CN104251856A - Peroxide gas sensor and preparation method thereof, and peroxide gas detection method - Google Patents
Peroxide gas sensor and preparation method thereof, and peroxide gas detection method Download PDFInfo
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- CN104251856A CN104251856A CN201310261721.3A CN201310261721A CN104251856A CN 104251856 A CN104251856 A CN 104251856A CN 201310261721 A CN201310261721 A CN 201310261721A CN 104251856 A CN104251856 A CN 104251856A
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Abstract
The invention provides a peroxide gas sensor and a preparation method thereof, and a peroxide gas detection method. The gas sensor comprises a quartz or glass package assembly with a gas inlet, a gas outlet and a sealing cover; an inner cavity of the quartz or glass package assembly is provided with a sensing element made of a nano-material; the nano-material contains a material sensitive to peroxide gas. The sensor performs enrichment and in-situ chemiluminescence detection by a nano-material thin film with high chemical activity, greatly improves the sensitivity of chemiluminescence detection, simplifies an instrument structure, also has the characteristics of low energy consumption, low background, no reagent loss, good repeatability and long service life, and can be used as a miniaturized portable high-sensitivity chemiluminescence sensor.
Description
Technical field
The present invention relates to a kind of superoxide gas sensor, its preparation method and superoxide gas detection method, particularly a kind of trace superoxide gas sensor, its preparation method and trace superoxide gas detection method.
Background technology
Superoxide gas is a kind of oxygenant of danger, is extensively present in chemistry, living things system and surroundings.Because superoxide gas is (as H
2o
2gas) strong volatility and its to biological hazard, how to realize superoxide gas (as H
2o
2gas) detection just become a difficult problem of pendulum before people.A series of detection system and detection method has been had about the detection of gas in prior art, such as, infrared spectrum, Raman spectrum, mass spectrum, galvanochemistry, chromatogram, fluorescence spectrum etc., but above method often all depends on expensive large-scale instrument and equipment, lengthy and tedious sample handling processes or detection limit is low not.Therefore, development one is needed to superoxide gas (as H
2o
2gas) the superoxide gas of especially super low concentration is (as H
2o
2gas) quick, efficient, easy, sensitive detection means.
Chemiluminescence analysis obtains a kind of high sensitivity trace and Analytical Methods of Trace that develop rapidly in recent years, because its analysis speed is fast, instrument and equipment is simple, the feature such as easily to be automated, to be widely used in the fields such as chemical analysis, immunoassay, rock-mineral analysis, Food Inspection, environmental monitoring.We notice, oxalate ester peroxide and derivant thereof, can with superoxide gas (as H as the chemiluminescence compound of a quasi-representative
2o
2gas) occur chemical reaction release and transferring energy to organic dye molecule.Due to specificity and the sensitivity of its chemical reaction, chemiluminescence just provides one and is detected oxide gas (as H
2o
2gas) highly effective new way.But this method also has itself limitation, as strong in portability, be only applicable to liquid-phase system etc.Therefore, develop a kind of easy and simple to handle, testing cost is cheap, detection sensitivity is high, be convenient to safeguard and the chemiluminescence gas sensor of Site Detection needs can be met people are looked forward to for many years just.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of superoxide gas sensor is provided.
Another object of the present invention is the preparation method providing a kind of described superoxide gas sensor.
Another object of the present invention is the purposes providing above-mentioned superoxide gas sensor.
Another object of the present invention is that providing a kind of uses above-mentioned superoxide gas sensor to be detected the method for oxide gas.
The present invention is achieved by the following technical solutions:
A kind of superoxide gas sensor, it comprises quartz with air intake opening, gas outlet and gland bonnet or glass-encapsulated assembly; In the inner chamber of described quartz or glass-encapsulated assembly, be provided with sensing element prepared by nano material; Containing the material to superoxide gas sensitization in described nano material.
According to the present invention, described sensing element is comprise chemiluminescent material and the nano material laminated film to the material of superoxide gas sensitization.
