CN106990152B - 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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- CN106990152B CN106990152B CN201710219525.8A CN201710219525A CN106990152B CN 106990152 B CN106990152 B CN 106990152B CN 201710219525 A CN201710219525 A CN 201710219525A CN 106990152 B CN106990152 B CN 106990152B
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Abstract
The invention belongs to environment monitoring device technical fields, disclose a kind of sensitive portable light electro-catalysis COD sensor.The sensor is made of the reaction tank three parts that light source casing, three electrodes suit and volume are 0.1~1L, and light source casing and three electrodes suit are inserted vertically into reaction tank；LED ultraviolet lamp is set in the light source casing and is used for light transmission in side setting transparent window；Reference electrode is inserted into, to the TiO of electrode and hydrogenation in three ducts of setting respectively in the three electrodes suit2Nano-array thin film working electrode, the duct side of working electrode open up reacting hole, the transparent window face on reacting hole and light source casing.TiO of the present invention to hydrogenate2Nano-array is light source as photochemical catalyst, built-in LED ultraviolet lamp, 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 is small in size, and it is easy to carry, avoid damage of the ultraviolet source to operator.
Description
Technical field
The invention belongs to environment monitoring device technical fields, and in particular to a kind of sensitive portable light electro-catalysis chemistry need
Oxygen amount sensor.
Background technique
Water resource is the indispensable part of nature, is the origin of life of all species and the weight depended on for existence in the world
Want basis.China be on the earth water resource there is a serious shortage of one of country, 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 of China human mortality and urbanization, industrialized fast
Exhibition is hailed, constantly having sanitary sewage and industrial wastewater to be drained into, river is marine, and a large amount of nutrient and organic pollutant cause
Planktonic organism sharply breeds in water body, and water quality is caused seriously to pollute and deteriorate, so as to cause ecological balanced system destruction.Especially
Pearl River Delta and Yangtze River Delta Area, the density of population is big, industrial development is rapid, to cause water resource pollution especially serious, has given people
Primary serious warning, the problem of water quality monitoring obtain unprecedented concern.COD (COD) is to use chemical oxidation
Method measures the amount of reducing substances in water sample.The amount of oxidant consumed by every liter of water sample is converted to the quality of the oxygen of needs,
It as unit of mg/L, can reflect the degree that water body is polluted by organic matter, be an important water quality indicator 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 measuring.The method of conventional determining COD mainly has height at present
Potassium manganate method or potassium dichromate method.But it is numerous that these above-mentioned methods generally require a large amount 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 measurements
New method, such as chemiluminescence, Flow Injection Technique, Ozonation, electrochemical process, photocatalytic method and photoelectrocatalysioxidization oxidization
Method etc..Since photocatalysis can carry out at normal temperatures and pressures, secondary pollution is not generated, and equipment is simple, catalyst can return
It receives and reuses.Currently, photocatalytic method is always the hot spot 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 variation of these material concentrations, can measure COD in water
Content.Based on this principle, some new photochemical catalytic oxidation systems have been developed to measure COD.Zhang Shanqing et al.
(Sensors and Actuators:B Chemical, 2009,141 (2): 634) grows TiO on ITO2Film is urged as light
Polarizing electrode, this portable, electrode material low in cost and environmentally friendly can be used for COD detection, have quickly, efficiently
With accurate feature.TiO2Electrode is the key factor of photoelectrocatalysioxidization oxidization method measurement 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 binding force of substrate is strong, and photogenerated charge is compound low, and transmission is fast, be conducive to improve the stability of titanium-based nano pipe sensor array,
Working life and PhotoelectrocatalytiPerformance Performance, thus be conducive to improve the stability and reproducibility of measuring method.Due to TiO2Only in purple
There is response under outer light, ultraviolet light is as excitation light source, and ultraviolet light has certain radiation injury to human body in operation.Zhang Sheng
It is gloomy etc. to disclose a kind of TiO of hydrogenation2Nanometer stick array is applied to the preparation of visible light photoelectrocatalysis COD sensor
Method (ZL201410570773.3), the range for detecting COD is 0~300mg/L.But the TiO hydrogenated under visible light2To one
A little organic matters difficult to degrade are unable to permineralization, and the error of generation can be bigger.The light of the COD of photoelectrocatalysioxidization oxidization method measurement at present
Source is all placed in except photocell, and the light source of this external is typically necessary large-scale light source generator and provides, such as xenon lamp, this
Sample will lead to most luminous energy and be wasted, and the ultraviolet light that xenon lamp issues in operation has certain radiation to damage human body
Wound.Moreover, being especially unsuitable for field work as light source using large-scale xenon lamp.
