CN110006876B - A kind of carbon dioxide gas detection device and detection method - Google Patents
A kind of carbon dioxide gas detection device and detection method Download PDFInfo
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Abstract
本发明公开了二氧化碳气体检测装置及检测方法，检测装置包括检测单元、液路单元、气路单元和控制单元，检测单元包括避光外壳、管式气液界面反应器和光电检测传感器，避光外壳具有避光腔体，管式气液界面反应器和光电检测传感器设置在避光腔体内，液路单元包括与进液口和出液口相连的输液模块和储液模块，气路单元包括与出气口相连的抽气模块，控制单元与检测单元的光电检测传感器、液路单元中的输液模块和气路单元中的抽气模块电连接。所述二氧化碳气体检测方法采用上述二氧化碳气体管式检测装置进行二氧化碳气体浓度的检测。本发明基于气液相界面化学发光技术，实现二氧化碳气体的高灵敏度在线检测，成本低、速度快，具有较高的准确性及稳定性。
The invention discloses a carbon dioxide gas detection device and a detection method. The detection device includes a detection unit, a liquid circuit unit, a gas circuit unit and a control unit. The detection unit includes a light-proof casing, a tubular gas-liquid interface reactor and a photoelectric detection sensor. The shell has a light-shielding cavity, and the tubular gas-liquid interface reactor and the photoelectric detection sensor are arranged in the light-shielding cavity. The liquid circuit unit includes an infusion module and a liquid storage module connected with the liquid inlet and the liquid outlet. The air extraction module connected with the air outlet, the control unit is electrically connected with the photoelectric detection sensor of the detection unit, the infusion module in the liquid circuit unit and the air extraction module in the air circuit unit. The carbon dioxide gas detection method adopts the carbon dioxide gas tubular detection device to detect the carbon dioxide gas concentration. Based on the gas-liquid interface chemiluminescence technology, the invention realizes high-sensitivity on-line detection of carbon dioxide gas, has low cost, high speed, and high accuracy and stability.
Description
Technical Field
The invention relates to the technical field of chemiluminescence detection, in particular to a carbon dioxide gas detection device and a detection method.
Background
At present, a non-dispersive infrared absorption method is generally adopted for detecting carbon dioxide gas, the detection cost is low, the operation is simple, the detection speed is high, and continuous online detection can be realized. However, the method is easily influenced by the interference of moisture and aerosol in the gas in the detection process, the error is large, and the accuracy and the stability are difficult to guarantee. The gas-liquid phase interface chemiluminescence detection technology is a high-sensitivity detection method, and has been successfully applied to online detection of trace gases such as nitrogen dioxide, ozone, sulfur dioxide, formaldehyde and the like in the atmosphere. Compared with the traditional detection method, the technology has the advantages of low detection cost, simple equipment structure and the like, and has better application prospect. However, the technology is not applied to the detection of carbon dioxide gas at present.
In practical application, a gas-liquid interface chemiluminescence detection technology needs to provide a flowing gas-liquid reaction interface through a specific reaction bed structure to realize gas-liquid interface chemiluminescence reaction. In the prior art, the reaction bed generally adopts high hydrophilic thin film materials (such as silk, filter paper, PP fiber non-woven fabric, polyester fiber cloth, and the like), and has the advantages of providing a larger reaction interface and obtaining higher detection sensitivity. However, the high hydrophilicity and high wettability of the reaction bed mainly depend on the internal multi-dimensional structure supported by the superfine fibers. Along with the repeated use of the reaction bed, the multidimensional structure in the reaction bed is gradually hardened and collapsed, so that the hydrophilicity and the wettability of the reaction bed are gradually poor. Meanwhile, the reaction bed is soft and has certain tensile ductility, so that the reaction bed is difficult to be uniformly and flatly fixed in a reactor, and the detection performance of the equipment is influenced due to poor consistency.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a carbon dioxide gas detection device and a detection method, which can better realize high-sensitivity online detection of carbon dioxide gas based on a gas-liquid phase interface chemiluminescence technology.