According to the present invention, the described material to superoxide gas sensitization is selected from oxalic acid ester type compound, such as two (2,4,5 – tri-chloro-salicylic acids are just for ester) oxalate (CPPO).
According to the present invention, described chemiluminescent material is selected from dyestuff, luminol (have another name called luminol, chemical name is luminol), lucigenin (lucigenin; Bis-N-methylacridinium nitrate) etc.Preferably, described dyestuff is 9,10-tolane base anthracene (BPEA).
According to the present invention, described sensor also comprises the optical signal receiver be located at below described quartz or glass-encapsulated assembly.
According to the present invention, described optical signal receiver is made up of monochromator and photomultiplier.
The present invention also provides following technical scheme:
Prepare a method for the sensing element in above-mentioned superoxide gas sensor, comprise the steps:
1) mixing comprising the solution of chemiluminescent material with each raw material in the chemical luminous system of the material to superoxide gas sensitization, stirring;
2) mixed solution being watered the bottom casting from quartz or glass assembly, after gelation, drying, namely obtain described sensing element, is nano material laminated film.
According to the present invention, the described material to superoxide gas sensitization is selected from oxalic acid ester type compound, such as two (2,4,5 – tri-chloro-salicylic acids are just for ester) oxalate.
According to the present invention, described chemiluminescent material is selected from dyestuff, luminol (have another name called luminol, chemical name is luminol), lucigenin (lucigenin; Bis-N-methylacridinium nitrate) etc.Preferably, described dyestuff is 9,10-tolane base anthracene (BPEA).
According to the present invention, in described step 1), described chemiluminescent material be 1:0.1 ~ 1:10 to the mol ratio of the material of peroxide-sensitive, preferred 1:1.
The present invention also provides following technical scheme:
A purposes for above-mentioned superoxide gas sensor, it is particularly useful for the detection of trace superoxide for the detection of superoxide.
According to the present invention, described detected object comprises ultraviolet degradation can produce H
2o
2the superoxide solid of gas and gas, comprise superoxide explosive, dangerous material (such as TATP, HMTD etc.) etc.
According to the present invention, described detected object comprises H
2o
2gas.
The present invention also provides following technical scheme:
Be detected a method for oxide, comprise the steps:
(1) by H that described superoxide produces
2o
2gas and carrier gas pass into gas sensor by the air intake opening of above-mentioned superoxide gas sensor;
(2) chemiluminescence signal being entered sensing element after sensor by above-mentioned superoxide gas is detected.
According to the present invention, described H
2o
2gas is that superoxide is produced, as produced by ultraviolet degradation.
According to the present invention, H described in the surface enrichment of the sensing element in described superoxide gas sensor
2o
2, there is chemical reaction in gas molecule.
According to the present invention, described H
2o
2the flow velocity of gas and carrier gas is 75-350mL/min, preferred 100-200mL/min.
According to the present invention, described enrichment time is 1-30min, preferred 5-20min.
According to the present invention, the combination gas that described carrier gas is nitrogen or air or mixes with any ratio.
According to the present invention, described sensor also comprises the optical signal receiver be located at below described quartz packaged assembly.Preferably, described optical signal receiver is made up of monochromator and photomultiplier.
According to the present invention, described H
2o
2gas and carrier gas are passed into by the air intake opening of above-mentioned superoxide gas sensor, H described in the surface enrichment of the sensing element in described superoxide gas sensor
2o
2gas molecule, chemical reaction occurs luminous, the light of generation enters conduction optical fiber by photomultiplier, and light signal is finally passed to signal detector by optical fiber.
The actively useful effect that the present invention has:
1. provide a kind ofly to be easy to carry, the replaceable simple and convenient operation and maintenance of material can be used in the high sensitivity chemistry luminous gas sensor that on-the site analysis detects.
2. effectively reduce the cost of detection, be conducive to the popularization and application of chemiluminescence analytical technique in fields such as chemical analysis, immunoassay, rock-mineral analysis, Food Inspection, environmental monitorings.
describe in detail
The invention discloses a kind of method of the sensing element prepared in above-mentioned superoxide gas sensor, comprise the steps:
1) mixing comprising the solution of chemiluminescent material with each raw material in the chemical luminous system of the material to superoxide gas sensitization, stirring;
2) mixed solution being watered the bottom casting from quartz or glass assembly, after gelation, drying, namely obtain described sensing element, is nano material laminated film.
