pt respectively to electricity in three electrodes suit
Pole 3 and the TiO of hydrogenation2Nano-array thin film working electrode 4, wherein reference electrode and the duct bottom to electrode are not closed, work
Make the duct bottom lock of electrode and open up circular hole 9 (Circularhole diameter is 10mm), the circular hole 9 of working electrode duct side in side
With the transparent window 8 on light source sleeve pipe just to (distance is 5mm).
" the TiO of hydrogenation in the present embodiment2Nano-array film " is prepared via a method which：
1)TiO2The preparation of nanometer stick array
(1) by FTO electro-conductive glass successively successively in deionized water, acetone and ethanol solution ultrasound 30 minutes, through go from
Sub- water is cleaned, and is dried up standby；
(2) precursor solution of titanium source is prepared：First by 30ml concentrated hydrochloric acids (mass concentration is 37.5%) and 30ml go from
Sub- water mixing, stirring adds l ml butyl titanates and continues stirring 5 minutes after 5 minutes, obtain titanium source precursor solution；
(3) conducting surface of FTO electro-conductive glass is placed in reactor obliquely, titanium source precursor solution is added, at 150 DEG C
Under the conditions of Hydrothermal Synthesiss 7 hours, prepare TiO2Nanometer stick array, deionized water is washed, and is dried at 80 DEG C.
2)TiO2The hydrogenation of nanometer stick array, hydrogen atmosphere is the mixed gas of hydrogen argon gas.The flow velocity of hydrogen is
20SCCM, the flow velocity of argon gas is 80SCCM, and hydrogenation temperature is 350 DEG C, and hydrogenation time is 1h.The TiO hydrogenated2Nano-array
Film.
The TiO of gained hydrogenation2The front elevation and side view of the field emission scanning electron microscope figure (FESEM) of nano-array film point
Not as shown in Figure 4 and Figure 5.ESEM uses LEO 1530VP/Inca 300, and accelerating potential is 5KV.By Fig. 4 and Fig. 5 results
It can be seen that, the TiO of hydrogenation2The rod footpath of nanometer stick array is about 130nm, and rod length is about 1.7 μm.
Application of the portable light electro-catalysis COD sensor of the present embodiment in water in COD detections, specifically should
It is with process：Water sample solution is injected in reaction tank, addition inorganic salts are electrolyte, and three electrodes during three electrodes are set with connect
Electrochemical workstation is connect, is biased on the working electrode (s, while opening LED uviol lamps and its is strong by light-source controller controls
(light intensity at 365nm is 5mW/cm to degree2), TiO of the ultraviolet light in hydrogenation2It is 0.9V's in bias on nano-array film
Under the conditions of determine water body in COD, by the change of electrochemical signals during organic matter photoelectrocatalysioxidization oxidization, determine in water sample
COD value.Photoelectric current during the fully visible smooth photoelectrocatalysioxidization oxidization of one organic matter of each COD standard liquids correspondence.Fig. 6
For the photocurrent response figure (a for the glucose solution for determining various concentrations:0mg/L COD, b:3.84mg/L COD, c:19.2mg/
L COD, d:38.4mg/L COD, e:76.8mg/L COD, f:153.6mg/L COD, j:307.3mg/L COD, h:
307.2mg/L COD, i:614.4mg/L COD).The corresponding photocurrent values of difference concentration of glucose are calculated when taking 35 seconds,
Obtain the relation curve (such as Fig. 7) of COD in photoelectric current value added and solution, in the range of 0~460mg/L, photoelectric current
The COD value of the solution of value added and glucose is linear, working curve coefficient R2=0.9945.In identical work
Under curve, 3 certain sanitary wastewater COD values of parallel determination are 152mg/L, and the sanitary wastewater is measured with potassium dichromate standard method
COD value is 155mg/L.Use the COD value that the present embodiment sensor determines the 50mg/L malonic acid aqueous solution for 31.6mg/L, be somebody's turn to do
The theoretical COD of the standard malonic acid aqueous solution is 30.8mg/L.
The present invention compared for the TiO before and after hydrogenation2The photocurrent response of nano-array film, as a result as shown in Figure 8.In phase
With under conditions of, the TiO after hydrogenation2The photocurrent response of nanometer stick array is 2.2 times not hydrogenated, and is illustrated after hydrogenation
Film has the advantages that strong photoelectric respone, photo-generated carrier recombination rate are low and transfer velocity is fast, is conducive to improving TiO2Nanometer
The PhotoelectrocatalytiPerformance Performance and detection range of sensor array.Under the same terms, with the TiO without hydrogenation2Nano-array film enters
COD relation curves in water-filling solution, its range of linearity only has 0~260mg/L, working curve coefficient R2=0.9853.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of sensitive portable light electro-catalysis COD sensor, it is characterised in that：The sensor is by light source set
Pipe, three electrodes suit and the part of reaction tank three composition that volume is 0.1~1L, light source sleeve pipe and three electrodes suit are inserted vertically into anti-
In Ying Chi；LED uviol lamps, and the light source sleeve pipe side setting transparent window at LED uviol lamps are set in the light source sleeve pipe
For printing opacity；Three ducts are set to insert Ag/AgCl reference electrodes, Pt respectively to electrode and hydrogenation in three electrode suit
TiO2Nano-array thin film working electrode, wherein reference electrode and the duct bottom to electrode are not closed, the duct of working electrode
The transparent window of bottom lock simultaneously on reacting hole, the reacting hole and light source sleeve pipe of working electrode duct side is opened up sideways is just
It is right.