One aspect of the present invention provides a carbon dioxide gas detecting apparatus including a detecting unit, a liquid path unit, a gas path unit, and a control unit, wherein,
the detection unit comprises a light-proof shell, a tubular gas-liquid interface reactor and a photoelectric detection sensor, wherein the light-proof shell is provided with a light-proof cavity, and the tubular gas-liquid interface reactor and the photoelectric detection sensor are arranged in the light-proof cavity;
the tubular gas-liquid interface reactor comprises an upper joint, a lower joint, a transparent pipe body, a fiber column and an isolation sleeve, wherein the upper joint is provided with a liquid inlet, a liquid inlet channel, a gas outlet and a gas outlet channel;
the fiber column is arranged in the transparent tube body, and two ends of the fiber column are respectively and fixedly arranged in the liquid inlet channel and the liquid outlet channel; the isolation sleeve is arranged on the outer surface of the fiber column, and an opening part is arranged on one side of the isolation sleeve; an annular cavity is formed between the transparent tube body and the fiber column, and is communicated with the air inlet channel and the air outlet channel and communicated with the fiber column through the opening part of the isolation sleeve; the light-sensing part of the photoelectric detection sensor is over against the transparent tube body of the tubular gas-liquid interface reactor and over against the opening part of the isolation sleeve.
The liquid path unit comprises a liquid conveying module and a liquid storage module which are connected with a liquid inlet and a liquid outlet;
the gas circuit unit comprises a gas extraction module connected with the gas outlet;
the control unit is electrically connected with the photoelectric detection sensor of the detection unit, the infusion module in the liquid path unit and the air extraction module in the air path unit.
According to one embodiment of the carbon dioxide gas detection device, the light-proof shell comprises a light-proof shell and a light-proof front cover, the light-proof shell and the light-proof front cover are assembled to form the light-proof shell with a light-proof cavity, hole sites corresponding to the upper joint and the lower joint of the tubular gas-liquid interface reactor are arranged on the light-proof front cover, and the tubular gas-liquid interface reactor is fixed on the light-proof front cover.
According to one embodiment of the carbon dioxide gas detection device, annular grooves are formed in the positions where the upper joint and the lower joint are connected with the transparent tube body, the transparent tube body is installed in the annular grooves and is sealed and fixed, and black silica gel is filled when the transparent tube body is installed.
According to one embodiment of the carbon dioxide gas detection device, the upper joint and the lower joint are made of opaque corrosion-resistant materials, the air outlet channel of the upper joint and the air inlet channel of the lower joint are tubular channels, and the inner diameter of the tubular channels is the same as that of the transparent tube body.
According to one embodiment of the carbon dioxide gas detection device of the present invention, the isolation sleeve is made of a light-tight corrosion-resistant material, the outer diameter of the fiber column is smaller than the inner diameter of the isolation sleeve and smaller than the inner diameter of the transparent tube, the fiber column is vertically installed at the central position of the transparent tube, the fiber column is made of a hard PP fiber column, and a portion of the fiber column corresponding to the opening portion of the isolation sleeve is recessed to form a terrace portion.
According to one embodiment of the carbon dioxide gas detection device, the liquid storage module comprises a first reagent storage subunit, a second reagent storage subunit, a cleaning reagent storage subunit and a waste liquid collection subunit, the liquid infusion module comprises a reagent pump and a cleaning pump, and the air pumping module comprises an air pumping pump.
According to one embodiment of the carbon dioxide gas detection device, the reagent pump is a three-channel miniature ball peristaltic pump, the first reagent storage subunit and the second reagent storage subunit are respectively connected with the liquid inlet through two channels of the reagent pump, and the liquid outlet is connected with the waste liquid collecting subunit through the other channel of the reagent pump; the cleaning pump is a double-channel miniature ball type peristaltic pump, the cleaning reagent storage subunit is connected with the liquid inlet through one channel of the cleaning pump, and the liquid outlet is connected with the waste liquid collecting subunit through the other channel of the cleaning pump.
In another aspect of the present invention, a carbon dioxide gas detection method is provided, in which the carbon dioxide gas detection device is adopted to detect the concentration of carbon dioxide gas.