According to the present invention, described nano material is nano compound film, and nano material specific surface area is very large, is conducive to the absorption of detected gas molecule on CPPO surface and diffusion, which results in the persistent accumulation of gas molecule, and reaches the object that detection signal amplifies.H
2o
2cause CPPO surface and produce following chemical reaction: H
2o
2react with CPPO and generate the dioxane diacetyl of high chemical energy, by electron exchange luminescence (CIEEL) mechanism by energy trasfer to dyestuff (as BPEA) molecule, be degraded into carbon dioxide simultaneously and send fluorescence.
The dynamic process of chemiluminescence reaction is undertaken studying (device and experimental technique are as shown in Figure 1) by an inert gas flows device improved and a ultraweak Chemiluminescence Apparatus.Be exposed to H
2o
2after in steam, nano compound film produces the luminescence of high strength in the mode of chemical reaction.At H
2o
2concentration (C
h2O2) from 62ppb to 65ppm in scope, chemiluminescent intensity and H
2o
2the relation function of concentration as shown in Figure 2.Chemiluminescence measures with the integrated form of unit of luminous intensity's light intensity relative to the whole reaction time.(peak area is to H for typical calibration curve
2o
2concentration) as shown in Figure 2, in figure, each point represents the mean value of 3 revision tests, and error range is between 6% to 10%.What represent in figure is from 62ppb to 1.24ppm(, comprise four orders of magnitude) scope in close to linear kinetic curve.Chemiluminescent mean intensity is along with H
2o
2the increase of concentration and increasing, along with H
2o
2dividing potential drop increase and be tending towards saturated, this can owing to the Langmuir adsorption process of molecule on surface.As shown in Figure 2, at low H
2o
2under concentration (≤1.24ppm), nano compound film has shown the linear response to concentration, calculates H
2o
2detectability be 40ppb, than current business-like H
2o
2gas detection method (0.1 ~ 1ppm) is sensitiveer.Compared with the signal be exposed in other volatile active oxygen species (ROS), this nano compound film is to H
2o
2show very high selectivity, because the chemiluminescence of oxalate ester peroxide needs 1,2-dioxane diacetyl intermediate of a generation transient state, it can only pass through and H
2o
2reaction generate.
In order to make gas fully contact with sensing element, have employed diameter is 2cm, is highly quartz or the glass-encapsulated assembly of 0.2cm.In testing process, certain density hydrogen peroxide gas is driven to pass in described assembly with pure nitrogen.With the change of spectrometer monitoring spectrum, after Wavelength stabilized, record this intensity.Repeat above step, can H be obtained
2o
2gas concentration-luminous intensity standard curve.By the intensity of photometer measurement light during on-the-spot test, look into typical curve H
2o
2gas concentration.Due to this H
2o
2gas sensor adopts chemiluminescence to do sensing, carrys out measure gas concentrations by detecting luminous intensity, so have not by external electromagnetic field interference, good stability, highly sensitive, the advantage such as impact that is not subject to light source optical power fluctuation.
Accompanying drawing explanation
Fig. 1 is the example schematic of detection method provided by the invention.1. nitrogen cylinder, 2. gas meter, 3. superoxol, 4. valve, 5. air intake opening, 6. gas outlet 7. package assembling, 8. cotton, 9. sensing element, 10. photomultiplier, 11. gas sensors, 12. analytic systems
Fig. 2 is chemiluminescence intensity and H
2o
2the graph of relation of concentration.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but the present invention is not limited to following examples.Any improvement of making on basis of the present invention and change are all within scope.
