CN111693514A - Online detection device and method utilizing online liquid-gas conversion - Google Patents

Online detection device and method utilizing online liquid-gas conversion Download PDF

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Publication number
CN111693514A
CN111693514A CN202010375130.9A CN202010375130A CN111693514A CN 111693514 A CN111693514 A CN 111693514A CN 202010375130 A CN202010375130 A CN 202010375130A CN 111693514 A CN111693514 A CN 111693514A
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liquid
channel
reaction
gas
light
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CN111693514B (en
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王风青
毕长富
杨冰
王川
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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
    • G01N21/75Systems 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
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/76Chemiluminescence; Bioluminescence
    • G01N21/766Chemiluminescence; Bioluminescence of gases
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Abstract

The invention discloses an online detection device and method by utilizing online liquid-gas conversion, wherein the online detection device comprises a double-flow-path reactor, a light-shading shell and a photoelectric sensor; a reaction cavity is arranged in the body of the double-flow-path reactor, and the top of the reaction cavity is sealed and light-transmitting through a light-transmitting sheet; the bottom of the reaction cavity is provided with a first channel and a second channel which are vertically arranged, and the two sides of the reaction cavity are respectively provided with an air inlet and an air outlet; a first reaction bed and a second reaction bed are respectively arranged in the first channel and the second channel; the light-resistant shell is assembled on the body of the double-flow-path reactor and is formed with a light-resistant cavity, the photoelectric sensor is arranged in the light-resistant cavity, and the photosensitive position penetrates through the light hole to be opposite to the light-transmitting sheet and the reaction cavity of the double-flow-path reactor. The method utilizes the device to solve the problems of low sensitivity, large interference and the like existing in the prior liquid phase chemiluminescence method for detecting nitrite and the like.