According to one embodiment of the carbon dioxide gas detection method of the present invention, the detection method comprises the steps of:
step 1: assembling a detection device, continuously controlling a liquid path unit to introduce a detection reagent into a liquid inlet channel of a tubular gas-liquid interface reactor through a liquid inlet and lead the detection reagent out of a liquid outlet channel and discharge the detection reagent out of the tubular gas-liquid interface reactor through a liquid outlet, wherein the detection reagent comprises a first reagent and a second reagent, the first reagent is a hydrogen peroxide solution, the second reagent is a mixed solution of potassium hydroxide and potassium carbonate, the liquid inlet flow rates of the first reagent and the second reagent are the same, and the liquid outlet flow rate is slightly larger than the sum of the liquid inlet flow rates of the first reagent and the second reagent;
step 2: the control gas circuit unit leads the detection gas into a gas inlet channel of the tubular gas-liquid interface reactor through a gas inlet and leads the reacted gas out of a gas outlet channel and discharges the gas out of the tubular gas-liquid interface reactor through a gas outlet;
and step 3: detecting a chemiluminescence signal generated by gas-liquid interface chemiluminescence reaction in the tubular gas-liquid interface reactor through a photoelectric detection sensor, converting the chemiluminescence signal into an electric signal, and recording and calculating to obtain the actual concentration of the carbon dioxide;
and 4, step 4: and after the detection is finished, the liquid path unit is controlled to introduce a cleaning reagent into a liquid inlet channel of the tubular gas-liquid interface reactor through the liquid inlet, and the cleaning reagent is led out from the liquid outlet channel and is discharged out of the tubular gas-liquid interface reactor through the liquid outlet to complete cleaning, wherein the cleaning reagent is a mixed liquid of deionized water, ethanol and glycerol, and the liquid outlet flow rate of the cleaning reagent is 3-5 times of the liquid inlet flow rate.
Compared with the prior art, the invention provides a carbon dioxide gas detection device and a detection method, which realize high-sensitivity online detection of carbon dioxide gas based on a gas-liquid phase interface chemiluminescence technology. Compared with the prior art, the method has the advantages that the influence of moisture and aerosol can be avoided, the influence of other interference gases in the environmental gas can be avoided, the detection cost is low, the detection speed is high, and meanwhile, the method has high accuracy and stability.
Drawings
Fig. 1 shows an overall connection structure diagram of a carbon dioxide gas detecting apparatus according to an exemplary embodiment of the present invention.
Fig. 2 shows a schematic configuration diagram of a detection unit in a carbon dioxide gas detection device according to an exemplary embodiment of the present invention.
Fig. 3 shows a schematic structural view of a tubular gas-liquid interface reactor of a detection unit in a carbon dioxide gas detection device according to an exemplary embodiment of the present invention.
Description of reference numerals:
1-a detection unit; 11-light-proof front cover, 111-liquid inlet hole, 112-liquid outlet hole, 113-gas outlet hole and 114-gas inlet hole; 12-tubular gas-liquid interface reactor, 121-upper joint, 122-lower joint, 123-isolation sleeve, 1231-opening part, 124-fiber column, 1241-platform part, 125-transparent tube, 126-annular groove, 127-annular cavity, 1211-liquid inlet, 1212-gas outlet, 1213-liquid inlet channel, 1214-gas outlet channel, 1221-liquid outlet, 1222-gas inlet, 1223-liquid outlet channel, 1224-gas inlet channel; 13-light-shielding shell and 14-photoelectric detection sensor;
2-liquid path unit, 21-liquid storage module, 211-first reagent storage subunit, 212-second reagent storage subunit, 213-waste liquid collection subunit and 214-cleaning reagent storage subunit; 22-infusion module, 221-reagent pump, 222-cleaning pump; 3-gas path unit, 4-control unit.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
The following will specifically describe the carbon dioxide gas detection device of the present invention with reference to the accompanying drawings.
Fig. 1 shows an overall connection structure diagram of a carbon dioxide gas detecting apparatus according to an exemplary embodiment of the present invention.
