CN107941867B - Electrochemical gas sensor capable of jointly detecting nitric oxide in expired air and hydrogen sulfide in expired air - Google Patents
Electrochemical gas sensor capable of jointly detecting nitric oxide in expired air and hydrogen sulfide in expired air Download PDFInfo
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 60
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 55
- 239000007789 gas Substances 0.000 title claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 239000007772 electrode material Substances 0.000 claims abstract description 13
- 239000003792 electrolyte Substances 0.000 claims abstract description 5
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 3
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 3
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 3
- 239000010439 graphite Substances 0.000 claims abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 14
- 239000003575 carbonaceous material Substances 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 229910052725 zinc Inorganic materials 0.000 claims description 14
- 239000011701 zinc Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- 238000009792 diffusion process Methods 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000002134 carbon nanofiber Substances 0.000 claims description 2
- 238000013461 design Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000004745 nonwoven fabric Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 claims 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims 1
- 239000004809 Teflon Substances 0.000 claims 1
- 229920006362 Teflon® Polymers 0.000 claims 1
- 239000004917 carbon fiber Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 238000004364 calculation method Methods 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 208000015181 infectious disease Diseases 0.000 description 3
- 230000002458 infectious effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 208000037883 airway inflammation Diseases 0.000 description 2
- 230000000172 allergic effect Effects 0.000 description 2
- 208000010668 atopic eczema Diseases 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003550 marker Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 210000000440 neutrophil Anatomy 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 1
- DBTDEFJAFBUGPP-UHFFFAOYSA-N Methanethial Chemical compound S=C DBTDEFJAFBUGPP-UHFFFAOYSA-N 0.000 description 1
- 206010036790 Productive cough Diseases 0.000 description 1
- 208000037884 allergic airway inflammation Diseases 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002327 eosinophilic effect Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002757 inflammatory effect Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 210000003802 sputum Anatomy 0.000 description 1
- 208000024794 sputum Diseases 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
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Abstract
The invention discloses a four-electrode electrochemical gas sensor capable of simultaneously measuring nitric oxide and hydrogen sulfide in expired air, which is a four-electrode system consisting of two working electrodes, an auxiliary electrode, a reference electrode, a hydrogen sulfide filter and electrolyte, and is characterized in that: the two working electrodes are positioned on the same horizontal plane and are relatively independent in space, the two working electrodes are made of the same electrode material, and the hydrogen sulfide filter is positioned above one of the working electrodes. The working electrode is semicircular, and the electrode material is gold-doped carbon nanotube, graphite or graphene. The gold-doped working electrode is sensitive to hydrogen sulfide, so that a mixed response signal of nitric oxide and hydrogen sulfide can be obtained, and only a response signal of nitric oxide can be obtained on the working electrode provided with the hydrogen sulfide filter, so that the response signals of nitric oxide and hydrogen sulfide can be obtained on the sensor at the same time through difference calculation. The sensor can realize the simultaneous detection of the exhaled nitric oxide and the exhaled hydrogen sulfide.
Description
Technical Field
The invention relates to the field of breath detection, in particular to an electrochemical gas sensor capable of simultaneously measuring nitric oxide and hydrogen sulfide in breath.
Background
Exhaled NO is an internationally accepted marker of eosinophilic or allergic airway inflammation, normally in the 5-25 ppb range, and a number of commercial products have been used in clinical practice. Recent studies using laboratory instruments found exhaled breath H2S may be a neutrophil or infectious airway inflammatory marker, e.g., Jack FDummer study from Ottago university found exhaled breath H2There is a negative correlation between S concentration and sputum neutrophil levels, H2The S concentration is about 10 ppb. Thus, the exhaled gases NO and H2The combined detection of S is hopeful to distinguish the inflammation types and provides more effective basis for medication. Exhaled gases NO and H2The combined detection of S has important clinical significance.
Currently, chemiluminescence and electrochemical NO sensor technologies can achieve the detection of ppb levels of NO. Among them, the chemiluminescence apparatus is expensive in equipment, complex in maintenance method, and is subject to clinical applicationWith great limitation, the electrochemical NO sensor technology of the swedish NIOX and shanghao, china has been widely used for the detection of clinical exhaled NO. Expired air H2The detection of S has not been reported in the commercial clinical technology, and expired air H is detected in the laboratory2Most of the detection methods of S are gas chromatography and chemiluminescence methods, equipment is expensive, an analysis method is complex, and clinical application is greatly limited.