BEPA:9,10-tolane base anthracene
CPPO: two (2,4,5 – tri-chloro-salicylic acids are just for ester) oxalate
Embodiment 1
The preparation method of BEPACPPO nano material laminated film used in the method is as follows: be dissolved into respectively in acetone and ethanol by BPEA and CPPO, be configured to the solution of 1mM, is that 1:1 mixes with volume ratio.Then the mixed solution getting 100 μ L drips on test tube, and solvent at room temperature slowly volatilizees.In order to the growth of stabilized nanoscale material, sample is left standstill 3h.These sample tubes are placed on dark ventilation dry at room temperature over night, after solvent volatilization completely, can nano compound film be obtained.
Gas of carrier gas is nitrogen or air, and flow velocity is within the scope of 75-350mL/min.Bubbling in the aqueous hydrogen peroxide solution of concentration known, at room temperature take in described superoxide gas sensor by air intake opening, gas molecule to be measured is made to be adsorbed on nano compound film surface, realize the object of enrichment, there is chemical reaction on its surface and produce light signal, the automatic record of computer after photomultiplier amplifies.Light signal linearly changes with the change of gas concentration.As to H
2o
2gas, the range of linearity is 0.064-1.24ppm.
Embodiment 2
The preparation method of BEPA oxalate ester peroxide polymer nano material laminated film used in the method is as follows: BPEA and oxalic acid ester polymer being dissolved into respectively in acetone and methylene chloride, being configured to the solution of 1mM, is that 1:1 mixes with volume ratio.Then the mixed solution getting 100 μ L drips on test tube, and solvent at room temperature slowly volatilizees.In order to the growth of stabilized nanoscale material, sample is left standstill 3h.These sample tubes are placed on dark ventilation dry at room temperature over night, after solvent volatilization completely, can nano compound film be obtained.
Gas of carrier gas is nitrogen or air, and flow velocity is within the scope of 75-350mL/min.Bubbling in the aqueous hydrogen peroxide solution of concentration known, at room temperature take in described superoxide gas sensor by air intake opening, gas molecule to be measured is made to be adsorbed on nano compound film surface, realize the object of enrichment, there is chemical reaction on its surface and produce light signal, the automatic record of computer after photomultiplier amplifies.Light signal linearly changes with the change of gas concentration.As to H
2o
2gas, the range of linearity is 0.25-1.62ppm.
The synthetic route of oxalic acid ester polymer: under nitrogen atmosphere protection, 4-hydroxylphenylethyl alcohol (16mmol) and 1,8-ethohexadiol (2.4mmol) are dissolved in 10ml anhydrous tetrahydro furan.Triethylamine (40mmol) is dropwise added under zero degree.Under zero degree, in the oxalyl chloride that the anhydrous tetrahydro furan this potpourri being added 20ml dissolves (18.3mmol).Overnight at room temperature reacts, and finally adds saturated aqueous common salt cessation reaction, by extraction into ethyl acetate product.The organic product anhydrous Na obtained
2sO
4drying, concentrates in a vacuum.Last polymkeric substance passes through in methylene chloride/cyclohexane (1:1) precipitate and separate.
Embodiment 3
Dissolved in ethanol by CPPO, be configured to the solution of 1mM, the described solution getting 100 μ L drips on test tube, and solvent at room temperature slowly volatilizees.In order to the growth of stabilized nanoscale material, sample is left standstill 3h.These sample tubes are placed on dark ventilation dry at room temperature over night, after solvent volatilization completely, can nano material film be obtained.
Gas of carrier gas is N
2gas, flow velocity is within the scope of 75-350mL/min.Bubbling in the aqueous hydrogen peroxide solution of concentration known, at room temperature take in described superoxide gas sensor by air intake opening, gas molecule to be measured is made to be adsorbed on nano material film surface, realize the object of enrichment, there is chemical reaction on its surface and produce light signal, the automatic record of computer after photomultiplier amplifies.Light signal is lower than precedent hundred times, because do not have luminescent substance BPEA, chemiluminescence is very faint.
Embodiment 4
Being dissolved into respectively in acetone and ethanol by BPEA and CPPO, being configured to the solution of 1mM, is that 1:1 mixes with volume ratio.Then the mixed solution getting 100 μ L drips on test tube, and solvent at room temperature slowly volatilizees.In order to the growth of stabilized nanoscale material, sample is left standstill 3h.These sample tubes are placed on dark ventilation dry at room temperature over night, after solvent volatilization completely, can nano compound film be obtained.