As shown in fig. 1, according to an exemplary embodiment of the present invention, the carbon dioxide gas detection apparatus includes a detection unit 1, a liquid path unit 2, a gas path unit 3, and a control unit 4, where the detection unit 1 is a main component for detecting carbon dioxide by using a gas-liquid interface chemiluminescence detection technique, the liquid path unit 2 is used for supplying and recovering a reagent or a cleaning reagent to the detection unit 1, the gas path unit 3 is used for supplying a detection gas to the detection unit 1, and the control unit 4 controls an operation of the detection apparatus and realizes detection of carbon dioxide.
Fig. 2 shows a schematic configuration diagram of a detection unit in a carbon dioxide gas detection device according to an exemplary embodiment of the present invention.
As shown in fig. 2 and 3, the detection unit 1 of the present invention includes a light-shielding case, a tubular gas-liquid interface reactor 12, and a photoelectric detection sensor 14, the light-shielding case has a light-shielding cavity, and the tubular gas-liquid interface reactor 12 and the photoelectric detection sensor 14 are disposed in the light-shielding cavity. The gas-liquid interface chemiluminescence reaction of the detection gas occurs in the tubular gas-liquid interface reactor 12, the photoelectric detection sensor 14 detects a chemiluminescence signal, converts the chemiluminescence signal into an electrical signal and outputs the electrical signal, and the light-proof shell provides a light-proof environment for reaction and detection.
Fig. 3 shows a schematic structural view of a tubular gas-liquid interface reactor of a detection unit in a carbon dioxide gas detection device according to an exemplary embodiment of the present invention.
As shown in fig. 3, the tubular gas-liquid interface reactor comprises an upper joint 121, a lower joint 122, a transparent tube 125, a fiber column 124 and an isolation sleeve 123, wherein the upper joint 121 is provided with a liquid inlet 1211, a liquid inlet channel 1213, a gas outlet 1212 and a gas outlet channel 1214, and the lower joint 122 is provided with a liquid outlet 1221, a liquid outlet channel 1223, a gas inlet 1222 and a gas inlet channel 1224.
Preferably, the light-shielding shell comprises a light-shielding shell 13 and a light-shielding front cover 11, the light-shielding shell 13 and the light-shielding front cover 11 are assembled to form the light-shielding shell with the light-shielding cavity, the light-shielding front cover 11 is provided with hole sites corresponding to the upper joint 121 and the lower joint 122 of the tubular gas-liquid interface reactor, and the tubular gas-liquid interface reactor 12 is fixed on the light-shielding front cover 11.
The upper joint 121 and the lower joint 122 are preferably made of a light-tight corrosion-resistant material, the light-proof housing 13 and the light-proof front cover 11 are assembled to form a light-proof cavity after installation, the inner cavity of the tubular gas-liquid interface reactor 12 is communicated with the external liquid path unit 2 and the external gas path unit 3 through the liquid inlet hole 111, the liquid outlet hole 112, the gas outlet hole 113 and the gas inlet hole 114 which are formed in the light-proof front cover 11, and external light cannot enter the light-proof cavity and the tubular gas-liquid interface reactor through the gas-liquid path system, and the detection result cannot be influenced.
According to the present invention, a transparent tube 125 is connected between the upper joint 121 and the lower joint 122, the fiber column 124 is disposed in the transparent tube 125, and two ends of the fiber column 124 are respectively and fixedly installed in the liquid inlet channel 1213 and the liquid outlet channel 1223; the isolation sleeve 123 is arranged on the outer surface of the fiber column 124, and one side of the isolation sleeve 123 is provided with an opening part 1231; an annular cavity 127 is formed between the transparent tube body 125 and the fiber column 124, the annular cavity 127 is communicated with the air inlet channel 1224 and the air outlet channel 1214 and is communicated with the fiber column 124 through the opening part 1231 of the isolation sleeve 123; the light-sensing portion of the photodetection sensor 14 faces the transparent tube 125 of the tubular gas-liquid interface reactor 12 and faces the opening 1231 of the isolation sleeve 123.
Wherein, the positions where the upper joint 121 and the lower joint 122 are connected with the transparent tube 125 are both provided with an annular groove 126, and then the transparent tube 125 is installed in the annular groove 126 and sealed and fixed. Preferably, the transparent tube 125 is filled with black silicone when it is installed.
