CN110006876A - A kind of device for testing carbon dioxide gas and detection method - Google Patents

A kind of device for testing carbon dioxide gas and detection method Download PDF

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Publication number
CN110006876A
CN110006876A CN201910332948.XA CN201910332948A CN110006876A CN 110006876 A CN110006876 A CN 110006876A CN 201910332948 A CN201910332948 A CN 201910332948A CN 110006876 A CN110006876 A CN 110006876A
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gas
reagent
carbon dioxide
protected
liquid
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CN110006876B (en
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王竹青
付大友
袁东
谭文渊
廖琴瑶
李鲜萍
谭浩兰
李佳祁
陈雨琴
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Sichuan University of Science and Engineering
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Sichuan University of Science and Engineering
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/05Flow-through cuvettes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/76Chemiluminescence; Bioluminescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N2021/0325Cells for testing reactions, e.g. containing reagents
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/05Flow-through cuvettes
    • G01N2021/058Flat flow cell

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

The invention discloses device for testing carbon dioxide gas and detection methods, detection device includes detection unit, fluid path unit, gas circuit unit and control unit, detection unit includes being protected from light shell, tubular type gas-liquid interface reactor and photoelectric testing sensor, be protected from light shell have be protected from light cavity, tubular type gas-liquid interface reactor and photoelectric testing sensor setting are being protected from light in cavity, fluid path unit includes the infusion module being connected with inlet and liquid outlet and liquid storage module, gas circuit unit includes the air suction module being connected with gas outlet, the photoelectric testing sensor of control unit and detection unit, air suction module electrical connection in infusion module and gas circuit unit in fluid path unit.The carbon dioxide gas body detecting method carries out the detection of density of carbon dioxide gas using above-mentioned carbon dioxide gas tubular type detection device.The present invention is based on gas liquid film chemiluminescence, the highly sensitive on-line checking of carbon dioxide gas is realized, it is at low cost, speed is fast, accuracy and stability with higher.

Description

A kind of device for testing carbon dioxide gas and detection method
Technical field
The present invention relates to the technical fields of chemiluminescence detection, more particularly, are related to a kind of carbon dioxide gas detection Device and detection method.
Background technique
Currently, generally using non-dispersive infrared absorption method for the detection of carbon dioxide gas, testing cost is low, operates Simple and detection speed is fast, and continuous on-line determination may be implemented.But this method is easy by moisture in gas in the detection process And the interference effect of aerosol, error is larger, and Stability and veracity hardly results in guarantee.Gas liquid film chemiluminescence inspection Survey technology is a kind of detection method of high sensitivity, has been successfully applied to nitrogen dioxide in atmosphere, ozone, sulfur dioxide, first The on-line checking of the trace gas such as aldehyde.Relative to traditional detection method, it is excellent that the testing cost of the technology is low, device structure is simple etc. Point, with good application prospect.But the technology is not yet applied to the detection of carbon dioxide gas at present.
Gas liquid film chemiluminescence detection technology in practical applications, need by a specific reaction bed structure come One flowing gas liquid reaction interface is provided and realizes gas liquid film chemiluminescence reaction.In previous technology, the reaction bed one As use high hydrophilic film material (such as silk, filter paper, PP fabric nonwoven cloth, polyester fiber cloth), its advantage is that can mention For biggish reaction interface to obtain higher detection sensitivity.But the high-hydrophilic of such reaction bed and high wellability Characteristic depends on the fractal of its internal superfine fibre support.With being used for multiple times for reaction bed, in reaction bed The multidimensional structure in portion gradually hardened can collapse, so that its hydrophily and wellability are gradually deteriorated.Simultaneously as this kind of reaction bed compared with It is soft and there is certain tensile ductility, it is difficult being fixed in reactor for uniform ground, consistency difference and the inspection for influencing equipment Survey performance.
Summary of the invention
In order to solve the problems in the existing technology, the object of the present invention is to provide a kind of detections of carbon dioxide gas to fill It sets and detection method, the high sensitivity for more preferably realizing carbon dioxide gas based on gas liquid film chemiluminescence is online Detection.