Gas of carrier gas is nitrogen or air, flow velocity is within the scope of 75-350mL/min, at room temperature directly enter in described superoxide gas sensor by air intake opening, gas molecule to be measured is made to be adsorbed on nano compound film surface, realize the object of enrichment, there is chemical reaction on its surface and produce light signal, the automatic record of computer after photomultiplier amplifies.Light signal is very faint.
Embodiment 5
BPEA is dissolved in acetone, is configured to the solution of 1mM.Then the mixed solution getting 100 μ L drips on test tube, and solvent at room temperature slowly volatilizees.In order to the growth of stabilized nanoscale material, sample is left standstill 3h.These sample tubes are placed on dark ventilation dry at room temperature over night, after solvent volatilization completely, can nano material film be obtained.
Gas of carrier gas is nitrogen gas, and flow velocity is within the scope of 75-375mL/min.Bubbling in the aqueous hydrogen peroxide solution of concentration known, at room temperature take in described superoxide gas sensor by air intake opening, gas molecule to be measured is made to be adsorbed on nano material film surface, realize the object of enrichment, there is chemical reaction on its surface and produce light signal, the automatic record of computer after photomultiplier amplifies.Discovery does not have light signal, because do not have chemiluminescent active substance CPPO.
Embodiment 6
Being dissolved into respectively in acetone and ethanol by BPEA and CPPO, being configured to the solution of 1mM, is that 1:1 mixes with volume ratio.Then the mixed solution getting 100 μ L drips on test tube, and solvent at room temperature slowly volatilizees.In order to the growth of stabilized nanoscale material, sample is left standstill 3h.These sample tubes are placed on dark ventilation dry at room temperature over night, after solvent volatilization completely, can nano compound film be obtained.
Gas of carrier gas is nitrogen gas, and flow velocity is within the scope of 75-350mL/min.Bubbling in the peroxide liquid of concentration known, at room temperature take in described superoxide gas sensor by air intake opening, gas molecule to be measured is made to be adsorbed on nano compound film surface, realize the object of enrichment, there is chemical reaction on its surface and produce light signal, the automatic record of computer after photomultiplier amplifies.Light signal hundred times more weak than hydrogen peroxide, chemiluminescence probe shows high selectivity.
Embodiment 7
Being dissolved into respectively in acetone and ethanol by BPEA and CPPO, being configured to the solution of 1mM, is that 1:1 mixes with volume ratio.Then the mixed solution getting 100 μ L drips on test tube, and solvent at room temperature slowly volatilizees.In order to the growth of stabilized nanoscale material, sample is left standstill 3h.These sample tubes are placed on dark ventilation dry at room temperature over night, after solvent volatilization completely, can nano compound film be obtained.
Superoxide (as TATP, HMTD) gas of concentration known is passed through ultraviolet degradation, gas of carrier gas is nitrogen gas, flow velocity is within the scope of 75mL/min, at room temperature take in described superoxide gas sensor by air intake opening, gas molecule to be measured is made to be adsorbed on nano compound film surface, realize the object of enrichment, on its surface, chemical reaction occurs and produce light signal, the automatic record of computer after photomultiplier amplifies.Light signal linearly changes with the change of gas concentration.As to H
2o
2gas, the range of linearity is 0.064-1.24ppm.
Claims (10)
1. a superoxide gas sensor, it comprises quartz with air intake opening, gas outlet and gland bonnet or glass-encapsulated assembly; In the inner chamber of described quartz or glass-encapsulated assembly, be provided with sensing element prepared by nano material; Containing the material to superoxide gas sensitization in described nano material.
2. superoxide gas sensor according to claim 1, is characterized in that, described sensing element is comprise chemiluminescent material and the nano material laminated film to the material of superoxide gas sensitization; Preferably, the described material to superoxide gas sensitization is selected from oxalic acid ester type compound, such as two (2,4,5 – tri-chloro-salicylic acids are just for ester) oxalate (CPPO); Preferably, described chemiluminescent material is selected from dyestuff, luminol (have another name called luminol, chemical name is luminol), lucigenin (lucigenin; Bis-N-methylacridinium nitrate) etc.; Preferably, described dyestuff is 9,10-tolane base anthracene (BPEA).
