CN106018512A - Dissolved oxygen sensor - Google Patents
Dissolved oxygen sensor Download PDFInfo
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- CN106018512A CN106018512A CN201610422852.9A CN201610422852A CN106018512A CN 106018512 A CN106018512 A CN 106018512A CN 201610422852 A CN201610422852 A CN 201610422852A CN 106018512 A CN106018512 A CN 106018512A
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- dissolved oxygen
- electrode
- sensor
- oxygen sensor
- permeation membrane
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Abstract
The invention relates to a dissolved oxygen sensor. The sensor comprises a tubular shell (1), wherein an oxygen permeation membrane (2) is connected to one end of the shell (1) in a sealed mode, an insulator center bar (3) is arranged in a cavity of the shell, one end of the insulator center bar (3) is close to the oxygen permeation membrane (2), and the other end of the insulator center bar (3) extends to the tubular shell (1) in the direction away from the oxygen permeation membrane (2); a working electrode (6) is arranged at the tail of the end, close to the oxygen permeation membrane (2), of the insulator center bar (3), an auxiliary electrode (9) is wound around the outer surface of the insulator center bar (3), and the superficial area ratio of the working electrode to the auxiliary electrode is 0.1-0.5. The sensor can also comprise a stirring device and a temperature compensation device.
Description
Technical field
The present invention relates to a kind of Film electrode sensor, be specifically related to a kind of dissolved oxygen sensor.
Background technology
Dissolved oxygen is the important indicator that evaluation water quality is good and bad, water body is contaminated degree.Existing dissolved oxygen
Sensor is varied, and ultimate principle is all to utilize various Instrument measuring oxygen molecule at chemistry, electrochemistry and light
The electricity produced in chemical reaction or optical signalling, be then converted to electrical signal by unified for these signals,
The most amplified processing of circuit or analog to digital conversion circuit, finally export instrument display interface by measurement result, from
And realize the measurement of dissolved oxygen concentration.
It is complicated, expensive, minimum that the most conventional chemical type sensor and optical sensor have structure
The problems such as detection limit is limited, it is impossible to meet more measurement requirement.And electrochemical process sensor have precision high,
The features such as response is fast, the linearity is good, volume is little, length in service life, most common of which is Film electrode method.
Film electrode sensor mainly includes working electrode, auxiliary electrode and oxygen permeation membrane three part, dissolves in water
Oxygen, by having selective oxygen permeation membrane, directly produces the signal of telecommunication being directly proportional to oxygen concentration on electrode, logical
Cross and monitor this signal of telecommunication, it is achieved the measurement to dissolved oxygen content.Electrode material and electrode surface area, oxygen flow
Dissolved oxygen monitoring all can be had an impact by film thickness, TWS and agitating device, existing sensor production side
Method is the most complicated, and sensitivity and precision are low, and reaction rate has much room for improvement.
Summary of the invention
In view of the drawbacks described above of prior art, the present invention provides a kind of dissolved oxygen sensor, to solve existing overlay film
Electrode sensor is unreasonable due to structure, be vulnerable to detect environmental effect, and cause its detection sensitivity and
The technical problem that precision is low.
For achieving the above object, concrete technical scheme of the present invention is as follows:
A kind of dissolved oxygen sensor, including tubular shell (1), one end of described housing is sealed with oxygen permeation membrane (2)
Being additionally provided with insulator center bar (3) in the cavity of described housing, one end of described insulation center bar (3) is leaned on
Nearly described oxygen permeation membrane (2), and it is fixed with working electrode (6), described insulator center bar (3) at its end
The other end extend to the other end of tubular shell (1) along the direction deviating from oxygen permeation membrane (2);Described absolutely
Auxiliary electrode (9) also it is wound with on the outer surface of edge body center bar (3). wherein, and described working electrode (6)
It is 0.1-0.5 with auxiliary electrode (9) surface area.
Further, the working electrode (6) of described sensor can be gold electrode.
Further, the gold electrode of described dissolved oxygen sensor, for diameter 5-6mm principal column body and close
Oxygen permeation membrane (2) is held in circular arc type.