In addition, the air outlet channel 1214 of the upper joint 121 and the air inlet channel 1224 of the lower joint 122 are tubular channels, and the inner diameters of the air outlet channel 1214 and the air inlet channel 1224 are the same as the inner diameter of the transparent tube body 125, so that when the transparent tube body 125 is installed between the upper joint and the lower joint, a communicated air channel is formed, and no dead volume exists at the joint and the flow of air is not influenced.
The fiber column 124 is disposed in the liquid inlet channel 1213 and the liquid outlet channel 1223 of the upper and lower joints, respectively, and the fiber column 124 is preferably vertically installed at the center of the transparent tube 125. Therefore, after entering the inlet channel 1213 from the inlet 1211 of the upper joint 121, the reagent liquid participating in the reaction reaches the top end of the fiber column 124 and is uniformly distributed on the surface and inside of the fiber column 124 under the capillary action and the gravity action of the microfiber contained in the fiber column, and flows from the top end of the fiber column 124 to the bottom end of the fiber column 124 along with the continuous addition of the liquid and flows out from the outlet 1221 through the outlet channel 1223.
Wherein the outer diameter of the fiber column 124 is smaller than the inner diameter of the transparent tube 125 and smaller than the inner diameter of the isolation sleeve 123, an annular cavity 127 can be formed between the transparent tube 125 and the fiber column 124 and is installed in the isolation sleeve 123. The fiber column is preferably made of hard PP fiber column, has good hydrophilicity, is not easy to deform and damage, is easy to clean and is convenient to install and disassemble.
According to the present invention, an isolation sleeve 123 is provided on the outer surface of the fiber column 124, and an opening 1231 is provided on one side of the isolation sleeve 123, as shown in fig. 2. Specifically, on one hand, the isolation sleeve 123 can prevent the air flow from the air inlet channel in the oblique direction from generating large impact on the liquid distributed on the fiber column 124, so that the liquid is unevenly distributed or even separated from the fiber column to form liquid drops which enter the air channel to pollute the reactor and a subsequent air channel system, and meanwhile, can prevent the liquid from reacting due to premature contact with the gas to affect the detection effect; in another aspect. The partially open spacer sleeve 123 protects the fiber column and improves the effectiveness of the reaction. By the spacer 123, the liquid can be detected by contacting the gas and reacting with the gas only at a position on the fiber column 124 that is exposed from the opening 1231 and faces the light-sensing portion of the photodetection sensor 14.
The isolation sleeve 123 is preferably made of a light-proof material, which is beneficial to improving the light-proof effect; the isolation sleeve 123 is preferably made of corrosion-resistant material to prevent chemical reaction when contacting gas and liquid, which affects the use effect or detection effect. Preferably, the isolation sleeve 123 is a heat shrink tube of black teflon material. In addition, the fiber post 124 is preferably recessed to form a terrace portion 1241 in a portion corresponding to the opening 1231 of the isolation sleeve 123, which can produce better reaction and detection effects.
The isolation sleeve 123 can well support and fix the fiber column 124, and a notch such as an opening part is formed at a position facing the photoelectric detection sensor 14, so that gas and a detection reagent can be ensured to contact at the position and generate a chemiluminescence reaction. And at the position opposite to the photoelectric detection sensor, the gas-liquid separation is carried out by using the separation sleeve to prevent the gas-liquid reaction. The effective utilization rate of detection reagent and gas-liquid reaction is improved favorably like this to the partly indent of naked hourglass of fiber column forms platform portion, can prevent effectively that gas-liquid contact reaction department liquid from breaking away from fiber column and getting into gas circuit passageway pollution detector and gas circuit.
The transparent tube 125 used in the present invention is a tubular structure, preferably a high-purity quartz tube having a tubular structure.
As shown in fig. 3, the liquid path unit 2 of the present invention includes a liquid delivery module 22 and a liquid storage module 21 connected to a liquid inlet 1211 and a liquid outlet 1221 through a liquid inlet hole 111 and a liquid outlet hole 112 on the light-shielding front cover 11, wherein the liquid inlet hole 111 is communicated with the liquid inlet 1211, and the liquid outlet hole 112 is communicated with the liquid outlet 1221. The air path unit 3 of the present invention includes an air pumping module connected to the air outlet 1212 through the air outlet 113 of the light-shielding front cover 11, and of course, the air inlet 114 of the light-shielding front cover 11 is directly connected to the air source to be detected.