3. superoxide gas sensor according to claim 1 and 2, is characterized in that, described sensor also comprises the optical signal receiver be located at below described quartz or glass-encapsulated assembly; Preferably, described optical signal receiver is made up of monochromator and photomultiplier.
4. prepare a method for the sensing element in the superoxide gas sensor described in any one of claims 1 to 3, comprise the steps:
1) mixing comprising the solution of chemiluminescent material with each raw material in the chemical luminous system of the material to superoxide gas sensitization, stirring;
2) mixed solution being watered the bottom casting from quartz or glass assembly, after gelation, drying, namely obtain described sensing element, is nano material laminated film.
5. method according to claim 4, is characterized in that, in described step 1), described chemiluminescent material be 1:0.1 ~ 1:10 to the mol ratio of the material of peroxide-sensitive, preferred 1:1.
6. a purposes for the superoxide gas sensor described in any one of claims 1 to 3, it is particularly useful for the detection of trace superoxide for the detection of superoxide; Preferably, described detected object comprises ultraviolet degradation and can produce H
2o
2the superoxide solid of gas and gas, comprise superoxide explosive, dangerous material (such as TATP, HMTD etc.) etc.; More preferably, described detected object comprises H
2o
2gas.
7. be detected a method for oxide, comprise the steps:
(1) by H that described superoxide produces
2o
2gas (as produced by ultraviolet degradation) and carrier gas are passed into by the air intake opening of the superoxide gas sensor as described in any one of claims 1 to 3;
(2) chemiluminescence signal being entered sensing element after sensor by above-mentioned superoxide gas is detected.
8. method according to claim 7, is characterized in that, H described in the surface enrichment of the sensing element in described superoxide gas sensor
2o
2, there is chemical reaction in gas molecule.
9. the method according to claim 7 or 8, is characterized in that, described H
2o
2the flow velocity of gas and carrier gas is 75-350mL/min, preferred 100-200mL/min; Preferably, described enrichment time is 1-30min, preferred 5-20min; Preferably, the described carrier gas combination gas that is nitrogen or air or mixes with any ratio.
10. the method according to any one of claim 7 to 9, is characterized in that, described sensor also comprises the optical signal receiver be located at below described quartz or glass-encapsulated assembly; Preferably, described optical signal receiver is made up of monochromator and photomultiplier.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105806832A (en) * | 2016-03-16 | 2016-07-27 | 济南大学 | Preparation method and application of hydrogen peroxide sensor based on double functions of electrochemiluminescence and photoelectrochemistry |
| CN108088838A (en) * | 2017-12-13 | 2018-05-29 | 西南大学 | Application and method of double [2,4,6- trichlorophenyls] oxalates in the mould toxin of rod method is measured |
| CN112924424A (en) * | 2021-01-21 | 2021-06-08 | 重庆大学 | Preparation method of fluorescent thin block and TATP optical fiber fluorescent probe for trace explosives |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105806832A (en) * | 2016-03-16 | 2016-07-27 | 济南大学 | Preparation method and application of hydrogen peroxide sensor based on double functions of electrochemiluminescence and photoelectrochemistry |
| CN105806832B (en) * | 2016-03-16 | 2018-08-03 | 济南大学 | A kind of preparation method and application of the hydrogen peroxide sensor difunctional based on electrogenerated chemiluminescence and optical electro-chemistry |
| CN108088838A (en) * | 2017-12-13 | 2018-05-29 | 西南大学 | Application and method of double [2,4,6- trichlorophenyls] oxalates in the mould toxin of rod method is measured |
| CN112924424A (en) * | 2021-01-21 | 2021-06-08 | 重庆大学 | Preparation method of fluorescent thin block and TATP optical fiber fluorescent probe for trace explosives |
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Application publication date: 20141231 |