Further, the auxiliary electrode (9) of described dissolved oxygen sensor includes silver wire core body, and is plated in described
The silver chloride layer of silver core surface.
Further, described silver wire core diameter is 0.3-0.6mm, and described silver chloride layer is by described silver wire
Core body is placed in 0.1mol/L HCl solution, uses 10mA/cm2Current density electrolysis 3 hours prepare.
Further, the cavity limited capacity of described tubular shell (1) receives 3-5mL electrolyte (12).
Further, described dissolved oxygen sensor also comprises temperature compensation means, and it includes critesistor (10)
With function of temperature compensation control system, described critesistor (10) is welded on described working electrode (6), described
Temperature and dissolved oxygen are acquired by function of temperature compensation control system, and realize the compensation to temperature.
Further, described dissolved oxygen sensor also includes agitating device (11), described agitating device (11)
It is arranged on described tubular shell (1) and is sealed with the one end of oxygen permeation membrane (2).
Further, described agitating device (11), including stirring rod and blade, described blade is connected to stirring
On rod, a diameter of 300-500mm of described stirring rod, described blade is 45 degree of inclinations.
Further, described oxygen permeation membrane (2) is with low-density politef as material, and thickness is 20-25 μm.
In the present invention, working electrode (6) can be selected for this technology necks such as gold electrode, platinum electrode and glassy carbon electrode
Prepared by material conventional in territory.
In the present invention, auxiliary electrode (9) can also use the metal that Ag, Ni, W, Pb etc. are stable to prepare.
For ensureing that working electrode can fully be polarized, the area of auxiliary electrode needs bigger than working electrode,
In practice, it is found by the applicant that when the surface area of working electrode with auxiliary electrode is 0.1-0.5, preferably
During 0.2-0.4, sensitivity and the degree of accuracy of measurement are best.
The present invention uses above technical scheme, has the advantage that
1. due to working electrode and the special ratios of auxiliary electrode surface area, it is possible to increase the reaction speed of sensor
Degree and susceptiveness, make measurement result more accurate.
2. preferred, due to agitating device and the use of temperature compensation means, measured value is more accurate, reflection
The truth of sample.Agitating device makes the concentration of dissolved oxygen in water sample and distribution of water temperature more uniform, simultaneously
Temperature compensation means greatly reduces the TWS impact on measurement result.
Accompanying drawing explanation
Fig. 1 is a kind of dissolved oxygen sensor structural representation of the present invention;
Fig. 2 is the dissolved oxygen sensor current average under anaerobic of tool different-thickness oxygen permeation membrane;
Fig. 3 is the temperature impact on DO determination result;
Fig. 4 is the stirring impact on DO determination result.
In figure: the cavity of 1-tubular shell;2-oxygen permeation membrane;3-insulator center bar;4-the first wire;5-
Ammeter;6-working electrode;7-electrode base;8-the second wire;9-auxiliary electrode;10-temperature-sensitive electricity
Resistance;11-agitating device;12-electrolyte.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and reality
Execute example, the detailed description of the invention of the present invention is described in further detail.Following example are used for this is described
Bright, it is not intended to limit the scope of the present invention.
Fig. 1 shows the structural representation of a kind of dissolved oxygen sensor of the present invention, including tubular shell (1),
One end of described housing (1) is sealed with oxygen permeation membrane (2), and the other end of described insulator center bar (3) is along the back of the body
The other end of tubular shell (1) is extended to from the direction of oxygen permeation membrane (2);In one embodiment, tubulose
The other end of housing (1), that is to say to deviate from and is sealed with the end of oxygen permeation membrane (2) and is fixed with or activity sets
There is a top cover, for the other end of closed tube housing (1), wherein, insulator center bar (3) another
One end can be fixed and be located on top cover, and described insulator center bar (3) center can be conducted electricity, and outer surface is insulation
Body;Second wire (8) one end is connected with ammeter (5), and the other end is by insulator center bar (3)
The conductive structure of the heart, is connected with the working electrode (6) of insulator center bar (3) lower end;Described ammeter
(5) being connected with electrode base (7), the other end of electrode base (7) passes through the first wire (4) with auxiliary
Helping electrode (9) to connect, described auxiliary electrode (9) is coiled on insulator center bar (3), auxiliary electrode
(9) it is connected with the insulation of insulator center bar (3) outer surface, in described housing (1), is full of electrolyte (12),
Critesistor (10) is connected on working electrode (6) by the way of welding, and described working electrode (6)
It is 0.1-0.5 with auxiliary electrode (9) surface area.
