CN106092937A - Use the molecular absorption spectrometer of gas-liquid separation membrane - Google Patents

Use the molecular absorption spectrometer of gas-liquid separation membrane Download PDF

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Publication number
CN106092937A
CN106092937A CN201610683280.XA CN201610683280A CN106092937A CN 106092937 A CN106092937 A CN 106092937A CN 201610683280 A CN201610683280 A CN 201610683280A CN 106092937 A CN106092937 A CN 106092937A
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gas
separation membrane
liquid separation
reactor
detector
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Inventor
吴得福
高心岗
隋宗斌
铁振平
王强
熊思
李洪杰
张丹
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QINGDAO JIAMING MEASUREMENT AND CONTROL TECHNOLOGY Co Ltd
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QINGDAO JIAMING MEASUREMENT AND CONTROL TECHNOLOGY Co Ltd
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Priority to CN201610683280.XA priority Critical patent/CN106092937A/en
Publication of CN106092937A publication Critical patent/CN106092937A/en
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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
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/228Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26Drying gases or vapours
    • B01D53/268Drying gases or vapours by diffusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/08Cleaning containers, e.g. tanks
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • 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
    • 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
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/314Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
    • 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
    • G01N2021/0106General arrangement of respective parts
    • G01N2021/0112Apparatus in one mechanical, optical or electronic block
    • 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
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N2021/3125Measuring the absorption by excited molecules

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
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  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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Abstract

A kind of molecular absorption spectrometer using gas-liquid separation membrane, including reactor, detector.Being provided with gas-liquid separation membrane in the inner chamber of described reactor, the inner chamber of reactor is separated into the first reaction chamber and the second reaction chamber by described gas-liquid separation membrane up and down.Described first reaction chamber is connected by transfer pipeline with the inner chamber of detector.Described second reaction chamber connects sampling device and carrier gas device.Described detector is provided with light source and is able to receive that the detection device of light that light source sends.After the molecular absorption spectrometer using gas-liquid separation membrane makes water sample to be measured and reagent react in reactor, directly pass through gas-liquid separation membrane, water in the gas produce reaction filters, and gas-liquid separation membrane is positioned at reactor, makes reaction unit combine with drying device, enormously simplify system, equipment is simple to operate, it is easy to miniaturization and the portable design of instrument, testing sample can be carried out on-site measurement, add the range of instrument.