An aspect of of the present present invention provides device for testing carbon dioxide gas, and the detection device includes detection unit, liquid Road unit, gas circuit unit and control unit, wherein
The detection unit includes being protected from light shell, tubular type gas-liquid interface reactor and photoelectric testing sensor, described to be protected from light Shell, which has, is protected from light cavity, and the tubular type gas-liquid interface reactor and photoelectric testing sensor setting are being protected from light in cavity;
The tubular type gas-liquid interface reactor includes top connection, lower contact, transparent tube body, fibre columns and disrance sleeve, on Connector be equipped with inlet, feed pathway, gas outlet and outlet passageway, lower contact be equipped with liquid outlet, liquid outlet channel, air inlet and into Gas channel, is connected with transparent tube body between top connection and lower contact;
The fibre columns are arranged in transparent tube body, and the both ends of fibre columns are respectively and fixedly installed to feed pathway and liquid is logical out In road;The disrance sleeve is arranged on the outer surface of fibre columns, and the side of the disrance sleeve is provided with opening portion;It is described Ring-shaped cavity is formed between bright tube body and fibre columns, the ring-shaped cavity is connected to inlet channel and outlet passageway and passes through institute The opening portion for stating disrance sleeve is connected to fibre columns;The photographic department face tubular type gas-liquid interface of the photoelectric testing sensor reacts The opening portion of disrance sleeve described in the transparent tube body and face of device.
The fluid path unit includes the infusion module being connected with inlet and liquid outlet and liquid storage module;
The gas circuit unit includes the air suction module being connected with gas outlet;
The photoelectric testing sensor of described control unit and the detection unit, infusion module and gas circuit in fluid path unit Air suction module electrical connection in unit.
One embodiment of device for testing carbon dioxide gas according to the present invention, the shell that is protected from light includes being protected from light shell Be protected from light front cover, it is described to be protected from light shell and be assembled to form with front cover is protected from light with the shell that is protected from light for being protected from light cavity, it is described to be protected from light front cover On be provided with hole location corresponding with the top connection of the tubular type gas-liquid interface reactor and lower contact, the tubular type gas-liquid interface Reactor, which is fixed on, to be protected from light on front cover.
One embodiment of device for testing carbon dioxide gas according to the present invention, the top connection and lower contact with it is transparent Endless groove is provided at the position of tube body connection, the transparent tube body is mounted in endless groove and is fixed by sealing, wherein thoroughly It is perfused when bright tube body is installed using black silica gel.
One embodiment of device for testing carbon dioxide gas according to the present invention, the top connection and lower contact be not using The resistant material of light transmission is made, the inlet channel of the outlet passageway of top connection and lower contact be tubular conduit and internal diameter with it is transparent The internal diameter of tube body is identical.
One embodiment of device for testing carbon dioxide gas according to the present invention, the disrance sleeve is using lighttight Resistant material is made, and the outer diameter of the fibre columns is less than the internal diameter of disrance sleeve and is less than the internal diameter of transparent tube body, the fibre Dimension column is vertically installed at the central position of transparent tube body, and the fibre columns are made of the PP fibre columns of hard, wherein fiber Column part corresponding with the opening portion of disrance sleeve is recessed platform part.
One embodiment of device for testing carbon dioxide gas according to the present invention, the liquid storage module include the first reagent Store subelement, the second reagent storage subelement, cleaning reagent storage subelement and waste collection subelement, the infusion module Including reagent pump and cleaning pump, the air suction module includes aspiration pump.
One embodiment of device for testing carbon dioxide gas according to the present invention, the reagent pump are the miniature rolling of triple channel Bead peristaltic pump, the first reagent storage subelement, the second reagent storage subelement pass through the two paths of the reagent pump respectively It is connected with inlet, liquid outlet is connected by another paths of the reagent pump with waste collection subelement;The cleaning pump For binary channels Miniature ball formula peristaltic pump, cleaning reagent stores all the way channel and inlet phase of the subelement by the cleaning pump Even, liquid outlet is connected by another paths of the cleaning pump with waste collection subelement.
Another aspect provides a kind of carbon dioxide gas body detecting methods, using above-mentioned carbon dioxide gas physical examination Survey the detection that device carries out density of carbon dioxide gas.