Summary of the invention
In order to solve the disadvantage that the above prior art and shortcoming, the primary purpose of the present invention is that providing 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 sensors in water
Application in middle COD detection.
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 casing, three electrodes suit and volume
It is constituted for the reaction tank three parts of 0.1~1L, light source casing and three electrodes suit are inserted vertically into reaction tank；The light source casing
Interior setting LED ultraviolet lamp, and the light source casing side setting transparent window at LED ultraviolet lamp is used for light transmission；Three electrode
Ag/AgCl reference electrode, Pt are inserted into the TiO of electrode and hydrogenation in three ducts of setting respectively in suit2Nano-array film work
Make electrode, reference electrode and the duct bottom of electrode is not closed wherein, the duct bottom of working electrode, which is closed, simultaneously opens in side
If reacting hole, the reacting hole of working electrode duct side and the transparent window face on light source casing.
Further, reaction tank lid is set on the reaction tank, and reaction tank covers two openings of setting and is inserted into light source respectively
Casing and three electrodes are set with and fix.
Preferably, the light source casing is prepared using aluminium, and the transparent window material of light source casing side is quartz.
Preferably, the light wave that the LED ultraviolet lamp issues is 280~400nm, and voltage rating is 2~6V, power is 2~
20W。
Preferably, the reacting hole of working electrode duct side is the circular hole that diameter is 5~15mm.
Preferably, the transparent window distance on the reacting hole Yu light source casing of working electrode duct side 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 hydrogenates to obtain.
Preferably, the hydrogen atmosphere refer to containing volume fraction be 10%~50% hydrogen and inert gas it is mixed
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, (specific preparation method can refer to patent 201410570773.3 or corresponding document) is prepared through hydro-thermal reaction；
The substrate is to adulterate the SnO of 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.
Above-mentioned sensitive portable light electro-catalysis COD sensor in water COD detection in application, specifically answer
With process are as follows: inject water sample solution in reaction tank, addition inorganic salts are electrolyte, and three electrodes in three electrodes suit are connected
Electrochemical workstation is connect, is biased on the working electrode (s, LED ultraviolet lamp is opened simultaneously and adjusts its intensity, ultraviolet light
In the TiO of hydrogenation2On nano-array film, by the variation of electrochemical signals during organic matter photoelectrocatalysioxidization oxidization, determine
COD value in water sample.
Compared with the existing technology, the invention has the following advantages and beneficial effects:
(1) TiO of the present invention to hydrogenate2Nano-array is as photochemical catalyst, with unhydrided TiO2Nano-array sensor
It compares, has the advantages that photoelectric respone is strong, photo-generated carrier recombination rate is low and transfer velocity is fast, be conducive to improve TiO2Nanometer battle array
The PhotoelectrocatalytiPerformance Performance and detection range of sensor；
(2) present invention forms portable light electrocatalytic chemical oxygen demand (COD) sensor, built-in ultraviolet source body with built-in LED ultraviolet lamp
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.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the portable light electro-catalysis COD sensor of the embodiment of the present invention.
Fig. 2 is the top view of three electrodes suit in the portable light electro-catalysis COD sensor of the embodiment of the present invention
Scheme (A) and bottom view (B).
Fig. 3 is to be inserted into work during three electrode of portable light electro-catalysis COD sensor of the embodiment of the present invention is set with
The duct the schematic diagram of the section structure (C) and insertion reference electrode, the duct the schematic diagram of the section structure (D) to electrode of electrode.
Number is described as follows in Fig. 1~3: tri- electrode of 1- suit, 2- reference electrode, 3- is to electrode, 4- working electrode, 5- aluminium
Light source casing processed, 6- light source controller, 7-LED ultraviolet lamp, 8- quartz transparent window, the circular hole of 9- working electrode duct side,
10- reaction tank lid, 11- reaction tank.
Fig. 4 and Fig. 5 is the TiO of the hydrogenation of preparation of the embodiment of the present invention2The field emission scanning electron microscope figure of nano-array film
(FESEM) front elevation and side view.
Fig. 6 is that the portable light electro-catalysis COD sensor of the embodiment of the present invention measures the glucose of various concentration
The photocurrent response figure of solution.