The liquid storage module 21 includes a first reagent storage subunit 211, a second reagent storage subunit 212, a cleaning reagent storage subunit 214, and a waste liquid collection subunit 213, the liquid delivery module 22 includes a reagent pump 221 and a cleaning pump 222, and the air pumping module includes an air pumping pump. The control unit 4 is electrically connected with the photoelectric detection sensor 14 of the detection unit 1, the infusion module 22 in the liquid path unit 2 and the air extraction module in the air path unit 3, so as to realize automatic control during detection.
Preferably, the reagent pump 221 adopted in the present invention is a three-channel micro ball peristaltic pump, the first reagent storage subunit 211 and the second reagent storage subunit 212 are respectively connected to the liquid inlet 1211 through two channels of the reagent pump 221, the liquid outlet 1221 is connected to the waste liquid storage subunit 213 through another channel of the reagent pump 221, thereby forming an input channel for the detection reagent, and the first reagent and the second reagent can respectively enter the tubular gas-liquid interface reactor under the action of the reagent pump 221 and are discharged after the detection reaction.
Similarly, the cleaning pump 222 is a two-channel micro ball peristaltic pump, the cleaning reagent storage subunit 214 is connected with the liquid inlet 1211 through one channel of the cleaning pump 222, and the liquid outlet 1221 is connected with the waste liquid collecting subunit 213 through the other channel of the cleaning pump 222, so that an input channel of the cleaning reagent is formed, and the cleaning reagent can enter the tubular gas-liquid interface reactor under the action of the cleaning pump 222 and is discharged after the cleaning of the reactor.
The invention also provides a carbon dioxide gas detection method, which adopts the carbon dioxide gas detection device to detect the concentration of the carbon dioxide gas.
Specifically, the detection method may include the steps of:
step 1:
and assembling the detection device, continuously controlling the liquid path unit to introduce the detection reagent into the liquid inlet channel of the tubular gas-liquid interface reactor through the liquid inlet, and leading the detection reagent out of the liquid outlet channel and discharging the detection reagent out of the tubular gas-liquid interface reactor through the liquid outlet.
With the continuous entering of the detection reagent, the detection reagent is uniformly distributed on the surface and inside of the fiber column under the capillary action and the gravity action of the fiber column, moves downwards to reach the liquid outlet channel, and then is discharged out of the tubular gas-liquid interface reactor through the liquid outlet.
The carbon dioxide detection reagent adopted by the invention comprises a first reagent and a second reagent, wherein the first reagent is a hydrogen peroxide solution, and the second reagent is a mixed solution of potassium hydroxide and potassium carbonate. And during detection, the liquid inlet flow rate of the first reagent and the liquid outlet flow rate of the second reagent are preferably the same and slightly larger than the sum of the liquid inlet flow rates of the first reagent and the second reagent.
Step 2:
the control gas circuit unit leads the detection gas into the gas inlet channel of the tubular gas-liquid interface reactor through the gas inlet and leads the reacted gas out of the gas outlet channel and discharges the gas out of the tubular gas-liquid interface reactor through the gas outlet.
Therefore, carbon dioxide in the gas to be detected entering the tubular gas-liquid interface reactor reacts with the detection reagent on the surface of the fiber column exposed from the opening part of the isolation sleeve to generate a chemiluminescent signal, and the reacted gas is discharged out of the tubular gas-liquid interface reactor from the gas outlet.
And step 3:
and detecting a chemiluminescence signal generated by gas-liquid interface chemiluminescence reaction in the tubular gas-liquid interface reactor through a photoelectric detection sensor, converting the chemiluminescence signal into an electric signal, and recording and calculating to obtain the actual concentration of the carbon dioxide.
And 4, step 4:
after the detection is finished, the liquid path unit is controlled to lead the cleaning reagent into the liquid inlet channel of the tubular gas-liquid interface reactor through the liquid inlet and lead the cleaning reagent out of the liquid outlet channel and discharge the cleaning reagent out of the tubular gas-liquid interface reactor through the liquid outlet to finish the cleaning,
wherein, the cleaning reagent can be a mixed solution of deionized water, ethanol and glycerol. In the cleaning process, the effluent flow rate of the cleaning reagent is preferably controlled to be 3-5 times of the inlet flow rate.