One embodiment of carbon dioxide gas body detecting method according to the present invention, described detection method includes the following steps:
Step 1: assembling detection device, constantly control fluid path unit will test reagent and be passed through tubular type gas-liquid by inlet The feed pathway of interfacial reactor and will test reagent drawn from liquid outlet channel and by liquid outlet be discharged tubular type gas-liquid interface Reactor, wherein the detection reagent includes the first reagent and the second reagent, and the first reagent is hydrogenperoxide steam generator, the second examination Agent is the mixed solution of potassium hydroxide and potassium carbonate, and the feed liquor flow velocity of the first reagent and the second reagent is identical and flow velocity is bigger out In the sum of the first reagent and the feed liquor flow velocity of the second reagent;
Step 2: it is logical that control gas circuit unit will test the air inlet that gas is passed through tubular type gas-liquid interface reactor by air inlet Road and by the gas after reaction drawn from outlet passageway and by gas outlet be discharged tubular type gas-liquid interface reactor;
Step 3: gas-liquid interface chemiluminescence reaction in tubular type gas-liquid interface reactor is detected by photoelectric testing sensor The chemiluminescence signal of generation is simultaneously converted to electric signal, records and calculates the actual concentrations for obtaining carbon dioxide;
Step 4: controlling fluid path unit after detection for cleaning reagent and the reaction of tubular type gas-liquid interface is passed through by inlet The feed pathway of device and by cleaning reagent drawn from liquid outlet channel and by liquid outlet be discharged tubular type gas-liquid interface reactor it is complete At cleaning, wherein the cleaning reagent is the mixed liquor of deionized water, ethyl alcohol and glycerine, and the flow velocity that goes out of cleaning reagent is 3~5 times of feed liquor flow velocity.
Compared with prior art, the present invention provides a kind of device for testing carbon dioxide gas and detection methods, are based on gas Liquid interface chemiluminescence realizes the highly sensitive on-line checking of carbon dioxide gas.It, will not relative to current techniques The influence of other interference gas in environmental gas is influenced and will receive by moisture and aerosol, and testing cost is low, detects Speed is fast, while accuracy with higher and stability.
Detailed description of the invention
The Integral connection structure that Fig. 1 shows device for testing carbon dioxide gas according to an exemplary embodiment of the present invention shows It is intended to.
Fig. 2 shows the structures of detection unit in device for testing carbon dioxide gas according to an exemplary embodiment of the present invention Schematic diagram.
Fig. 3 shows the tubular type of detection unit in device for testing carbon dioxide gas according to an exemplary embodiment of the present invention The structural schematic diagram of gas-liquid interface reactor.
Description of symbols:
1- detection unit;11- is protected from light front cover, 111- inlet opening, 112- fluid hole, 113- venthole, 114- air inlet; 12- tubular type gas-liquid interface reactor, 121- top connection, 122- lower contact, 123- disrance sleeve, the opening portion 1231-, 124- fiber Column, 1241- platform part, 125- transparent tube body, 126- endless groove, 127- ring-shaped cavity, 1211- inlet, the gas outlet 1212-, 1213- feed pathway, 1214- outlet passageway, 1221- liquid outlet, 1222- air inlet, 1223- liquid outlet channel, 1224- air inlet are logical Road;13- is protected from light shell, 14- photoelectric testing sensor;
2- fluid path unit, 21- liquid storage module, the first reagent of 211- store subelement, the second reagent of 212- stores subelement, 213- waste collection subelement, 214- cleaning reagent store subelement;22- infusion module, 221- reagent pump, 222- cleaning pump; 3- gas circuit unit, 4- control unit.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics ?.
First device for testing carbon dioxide gas of the invention is specifically described in conjunction with attached drawing below.
The Integral connection structure that Fig. 1 shows device for testing carbon dioxide gas according to an exemplary embodiment of the present invention shows It is intended to.
As shown in Figure 1, an exemplary embodiment of the present invention, the device for testing carbon dioxide gas includes that detection is single Member 1, fluid path unit 2, gas circuit unit 3 and control unit 4, wherein detection unit 1 is to utilize gas liquid film chemiluminescence detection The primary clustering that technology detects carbon dioxide, fluid path unit 2 is used to provide to detection unit 1 and reclaim reagent or cleaning Reagent, gas circuit unit 3 are used to provide detection gas to detection unit 1, and control unit 3 controls the movement of detection device and realizes two The detection of carbonoxide.
Fig. 2 shows the structures of detection unit in device for testing carbon dioxide gas according to an exemplary embodiment of the present invention Schematic diagram.