2. a kind of sensitive portable light electro-catalysis COD sensor according to claim 1, it is characterised in that：
Reaction tank lid is set on the reaction tank, and reaction tank covers two openings of setting, and insertion light source sleeve pipe and three electrodes are set with simultaneously respectively
It is fixed.
3. a kind of sensitive portable light electro-catalysis COD sensor according to claim 1, it is characterised in that：
The light source sleeve pipe is prepared using aluminium, and the transparent window material of the light source sleeve pipe side is quartz.
4. a kind of sensitive portable light electro-catalysis COD sensor according to claim 1, it is characterised in that：
The light wave that the LED uviol lamps are sent is 280~400nm, and rated voltage is 2~6V, and power is 2~20W.
5. a kind of sensitive portable light electro-catalysis COD sensor according to claim 1, it is characterised in that：
The reacting hole of working electrode duct side is a diameter of 5~15mm circular hole.
6. a kind of sensitive portable light electro-catalysis COD sensor according to claim 1, it is characterised in that：
The reacting hole of working electrode duct side is 5~15mm with the transparent window distance on light source sleeve pipe.
7. a kind of sensitive portable light electro-catalysis COD sensor according to claim 1, it is characterised in that：
The TiO of the hydrogenation2Nano-array film is by by TiO2Nano-stick array thin film is hydrogenated in hydrogen atmosphere and obtained；It is described
Hydrogen atmosphere refer to containing volume fraction for 10%~50% hydrogen and inert gas mixed atmosphere, the temperature of the hydrogenation
Spend for 300~700 DEG C.
8. a kind of sensitive portable light electro-catalysis COD sensor according to claim 7, it is characterised in that：
The TiO2Nano-stick array thin film be by the way that substrate is put into the aqueous solution containing butyl titanate and hydrochloric acid, it is anti-through hydro-thermal
It should prepare；The substrate is FTO, ITO or metal titanium sheet.
9. a kind of sensitive portable light electro-catalysis COD sensor according to claim 1, it is characterised in that：
The TiO of the hydrogenation2TiO in nano-array film2The length of nano-array is 100~2000nm.
10. a kind of sensitive portable light electro-catalysis COD sensor described in any one of claim 1~9 is in water
Application in COD detections, it is characterised in that concrete application process is：Water sample solution is injected in reaction tank, adding inorganic salts is
Electrolyte, three electrodes during three electrodes are set with connect electrochemical workstation, are biased on the working electrode (s, open simultaneously
LED uviol lamps simultaneously adjust its intensity, TiO of the ultraviolet light in hydrogenation2On nano-array film, pass through organic matter photoelectrocatalysis
The change of electrochemical signals in oxidizing process, determines the COD value in water sample.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107910392A (en) * | 2017-11-20 | 2018-04-13 | 中国石油大学(华东) | Broadband photodetector based on hydrogenation titanic oxide nanorod array/silicon heterogenous and preparation method thereof |
| CN109999743A (en) * | 2019-04-22 | 2019-07-12 | 西安交通大学 | A kind of experimental provision and experimental method of electrical enhanced photocatalysis carbon dioxide methanol |
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| CN104316581A (en) * | 2014-10-23 | 2015-01-28 | 华南理工大学 | Visible light photoelectrocatalysis based COD (chemical oxygen demand) sensor and preparation method and application thereof |
| CN106153696A (en) * | 2014-11-05 | 2016-11-23 | 朝阳科技大学 | chemical oxygen demand detection device |
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| CN1774627A (en) * | 2003-04-04 | 2006-05-17 | 水体检测有限公司 | Photoelectrochemical determination of chemical oxygen demand |
| CN1721056A (en) * | 2005-05-26 | 2006-01-18 | 上海交通大学 | Photoelectrocatalytic thin-layered minisize reactor |
| CN102866186A (en) * | 2012-09-12 | 2013-01-09 | 合肥工业大学 | Circulating-type water chemical oxygen demand detection photoelectrochemical sensor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107910392A (en) * | 2017-11-20 | 2018-04-13 | 中国石油大学(华东) | Broadband photodetector based on hydrogenation titanic oxide nanorod array/silicon heterogenous and preparation method thereof |
| CN109999743A (en) * | 2019-04-22 | 2019-07-12 | 西安交通大学 | A kind of experimental provision and experimental method of electrical enhanced photocatalysis carbon dioxide methanol |
| CN109999743B (en) * | 2019-04-22 | 2024-04-09 | 西安交通大学 | Experimental device and experimental method for preparing methanol by photoelectrically and cooperatively catalyzing carbon dioxide |
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