Fig. 7 is that the portable light electro-catalysis COD sensor measurement different glucose of the embodiment of the present invention is molten
The relation curve of COD in the photoelectric current value added and solution of liquid.
Fig. 8 is TiO in the embodiment of the present invention2The photocurrent response comparison diagram of nano-array film hydrogenation front and back.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment
A kind of portable light electro-catalysis COD sensor of the present embodiment, structural schematic diagram such as Fig. 1~3 institute
Show.The portable light electro-catalysis COD sensor is by aluminum light source casing 5, three electrodes suit 1 and reaction tank 11 3
Part is constituted, and the internal diameter of reaction tank size is 44mm, outer diameter 50mm, a height of 70mm.It is (interior that reaction tank lid 10 is set on reaction tank
Diameter is 50mm, outer diameter 56mm), reaction tank covers two semicircle orifices of setting, and size can just be suitble to fixed light source casing
It is set with three electrodes, light source casing and three electrodes suit are all two semicircle orifices that are up big and down small, being covered respectively by reaction tank
Stabilization is inserted vertically into reaction tank.LED ultraviolet lamp 7 is set in the light source casing and is connected to light source controller 6, can be used for controlling
Light intensity output processed；Light source casing side at LED ultraviolet lamp is arranged quartzy transparent window 8 and is used for light transmission；The three electrodes suit
It is made of polytetrafluoroethylene material, Ag/AgCl reference electrode 2, Pt are inserted into electricity in three ducts of setting respectively in three electrodes suit
The TiO of pole 3 and hydrogenation2Nano-array thin film working electrode 4 reference electrode and is not closed the duct bottom of electrode, work wherein
It closes and opens up circular hole 9 (Circularhole diameter 10mm), the circular hole 9 of working electrode duct side in side in the duct bottom for making electrode
With 8 face of transparent window on light source casing (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, gone from
Sub- water is cleaned, and is dried up spare；
(2) prepare the precursor solution of titanium source: first by 30ml concentrated hydrochloric acid (mass concentration 37.5%) and 30ml go from
Sub- water mixing is added l ml butyl titanate and continues stirring 5 minutes, obtains titanium source precursor solution after stirring 5 minutes；
(3) conducting surface of FTO electro-conductive glass is placed in reaction kettle obliquely, titanium source precursor solution is added, at 150 DEG C
Under the conditions of hydrothermal synthesis 7 hours, prepare TiO2Nanometer stick array, deionized water are washed, dry at 80 DEG C.
2)TiO2The hydrogenation of nanometer stick array, hydrogen atmosphere are the mixed gas of hydrogen argon gas.The flow velocity of hydrogen is
20SCCM, the flow velocity of argon gas are 80SCCM, and hydrogenation temperature is 350 DEG C, hydrogenation time 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 not as shown in Figure 4 and Figure 5.Scanning electron microscope uses LEO 1530VP/Inca 300, acceleration voltage 5KV.By Fig. 4 and Fig. 5 result
As it can be seen that the TiO of hydrogenation2The stick diameter of nanometer stick array is about 130nm, and stick is about 1.7 μm long.
The portable light electro-catalysis COD sensor of the present embodiment in water COD detection in application, specifically answer
With process are as follows: inject water sample solution in reaction tank, addition inorganic salts are electrolyte, and three electrodes in three electrodes suit are connected
Electrochemical workstation is connect, is biased on the working electrode (s, LED ultraviolet lamp is opened simultaneously and it 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 measure water body in COD determined in water sample by the variation of electrochemical signals during organic matter photoelectrocatalysioxidization oxidization
COD value.Photoelectric current when the fully visible smooth photoelectrocatalysioxidization oxidization of the corresponding organic matter of each COD standard solution.Fig. 6
For photocurrent response figure (a:0mg/L COD, the b:3.84mg/L COD, c:19.2mg/ of the glucose solution of measurement various concentration
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, being measured in parallel 3 certain sanitary wastewater COD values is 152mg/L, measures the sanitary wastewater with potassium dichromate standard method
COD value is 155mg/L.Use the COD value of the malonic acid aqueous solution of the present embodiment sensor measurement 50mg/L for 31.6mg/L, it should
The theoretical COD of standard malonic acid aqueous solution is 30.8mg/L.