As shown in Figures 2 and 3, detection unit 1 of the invention includes being protected from light shell, tubular type gas-liquid interface reactor 12 and light Electro-detection sensor 14 is protected from light shell with cavity is protected from light, and tubular type gas-liquid interface reactor 12 and photoelectric testing sensor 14 are set It sets and is being protected from light in cavity.Wherein, the gas-liquid interface chemiluminescence reaction of detection gas is sent out in tubular type gas-liquid interface reactor 12 Raw, photoelectric testing sensor 5 detects chemiluminescence signal and exports after being converted to electric signal, and being protected from light shell then is reaction and detection Light protected environment is provided.
Fig. 3 shows the tubular type of detection unit in device for testing carbon dioxide gas according to an exemplary embodiment of the present invention The structural schematic diagram of gas-liquid interface reactor.
As shown in figure 3, tubular type gas-liquid interface reactor includes top connection 121, lower contact 122, transparent tube body 125, fiber Column 124 and disrance sleeve 123, top connection 121 are equipped with inlet 1211, feed pathway 1213, gas outlet 1212 and outlet passageway 1214, lower contact 122 is equipped with liquid outlet 1221, liquid outlet channel 1223, air inlet 1222 and inlet channel 1224.
Preferably, being protected from light shell includes being protected from light shell 13 and being protected from light front cover 11, is protected from light shell 13 and is protected from light the assembly of front cover 11 Being formed has be protected from light cavity to be protected from light shell, is protected from light the top connection 121 being provided on front cover 11 with tubular type gas-liquid interface reactor With the corresponding hole location of lower contact 122, tubular type gas-liquid interface reactor 12, which is then fixed on, to be protected from light on front cover 11.
Top connection 121 and lower contact 122 are preferably made of lighttight resistant material, and shell 13 is protected from light after installation It is protected from light cavity with being protected from light front cover 11 and being assembled to form, the internal cavity of tubular type gas-liquid interface reactor 12 is set by being protected from light on front cover 11 It sets inlet opening 111, fluid hole 112, venthole 113, air inlet 114 to be connected to external fluid path unit 2 and gas circuit unit 3, outside Portion's light will not be entered by gas liquid channel system to be protected from light in cavity and tubular type gas-liquid interface reactor, will not be produced to testing result It is raw to influence.
According to the present invention, transparent tube body 125 is connected between top connection 121 and lower contact 122, the setting of fibre columns 124 exists In transparent tube body 125, the both ends of fibre columns 124 are respectively and fixedly installed in feed pathway 1213 and liquid outlet channel 1223;Isolation Casing 123 is arranged on the outer surface of fibre columns 124, and the side of disrance sleeve 123 is provided with opening portion 1231;Transparent tube body Ring-shaped cavity 127 is formed between 125 and fibre columns 124, ring-shaped cavity 127 is connected to inlet channel 1224 and outlet passageway 1214 And it is connected to by the opening portion 1231 of disrance sleeve 123 with fibre columns 124;The photographic department face pipe of photoelectric testing sensor 14 The transparent tube body 125 of formula gas-liquid interface reactor 12 and the opening portion 1231 of face disrance sleeve 123.
Wherein, it above connects and is provided with endless groove 126 at 121 and the position that connect with transparent tube body 125 of lower contact 122, then Transparent tube body 125 is mounted in endless groove 126 and is fixed by sealing.Preferably, black silica gel is used when transparent tube body 125 is installed Perfusion.
Also, the outlet passageway 1214 of top connection 121 and the inlet channel 1224 of lower contact 122 are tubular conduit and internal diameter Identical as the internal diameter of transparent tube body 125, then the gas circuit that connection is formed after transparent tube body 125 is installed between upper lower contact is logical Road is not present dead volume in junction and will not influence the flowing of gas.
The both ends of fibre columns 124 are respectively placed in the feed pathway 1213 and liquid outlet channel 1223 of lower contact, fibre columns 124 are preferably vertically installed at the central location of transparent tube body 125.The reagent liquid reacted is participated in as a result, from top connection 121 After inlet 1211 enters feed pathway 1213, the top of fibre columns 124 and the capillary of the superfine fibre contained by fibre columns are reached The surface and inside of fibre columns 124 are evenly distributed under effect and gravity, with being continuously added into from fibre columns 124 for liquid Top flow to fibre columns 124 bottom end and by liquid outlet channel 1223 from liquid outlet 1221 flow out.