Description

Use the molecular absorption spectrometer of gas-liquid separation membrane
Technical field
The present invention relates to water quality monitoring technical field, a kind of molecule absorption utilizing macromolecule gas-liquid separation membrane of specific design Spectrogrph.
Background technology
Water resource is the most important natural resourcess of the mankind, is the primary conditions depended on for existence and development of the mankind.In recent years with Water resource pollution day by day serious, water quality monitoring is as the basic work in water pollution control work, for water environment management, dirt The control of dye source, environmental planning etc. provide scientific basis, to whole water environment protection, water pollution control and safeguard that water environment is healthy Aspect plays vital effect.
Water analysis index subjet is various, because the different detection methods of purposes are the most different.Gas-phase molecular absorption spectrometry Method (Gas-Phase Molecular Absorption Spectrometry, hereinafter referred to as GPMAS) is according to water sample component to be measured The gas concentration decomposed is followed Lamber-Beer's Law (Beer-Lambert Law) this principle with characteristic light absorption intensity and is surveyed Determine the quantitative analysis of water pollutant composition.
Ammonia nitrogen (NH is measured utilizing GPMAS3-N), nitrate nitrogen (NO3-N) etc. water pollutant time, by sample and reagent (titanous chloride .) injects a mixing reactor, and the component to be measured realized in 70 DEG C of environment above in liquid phase is converted to gas, By being dried except sending into measurement system after gas being removed water after water.
In order to effectively the component to be measured in liquid phase is converted to gas by chemical reaction, make gas from liquid phase sample Separating and be loaded into measurement system, current instrument includes sampling device, heater, reaction unit, drying device, inspection mostly Survey device, clean device, air mix facilities.And the drying device used is desiccant or semiconductor refrigerating water trap mostly, Desiccant easily hardens after absorbing moisture or makes moist, and causes the permeability of gas to be deteriorated, and then measurement result is produced impact, needs Often change.Semiconductor refrigerating is used to remove water, owing to reactant liquor reacts at relatively high temperatures, therefore to reach effectively to freeze Water removal effect, needs the refrigerating plant of relatively high power, and the gas produced in cooling procedure is readily adsorbed on tube wall, impact inspection Survey precision.Therefore, the major defect of this molecular absorption spectrometer device is that device structure is complicated, complex operation, scavenging period Long, need a large amount of deionized water, volume and power consumption relatively big and the most portable, it is impossible to meet the need of on-the-spot outdoor environment monitoring Ask.
Summary of the invention
The present invention is directed to current molecular absorption spectrometer appliance arrangement structure complicated, need drying device is separately configured, Volume and power consumption are relatively big, and the most portative problem, propose a kind of molecular absorption spectrometer using gas-liquid separation membrane.
The molecular absorption spectrometer of the employing gas-liquid separation membrane of the present invention, including reactor, detector.
Being provided with gas-liquid separation membrane in the inner chamber of described reactor, the inner chamber of reactor is divided by described gas-liquid separation membrane up and down It is divided into the first reaction chamber and the second reaction chamber.
Described first reaction chamber is connected by transfer pipeline with the inner chamber of detector.
Described second reaction chamber connects sampling device and carrier gas device.
Described detector is provided with light source and is able to receive that the detection device of light that light source sends.
Preferably, described detector two ends are respectively arranged with air inlet and exhaust outlet, described air inlet and transfer pipeline Being connected, described exhaust outlet connects purifier.
Preferably, described light source and detection device lay respectively at the two ends of detector.
Preferably, described first reaction chamber is provided with gas outlet, and described gas outlet is provided with leaving air control valve.
Preferably, described transfer pipeline is provided with delivery control valve.
Preferably, in described second reaction chamber, heater is installed.
Preferably, described heater is arranged on the injection port that the second reaction chamber is arranged, and described injection port fills with sample introduction Put connected.
Preferably, described second reaction chamber is provided with leakage fluid dram, and described leakage fluid dram connects bat liquid pump.
The invention has the beneficial effects as follows: use the molecular absorption spectrometer of gas-liquid separation membrane to make water sample to be measured and reagent instead After reacting in answering device, directly by gas-liquid separation membrane, the water in the gas produce reaction filters, and gas-liquid separation membrane is positioned at In reactor, making reaction unit combine with drying device, enormously simplify system, equipment is simple to operate, it is simple to instrument little Type and portable design, can carry out on-site measurement to testing sample, add the range of instrument.Utilize gas-liquid separation membrane The most except water drier, it is not necessary to re-use any dry medium or gas dewatering device, water rem oval is high, reduces gas to be measured Tube wall absorption, improve the service life of instrument, determination data precision is more preferably.
Air inlet and the aerofluxus of detector are positioned at two ends, enable the gas to be measured longer time that reaction produces at detector Interior flowing, it is ensured that the accuracy of gas detecting.The waste gas that detector is discharged is sent in air after being purified by purifier, it is to avoid Detection operation pollutes.
The light source of detector and detection device also are located at two ends, and the scope making light be distributed maximizes, and carries from another point of view The high accuracy of gas detecting.
First reaction chamber arranges the gas outlet that leaving air control valve controls, and equipment can be to the pressure in reactor during using Power is balanced, and enables water sample to be measured and reagent to smoothly enter in reactor;Can when gas concentration to be measured is too high, Gas is shunted, it is to avoid reactor pressure is excessive, cause the danger of blast;Equipment can be made to carry out water sample detection before, The carrier gas carrying out reactor cleaning can enter smoothly, and is discharged by the gas in reactor.
Delivery control valve controls the break-make being connected between reactor and detector, and gas concentration the most to be measured is relatively low Time, enable gas to be measured to be enriched with in the reactor, it is ensured that to send into the concentration of gas in detector, it is ensured that the essence of gas detecting Degree.
Water sample to be measured and reagent can be heated by heater, accelerate response speed.And heater is positioned at injection port On, make water sample to be measured and reagent just enter reactor the most heated, strengthen the effect of heatable catalytic reaction.