The critical piece preparation method of this dissolved oxygen sensor is as follows:
1. the preparation of working electrode (6)
Using high-purity gold (99.9%) as the material of working electrode (6).First by the gold of a diameter of 5mm
Electrode cutting becomes to be about 50mm, and wherein one end is polished into arc-shaped.Then to gold electrode surfaces through 200#,
The sand paper of 600#, 1000# and 1200# is polished step by step, then carries out deoiling treatment, then with acetone
It is carried out 3 times, and ultrasonic 5min with dehydrated alcohol, then cleans with distilled water.After cleaning with distilled water,
With the oxide on hot nitric acid cleaning electrode surface, then clean with distilled water.Next a-Al is used2O3Polishing powder
It is polished to minute surface, the most ultrasonic, clean up with distilled water, standby.The surface area of working electrode excessive or
Person is too small is all unfavorable for dissolved oxygen sensing.Surface area is the biggest, and aftercurrent is the biggest;Surface area is the least, anaerobic
Under the conditions of current value the least, be less susceptible to process.Consider, the present embodiment uses diameter 5-6mm
The principal column body of left and right, as working electrode, makes circular arc type near oxygen permeation membrane end face.
The selection of working electrode to consider following factor: electrochemical window, electrical conductance, repeatability, mechanicalness
Energy, cost, toxicity etc..Working electrode itself does not produce the material unrelated with studying reaction, and can be wider
Potential windows region in be measured;Electrode not with studied material or react with electrolyte solution;
The work area of working electrode should be smooth homogeneous, and is prone to surface cleaning process.Typically use inertia
Electrode, platinum, gold etc. are the more commonly used electrodes.
2. the preparation of auxiliary electrode (9)
It is that material makes silver/silver chloride electrode as auxiliary electrode using the high-purity filamentary silver (99.9%) that resistance is little.
The present embodiment employing galvanoplastic are at filamentary silver plated surface silver chloride, thus obtain silver/silver chloride electrode.Can use straight
Footpath is the filamentary silver of 0.3-0.6mm, a diameter of 0.5mm of selection in the present embodiment, the filamentary silver of a length of 10cm
As electrode matrix, in 0.1mol/L HCl solution, filamentary silver is connected on the positive pole of battery, and platinum filament is connected on negative pole,
Use 10mA/cm2Current density electrolysis 3h, now filamentary silver surface cover one layer of brown silver chloride coating, plating
Layer is the finest and closely woven to be preferred, and electrolysis is cleaned with distilled water after terminating, and is then stored in 0.1mol/L HCl solution
Standby, keep in Dark Place.In certain embodiments, electrolysis time is 6 hours, depends on concrete anti-
Answer condition, to obtain the finest and closely woven coating.For ensureing that working electrode can fully be polarized, auxiliary electrode
Area ratio working electrode bigger, so can reduce the electric current density on electrode.In the present embodiment, work
Electrode and auxiliary electrode surface area are 0.1-0.5, in some embodiments more preferably, and work electricity
Pole and auxiliary electrode surface area are 0.2-0.4.In the present invention, filamentary silver bobbin winoler is turned to spiral
Shape, is enclosed within insulator center bar.Generally auxiliary electrode commonly uses carbon electrode and platinum black electrode, it is possible to
Use and keep inert electrode such as platinum, silver, nickel etc. in the electrolyte, actual application can select as required
Auxiliary electrode.