Wherein, the outer diameter of fibre columns 124 is less than the internal diameter of transparent tube body 125 and is less than the internal diameter of disrance sleeve 123, then Ring-shaped cavity 127 can be formed between transparent tube body 125 and fibre columns 124, and is mounted in disrance sleeve 123.Fiber Column preferably uses the PP fibre columns of hard to be made, and good hydrophilic property is unlikely to deform damage, is readily cleaned and is easily installed disassembly.
According to the present invention, the outer surface of fibre columns 124 is equipped with disrance sleeve 123, and the side of disrance sleeve 123 is provided with Opening portion 1231, specific structure is as shown in Figure 2.Specifically, on the one hand, disrance sleeve 123 can be prevented from inlet channel The air-flow of inclined direction generates biggish impact to liquid be distributed in fibre columns 124, causes liquid distribution uneven or even Be detached from fiber columnar and enter gas channels pollution reactor and subsequent air-channel system at drop, at the same can prevent again liquid with Gas premature contact generates reaction and influences detection effect;On the other hand.The disrance sleeve 123 of outs open can protect fiber Column improves the validity of reaction.Under the action of disrance sleeve 123, liquid is in fibre columns 124 only from opening portion 1231 When exposing and the position of the photographic department of face photoelectric testing sensor 14, it can be contacted with gas and react and be detected It measures.
Disrance sleeve 123 is preferably made of light-proof material, is conducive to improve light-shading effect;Disrance sleeve 123 is excellent Selection of land is made of resistant material, is prevented from chemically reacting when contacting gas with liquid, is influenced using effect or inspection Survey effect.Preferably, disrance sleeve 123 is the heat-shrink tube of black polytetrafluoroethylene material.Furthermore it is preferred that in fibre columns 124 Part corresponding with the opening portion 1231 of disrance sleeve 123 is recessed platform part 1240, can generate and more preferably react and examine Survey effect.
Disrance sleeve 123 can play preferable support fixed function to fibre columns 124, in face photoelectric testing sensor 14 position is provided with the notch such as opening portion, it is ensured that gas and detection reagent can contact concurrent biochemical hair in the position Light reaction.And in the position back to photoelectric testing sensor, then gas-liquid isolation is carried out using disrance sleeve, prevents gas liquid reaction Occur.Be conducive to improve the effective rate of utilization of detection reagent and gas liquid reaction, and the naked leakage part concave shaped of fibre columns in this way At platform part, liquid disengaging fibre columns at gas-liquid contact reaction can be effectively prevented and enter gas channels pollution detection device and gas Road.
Transparent tube body 125 used in the present invention is tubular structure, preferably the high purity quartz pipe of tubular structure.
As shown in figure 3, fluid path unit 2 of the invention includes the inlet opening 111 and fluid hole 112 by being protected from light on front cover 11 The infusion module 22 and liquid storage module 21 being connected with inlet 1211 and liquid outlet 1221, wherein inlet opening 111 and feed pathway 1211 connections, fluid hole 112 are connected to liquid outlet channel 1221.Gas circuit unit 3 of the invention then includes by being protected from light on front cover 11 The air suction module that is connected with gas outlet 1212 of venthole 113, be protected from light certainly air inlet 114 on front cover 11 directly with it is to be detected Gas source connection.
Liquid storage module 21 includes the first reagent storage subelement 211, the second reagent storage subelement 212, cleaning reagent storage Subelement 214 and waste collection subelement 213 are deposited, infusion module 22 includes reagent pump 221 and cleaning pump 222, air suction module packet Include aspiration pump.Control unit 4 is then gentle with the infusion module 22 in the photoelectric testing sensor 14 of detection unit 1, fluid path unit 2 Air suction module electrical connection in road unit 3, to realize automatic control when detection.
Preferably, the reagent pump 221 used in the present invention is triple channel Miniature ball formula peristaltic pump, the first reagent storage Unit 211, the second reagent storage subelement 212 are connected by the two paths of reagent pump 221 with inlet 1211 respectively, out liquid Mouth 1221 stores subelement 213 by another paths and waste liquid of reagent pump 221 and is connected, and thus forms the defeated of detection reagent Enter access, the first reagent and the second reagent can enter in tubular type gas-liquid interface reactor under the action of reagent pump 221 respectively And it is discharged after detection reaction.