Exhaled gas NO and exhaled gas H2The concentration of S is ppb level, and the joint detection is a very challenging and innovative technology. The invention aims to develop a method for simultaneously measuring NO and H in exhaled breath2Electrochemical gas sensing of S for breath detection of allergic and infectious airway inflammation and related diseases.
Disclosure of Invention
The invention aims to provide a four-electrode electrochemical gas sensor capable of simultaneously measuring nitric oxide and hydrogen sulfide in expired air. The sensor consists of two working electrodes, an auxiliary electrode, a reference electrode, a hydrogen sulfide filter, a buffer and electrolyte, wherein the two working electrodes are positioned on the same horizontal plane, the space is relatively independent, the electrode materials are the same, the hydrogen sulfide filter is positioned above one of the working electrodes, and the buffer is positioned above the other working electrode.
The two working electrodes are located on the same horizontal plane and are relatively independent in space, the two working electrodes can be separated through the design of the sensor shell, and the interference caused by mutual diffusion of gas passing through the filter and gas not passing through the filter is avoided. A baffle plate can be arranged in the middle of the sensor shell and extends from the upper edges of the hydrogen sulfide filter and the buffer to the inside of the sensor, so that the hydrogen sulfide filter and the buffer can be separated, the two working electrodes can be separated, and relatively independent spaces are created for the two working electrodes. The thicknesses of the hydrogen sulfide filter and the buffer are the same, and the carriers of the materials are the same, so that the diffusion rates of the gases in the hydrogen sulfide filter and the buffer are the same, and the phenomenon that the same gas responds differently on the two working electrodes due to different diffusion rates is avoided.
The two working electrodes are made of the same electrode material and are semicircular in shape, and the electrode material is a gold-doped carbon nanotube, graphite or graphene. The electrode of the sensor adopts an inverted triangle installation mode: the two working electrodes, the reference electrode and the auxiliary electrode are respectively parallel from top to bottom. The reference electrode and the auxiliary electrode are both platinum electrodes. The hydrogen sulfide filter is located above one of the working electrodes (S1), and the main component of the hydrogen sulfide filter is a carbon material loaded with zinc and copper, and the shape of the carbon material is semicircular. The buffer is located above the other working electrode (S2). The gold-doped working electrode is sensitive to hydrogen sulfide gas, so that a mixed response signal of nitric oxide and hydrogen sulfide can be obtained, and only a response signal of nitric oxide can be obtained on the working electrode provided with the hydrogen sulfide filter, so that the response signals of nitric oxide and hydrogen sulfide can be obtained on the sensor at the same time through difference calculation, the test method is simplified, and the practical application cost is greatly reduced. The specific algorithm is as follows: let the concentration coefficient of nitric oxide be K1Concentration coefficient of hydrogen sulfide of K2The response current value I of the nitric oxide is obtained on the working electrode S11The mixed response current value I of the nitric oxide and the hydrogen sulfide is obtained on the working electrode S22And therefore, the first and second electrodes are,
CNO= K1*I1
CH2S= K2*( I2- I1)
the carbon material can be a material with a large specific surface area, such as carbon nanofibers, porous activated carbon, activated carbon nanofibers, activated carbon cloth, fiber non-woven fabrics and the like, and the carbon material is prepared by adding the carbon material into a mixed solution of 7-8 mo L/L zinc chloride and 5.8-7 mo L/L copper chloride, adding ammonia water, stirring and reacting for 4.5-5 hours at 65-80 ℃, filtering and separating after the reaction is finished, washing three times by using a 30% methanol solution, drying the solid obtained by filtering and separating at 100 ℃ for 12 hours, and preparing the carbon material loaded with zinc and copper.
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
the four-electrode electrochemical gas sensor prepared by the technical scheme of the invention has the following maximum advantages: the method can simultaneously measure the nitric oxide and the hydrogen sulfide in the expired air, the working electrodes are made of the same electrode material, the drifts caused by environmental factors such as temperature and the like are consistent, and the calculation deviation caused by the difference of the two working electrode materials is solved. The hydrogen sulfide filter is a carbon material loaded with zinc and copper, and the material carrier has the advantages of large specific surface area, small zinc and copper particles, large loading capacity, strong removal effect on hydrogen sulfide and long service life. The four-electrode electrochemical gas sensor prepared by the technical scheme of the invention realizes the combined detection of nitric oxide and hydrogen sulfide in expiration, and can be applied to expiration detection of allergic and infectious airway inflammation and related diseases.
Drawings
FIG. 1 is a schematic diagram of the structure of an electrochemical gas sensor.
