CN110082488A - A kind of dissolved oxygen metering calibrating installation and method - Google Patents
A kind of dissolved oxygen metering calibrating installation and method Download PDFInfo
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Abstract
The present invention relates to dissolved oxygen sensing instrument meter amount calibrating installation and its application methods, belong to product quality detection field.Solves the technical problem that current dissolved oxygen meter collimation technique is higher to the surge requirements of water temperature and operation calculating is very cumbersome.A kind of dissolved oxygen metering calibrating installation, including the internal constant temperature water bath for being equipped at least one temperature sensor；Constant temperature water bath top cover is provided with by compared with dissolved oxygen meter entrance；Constant temperature water bath top cover lower surface is equipped with fluorescence method normal electrode；It further include oxygen calibrating gas bottle in nitrogen, industrial personal computer and the air pump controlled by industrial personal computer；Oxygen calibrating gas bottle is connected by pipeline with air pump in the nitrogen, and air pump is protruded into constant temperature water bath by gas supply pipeline；The signal output end of the fluorescence method normal electrode is connected with the signal input part of industrial personal computer.It is very complicated that the method for the invention solves the problems, such as that operation of the existing technology calculates, and improves work efficiency.
Description
Technical field
The present invention relates to dissolved oxygen sensing instrument meter amount calibrating installation and its application methods, belong to product quality detection field.
Background technique
Dissolved oxygen meter belongs to environment measuring quasi-instrument, is widely used in metallurgy, petroleum, chemical industry, petrochemical industry, coal industry
Etc. industries, can accurately show water outlet in total organic carbon concentration, protect people life property safety to curbing environmental pollution
With extremely important effect.Metering or measurement and calibration are carried out to dissolved oxygen meter, conventional metered dose standard set-up is mainly by two
Etc. standard mercuries thermometer, electronic stopclock and water bath with thermostatic control corollary equipment composition.According to the requirement of national measurement regulation, by water temperature
The different water temperatures (0~50) DEG C for adjusting national measurement regulatory requirements stir water sample using blender, bubbler, Xiang Shui are added
Middle exposure air, preparation saturated dissolved oxygen water；Tested dissolved oxygen meter is put into water, it is direct to be detected dissolved oxygen meter
Mensuration measures the dissolved oxygen content of different temperatures Shi Shuizhong, from " oxygen different water temperatures, atmospheric pressure water in be saturated concentration value
Table " comparing calculates the metering performance of tested dissolved oxygen meter.
Existing dissolved oxygen meter calibration method and device:
There is temperature adjustment function constant temperature water bath using one kind, setting a temperature is able to maintain its temperature in a certain range
It is interior, then by bubbler continuous aeration 60 minutes into constant temperature water bath, then after standing 30 minutes or so, obtain calibration
Then dissolved oxygen electrode is measured the dissolved oxygen concentration in water into the water, then measures the atmospheric pressure in air by dissolved oxygen water,
Then with " oxygen different water temperatures, atmospheric pressure water in be saturated concentration value table " compared to pair, measure obtain dissolved oxygen meter
Metering performance；Existing measurement and calibration device labor efficiency is low, and the experiment condition reproduction time is long, and working efficiency is low.
Equipment dissolved oxygen water temperature is needed when calibration, and controls water temperature fluctuation range, is calibrated and is used due to the dissolved oxygen of calibration
Water is an exposure in air, so that water temperature is changed control at 0.2 DEG C, existing determination device is 0.1 DEG C of scale division value, passes through heating
Afterwards, water temperature is stirred, even water temperature is made, and is maintained at a lesser range fluctuation, there are certain difficulties.
Existing measurement calibration method
Condition:
1, saturated dissolved oxygen water is prepared, is that (existing scheme requires to do 10 by the temperature of water bath with thermostatic control temperature adjusting to needs
DEG C, 20 DEG C, 30 DEG C of three temperature spots), temperature fluctuation is no more than ± 0.2 DEG C, and 60 points are continuously aerated into water by starting air pump
Clock (oxygen content about 21% in air) after the completion of aeration, stands 30 minutes or so.