The present invention compared the TiO of hydrogenation front and back2The 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, after illustrating hydrogenation
Film has the advantages that strong photoelectric respone, photo-generated carrier recombination rate are low and transfer velocity is fast, is conducive to improve TiO2Nanometer
The PhotoelectrocatalytiPerformance Performance and detection range of sensor array.Under the same terms, with the TiO not hydrogenated2Nano-array film into
COD relation curve in row aqueous solution, the range of linearity only have 0~260mg/L, working curve coefficient R2=0.9853.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (7)
1. a kind of application in COD detection in water of sensitive portable light electro-catalysis COD sensor, feature exists
In: the sensor is made of the reaction tank three parts that light source casing, three electrodes suit and volume are 0.1~1L, light source casing
It is inserted vertically into reaction tank with three electrodes suit；LED ultraviolet lamp, and the light at LED ultraviolet lamp are set in the light source casing
Source casing side is arranged transparent window and is used for light transmission；Ag/AgCl ginseng is inserted into three ducts of setting respectively in the three electrodes suit
Than electrode, Pt to the TiO of electrode and hydrogenation2Nano-array thin film working electrode, wherein reference electrode and the duct bottom to electrode
Portion does not close, and the closing of the duct bottom of working electrode simultaneously opens up reacting hole in side, the reacting hole of working electrode duct side with
Transparent window face on light source casing；The application process are as follows: water sample solution is injected in reaction tank, it is electricity that inorganic salts, which are added,
Three electrodes in three electrodes suit are connected electrochemical workstation, are biased, open simultaneously on the working electrode (s by Xie Zhi
LED ultraviolet lamp simultaneously adjusts its intensity, TiO of the ultraviolet light in hydrogenation2On nano-array film, pass through organic matter photoelectrocatalysis
The variation of electrochemical signals in oxidation process, determines the COD value in water sample；
The TiO of the hydrogenation2Nano-array film is by by TiO2Nano-stick array thin film is hydrogenated in hydrogen atmosphere and is obtained；
The hydrogen atmosphere refers to the mixed atmosphere of the hydrogen and inert gas that are 10%~50% containing volume fraction, the hydrogenation
Temperature be 300~700 DEG C；
The TiO2Nano-stick array thin film is by being put into substrate in the aqueous solution containing butyl titanate and hydrochloric acid, through water
Thermal response is prepared；The substrate is FTO, ITO or metal titanium sheet.
2. COD is examined a kind of sensitive portable light electro-catalysis COD sensor according to claim 1 in water
Application in survey, it is characterised in that: reaction tank lid is set on the reaction tank, and reaction tank covers two openings of setting and is inserted into respectively
Light source casing and three electrodes are set with and fix.
3. COD is examined a kind of sensitive portable light electro-catalysis COD sensor according to claim 1 in water
Application in survey, it is characterised in that: the light source casing is prepared using aluminium, the transparent window material of light source casing side
For quartz.
4. COD is examined a kind of sensitive portable light electro-catalysis COD sensor according to claim 1 in water
Application in survey, it is characterised in that: the light wave that the LED ultraviolet lamp issues is 280~400nm, and voltage rating is 2~6V, function
Rate is 2~20W.
5. COD is examined a kind of sensitive portable light electro-catalysis COD sensor according to claim 1 in water
Application in survey, it is characterised in that: the reacting hole of working electrode duct side is the circular hole that diameter is 5~15mm.
6. COD is examined a kind of sensitive portable light electro-catalysis COD sensor according to claim 1 in water
Application in survey, it is characterised in that: the reacting hole of working electrode duct side and the transparent window distance on light source casing
For 5~15mm.
7. COD is examined a kind of sensitive portable light electro-catalysis COD sensor according to claim 1 in water
Application in survey, it is characterised in that: the TiO of the hydrogenation2TiO in nano-array film2The length of nano-array be 100~
2000nm。
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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 |
| 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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|---|---|---|---|---|
| CN1721056A (en) * | 2005-05-26 | 2006-01-18 | 上海交通大学 | Photoelectrocatalytic thin-layered minisize reactor |
| CN1774627A (en) * | 2003-04-04 | 2006-05-17 | 水体检测有限公司 | Photoelectrochemical determination of chemical oxygen demand |
| CN102866186A (en) * | 2012-09-12 | 2013-01-09 | 合肥工业大学 | Circulating-type water chemical oxygen demand detection photoelectrochemical sensor |
| 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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2017
- 2017-04-06 CN CN201710219525.8A patent/CN106990152B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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