3. sensor housing structure design
Sensor internal is tubular casing structure, and housing tip can be i.e. the overall structure connected with housing wall,
Can also be can the structure of opening and closing, it is ensured that Guan Bi back casing is enclosed construction.The present embodiment senses
Device is closed cavity.Oxygen permeation membrane (2) can realize with tubular shell (1) main part by the way of screw thread
Sealing-in, it is possible to take other sealing-in modes, it is ensured that after connection, whole housing is enclosed construction.Oxygen permeation membrane
(2) polytetrafluoroethylmaterial material is used to make, because it has excellent chemical stability, in strong oxidizing property
Acid, concentrated alkali solution do not change, is also insoluble in any known organic solvent simultaneously and also there is electrical insulating property
Good feature, is the more stable material of current chemical property.Sensor cavity there is insulant make
Center sensor rod (3), is coiled in auxiliary electrode (9) on insulator center bar (3).At insulator
The one end end of center bar arranges working electrode (6), uses high-insulativity, the epoxy resin of high water proofing property
Glue is bonding with insulator center bar (3) by working electrode (6).The shell structure of sensor is wanted and electrode
Size suitable, and housing cavity body volume is reasonable, if cavity volume is excessive, then electricity during measuring
Solving the oxygen consumption time in matter long, reach stabilization time longer, when measuring low oxygen content, error is big.This enforcement
The sensor housing volume of example, can only accommodate 3-5mL electrolyte, and therefore sensor can quickly reach stable
Electric current such that it is able to accurately measure.Additionally, the distance between housing and working electrode surface should be tried one's best
Reduce, so that sensor produces dissufion current and is rapidly reached stable, reduce the sensor response time to oxygen,
Ensure sensor service life.
4. oxygen permeation membrane
In some embodiments with thickness be 20-25 μm low-density politef as material, preferable film has
Relatively low oxygen permeability and high oxygen diffusibility.Low can be used to of permeability guarantees that the film that oxygen spreads controls,
High diffusion can have quick sonde response, and the sensitivity of sensor probe is directly by the change of film character
Impact, oxygen permeation membrane is the thinnest, and sensitivity is the highest.Swelling or the change of film cause probe on the osmotic pressure of oxygen
The change of sensitivity.The present invention selects poly tetrafluoroethylene, and it has higher thermal resistance, high temperature resistant, and has
Extremely low water penetration.For the sensor of different-thickness oxygen permeation membrane, film is the thinnest, and oxygen transmission rate is the highest, sensor
Average current value the biggest, but sensor stability is more easily subject to the interference of sample flow rate;Oxygen permeation membrane is the thickest,
Oxygen transmission rate is the lowest, and the average current value of sensor is the least.Owing to dissolved oxygen sensor needs to be operated in some spies
In different environment, such as under the conditions of the high-temperature cooling water discharged in Aeration tank and the power plant of some sewage treatment plants etc.,
Requiring to consider thickness and the toughness of sensor oxygen permeation membrane, the thin toughness of oxygen permeation membrane is the poorest, sensor
The use time is short and later stage maintenance is frequent;Oxygen flow thickness, good toughness, use the time long, but sensitivity declines.
Select the polytetrafluoroethylene film after 20-25 μm in some preferred embodiments.
5. temperature compensation means
The critesistor (10) of built-in positive temperature coefficient is close-coupled at working electrode (6) with welding manner
On.Water temperature is more obvious on sensor impact, under conditions of oxygen in water concentration is constant, from
In 0-40 DEG C of temperature range, electrode output signal difference is up to more than 3 times.The present invention is to use temperature and molten
Solve oxygen to gather respectively, compensate with software, it is not necessary to circuit is carried out temperature-compensating debugging.Set at software
Meter is taked three kinds of methods temperature coefficient is compensated: first, according to relevant the most empty in GB
The actual value of the oxygen in water that gas is saturated, makes the curve of temperature and saturated dissolved oxygen, obtains fit equation
It is stored in PLC, second reason of temperature coefficient of eliminating the effects of the act;Second, measure probe at each temperature by
Analog/digital conversion value in the water of the saturation of the air, makes the curve of temperature and conversion value, obtains fit equation and is stored to
In PLC, first reason of temperature coefficient of eliminating the effects of the act;3rd, carrying out in atmosphere time actually used
Parameter during saturation crrection joins in fit equation in real time, eliminates probe error in use.
