CN102706828A - Chemical oxygen demand detecting device and detecting method - Google Patents
Chemical oxygen demand detecting device and detecting method Download PDFInfo
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- CN102706828A CN102706828A CN2012101718890A CN201210171889A CN102706828A CN 102706828 A CN102706828 A CN 102706828A CN 2012101718890 A CN2012101718890 A CN 2012101718890A CN 201210171889 A CN201210171889 A CN 201210171889A CN 102706828 A CN102706828 A CN 102706828A
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Abstract
The invention discloses a chemical oxygen demand detecting device. A water sample chamber of a measuring tank is provided with a sample inlet through hole, a sample outlet through hole and a valve; two opposite permanent magnetic iron blocks with magnetic poles being opposite are arranged at two sides of the water sample chamber respectively; shells at the other two sides of the water sample chamber are provided with an incident light window and an emergent light window; a collimation optical module and a spectroscope are arranged outside the incident light window; an angle of 45 degrees is formed between the the spectroscope and an incident light path; and an ultraviolet light source is arranged in a photovoltaic chamber and connected with a light source driving module. In the photovoltaic chamber, the reflected light path of the spectroscope is provided with a photovoltaic conversion circuit. A light collection module is arranged outside the emergent light window, the other photovoltaic conversion circuit is arranged behind the emergent light window and the two photovoltaic conversion circuits are connected with a data processing module. The data processing module is connected with an output port. The centers of the ultraviolet light source, the collimation optical module, the incident light window, the emergent light window and the light collection module are positioned on the same straight line. The detecting device and the detecting method are fast in detection speed, free of secondary pollution, low in cost and applicable to online detection.
Description
Technical field the present invention relates to a kind of detecting instrument, particularly detects the device and method of COD.
Background technology COD (Chemical Oxygen Demand is called for short COD) is to be prone in the water be converted into the mass concentration of oxygen, in mg/L by the amount of the oxygenant that reducing substances consumed of strong oxidizer oxidation.Reducing substances has organism, nitrite, ferrous salt and sulfide etc. in the water, and COD has reflected the degree that water body is polluted by reducing substances, is one of relative indicatrix of organic content.
At present; What the COD on-line monitoring instrument of exploitation used both at home and abroad is chemical method mostly; Utilize the on-line monitoring instrument of chemical method exploitation, need the regular hour owing to clear up sample, and clear up heavy metal ion such as containing chromium ion, silver ion in the agent; When not focusing on, easily environment is caused secondary pollution; Simultaneously, chemical method COD on-line monitoring appearance has long, the shortcomings such as failure rate is high, experimental cost height of test data time-delay, the COD analyser of U.S.'s Hash company exploitation for example, the online COD analyser of German LAR exploitation.In addition the method that also has application of pure physics, ultraviolet method for example, near infrared spectroscopy etc., these methods can be carried out continuous monitoring, and need not to use chemical reagent, and the test duration is short, and the error that can avoid some conventional methods to bring.But traditional ultraviolet method measurement range is little, and bigger to the water-quality constituents restriction; The near infrared method only limits to the laboratory study stage because hydrone seriously is restricted infrared light scattering, can not generally use.
Summary of the invention the object of the present invention is to provide that detection speed is fast, the pick-up unit and the detection method of non-secondary pollution, cost is low, usable range is wide online detection COD.
COD pick-up unit of the present invention mainly includes measuring cell, light source driver module, ultraviolet source, collimating optics module, light convergence module, opto-electronic conversion and data processing module and optical window cleaning mechanism.Wherein, measuring cell is two continuous closure casings, and one is the water sample chamber, and another is the photoelectricity chamber, and its water sample chamber upper body is provided with sample introduction through hole and the sample holes valve supporting with it, and the sample introduction through hole is provided with screen pack; Its water sample chamber lower case is provided with out kind through hole and sample outlet hole valve and the screen pack supporting with it.On the inner housing of both sides, above-mentioned water sample chamber, be respectively equipped with two relatively also permanent magnetic iron blocks of sealing, and both magnetic poles are opposite.Belong to the through hole that is respectively equipped with two coaxial cables on vertical two side bodies in addition of face in the water sample chamber with permanent magnet, it is incident and outgoing optical window that the side of through hole towards the water sample chamber is provided with transparent optical window, and the distance between two optical windows is the transmission light path.Incident light outside window side be provided with the photoelectricity chamber housing that is connected as a single entity and seals with the water sample chamber; Incident optical window in it is provided with collimating optics module and spectroscope; Spectroscope becomes 45 ° with input path; At indoor ultraviolet source such as the deuterium lamp of being provided with of photoelectricity, this ultraviolet source links to each other with light source driver module, and this light source driver module comprises power supply and driving circuit.The light that ultraviolet source sends shines emergent light set light convergence module such as convex lens in the side opening outside window through the transmissive part of sample cell as flashlight after the beam split of collimating optics module, shine behind the collimation on the photodetector of photoelectric switching circuit; Reflected light shines on the photodetector of photoelectric switching circuit on the reference path, and light path is the transmission light path.Above-mentioned two photoelectric switching circuits all link to each other with data processing module.The effect of this data processing module is a electric signal that the photoelectric switching circuit on the reflected light path is obtained and pass electric signal that water sample chamber photoelectric switching circuit obtains and handle the output port that warp then links to each other with data processing module and pass.The center of above-mentioned ultraviolet source, collimating optics module, incident optical window and outgoing optical window and light convergence module all point-blank.At the indoor optical window cleaning mechanism that is provided with of water sample, it mainly includes: motor, drive link, gear, connecting rod and brush in addition.Wherein, motor is the clockwise and anticlockwise motor that links to each other with the photoelectricity driver module, is arranged on the housing of top, water sample chamber, and the motor outside is provided with the under shed flute profile outer cover with its containing, and the outer cover lower ending opening is connected with the housing seal of water sample chamber.Above-mentioned motor output shaft links to each other with the drive link upper end, and the through hole lower end that this drive link passes on the housing of top links to each other with driving gear, and this driving gear meshes with a follower gear again.Half cycle is promptly reverse to be changeed because motor output shaft changes, and therefore two gears only have half to be meshing with each other, and each links to each other second half of the non-engagement of two gears with a connecting rod, and the other end of these two connecting rods respectively is provided with the helical blade brush that can clean optical window.