2, the calibration of the dissolved oxygen error of indication will be calibrated dissolved oxygen meter electrode by air and be put into water termostat water-bath simultaneously
It gently swings, the indicating value of dissolved oxygen meter is read after stablizing, duplicate measurements twice, calculates the average value of dissolved oxygen sensing
The dissolved oxygen concentration error of indication is calculated by formula (1), take absolute value maximum Δ C1For calibration result.
In formula: Δ C1--- the dissolved oxygen concentration error of indication, mg/L；
--- apparatus measures average value, mg/L；
Cs1--- dissolved oxygen concentration reference value, table look-up (appendix C) and interpolation calculation, mg/L.
It is attached to examine and determine instrument indication error's process according to existing " dissolved oxygen meter " vertification regulation.For example, atmospheric pressure is
The dissolved oxygen meter measurement result of 932hPa, a routine are as shown in the table:
I, interpolation calculation water temperature is 9.9 DEG C, 20.0 DEG C, 30.0 DEG C, is saturated dissolution in the water under atmospheric pressure 932hpa
Oxygen concentration:
1. calculating water temperature is 9.9 DEG C, dissolved oxygen concentration is saturated in the water under atmospheric pressure 932hpa:
Table look-up " oxygen different water temperatures, atmospheric pressure water in be saturated concentration value " obtain 9 DEG C, 900hPa saturated dissolved oxygen is dense
Degree is 10.25mg/L, and 10 DEG C, 900hPa saturated dissolved oxygen concentration is 10.01mg/L；9 DEG C, 933hPa saturated dissolved oxygen concentration be
10.64mg/L, 10 DEG C, 933hPa saturated dissolved oxygen concentration be 10.39mg/L.
Under (9~10) DEG C neighbouring, 900hPa, temperature is every to increase 1 DEG C, saturated dissolved oxygen concentration variable quantity:
(1 DEG C=- 0.24mgL of 10.01mg/L-10.25mg/L ÷- 1·℃- 1
Under (9~10) DEG C neighbouring, 933hPa, temperature is every to increase 1 DEG C, saturated dissolved oxygen concentration variable quantity:
(1 DEG C=- 0.25mgL of 10.39mg/L-10.64mg/L ÷- 1·℃- 1
9.9 DEG C, be saturated dissolved oxygen concentration in the water under 900hPa:
10.01mg/L+ (- 0.24mgL- 1·℃- 19.9 DEG C -10 DEG C of) × ()=10.03mg/L
9.9 DEG C, be saturated dissolved oxygen concentration in the water under 933hPa:
10.39mg/L+ (- 0.25mgL- 1·℃- 19.9 DEG C -10 DEG C of) × ()=10.42mg/L
At 9.9 DEG C, (900~933) hPa, the every raising 1hPa of atmospheric pressure, saturated dissolved oxygen concentration variable quantity:
(10.42mg/L-10.03mg/L) ÷ 33hPa=0.01182mgL- 1·℃- 1·hPa- 1
9.9 DEG C, be saturated dissolved oxygen concentration in the water under 932hPa:
10.42mg/L+0.01182mg·L- 1·℃- 1·hPa- 1× (932hPa-933hPa)=10.43mg/L
That is it is 10.43mg/L that water temperature is saturated dissolved oxygen concentration under 9.9 DEG C, atmospheric pressure 932hPa, in water
2. calculating 20.0 DEG C of water temperature, dissolved oxygen concentration is saturated in the water under atmospheric pressure 932hpa:
Table look-up " oxygen different water temperatures, atmospheric pressure water in be saturated concentration value " obtain 20.0 DEG C, 900hPa saturation dissolution
Oxygen concentration is 8.05mg/L, and 933hPa saturated dissolved oxygen concentration is 8.36mg/L.
At 20.0 DEG C, (900~933) hPa, the every raising 1hPa of atmospheric pressure, saturated dissolved oxygen concentration variable quantity:
(8.36mg/L-8.05mg/L) ÷ 33hPa=0.0094mgL- 1·℃- 1·hPa- 1
20 DEG C, be saturated dissolved oxygen concentration in the water under 932hPa:
8.36mg/L+0.0094mg·L- 1·℃- 1·hPa- 1× (932hPa-933hPa)=8.35mg/L
That is it is 8.35mg/L that water temperature is saturated dissolved oxygen concentration under 20.0 DEG C, atmospheric pressure 932hPa, in water
3. calculating 30.0 DEG C of water temperature, dissolved oxygen concentration is saturated in the water under atmospheric pressure 932hpa:
Table look-up " oxygen different water temperatures, atmospheric pressure water in be saturated concentration value " obtain 30.0 DEG C, 900hPa saturation dissolution
Oxygen concentration is 6.68mg/L, and 933hPa saturated dissolved oxygen concentration is 6.94mg/L.