6. agitating device
Agitating device is with politef as raw material, and including blade and stirring rod, blade is connected to stirring rod
On, stirring rod uses helical gear drive, and stirring rod diameter can be 300-500mm, and the present embodiment stirs
The a diameter of 450mm of rod, is axial stirring paddle with 45 ° of tilt flat plate blades, is stirred.Polytetrafluoroethyl-ne
Alkene has excellent chemical stability, corrosion resistance, sealing, high lubrication non-stick, electrical insulating property and good
Good aging resistance endurance, politef does not reacts with water sample to be measured, does not interferes with measurement result.
After being connected with temperature compensation means, agitating device by above-mentioned electrode, it is placed in injection casing molding in mould.
The present embodiment is using gold electrode as working electrode, and silver electrode, as auxiliary electrode, constitutes two-electrode system,
Oxygen permeation membrane isolation electrolyte and detected water sample, provide a constant voltage, thoroughly between gold electrode and silver electrode
The oxygen crossing film will occur reduction reaction on auxiliary electrode, produces fainter dissufion current, auxiliary
Size of current between electrode and working electrode is linear with by the amount of oxygen of oxygen permeation membrane, and then it is dense to obtain oxygen
Degrees of data.
The above is only the preferred embodiment of the present invention, is not limited to the present invention, it is noted that
For those skilled in the art, on the premise of without departing from the technology of the present invention principle, also
Can make some improvement and modification, these improve and modification should also be as being considered as protection scope of the present invention.
Now carry out dissolved oxygen detection with embodiment of the present invention dissolved oxygen sensor, so that the present invention is further described.
Embodiment 1
Fig. 2 shows that the dissolved oxygen sensor electric current under anaerobic of tool different-thickness oxygen permeation membrane is average
Value.
Make oxygen permeation membrane thickness and be respectively the sensor of 10,25,35 μm, at auxiliary electrode and working electrode
On add the polarizing voltage polarization 2h of 0.7V, measure the electric current in sensor 30min under anaerobic respectively
Meansigma methods.As in figure 2 it is shown, test result shows, for the sensor of different-thickness oxygen permeation membrane, film is the thinnest,
Oxygen transmission rate is the highest, and the current average in 30min is the biggest, but sensor stability is more easily subject to sample stream
The interference of speed;Oxygen permeation membrane is the thickest, and oxygen transmission rate is the lowest, and the average current value in sensor 30min is the least.Due to
Dissolved oxygen sensor often needs to work in some special environments, such as at the Aeration tank of some sewage treatment plants
Under the conditions of the high-temperature cooling water etc. discharged with power plant, this requires to carry out thickness and the toughness of sensor oxygen permeation membrane
Considering, the thin toughness of oxygen permeation membrane is the poorest, and sensor uses the time short and later stage maintenance is frequent;Oxygen flow thickness,
Good toughness, uses the time long, but sensitivity declines.Consider, poly-four after general selection 20-25 μm
Fluoroethylene film.
Embodiment 2
Fig. 3 shows the temperature impact on DO determination result.
To there is temperature-compensating and do not have the sensor of temperature-compensating to measure same saturated with YSI dissolved oxygen instrument simultaneously
Oxygen solution, changes detected solution temperature, measures dissolved oxygen value in different temperatures solution.YSI dissolved oxygen sensing
Instrument is the optic dissolution oxygen measuring device of imported from America, is not limited by flow velocity, without flow velocity or stirring dependency, surveys
Amount result is accurate.Using the measured value of YSI sensor as actual value, the survey of detection oligodynamical oxygen sensor
Accuracy of measurement and uncertainty.As it is shown on figure 3, measurement result shows, with the sensor without temperature-compensating
Comparing, the detection of dissolved oxygen is followed the trail of effective by the dissolved oxygen sensor of band temperature-compensating, and certainty of measurement is high,
It is more nearly actual value.
Embodiment 3
Fig. 4 shows the stirring impact on DO determination result.
By self-carrying mixing with do not have the sensor of agitating device to measure same saturated aqueous solution simultaneously, observation
The change of dissolved oxygen in 15min.As shown in Figure 4, measurement result shows, DO determination result during stirring
More stable, if do not stirred, during the moment contacted with film, in this position sample, dissolved oxygen is constantly consumed, and leads
Causing measurement result to decline, measurement result is unstable always.