FIG. 2 is a response curve of an electrochemical gas sensor to a gas mixture.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Structure of electrochemical gas sensor of this example: as shown in fig. 1, the sensor includes a case 10, a working electrode (S1) 21, a working electrode (S2) 22, a reference electrode (R) 23, a counter electrode (C) 24, an electrolyte 30, a hydrogen sulfide filter 40, and a buffer 50. An air inlet hole 11 is arranged in the middle of the top end of the sensor shell 10, an air outlet hole 12 is arranged on the left side of the top end of the shell 10, an air outlet hole 13 is arranged on the right side of the top end of the shell 10, and a baffle 14 is arranged in the middle of the shell. The hydrogen sulfide filter 40 is located above the working electrode (S1) 21, and the buffer 50 is located above the working electrode (S2) 22.
The two working electrodes are positioned on the same horizontal plane and are relatively independent in space. The electrode materials of the two working electrodes are the same and are gold-doped graphene. The working potential of the working electrode was 300 mV. The material of the reference electrode and the counter electrode is a platinum electrode. The working electrodes are made of the same electrode material, the drifts caused by environmental factors such as temperature and the like are consistent, and the calculation deviation caused by the difference of the two working electrode materials is solved.
The thickness of the baffle 13 is 1 mm, the total height is 4mm, the baffle 13 extends to the interior of the sensor from the upper edges of the hydrogen sulfide filter 40 and the buffer 50, the height of the hydrogen sulfide filter 40 and the buffer 50 is 2 mm, the height of the baffle 13 extending to the interior of the sensor is 2 mm, the baffle 13 can separate the hydrogen sulfide filter from the buffer, and can separate two working electrodes, so that the two working electrodes are in relatively independent spaces, and the interference caused by mutual diffusion of gases passing through the filter and gases not passing through the filter is avoided, the PIN 14 is a conductor for connecting four electrodes and is respectively connected with the working electrode (S1) 21, the working electrode (S2) 22, the reference electrode (R) 23 and the counter electrode (C) 24, the electrolyte 30 is 6 mol/L H2SO4And (3) solution. The material of the sensor housing 10 is ABS.
The preparation method of the porous active carbon loaded with the zinc and the copper comprises the steps of adding 3 g of the porous active carbon into a mixed solution containing 7.5 mo L/L zinc chloride and 6 mo L/L copper chloride in 30 m L, adding 20 m L ammonia, stirring and reacting for 5 hours at 75 ℃, filtering and separating after the reaction is finished, washing the solid obtained by filtering and separating for three times at 100 ℃ for 12 hours, drying the solid obtained by filtering and separating for 12 hours to obtain the porous active carbon loaded with the zinc and the copper, wherein the size of the obtained zinc and copper particles is in a range of 4-8 nm, the loading mass ratio of the zinc and the copper reaches 26.5%, the specific surface area of the material carrier is large, the zinc and the copper particles are small and large, and the porous active carbon loaded with the zinc and the copper has a strong hydrogen sulfide removal effect and a long service life.
The response curve of the electrochemical gas sensor manufactured in this example to a mixture of 20 ppb of nitric oxide and 15ppb of hydrogen sulfide is shown in fig. 2. In fig. 2, curve a is a response curve of the working electrode S1 provided with the hydrogen sulfide filter, and curve b is a response curve of the working electrode S2 provided with the buffer. The first 30s of the curve is the response of the sensor to the mixed gas, and the last 30s is the response of the sensor to the high purity air. The calculation shows that the concentration of the nitric oxide in the mixed gas is 19ppb, the concentration of the hydrogen sulfide is 15ppb, the error is within +/-10 percent, and the mixed gas meets the clinical requirement.
The above-mentioned embodiments are only preferred embodiments of the present invention, and do not limit the scope of the present invention, but all the modifications made by the principles of the present invention and the non-inventive efforts based on the above-mentioned embodiments shall fall within the scope of the present invention.
Claims (11)
1. A four-electrode electrochemical gas sensor capable of jointly detecting nitric oxide and hydrogen sulfide in expired air is characterized in that a four-electrode system is composed of two working electrodes, an auxiliary electrode, a reference electrode and electrolyte and is characterized in that: the two working electrodes are positioned on the same horizontal plane and are relatively independent in space, the two working electrodes are made of the same electrode material, the hydrogen sulfide filter is positioned above one of the working electrodes, and the buffer is positioned above the other working electrode;
the main component of the hydrogen sulfide filter is a carbon material loaded with zinc and copper;
the preparation method of the zinc-copper loaded carbon material comprises the steps of adding the carbon material into a mixed solution of 7-8 mo L/L zinc chloride and 5.8-7 mo L/L copper chloride, adding ammonia water, stirring and reacting for 4.5-5 hours at 65-80 ℃, filtering and separating after the reaction is finished, washing for three times by using 30% methanol solution, and drying the solid obtained by filtering and separating for 12 hours at 100 ℃ to prepare the zinc-copper loaded carbon material.