At 30.0 DEG C, (900~933) hPa, the every raising 1hPa of atmospheric pressure, saturated dissolved oxygen concentration variable quantity:
(6.94mg/L-6.68mg/L) ÷ 33hPa=0.0079mgL- 1·℃- 1·hPa- 1
20 DEG C, be saturated dissolved oxygen concentration in the water under 932hPa:
6.94mg/L+0.0079mg·L- 1·℃- 1·hPa- 1× (932hPa-933hPa)=6.93mg/L
That is it is 6.93mg/L that water temperature is saturated dissolved oxygen concentration under 30.0 DEG C, atmospheric pressure 932hPa, in water
II, the dissolved oxygen concentration error of indication is calculated according to formula:
Water temperature 9.9 DEG C: 10.01mg/L-10.43mg/L=-0.42mg/L
Water temperature 20.0 DEG C: 7.97mg/L-8.35mg/L=-0.38mg/L
Water temperature 30.0 DEG C: 6.59mg/L-6.93mg/L=-0.34mg/L
Instrument is examined and determine according to existing " dissolved oxygen meter " vertification regulation, need to be calculated under different temperatures, different atmospheric pressure
Standard saturated dissolved oxygen concentration value, this process is than relatively time-consuming and cumbersome.
Summary of the invention
The present invention is that the current dissolved oxygen meter collimation technique of solution is higher to the surge requirements of water temperature and operation calculating is non-
Often cumbersome technical problem provides a kind of dissolved oxygen metering calibrating installation and method.
Dissolved oxygen metering calibrating installation of the present invention adopts the following technical scheme that realization: a kind of dissolved oxygen metering school
Standard apparatus, including the internal constant temperature water bath for being equipped at least one temperature sensor；Constant temperature water bath top cover, which is provided with, relatively to be dissolved
Oxygen analyzer entrance；Constant temperature water bath top cover lower surface is equipped with fluorescence method normal electrode；Further include oxygen calibrating gas bottle in nitrogen,
Industrial personal computer and the air pump controlled by industrial personal computer；Oxygen calibrating gas bottle is connected by pipeline with air pump in the nitrogen, and air pump is logical
Gas supply pipeline is crossed to protrude into constant temperature water bath；The signal output end of the fluorescence method normal electrode and the signal input part of industrial personal computer
It is connected；
It further include the high photographing instrument supported by bracket；The signal output end of high photographing instrument is connected with the signal input part of industrial personal computer
It connects.
Device of the present invention directly measures oxygen in water according to fluorescence quenching principle, by fluorescence method normal electrode
Concentration is calibrated the image information of dissolved oxygen meter using high photographing instrument acquisition as the standard dissolved oxygen concentration value of measurement and calibration
(show value), and know the dissolved oxygen concentration value for taking and being calibrated dissolved oxygen meter measurement, it is counted with the concentration value of calibrating installation
According to processing, electronical record is generated.
Dissolved oxygen measurement calibration method of the present invention adopts the following technical scheme that realization: a kind of dissolved oxygen metering school
Quasi- method, includes the following steps:
(1) saturated dissolved oxygen water is prepared
After distilled water or high purity water are put into constant temperature water bath, it is passed through the calibrating gas of oxygen in a certain concentration nitrogen, is observed
The numerical value of dissolved oxygen on industrial personal computer, when the numerical value of dissolved oxygen sensing is when decimal point third position changes, it is believed that be passed through oxygen mark in nitrogen
After quasi- gas, the molecular oxygen in water has been saturated；
(2) whether the temperature for observing water temperature and surrounding air in constant temperature water bath approaches, when the two temperature difference is less than
At 0.2 DEG C, it is believed that calibration environment condition has；
(3) by the probe for the dissolved oxygen meter being calibrated by being put into constant temperature water bath compared with dissolved oxygen meter entrance
In, after the dissolved oxygen meter measured value that is calibrated is stablized, the dissolved oxygen meter measured value 2 significant digits that are calibrated
Numerical value changes once, and high photographing instrument identifies once with regard to auto Image Collection, continuously three times, is averaged as a measurement result；
(4) the dissolved oxygen concentration error of indication is calculated by formula (2)；
In formula: Δ C2--- the dissolved oxygen concentration error of indication, unit mg/L；
--- the dissolved oxygen meter measurement average value being calibrated, unit mg/L；
Cs2--- the dissolved oxygen concentration reference value surveyed on industrial personal computer by fluorescence method normal electrode, unit mg/L；
(5) concentration value of nitrogen is changed the step in (one) in nitrogen in the calibrating gas of oxygen at least twice, after changing every time all
Step (1)~(four) are repeated, at least three Δ C are finally obtained2Value；
(6) at least three Δ C2A maximum value is selected in value, as calibration result, completes calibration.