Similar, cleaning pump 222 is binary channels Miniature ball formula peristaltic pump, and cleaning reagent stores subelement 214 and passes through clearly The channel all the way for washing pump 222 is connected with inlet 1211, and liquid outlet 1221 is received by another paths and waste liquid of cleaning pump 222 Collect subelement 213 to be connected, thus forms the input channel of cleaning reagent, cleaning reagent can be under the action of cleaning pump 222 It is discharged into tubular type gas-liquid interface reactor and after cleaning reactor.
The present invention also provides carbon dioxide gas body detecting method, which employs above-mentioned device for testing carbon dioxide gas into The Concentration Testing of row carbon dioxide gas.
Specifically, which may comprise steps of:
Step 1:
Detection device is assembled, constantly controlling fluid path unit will test reagent by inlet to be passed through tubular type gas-liquid interface anti- It answers the feed pathway of device and will test reagent and drawn from liquid outlet channel and tubular type gas-liquid interface reactor is discharged by liquid outlet.
With continuing into for detection reagent, detection reagent is equably divided under fibre columns capillarity and gravity Cloth is in the surface of fibre columns and inside and moves down arrival liquid outlet channel, and it is anti-that tubular type gas-liquid interface then is discharged by liquid outlet Answer device.
Wherein, the carbon dioxide detection reagent that the present invention uses includes the first reagent and the second reagent, and the first reagent was Hydrogen peroxide solution, the second reagent are the mixed solution of potassium hydroxide and potassium carbonate.And when detecting, preferably the first reagent and The feed liquor flow velocity of second reagent is identical and flow velocity is slightly larger than the sum of the first reagent and the feed liquor flow velocity of the second reagent out.
Step 2:
Control gas circuit unit will test gas by air inlet be passed through tubular type gas-liquid interface reactor inlet channel and Gas after reaction is drawn from outlet passageway and tubular type gas-liquid interface reactor is discharged by gas outlet.
It as a result, can be with the opening from disrance sleeve into the carbon dioxide in the under test gas of tubular type gas-liquid interface reactor The detection reagent on the fibre columns surface that portion exposes reacts and generates chemiluminescence signal, and the gas after reaction is arranged from gas outlet Tubular type gas-liquid interface reactor out.
Step 3:
Detect what gas-liquid interface chemiluminescence reaction in tubular type gas-liquid interface reactor generated by photoelectric testing sensor Chemiluminescence signal is simultaneously converted to electric signal, records and calculates the actual concentrations for obtaining carbon dioxide.
Step 4:
After detection control fluid path unit by cleaning reagent by inlet be passed through tubular type gas-liquid interface reactor into Liquid channel and by cleaning reagent drawn from liquid outlet channel and by liquid outlet be discharged tubular type gas-liquid interface reactor complete cleaning,
Wherein, cleaning reagent can be deionized water, the mixed liquor of ethyl alcohol and glycerine.In the process of cleaning, preferably The flow velocity out for controlling cleaning reagent is 3~5 times of feed liquor flow velocity.
Below with reference to specific carbon dioxide detection embodiment, the present invention will be further described.
Embodiment:
Utilize the concentration of carbon dioxide detection detection device detection Carbon Dioxide in Air of the invention.
The preparation of detection reagent: naturally cooling to room temperature after deionized water is boiled 30 minutes, for preparing the first reagent With the second reagent, wherein the first reagent is hydrogenperoxide steam generator, the concentration of hydrogen peroxide are as follows: 0.0001~1mol/L, peroxidating The concentration of hydrogen is preferably 0.1mol/L;Second reagent is the mixed solution of potassium hydroxide and potassium carbonate, and the concentration of potassium hydroxide is The concentration of 0.0001~1mol/L, potassium carbonate are 0.0001~1mol/L, and the concentration of potassium hydroxide is preferably 0.5mol/L, carbonic acid The concentration of potassium is preferably 0.25mol/L.
The preparation of cleaning reagent: glycerine is dissolved in the mixed liquor of deionized water and ethyl alcohol and is configured to cleaning solution, wherein Deionized water and the mixed proportion of ethyl alcohol are 1:1, and the volumetric concentration of glycerine is 5%.