Embodiment 4
Take 5 earth's surface water samples, respectively by the dissolved oxygen sensor made and iodimetric titration (GB 7489-87)
Measure oxygen in water, compare the measurement result of two kinds of methods.Iodimetric titration has measurement result feature accurately,
But its operating process is complicated.As shown in table 1, comparing result finds, iodimetric titration and the measurement result of instrumental method
Concordance is fine.
Table 1 dissolved oxygen meter and iodometric determination result
Water sample is numbered | Dissolved oxygen meter method | Iodimetric titration |
1 | 8.34 | 8.36 |
2 | 8.51 | 8.52 |
3 | 7.93 | 7.96 |
4 | 8.02 | 8.03 |
5 | 8.33 | 8.34 |
Embodiment 2-5 from different angles, demonstrates the performance of dissolved oxygen sensor prepared by the present invention,
Confirm the effect of temperature compensation means and agitating device, and by having been found to as measuring reliably with two kinds
The comparison of mode, demonstrates the accuracy of dissolved oxygen sensor measurement result prepared by the present invention.
Claims (10)
1. a dissolved oxygen sensor, including tubular shell (1), is sealed with in one end of described housing (1)
Oxygen permeation membrane (2), it is characterised in that be additionally provided with insulator center bar (3) in the cavity of described housing,
One end of described insulation center bar (3) is near described oxygen permeation membrane (2), and sets its end is fixing
Having working electrode (6), the other end of described insulator center bar (3) is along deviating from oxygen permeation membrane (2)
Direction extend to the other end of tubular shell (1);Described insulator center bar (3)
Auxiliary electrode (9), wherein, described working electrode (6) and auxiliary electricity also it is wound with on outer surface
Pole (9) surface area is 0.1-0.5.
Dissolved oxygen sensor the most according to claim 1, it is characterised in that: described working electrode (6)
For gold electrode.
Dissolved oxygen sensor the most according to claim 2, a diameter of 5-6mm principal column of described gold electrode
Body, and hold in circular arc type near oxygen permeation membrane (2).
Dissolved oxygen sensor the most according to claim 1, it is characterised in that: described auxiliary electrode (9)
Including silver wire core body, and it is plated in the silver chloride layer of described silver wire core surface.
Dissolved oxygen sensor the most according to claim 4, it is characterised in that: described silver wire core body straight
Footpath is 0.3-0.6mm, and described silver chloride layer is molten for described silver wire core body is placed in 0.1mol/L HCl
In liquid, use 10mA/cm2Current density electrolysis 3 hours prepare.
Dissolved oxygen sensor the most according to claim 1, it is characterised in that: described tubular shell (1)
Cavity limited capacity receive 3-5mL electrolyte (12).
Dissolved oxygen sensor the most according to claim 1, it is characterised in that: also comprise temperature-compensating dress
Putting, it includes critesistor (10) and function of temperature compensation control system, described critesistor (10)
Being welded on described working electrode (6), described function of temperature compensation control system is to temperature and dissolved oxygen
It is acquired, and realizes the compensation to temperature.
Dissolved oxygen sensor the most according to claim 1, it is characterised in that: also include agitating device
(11), described agitating device is arranged on described tubular shell (1) and is sealed with oxygen permeation membrane (2)
One end.
Dissolved oxygen sensor the most according to claim 8, it is characterised in that: described agitating device (11)
Including stirring rod and blade, and a diameter of 300-600mm of stirring rod, described blade is 45 degree of inclinations.
Dissolved oxygen sensor the most according to claim 1, it is characterised in that: described oxygen permeation membrane (2)
With low-density politef as material, thickness is 20-25 μm.
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CN110057895A (en) * | 2019-04-30 | 2019-07-26 | 北京化工大学 | The optimization method of two electrode Clark type oligodynamical lambda sensor polarization parameters |
CN111239355A (en) * | 2020-01-22 | 2020-06-05 | 东北大学秦皇岛分校 | Dissolved oxygen detector based on machine learning feedback compensation optimization |
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CN111239355A (en) * | 2020-01-22 | 2020-06-05 | 东北大学秦皇岛分校 | Dissolved oxygen detector based on machine learning feedback compensation optimization |
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