The invention patent is contained using oxygen gas mixture in the nitrogen of various concentration is passed through into constant temperature (consistent with room temperature) water
Oxygen amount is generally 5%, 10%, 20% or so, the solution oxygen for measuring the dissolved oxygen content in water by normal electrode and being calibrated
Analyzer be compared, calculate and be accordingly calibrated the metering performance of dissolved oxygen meter, with present national metrological verification regulations
Compared to mainly there is following advantage: 1, standard value can be directly acquired by normal electrode measurement；2, temperature control is simple, saturation dissolution
Calibration water is obtained and temperature similar in room temperature by the standing in room temperature condition.3, existing national metrological verification regulations are logical
It crosses and is passed through air (oxygen content about 21% in air) into thermostatted water, then by changing the temperature in water and being maintained at certain temperature
Spend in range (regulatory requirements control temperature within the scope of ± 0.2 DEG C, regulatory requirements in 10 DEG C, 20 DEG C, 30 DEG C of three points, when
When dissolved oxygen water differs bigger temperature with environment temperature, to make water temperature control in ± 0.2 DEG C of range, because satisfying when calibration
Exposed to the open air in the environment with dissolved oxygen with water, keep water temperature under certain temperature, there are certain difficulty), make the oxygen content in water
It changes, needs to calculate the oxygen content in water by temperature and atmospheric pressure, entire calculating process is sufficiently complex.The application is then
Calculating and the temperature control process of above-mentioned complexity are avoided, calibration process is simply accurate, high-efficient.
Detailed description of the invention
The structural schematic diagram of Fig. 1 device of the present invention.
The configuration schematic diagram of Fig. 2 high photographing instrument.
1- constant temperature water bath, 2- temperature sensor, 3- fluorescence method normal electrode, 4- is by compared with dissolved oxygen meter entrance, 5-
Oxygen calibrating gas bottle in nitrogen, 6- industrial personal computer, 7- air pump, 8- gas supply pipeline, the dewatering outlet 9-, 10- high photographing instrument, 11- bracket, the bottom 12-
Seat.
Specific embodiment
The gas supply pipeline 8 includes vertical section and horizontal segment, and vertical section is protruded by 1 top cover of constant temperature water bath, and horizontal segment leans on
Nearly 1 bottom of constant temperature water bath and it is provided with multiple ventholes thereon.The above structure of air duct facilitates oxygen calibrating gas in nitrogen
It is sufficiently quickly dissolved in the water of constant temperature water bath, is conducive to calibration process and more quickly finishes.
The temperature sensor 2 is multiple it can be seen from Fig. 1, wherein having is in be horizontally set in constant temperature water bath 1
Wall, and in being vertically arranged in below constant temperature water bath top cover.It could be aware that the temperature feelings of constant temperature water bath everywhere in this way
Condition.
Side wall of the constant temperature water bath 1 close to bottom is provided with dewatering outlet 9.
The bracket 11 is mounted on one for placing by the pedestal 12 compared with dissolved oxygen meter.