Description

Online detection device and method utilizing online liquid-gas conversion
Technical Field
The present invention relates to the technical field of chemiluminescence detection devices, and more particularly, to an online detection device and method using online liquid-gas conversion.
Background
The chemiluminescence detection technology is a high-sensitivity analysis detection method with wide application, generally has the advantages of low detection cost, simple equipment structure and the like compared with the traditional detection method, and has better application prospect.
Nitrite is a key indicator of concern in the fields of water quality, environment, food, and the like, due to its harm to the body. However, the application of the chemiluminescence technology in the field of nitrite detection has many problems, and the most important problems are low sensitivity and more interference factors. Based on a gas-liquid phase interface chemiluminescence detection technology, ultra-high sensitivity detection of nitrogen dioxide gas can be realized by utilizing a luminol detection system, and the detection limit can reach pptv level. The results of the current research have confirmed that the luminol detection system does not respond to nitrite, and therefore cannot be applied to the detection of nitrite.
Disclosure of Invention
In order to solve the problems in the prior art, the present invention provides an online detection device and method using online liquid-gas conversion.
The invention discloses an online detection device utilizing online liquid-gas conversion, which comprises a double-flow-path reactor, a light-shading shell and a photoelectric sensor, wherein the double-flow-path reactor is connected with the light-shading shell;
a reaction cavity is arranged in the body of the double-flow-path reactor, and the top of the reaction cavity is sealed and light-transmitting through a light-transmitting sheet; the bottom of the reaction cavity is provided with a first channel and a second channel which are vertically arranged, two ends of the first channel respectively extend into the body and are communicated with a first liquid inlet hole and a first liquid outlet hole which are arranged on the body, two ends of the second channel respectively extend into the body and are communicated with a second liquid inlet hole and a second liquid outlet hole which are arranged on the body, and two sides of the reaction cavity are respectively provided with an air inlet hole and an air outlet hole; a first reaction bed and a second reaction bed are respectively arranged in the first channel and the second channel, and the parts of the first channel and the second channel, which are positioned in the reaction cavity, are cut open to form an exposed area and expose the first reaction bed and the second reaction bed in the reaction cavity;
the light-resistant shell is assembled on the body of the double-flow-path reactor and is provided with a light-resistant cavity, the photoelectric sensor is arranged in the light-resistant cavity, and the photosensitive position of the photoelectric sensor penetrates through the light hole to be opposite to the light-transmitting sheet and the reaction cavity of the double-flow-path reactor.
According to one embodiment of the online detection device utilizing online liquid-gas conversion, the reaction chamber is a rhomboid chamber, the first channel and the second channel are arranged in parallel, and the air inlet hole and the air outlet hole are arranged on the left side and the right side of the reaction chamber.
According to one embodiment of the on-line detection device utilizing on-line liquid-gas conversion of the present invention, the flow direction of the fluid in the first channel and the second channel is perpendicular to the flow direction of the gas in the reaction chamber from the gas inlet hole to the gas outlet hole.
According to one embodiment of the on-line detection device utilizing on-line liquid-gas conversion according to the present invention, the first reaction bed and the second reaction bed are columnar ultrafine fibrous material pieces.
According to an embodiment of the present invention, the online detection device using online liquid-gas conversion further comprises a first peristaltic pump communicated with the first liquid inlet or the first liquid outlet, a second peristaltic pump communicated with the second liquid inlet or the second liquid outlet, a gas filter communicated with the gas inlet, and a vacuum pump communicated with the gas outlet.
According to one embodiment of the online detection device utilizing online liquid-gas conversion, the online detection device further comprises a processing system electrically connected with the photoelectric sensor and a control system electrically connected with the first peristaltic pump, the second peristaltic pump, the vacuum pump and the photoelectric sensor.
Another aspect of the present invention provides an online detection method using online liquid-gas conversion, which uses the above online detection apparatus using online liquid-gas conversion and includes the steps of:
A. after being mixed with acid liquid on line, the liquid to be detected is introduced into a first channel through a first liquid inlet hole, a detection reagent is introduced into a second channel through a second liquid inlet hole, and meanwhile, zero air enters a reaction cavity of the double-flow-path reactor through an air inlet hole;
B. the detected gas generated by the reaction of the mixed liquid entering the first channel is separated from the exposed first reaction bed and is conveyed to the surface of the exposed second reaction bed in the second channel under the carrying effect of zero air to contact with the detection reagent and generate a chemiluminescence reaction;
C. and converting the chemiluminescence signal detected by the photoelectric sensor into an electric signal, calculating to obtain the concentration of the detected gas, and calculating to obtain the concentration of the detected object in the detected liquid according to the flow velocity of the zero air and the flow velocity of the detected liquid.
According to an embodiment of the online detection method using online liquid-gas conversion of the present invention, the detected liquid contains a solution of nitrite, the acid solution is hydrochloric acid or sulfuric acid with a volume concentration of 0.1% to 10%, the detection reagent is a nitrogen dioxide detection reagent, the detected gas is nitrogen dioxide, and the detected substance in the detected liquid is nitrite.
The invention provides an online detection device and method utilizing online liquid-gas conversion, which simultaneously realize online liquid-gas conversion of nitrite, methanol and the like and high-sensitivity online detection of converted gas, thereby indirectly realizing high-sensitivity online detection of nitrite and the like and effectively avoiding interference of coexisting ions in detected liquid. The invention realizes the high-sensitivity on-line detection of nitrite and the like by means of a high-sensitivity gas-liquid phase detection technology, and solves the problems of low sensitivity, large interference and the like in the conventional liquid-phase chemiluminescence method for detecting nitrite and the like.
Drawings
Fig. 1 illustrates an overall sectional structural view of an online detection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention.
Fig. 2a is a schematic top view showing a structure of a dual-flow-path reactor in an on-line inspection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention, fig. 2b is a schematic cross-sectional structure of a dual-flow-path reactor in an on-line inspection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention, and fig. 2c is a schematic bottom view showing a structure of a dual-flow-path reactor in an on-line inspection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention.
Description of reference numerals:
1-double-flow-path reactor, 11-reaction cavity, 12-light-transmitting sheet, 131-air inlet, 132-air outlet, 141-first liquid inlet, 142-first liquid outlet, 143-first channel, 144-first reaction bed, 151-second liquid inlet, 152-second liquid outlet, 153-second channel and 154-second reaction bed; 2-light-proof shell, 21-light-transmitting hole and 3-photoelectric sensor.