The detection of nitrogen dioxide gas: the first reagent and the second reagent are under the action of reagent pump, with 30ul/min's Flow extraction from corresponding reagent storage subelement enters liquid line, and mixes in the rear end of reagent pump, mixed mixed Close the feed pathway that reagent enters tubular type gas-liquid interface reactor.With continuing into for detection reagent, detection reagent contact is fine Dimension column is simultaneously evenly distributed in the surface of fibre columns and inside and moving down reaches out under its capillarity and gravity Liquid channel, and as the flow with about 80~100ul/min in reagent pump backward channel (is slightly larger than two-way detection reagent stream The sum of amount) it is extracted detection unit and is collected in waste liquid storage subelement.
Inlet channel of the gas circuit unit by air from air inlet sucking tubular type gas-liquid interface reactor is controlled, and will reaction Gas afterwards draws from outlet passageway and tubular type gas-liquid interface reactor is discharged by gas outlet.It is reacted into tubular type gas-liquid interface Carbon dioxide in the air of device can occur with the hybrid detection reagent on the fibre columns surface exposed from the opening portion of disrance sleeve Chemiluminescence signal is reacted and generates, tubular type gas-liquid interface reactor is discharged from gas outlet in the gas after reaction.
Gas-liquid interface chemiluminescence signal is detected and is converted to by photoelectric testing sensor in tubular type gas-liquid interface reactor Electric signal records and calculates the actual concentrations for obtaining carbon dioxide.The calculation formula of content of nitrogen dioxide are as follows: C=kS+b, In, C by survey carbon dioxide actual concentrations value, S is the output signal of photoelectric testing sensor, and k and b are constant, can be passed through The surveyed luminous signal of the carbon dioxide calibrating gas of various concentration level carries out linear fit and obtains.
After detection control fluid path unit by cleaning reagent by inlet be passed through tubular type gas-liquid interface reactor into Liquid channel and by cleaning reagent drawn from liquid outlet channel and by liquid outlet be discharged tubular type gas-liquid interface reactor complete cleaning. Cleaning process is generally 10min, and cleaning speed is about 200ul/min.
Device for testing carbon dioxide gas and detection method of the invention is realized based on gas liquid film chemiluminescence The high sensitivity of carbon dioxide gas, high time resolution real-time online continuously detect, detection sensitivity is up to ppmv grades Below.Compared with currently widely used non-dispersive infrared absorption spectral technique, not will receive ambient moisture and aerosol and The influence of other interference gas, and testing cost is low, detection speed is fast, while accuracy with higher and stability.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed New feature or any new combination, and disclose any new method or process the step of or any new combination.

Claims (9)

1. a kind of device for testing carbon dioxide gas, which is characterized in that the detection device include detection unit, fluid path unit, Gas circuit unit and control unit, wherein
The detection unit includes being protected from light shell, tubular type gas-liquid interface reactor and photoelectric testing sensor, described to be protected from light shell With cavity is protected from light, the tubular type gas-liquid interface reactor and photoelectric testing sensor setting are being protected from light in cavity;
The tubular type gas-liquid interface reactor includes top connection, lower contact, transparent tube body, fibre columns and disrance sleeve, top connection Equipped with inlet, feed pathway, gas outlet and outlet passageway, it is logical that lower contact is equipped with liquid outlet, liquid outlet channel, air inlet and air inlet Road is connected with transparent tube body between top connection and lower contact;
The fibre columns are arranged in transparent tube body, and the both ends of fibre columns are respectively and fixedly installed to feed pathway and liquid outlet channel In;The disrance sleeve is arranged on the outer surface of fibre columns, and the side of the disrance sleeve is provided with opening portion;It is described transparent Ring-shaped cavity is formed between tube body and fibre columns, the ring-shaped cavity is connected to inlet channel and outlet passageway and by described The opening portion of disrance sleeve is connected to fibre columns;The photographic department face tubular type gas-liquid interface reactor of the photoelectric testing sensor Transparent tube body and face described in disrance sleeve opening portion.
The fluid path unit includes the infusion module being connected with inlet and liquid outlet and liquid storage module;
The gas circuit unit includes the air suction module being connected with gas outlet;
Photoelectric testing sensor, the infusion module in fluid path unit and the gas circuit unit of described control unit and the detection unit In air suction module electrical connection.