A kind of dissolved oxygen measurement calibration method, includes the following steps:
(1) saturated dissolved oxygen water is prepared
After distilled water or high purity water are put into constant temperature water bath, the calibrating gas for being passed through oxygen in a certain concentration nitrogen (passes through
Oxygen calibrating gas bottle in nitrogen), the numerical value of dissolved oxygen on industrial personal computer is observed, when the numerical value of dissolved oxygen sensing becomes in decimal point third position
When dynamic, it is believed that be passed through the molecular oxygen in nitrogen after oxygen calibrating gas, in water and be saturated；
(2) whether the temperature for observing water temperature and surrounding air in constant temperature water bath approaches, when the two temperature difference is less than
At 0.2 DEG C, it is believed that calibration environment condition has；
(3) by the probe for the dissolved oxygen meter being calibrated by being put into constant temperature water bath compared with dissolved oxygen meter entrance 4
In, after the dissolved oxygen meter measured value that is calibrated is stablized, the dissolved oxygen meter measured value 2 significant digits that are calibrated
Numerical value changes primary, and high photographing instrument is primary (can also manual control) with regard to auto Image Collection identification, continuously three times, be averaged as
One measurement result；The variation of decimal point on high photographing instrument automatic identification dissolved oxygen meter display screen, this is that the prior art is easy
It realizes；
(4) the dissolved oxygen concentration error of indication is calculated by formula (2)；
In formula: Δ C2--- the dissolved oxygen concentration error of indication, unit mg/L；
--- the dissolved oxygen meter measurement average value being calibrated, unit mg/L；
Cs2--- the dissolved oxygen concentration reference value surveyed on industrial personal computer by fluorescence method normal electrode, unit mg/L；
(5) concentration value of nitrogen is changed the step in (one) in nitrogen in the calibrating gas of oxygen at least twice, after changing every time all
Step (1)~(four) are repeated, at least three Δ C are finally obtained2Value；
(6) at least three Δ C2A maximum value is selected in value, as calibration result, completes calibration.
Fluorescence method normal electrode is corrected by the phase difference of measurement excitation feux rouges and reference light in conjunction with air pressure, is marked with inside
As the standard dissolved oxygen concentration value of measurement and calibration, the above process is existing for definite value comparison, the directly concentration of measurement oxygen in water
What some fluorescence method normal electrodes can be completed.
Dissolved oxygen calibration 25 DEG C ± 5 DEG C of water temperature of distilled water or high purity water in step (1), this water can pass through room temperature
Natural equilibrium obtains, this temperature water is put into constant temperature water bath, can eliminate influence of the environment temperature to water temperature substantially.
Oxygen calibrating gas is pre-charged in nitrogen in oxygen calibrating gas bottle in nitrogen, is passed through in constant temperature water bath by air pump.Nitrogen
Middle oxygen standard gas concentration can choose 5%, 10%, 20% (nitrogen volume ratio concentration).
Claims (7)
1. a kind of dissolved oxygen measures calibrating installation, including the internal constant temperature water bath for being equipped at least one temperature sensor (2)
(1)；It is characterized in that, constant temperature water bath (1) top cover is provided with by compared with dissolved oxygen meter entrance (4)；Constant temperature water bath (1) top cover
Lower surface is equipped with fluorescence method normal electrode (3)；It further include oxygen calibrating gas bottle (5) in nitrogen, industrial personal computer (6) and by industrial personal computer
(6) air pump (7) controlled；Oxygen calibrating gas bottle (5) is connected with air pump (7) in the nitrogen, and air pump (7) passes through gas supply pipeline
(8) it protrudes into constant temperature water bath (1)；The signal output end of the fluorescence method normal electrode (3) and the signal of industrial personal computer (6) input
End is connected；
It further include the high photographing instrument (10) supported by bracket (11)；The signal output end of high photographing instrument (10) and the letter of industrial personal computer (6)
Number input terminal is connected.
2. a kind of dissolved oxygen as described in claim 1 measures calibrating installation, which is characterized in that the gas supply pipeline (8) includes
Vertical section and horizontal segment, vertical section are protruded by constant temperature water bath (1) top cover, horizontal segment close to constant temperature water bath (1) bottom and its
On be provided with multiple ventholes.
3. a kind of dissolved oxygen as claimed in claim 1 or 2 measures calibrating installation, which is characterized in that the temperature sensor (2)
To be multiple, wherein having is in be horizontally set on constant temperature water bath (1) inner wall, and push up in constant temperature water bath (1) is vertically arranged in
Lid lower section.