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 describes the online detection device and method using online liquid-gas conversion according to the present invention with reference to the accompanying drawings.
Fig. 1 illustrates an overall sectional structural view of an online detection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention.
As shown in fig. 1, according to an exemplary embodiment of the present invention, the online detection device using online liquid-gas conversion includes a dual-flow-path reactor 1, a light-shielding housing 2, and a photoelectric sensor 3, wherein the light-shielding housing 2 is used to provide a light-shielding environment in a matching manner, the photoelectric sensor 3 is used to receive and transmit a chemiluminescent signal, and the dual-flow-path reactor 1 is a main component for a chemiluminescent reaction.
Fig. 2a is a schematic top view showing a structure of a dual-flow-path reactor in an on-line inspection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention, fig. 2b is a schematic cross-sectional structure of a dual-flow-path reactor in an on-line inspection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention, and fig. 2c is a schematic bottom view showing a structure of a dual-flow-path reactor in an on-line inspection apparatus using online liquid-gas conversion according to an exemplary embodiment of the present invention.
As shown in fig. 2a to 2c, a reaction chamber 11 is provided in the body of the dual flow-path reactor 1 of the present invention, and the top of the reaction chamber 11 is sealed by a light-transmitting sheet 12 and transmits light. The bottom of the reaction chamber 11 is provided with a first channel 143 and a second channel 153 which are vertically arranged, two ends of the first channel 143 extend into the body and are communicated with a first liquid inlet hole 141 and a first liquid outlet hole 142 which are arranged on the body, so that a flow channel of a liquid can be formed. Two ends of the second channel 153 extend into the body and are communicated with the second liquid inlet hole 151 and the second liquid outlet hole 152 arranged on the body, so that another liquid flow channel can be formed, and the two liquid flow channels are independent of each other. The two sides of the reaction chamber 11 are further provided with an air inlet 131 and an air outlet 132 respectively for introducing carrier gas into the reaction chamber.
And, the first channel 143 and the second channel 153 are respectively provided with a first reaction bed 144 and a second reaction bed 154 therein, and the parts of the first channel 143 and the second channel 153 in the reaction chamber 11 are cut open to form an exposed area and expose the first reaction bed 144 and the second reaction bed 154 in the reaction chamber 11. That is, the first channel and the second channel are cut open to expose the first reaction bed and the second reaction bed in the reaction chamber 11, so that the liquid entering the first channel and the second channel can realize on-line liquid-gas conversion and chemiluminescence detection of the converted gas under the action of the carrier gas introduced into the reaction chamber, and the detection of the object to be detected in the detected liquid is realized.
As shown in fig. 1, the light-shielding case 2 is assembled on the body of the dual-flow-path reactor 1 and is formed with a light-shielding cavity, the photoelectric sensor 3 is disposed in the light-shielding cavity, and the photosensitive portion of the photoelectric sensor is directly opposite to the light-transmitting sheet 12 and the reaction cavity 11 of the dual-flow-path reactor 1 through the light-transmitting hole 21.
Preferably, the reaction chamber 11 of the dual-flow-path reactor of the present invention is a rhomboid chamber, the first channel 143 and the second channel 153 are arranged in parallel, and the air inlet 131 and the air outlet 132 are arranged on the left and right sides of the reaction chamber 11, so that the flow direction of the fluid in the first channel 143 and the second channel 153 is perpendicular to the flow direction of the gas between the air inlet 131 and the air outlet 132 in the reaction chamber 11, so as to facilitate the carrying of the gas to achieve a better carrying effect, and ensure the accuracy of the detection.
The first and second reaction beds 144 and 154 of the present invention are preferably cylindrical pieces of microfiber material that can be rapidly diffused and infiltrated.
According to the present invention, the on-line detecting device of the present invention further comprises a first peristaltic pump (not shown) in communication with the first liquid inlet 141 or the first liquid outlet 142, a second peristaltic pump (not shown) in communication with the second liquid inlet 151 or the second liquid outlet 152, a gas filter (not shown) in communication with the gas inlet 131, and a vacuum pump (not shown) in communication with the gas outlet 132. In addition, the online detection device also comprises a processing system electrically connected with the photoelectric sensor 3 and a control system electrically connected with the first peristaltic pump, the second peristaltic pump, the vacuum pump and the photoelectric sensor so as to realize online real-time control and result acquisition.
The invention also provides an online detection method utilizing online liquid-gas conversion, and an online detection device utilizing online liquid-gas conversion, and the online detection method comprises the following steps.
Step A:
and after the liquid to be detected and the acid liquid are mixed on line, the liquid is introduced into the first channel through the first liquid inlet hole, a detection reagent is introduced into the second channel through the second liquid inlet hole, and meanwhile, zero air enters the reaction cavity of the double-flow-path reactor through the air inlet hole.
Wherein the filtered zero air is preferably caused to enter the reactor through the air inlet hole and sequentially pass through the surfaces of the first reaction bed and the second reaction bed and finally to be discharged through the air outlet hole under the action of the back-end vacuum pump.
And B:
the detected gas generated by the reaction of the mixed liquid entering the first channel is separated from the exposed first reaction bed and is conveyed to the surface of the exposed second reaction bed in the second channel under the carrying effect of zero air to contact with the detection reagent and generate a chemiluminescence reaction;
the mixed liquid entering the first liquid inlet hole is diffused and soaked on the first reaction bed, and the detected gas generated by the reaction is separated from the first reaction bed. Then, the separated gas to be detected is conveyed to the surface of the second reaction bed under the action of zero air flow in the reactor, and contacts with the detection reagent soaked on the second reaction bed to generate a chemiluminescence reaction.
And C:
and converting the chemiluminescence signal detected by the photoelectric sensor into an electric signal, calculating to obtain the concentration of the detected gas, and calculating to obtain the concentration of the detected object in the detected liquid according to the flow velocity of the zero air and the flow velocity of the detected liquid.
In addition, the method also comprises the step of introducing a cleaning reagent into the reactor after the detection is finished to complete the cleaning of the first reaction bed and the second reaction bed.
According to an embodiment of the present invention, the detected liquid in the present invention may be a solution containing nitrous acid, the acid solution may be hydrochloric acid or sulfuric acid with a volume concentration of 0.1% to 10%, the detection reagent may be a nitrogen dioxide detection reagent, the detected gas may be nitrogen dioxide, and the detected object in the detected liquid may be nitrite, thereby indirectly realizing high-sensitivity online detection of nitrite in the detected liquid.
In conclusion, the invention realizes high-sensitivity online detection of nitrite and the like by means of a high-sensitivity gas-liquid phase detection technology, and solves the problems of low sensitivity, large interference and the like in the conventional liquid-phase chemiluminescence method for detecting nitrite and the like.
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.