Leakage fluid dram connects claps liquid pump, it is possible to is quickly discharged by reacted waste liquid, it is simple to the cleaning of reactor, then carries out Detect next time.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of the molecular absorption spectrometer using gas-liquid separation membrane.
Detailed description of the invention
In order to be able to further appreciate that the structure of the present invention, feature and other purpose, detailed in conjunction with appended preferred embodiment Being described as follows, illustrated preferred embodiment is merely to illustrate technical scheme, and the non-limiting present invention.
The detailed description of the invention of the present invention is as follows:
As it is shown in figure 1, use the molecular absorption spectrometer of gas-liquid separation membrane to include reactor 1, detector 2.
Being provided with gas-liquid separation membrane 3 in the inner chamber of reactor 1, the inner chamber of reactor is separated into by gas-liquid separation membrane 3 up and down First reaction chamber 1.1 and the second reaction chamber 1.2.
Gas-liquid separation membrane i.e. macromolecule gas-liquid separation membrane, is that a kind of selectivity is through film, it is possible to pass the gas through, in gas Moisture then cannot pass through.
First reaction chamber 1.1 is connected by transfer pipeline with the inner chamber of detector 1.
Second reaction chamber 1.2 connects sampling device 4 and carrier gas device 5.Water sample and reagent can be sent to by sampling device 4 In second reaction chamber 1.2, carrier gas then can be passed in the second reaction chamber 1.2 by carrier gas device 5, carrier gas can be high pure nitrogen or Air after purification.
Detector 2 is provided with light source 6 and is able to receive that the detection device 7 of light that light source 6 sends.Light source 6 uses Zn Lamps etc. can send the light-emitting device of specific wavelength spectral line, and the light sent is injected in the inner chamber of detector 2, is then detected by device 7 receive, and detection device 7 records the light intensity receiving light.
When carrying out water sample detection, by sampling device, water sample and reagent are sent in reactor 1.Water sample and reagent exist The second reaction chamber 1.2 in reactor 1 reacts, produces gas to be measured.Gas to be measured produces and is enriched with to finite concentration, reaction After being malleation in device 1, close sampling device 4, open carrier gas device 5, in reactor 1, be passed through the carrier gas of high pressure.Carrier gas will be treated Survey gas upwards pushing and withstanding, by gas-liquid separation membrane 3, by the filter moisture in gas to be measured, be then fed in detector 2.Inspection Surveying the light that in device 2, light source 6 is launched to be received by Jian Cezhuanzhi 7, the gas to be measured being passed in detector 2 makes detection device 7 connect The light intensity received changes.The measurement signal value of device for recording and detecting 7, determines pollutant component in water sample, goes forward side by side Row quantitative analysis.
In order to improve the precision of gas detecting to be measured, detector 2 two ends are respectively arranged with air inlet and exhaust outlet, light source 6 lay respectively at the two ends of detector 2 with detection device 7.Air inlet is connected with transfer pipeline, and exhaust outlet connects purifier 8.
Gas to be measured enters from air inlet, discharges from exhaust outlet so that it is can cover in detector 2 comprehensively, and light source 6 The light of injection covers whole detector 2 the most simultaneously, adds the degree of gases affect light intensity to be measured, makes light intensity Change becomes apparent from, and is more prone to detect, improves detection sensitivity, strengthens accuracy of detection.
After gas to be measured completes to detect operation, entering purifier 8 by exhaust outlet, purifier 8 is by harmful in gas Composition filters, and makes the gas entering in air meet discharge standard, it is to avoid atmosphere pollution.
For the pressure in balancing response device 1, the first reaction chamber arranges 1.1 has gas outlet, gas outlet to be provided with out gas control Valve 9 processed.When carrying out water sample detection, during water sample and reagent pass through in reactor 1, gas outlet is beaten by leaving air control valve 9 Opening, original gas in reactor 1 is released by the entrance of water sample and reagent, enables water sample and reagent to enter smoothly in reactor 1.
Before water sample detection, open leaving air control valve 9, by carrier gas device 5 in reactor 1 by the load of high pressure Gas, is emptied original gas in reactor 1 by gas outlet, is carried out reactor 1.Carrier gas travels further into detector 2 In, original gas in detector 2 is released, is also carried out detector 2 cleaning.After carrier gas enters and is full of detector 2, light source 6 Injection photoelectricity is received through carrier gas by Jian Cezhuanzhi 7, and detection device 7 records background signal, as the basic data of gas detecting.
During water sample detection is carried out, when gas concentration to be measured is too high, opens leaving air control valve 9, make a part Gas to be measured can be discharged by gas outlet, it is to avoid in reactor 1, pressure is excessive, explodes.
In order to control the break-make being connected between reactor with detector, transfer pipeline is provided with delivery control valve 10.Instead When answering that in device 1, gas concentration to be measured is relatively low, close delivery control valve 10, disconnect transfer pipeline, enable gas to be measured in reaction Device 1 is enriched with, after gas to be measured reaches concentration requirement, is opening guarantee delivery control valve 10, gas to be measured is sent into detection In device 2, make the gas concentration to be measured in entrance detector 2.
When carrying out reactor 1 and cleaning, close delivery control valve 10, make carrier gas all be led to by original gas in reactor 1 Cross gas outlet emptying.After reactor 1 has cleaned, when cleaning reactor 2, open delivery control valve 10, close leaving air control valve 9, make carrier gas fully enter in detector 2, gas in detector 2 is emptied by exhaust outlet.
In order to accelerate the response speed of water sample and reagent, being provided with heater 11 in the second reaction chamber 1.2, heater 11 increases Add temperature in reactor 1, accelerate response speed.Heater 11 is arranged on the injection port that the second reaction chamber 1.2 is arranged, injection port It is connected with sampling device 4, makes the water sample just entered from injection port and reagent just receive the heating of heater 11, increase anti-further Answer speed, improve the efficiency that detection operation is overall.
In order to by the waste liquid emptying in reactor 1, the second reaction chamber 1.2 is provided with leakage fluid dram, and leakage fluid dram connects bat Liquid pump 12.Clap liquid pump 12 and power is provided, the discharge of waste liquid in quickening reactor 1.Carry out the carrier gas that is passed through when reactor 1 cleans also Original liquid in reactor 1 is discharged by leakage fluid dram, it is ensured that clean in reactor 1, in order to carry out water sample detection next time, protect Demonstrate,prove the accuracy of water sample detection next time.