2. The four-electrode electrochemical gas sensor capable of jointly detecting nitric oxide and hydrogen sulfide in exhaled breath as claimed in claim 1, wherein the loading mass ratio of zinc and copper in the zinc and copper loaded carbon material is 10-30%, and the size of zinc and copper particles is 2-10 nm.
3. A four-electrode electrochemical gas sensor for the combined detection of nitric oxide and hydrogen sulfide in exhaled breath as in claim 1, wherein said two working electrodes are located on the same horizontal plane and are spatially separated from each other, and the two working electrodes are separated by the design of the sensor housing, so as to avoid the interference caused by the mutual diffusion of gases passing through the filter and gases not passing through the filter.
4. A four-electrode electrochemical gas sensor for the combined detection of nitric oxide and hydrogen sulfide in exhaled breath as in claim 1, wherein said two working electrodes are made of the same electrode material and have a semicircular shape.
5. The four-electrode electrochemical gas sensor capable of jointly detecting nitric oxide and hydrogen sulfide in exhaled breath as claimed in claim 1, wherein the electrode material of the working electrode is gold-doped carbon nanotube, gold-doped graphite or gold-doped graphene.
6. A four-electrode electrochemical gas sensor for combined detection of nitric oxide and hydrogen sulfide in exhaled breath as claimed in claim 1, wherein the electrodes of said sensor are mounted in an inverted triangle manner: the reference electrode and the auxiliary electrode are platinum electrodes.
7. A four-electrode electrochemical gas sensor for the combined detection of nitric oxide and hydrogen sulfide in exhaled breath as in claim 1, wherein said hydrogen sulfide filter is positioned above one of said working electrodes and has a semicircular shape.
8. A four-electrode electrochemical gas sensor for combined detection of nitric oxide and hydrogen sulfide in exhaled breath as claimed in claim 1, wherein said buffer is located above the other working electrode and is made of gas permeable material, and the gas permeable material is carbon fiber, teflon membrane or non-woven fabric, and is shaped as a semicircle.
9. A four-electrode electrochemical gas sensor for the combined detection of nitric oxide and hydrogen sulfide in exhaled breath as in claim 1, wherein said hydrogen sulfide filter and said buffer are of the same thickness and the same material as the carrier.
10. A four-electrode electrochemical gas sensor for combined detection of nitric oxide and hydrogen sulfide in exhaled breath as claimed in claim 6, wherein said carbon material is carbon nanofiber, porous activated carbon, activated carbon cloth or fiber non-woven cloth.
11. The four-electrode electrochemical gas sensor capable of jointly detecting nitric oxide and hydrogen sulfide in expired air as claimed in claim 6, wherein the carbon material is activated carbon nanofiber.
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| CN109813780A (en) * | 2019-02-01 | 2019-05-28 | 荆州市爱尔瑞科技有限公司 | A kind of electrochemistry nitric oxide gas sensor |
| CN110044980A (en) * | 2019-04-30 | 2019-07-23 | 西南大学 | Application of the pyrophosphoric acid cobalt nano material in building nitric oxide electrochemical sensor |
| DE102020125411A1 (en) * | 2020-09-29 | 2022-03-31 | Dräger Safety AG & Co. KGaA | Electrochemical multi-gas sensor |
| CN112697864B (en) * | 2020-12-16 | 2022-04-01 | 浙江大学 | An integrated four-electrode gas sensor and its preparation method and application |
| CN112924423B (en) * | 2021-01-21 | 2022-07-12 | 上海交通大学 | Graphene quantum dot-based assembled microparticle material and preparation method and application thereof |
| CN116642939A (en) * | 2023-06-14 | 2023-08-25 | 杨九亚 | Networked double-channel electrochemical gas detection circuit |
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| EP1154267A2 (en) * | 2000-05-13 | 2001-11-14 | Alphasense Limited | Electrochemical sensor for determining analyte in the presence of interferent |
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| CN103506071A (en) * | 2012-06-19 | 2014-01-15 | 中国石油化工股份有限公司 | Purificant used for absorbing hydrogen sulfide and carbonyl sulfide in tail gas of natural gas and preparation method thereof |
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