Claims (8)

1. An online detection device utilizing online liquid-gas conversion is characterized by comprising a double-flow-path reactor, a light-shading shell and a photoelectric sensor;
a reaction cavity is arranged in the body of the double-flow-path reactor, and the top of the reaction cavity is sealed and light-transmitting through a light-transmitting sheet; the bottom of the reaction cavity is provided with a first channel and a second channel which are vertically arranged, two ends of the first channel respectively extend into the body and are communicated with a first liquid inlet hole and a first liquid outlet hole which are arranged on the body, two ends of the second channel respectively extend into the body and are communicated with a second liquid inlet hole and a second liquid outlet hole which are arranged on the body, and two sides of the reaction cavity are respectively provided with an air inlet hole and an air outlet hole; a first reaction bed and a second reaction bed are respectively arranged in the first channel and the second channel, and the parts of the first channel and the second channel, which are positioned in the reaction cavity, are cut open to form an exposed area and expose the first reaction bed and the second reaction bed in the reaction cavity;
the light-resistant shell is assembled on the body of the double-flow-path reactor and is provided with a light-resistant cavity, the photoelectric sensor is arranged in the light-resistant cavity, and the photosensitive position of the photoelectric sensor penetrates through the light hole to be opposite to the light-transmitting sheet and the reaction cavity of the double-flow-path reactor.
2. The on-line detection device utilizing on-line liquid-gas conversion as claimed in claim 1, wherein the reaction chamber is a diamond-like chamber, the first channel and the second channel are arranged in parallel, and the air inlet and the air outlet are arranged at the left and right sides of the reaction chamber.
3. The on-line measuring device using on-line liquid-gas conversion as claimed in claim 2, wherein the flow direction of the fluid in the first channel and the second channel is perpendicular to the flow direction of the gas in the reaction chamber from the gas inlet hole to the gas outlet hole.
4. The on-line detection device utilizing on-line liquid-gas conversion as claimed in claim 1, wherein the first reaction bed and the second reaction bed are cylindrical ultrafine fibrous material pieces.
5. The on-line detection device utilizing on-line liquid-gas conversion as claimed in claim 1, further comprising a first peristaltic pump in communication with the first liquid inlet or the first liquid outlet, a second peristaltic pump in communication with the second liquid inlet or the second liquid outlet, a gas filter in communication with the gas inlet, and a vacuum pump in communication with the gas outlet.
6. The on-line detection device utilizing on-line liquid-gas conversion of claim 5, further comprising a processing system electrically connected to the photoelectric sensor and a control system electrically connected to the first peristaltic pump, the second peristaltic pump, the vacuum pump and the photoelectric sensor.
7. An online detection method using online liquid-gas conversion, characterized in that the online detection method uses the online detection device using online liquid-gas conversion according to any one of claims 1 to 6 and comprises the steps of:
A. after being mixed with acid liquid on line, the liquid to be detected is introduced into a first channel through a first liquid inlet hole, a detection reagent is introduced into a second channel through a second liquid inlet hole, and meanwhile, zero air enters a reaction cavity of the double-flow-path reactor through an air inlet hole;
B. the detected gas generated by the reaction of the mixed liquid entering the first channel is separated from the exposed first reaction bed and is conveyed to the surface of the exposed second reaction bed in the second channel under the carrying effect of zero air to contact with the detection reagent and generate a chemiluminescence reaction;
C. and converting the chemiluminescence signal detected by the photoelectric sensor into an electric signal, calculating to obtain the concentration of the detected gas, and calculating to obtain the concentration of the detected object in the detected liquid according to the flow velocity of the zero air and the flow velocity of the detected liquid.
8. The on-line detection method using online liquid-gas conversion as claimed in claim 7, wherein the detected liquid is a liquid containing nitrite, the acid solution is hydrochloric acid or sulfuric acid with a volume concentration of 0.1% -10%, the detection reagent is a nitrogen dioxide detection reagent, the detected gas is nitrogen dioxide, and the detected substance in the detected liquid is nitrite.
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