Claims (8)

1. the molecular absorption spectrometer using gas-liquid separation membrane, it is characterised in that include reactor (1), detector (2),
Being provided with gas-liquid separation membrane (3) in the inner chamber of described reactor (1), described gas-liquid separation membrane (3) is by the inner chamber of reactor It is separated into the first reaction chamber (1.1) and the second reaction chamber (1.2) up and down,
Described first reaction chamber (1.1) is connected by transfer pipeline with the inner chamber of detector (1),
Described second reaction chamber (1.2) connects sampling device (4) and carrier gas device (5),
Described detector (2) is provided with light source (6) and is able to receive that the detection device (7) of light that light source (6) sends.
The molecular absorption spectrometer of employing gas-liquid separation membrane the most according to claim 1, it is characterised in that described detector (2) two ends are respectively arranged with air inlet and exhaust outlet, and described air inlet is connected with transfer pipeline, and described exhaust outlet connects purification Device (8).
The molecular absorption spectrometer of employing gas-liquid separation membrane the most according to claim 1 and 2, it is characterised in that described light Source (6) and detection device (7) lay respectively at the two ends of detector (2).
The molecular absorption spectrometer of employing gas-liquid separation membrane the most according to claim 1, it is characterised in that described first anti- Answering chamber to arrange (1.1) has gas outlet, described gas outlet to be provided with leaving air control valve (9).
5. according to the molecular absorption spectrometer of the employing gas-liquid separation membrane described in claim 1 or 4, it is characterised in that described defeated Send pipeline that delivery control valve (10) is installed.
The molecular absorption spectrometer of employing gas-liquid separation membrane the most according to claim 1, it is characterised in that described second anti- Heater (11) is installed in answering chamber (1.2).
The molecular absorption spectrometer of employing gas-liquid separation membrane the most according to claim 6, it is characterised in that described heater (11) being arranged on the injection port that the second reaction chamber (1.2) is arranged, described injection port is connected with sampling device (4).
The molecular absorption spectrometer of employing gas-liquid separation membrane the most according to claim 1, it is characterised in that described second anti- Answering chamber (1.2) to be provided with leakage fluid dram, described leakage fluid dram connects bat liquid pump (12).
CN201610683280.XA 2016-08-17 2016-08-17 Use the molecular absorption spectrometer of gas-liquid separation membrane Pending CN106092937A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN106644665A (en) * 2017-01-17 2017-05-10 天津师范大学 Gas-liquid separation device
CN107782708A (en) * 2017-11-13 2018-03-09 青岛佳明测控科技股份有限公司 Microorganism in Water detection means and detection method
CN108333034A (en) * 2018-05-14 2018-07-27 中山大学 A kind of air film for Surface enhanced Raman spectroscopy detection detaches sample pretreatment device
CN111650389A (en) * 2020-06-12 2020-09-11 杭州准芯生物技术有限公司 Liquid detection cell and liquid analysis system
CN111974176A (en) * 2019-05-23 2020-11-24 奇鼎科技股份有限公司 Dehumidification module of mixed gas and detection system thereof
CN113447444A (en) * 2021-05-10 2021-09-28 镇江市空感科技有限公司 Detection apparatus based on gas-liquid reaction chamber reinforcing gas detection rate

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Publication number Priority date Publication date Assignee Title
CN106644665A (en) * 2017-01-17 2017-05-10 天津师范大学 Gas-liquid separation device
CN107782708A (en) * 2017-11-13 2018-03-09 青岛佳明测控科技股份有限公司 Microorganism in Water detection means and detection method
CN107782708B (en) * 2017-11-13 2023-10-13 青岛佳明测控科技股份有限公司 Water quality microorganism detection device and detection method
CN108333034A (en) * 2018-05-14 2018-07-27 中山大学 A kind of air film for Surface enhanced Raman spectroscopy detection detaches sample pretreatment device
CN111974176A (en) * 2019-05-23 2020-11-24 奇鼎科技股份有限公司 Dehumidification module of mixed gas and detection system thereof
CN111650389A (en) * 2020-06-12 2020-09-11 杭州准芯生物技术有限公司 Liquid detection cell and liquid analysis system
CN113447444A (en) * 2021-05-10 2021-09-28 镇江市空感科技有限公司 Detection apparatus based on gas-liquid reaction chamber reinforcing gas detection rate

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Application publication date: 20161109