The invention is further illustrated below with reference to specific carbon dioxide detection examples.
Example (b):
the carbon dioxide detection device of the invention is used for detecting the concentration of carbon dioxide in air.
Preparation of a detection reagent: boiling deionized water for 30 minutes, and naturally cooling to normal temperature for preparing a first reagent and a second reagent, wherein the first reagent is a hydrogen peroxide solution, and the concentration of hydrogen peroxide is as follows: 0.0001-1 mol/L, and the concentration of the hydrogen peroxide is preferably 0.1 mol/L; the second reagent is a mixed solution of potassium hydroxide and potassium carbonate, the concentration of the potassium hydroxide is 0.0001-1 mol/L, the concentration of the potassium carbonate is 0.0001-1 mol/L, the concentration of the potassium hydroxide is preferably 0.5mol/L, and the concentration of the potassium carbonate is preferably 0.25 mol/L.
Preparing a cleaning reagent: dissolving glycerol into a mixed solution of deionized water and ethanol to prepare a cleaning solution, wherein the mixing ratio of the deionized water to the ethanol is 1: 1, the volume concentration of the glycerol is 5%.
Detection of carbon dioxide gas: and the first reagent and the second reagent are pumped out from the corresponding reagent storage subunit at the flow rate of 30ul/min to enter a liquid pipeline under the action of the reagent pump, are mixed at the rear end of the reagent pump, and the mixed reagent enters a liquid inlet channel of the tubular gas-liquid interface reactor. Along with the continuous entering of the detection reagent, the detection reagent contacts the fiber column, is uniformly distributed on the surface and inside of the fiber column under the action of capillary action and gravity, moves downwards to reach the liquid outlet channel, is pumped out of the detection unit at a flow rate of about 80-100 ul/min (slightly larger than the sum of the flow rates of the two detection reagents) along with the reverse channel of the reagent pump, and is collected in the waste liquid storage subunit.
The control gas circuit unit sucks air into the gas inlet channel of the tubular gas-liquid interface reactor from the gas inlet, and leads the reacted gas out of the gas outlet channel and discharges the reacted gas out of the tubular gas-liquid interface reactor through the gas outlet. Carbon dioxide in the air entering the tubular gas-liquid interface reactor reacts with the mixed detection reagent on the surface of the fiber column exposed from the opening part of the isolation sleeve to generate a chemiluminescent signal, and the reacted gas is discharged out of the tubular gas-liquid interface reactor from the gas outlet.
And detecting the gas-liquid interface chemiluminescence signal in the tubular gas-liquid interface reactor by a photoelectric detection sensor, converting the gas-liquid interface chemiluminescence signal into an electric signal, and recording and calculating to obtain the actual concentration of the carbon dioxide. The calculation formula of the carbon dioxide concentration is as follows: and C is kS + b, wherein C is the actual concentration value of the measured carbon dioxide, S is the output signal of the photoelectric detection sensor, and k and b are constants and can be obtained by performing linear fitting on the luminescence signals measured by the carbon dioxide standard gas with different concentration levels.
And after the detection is finished, the liquid path unit is controlled to introduce the cleaning reagent into the liquid inlet channel of the tubular gas-liquid interface reactor through the liquid inlet, and the cleaning reagent is led out from the liquid outlet channel and is discharged out of the tubular gas-liquid interface reactor through the liquid outlet to finish cleaning. The cleaning process is generally 10min, and the cleaning speed is about 200 ul/min.
The carbon dioxide gas detection device and the detection method realize the real-time online continuous detection of the carbon dioxide gas with high sensitivity and high time resolution based on the gas-liquid phase interface chemiluminescence technology, and the detection sensitivity can reach below ppmv level. Compared with the currently commonly used non-dispersive infrared absorption spectrum technology, the method is not influenced by environmental moisture, aerosol and other interference gases, and has the advantages of low detection cost, high detection speed, and higher accuracy and stability.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
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