4. a kind of dissolved oxygen as claimed in claim 1 or 2 measures calibrating installation, which is characterized in that constant temperature water bath (1) is close
The side wall of bottom is provided with dewatering outlet (9).
5. a kind of dissolved oxygen as claimed in claim 1 or 2 measures calibrating installation, which is characterized in that bracket (11) installation
At one for placing by the pedestal (12) compared with dissolved oxygen meter.
6. a kind of dissolved oxygen measurement calibration method, is realized, feature using device as claimed in any one of claims 1 to 5
It is, includes the following steps:
(1) saturated dissolved oxygen water is prepared
After distilled water or high purity water are put into constant temperature water bath (1), it is passed through the calibrating gas of oxygen in a certain concentration nitrogen, observes work
The numerical value of dissolved oxygen on control machine (6), when the numerical value of dissolved oxygen sensing is when decimal point third position changes, it is believed that be passed through oxygen mark in nitrogen
After quasi- gas, the molecular oxygen in water has been saturated；
(2) whether the temperature for observing water temperature and surrounding air in constant temperature water bath (1) approaches, when the two temperature difference is less than 0.2
DEG C when, it is believed that calibration environment condition has；
(3) by the probe for the dissolved oxygen meter being calibrated by being put into constant temperature water bath compared with dissolved oxygen meter entrance (4)
(1) in, after the dissolved oxygen meter measured value being calibrated is stablized, two after the dissolved oxygen meter measured value decimal point being calibrated
Bit value changes once, and high photographing instrument (10) identifies once with regard to auto Image Collection, continuously three times, is averaged and measures as one
As a result；
(4) the dissolved oxygen concentration error of indication is calculated as follows；
In formula: Δ C2--- the dissolved oxygen concentration error of indication, unit mg/L；
--- the dissolved oxygen meter measurement average value being calibrated, unit mg/L；
Cs2--- the dissolved oxygen concentration reference value surveyed on industrial personal computer (6) by fluorescence method normal electrode, unit mg/L；
(5) change the step in (one) in nitrogen that the concentration value of nitrogen at least twice, all repeats after changing every time in the calibrating gas of oxygen
Step (1)~(four) finally obtain at least three Δ C2Value；
(6) at least three Δ C2A maximum value is selected in value, as calibration result, completes calibration.
7. a kind of dissolved oxygen measurement calibration method as claimed in claim 6, which is characterized in that dissolved oxygen is calibrated in step (1)
With 25 DEG C ± 5 DEG C of water temperature of distilled water or high purity water.
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| CN110320091A (en) * | 2019-08-15 | 2019-10-11 | 南京嘉恒仪器设备有限公司 | It is a kind of to prepare saturation dissolved oxygen water installations |
| CN110687269A (en) * | 2019-11-25 | 2020-01-14 | 河南省计量科学研究院 | Verification and calibration device for dissolved oxygen tester |
| CN110687266A (en) * | 2019-11-11 | 2020-01-14 | 广东省计量科学研究院 | Calibrating device for calibration of dissolved oxygen tester and working method thereof |
| CN110823976A (en) * | 2019-11-28 | 2020-02-21 | 河南省计量科学研究院 | Microbial membrane electrode method BOD analyzer calibration method |
| CN111239091A (en) * | 2020-02-23 | 2020-06-05 | 江苏省农业科学院 | Dissolved oxygen sensor calibration device and calibration method based on fluorescence quenching principle |
| CN113984855A (en) * | 2021-10-22 | 2022-01-28 | 福建福清核电有限公司 | Method and device for measuring concentration of target gas in radioactive waste gas |
| CN110687269B (en) * | 2019-11-25 | 2024-06-04 | 河南省计量测试科学研究院 | Calibrating device for dissolved oxygen meter |
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| CN111239091A (en) * | 2020-02-23 | 2020-06-05 | 江苏省农业科学院 | Dissolved oxygen sensor calibration device and calibration method based on fluorescence quenching principle |
| CN113984855A (en) * | 2021-10-22 | 2022-01-28 | 福建福清核电有限公司 | Method and device for measuring concentration of target gas in radioactive waste gas |
| CN113984855B (en) * | 2021-10-22 | 2024-01-23 | 福建福清核电有限公司 | Method and device for measuring concentration of target gas in radioactive waste gas |
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Application publication date: 20190802 |