2. device for testing carbon dioxide gas according to claim 1, which is characterized in that the shell that is protected from light includes being protected from light Shell and it is protected from light front cover, it is described to be protected from light shell and be assembled to form with front cover is protected from light with the shell that is protected from light for being protected from light cavity, it is described to be protected from light Hole location corresponding with the top connection of the tubular type gas-liquid interface reactor and lower contact, the tubular type gas-liquid are provided on front cover Interfacial reactor, which is fixed on, to be protected from light on front cover.
3. device for testing carbon dioxide gas according to claim 1, which is characterized in that the top connection and lower contact with Endless groove is provided at the position of transparent tube body connection, the transparent tube body is mounted in endless groove and is fixed by sealing, In, it is perfused when transparent tube body is installed using black silica gel.
4. device for testing carbon dioxide gas according to claim 1, which is characterized in that the top connection and lower contact are adopted Be made of lighttight resistant material, the inlet channel of the outlet passageway of top connection and lower contact be tubular conduit and internal diameter with The internal diameter of transparent tube body is identical, and the transparent tube body is the high purity quartz pipe of tubular structure.
5. device for testing carbon dioxide gas according to claim 1, which is characterized in that the disrance sleeve is using impermeable The resistant material of light is made, and the outer diameter of the fibre columns is less than the internal diameter of disrance sleeve and is less than the internal diameter of transparent tube body, institute The central position that fibre columns are vertically installed at transparent tube body is stated, the fibre columns are made of the PP fibre columns of hard, wherein Fibre columns part corresponding with the opening portion of disrance sleeve is recessed platform part.
6. device for testing carbon dioxide gas according to claim 1, which is characterized in that the liquid storage module includes first Reagent stores subelement, the second reagent storage subelement, cleaning reagent storage subelement and waste collection subelement, the infusion Module includes reagent pump and cleaning pump, and the air suction module includes aspiration pump.
7. device for testing carbon dioxide gas according to claim 6, which is characterized in that the reagent pump is that triple channel is micro- Type ball-type peristaltic pump, the first reagent storage subelement, the second reagent storage subelement pass through the two-way of the reagent pump respectively Channel is connected with inlet, and liquid outlet is connected by another paths of the reagent pump with waste collection subelement;It is described clear Washing pump is binary channels Miniature ball formula peristaltic pump, and cleaning reagent storage subelement passes through the channel all the way of the cleaning pump and feed liquor Mouth is connected, and liquid outlet is connected by another paths of the cleaning pump with waste collection subelement.
8. a kind of carbon dioxide gas body detecting method, which is characterized in that using dioxy described in any one of claims 1 to 7 Change the detection that carbon gas-detecting device carries out density of carbon dioxide gas.
9. carbon dioxide gas body detecting method according to claim 8, which is characterized in that the detection method includes following Step:
Step 1: assembling detection device, constantly control fluid path unit will test reagent and be passed through tubular type gas-liquid interface by inlet The feed pathway of reactor and will test reagent drawn from liquid outlet channel and by liquid outlet be discharged tubular type gas-liquid interface reaction Device, wherein the detection reagent includes the first reagent and the second reagent, and the first reagent is hydrogenperoxide steam generator, and the second reagent is The feed liquor flow velocity of the mixed solution of potassium hydroxide and potassium carbonate, the first reagent and the second reagent it is identical and out flow velocity slightly larger than the The sum of one reagent and the feed liquor flow velocity of the second reagent;
Step 2: control gas circuit unit will test gas and be passed through the inlet channel of tubular type gas-liquid interface reactor simultaneously by air inlet And the gas after reaction is drawn from outlet passageway and tubular type gas-liquid interface reactor is discharged by gas outlet;
Step 3: gas-liquid interface chemiluminescence reaction in tubular type gas-liquid interface reactor being detected by photoelectric testing sensor and is generated Chemiluminescence signal and be converted to electric signal, record and calculate the actual concentrations for obtaining carbon dioxide;
Step 4: controlling fluid path unit after detection for cleaning reagent and tubular type gas-liquid interface reactor is passed through by inlet Feed pathway and by cleaning reagent drawn from liquid outlet channel and by liquid outlet be discharged tubular type gas-liquid interface reactor complete it is clear It washes, wherein the cleaning reagent is the mixed liquor of deionized water, ethyl alcohol and glycerine, and the flow velocity that goes out of cleaning reagent is feed liquor 3~5 times of flow velocity.
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