Detection method of the present invention is following:
1, with the water sample chamber sample holes valve open of above-mentioned COD pick-up unit, places the underwater then, gather detected water sample.
After the water sample chamber of 2, treating this device is full of water sample, open ultraviolet source through triggering light source driver module, this ultraviolet source (deuterium lamp) sends ultraviolet light; Available band is 200nm ~ 400nm; After the spectroscope beam split, one tunnel transmittance is crossed water sample and after converging, is transmitted the arrival photoelectric switching circuit, and another road is directly delivered on the photodetection module after reflection; Two-way light converts the light signal of receiving to electric signal and sends into data processing module; Obtain electric signal V through after the signal Processing, output terminal transfers out through antenna radiation pattern, is received, shows and analyzed by the base station.
3, the COD value of this water sample adopts following formula to calculate:
The present invention adopts full spectra measurement, according to Lambert-Beer's law, and I=I
0E
-KCL, can get absorbance
Wherein A is the absorbance of sample solution, I
0Be with reference to light intensity value, I is the transmitted intensity after absorbing through sample, and K is an absorption coefficient, and C is the concentration of sample solution, and L is the length of optical propagation direction sample cell.To magnetize the seawater sample and be diluted to n different concentration; Measure the absorbance of magnetization seawater on the full spectrum of ultraviolet and reach the COD that measures the seawater sample of variable concentrations through National Standard Method (GB 11892-1989) (basic potassium permanganate method); Be used for predicting the COD of seawater sample to be measured after the modeling, A
B=k
1A
1+ k
2A
2+ k
3A
3+ ... + k
nA
n, k wherein
i, i=1,2 ..., n is the constant relevant with magnetic field intensity, is in 0.1T ~ 0.5T scope adding magnetic field B, obtains the ultraviolet absorptivity A at the every 10nm of 200 ~ 400nm place respectively through spectrometer
200+10*i, i=0,1,2 ..., 20.Because the COD under the same case, it is consistent to adopt magnetization to handle back reduction amplitude.Back COD is handled in magnetization, and to reduce amplitude ζ relevant with magnetic field intensity, when outside magnetic field is 0.35T, COD measure the upper limit compare when not adding magnetic field change big about 17.6%.The photoelectricity flow valuve be can obtain after the opto-electronic conversion, corresponding measuring voltage V and reference voltage V are transformed into through current-to-voltage convertor then
0, and A
B=lnV
0/ V/ (1-ζ), predicted value COD=k
BA
B, k wherein
BFor response sensitivity is the slope of matched curve, can obtain by National Standard Method (GB11892-1989) (basic potassium permanganate method) match.
Be to guarantee measuring accuracy, be preferably in that entrance window and the exit window to the water sample chamber cleans before detecting, i.e. actuating motor, motor cleans incident optical window and outgoing optical window through drive link, gear and connecting rod drive brush.After finishing, cleaning packs up two brushes, to guarantee that ultraviolet light can pass through the water sample chamber smoothly through corresponding control circuit and mechanical hook-up.
The present invention compared with prior art has following advantage: 1, simple in structure, be convenient to realize online detection; 2, utilize the method for Photoelectric Detection, detection speed is accelerated; 3, do not use chemical reagent, reduced the detection cost, do not increase secondary pollution; 4, introduce strong magnetic field action, enlarged measurement range; Adaptable across natural water samples such as seawater, river, lake water.
Description of drawings
Fig. 1 is that the master of the device for detecting chemical oxygen demand of the embodiment of the invention looks the section simplified schematic diagram.
Fig. 2 is the solid signal meaning sketch of the device for detecting chemical oxygen demand of the embodiment of the invention.
Fig. 3 is the course of work block diagram of the device for detecting chemical oxygen demand of the embodiment of the invention.
Embodiment
In the simplified schematic diagram of the device for detecting chemical oxygen demand of the embodiment of the invention illustrated in figures 1 and 2; Measuring cell is two continuous closure casings; One is water sample chamber 1, and water sample chamber upper left quarter housing is provided with sample introduction through hole and the sample holes valve 2 supporting with it, and the sample introduction through hole is provided with screen pack 3; Its water sample chamber lower case is provided with sample outlet hole valve and screen pack 4,5.In addition at the indoor optical window cleaning mechanism that is provided with of water sample; Its motor 6 is the promptly reverse clockwise and anticlockwise motor that changes of commentaries on classics half cycle that links to each other with light source driver module; Be arranged on the housing of top, water sample chamber; The motor outside is provided with the under shed flute profile outer cover with its containing, and the outer cover lower ending opening is connected with the housing seal of water sample chamber.Above-mentioned motor output shaft links to each other with drive link 7 upper ends; The through hole lower end that this drive link passes on the housing of top links to each other with driving gear 8; This driving gear meshes with a follower gear again; Each links to each other second half of the non-engagement of two gears with a connecting rod 9, and the other end of these two connecting rods respectively is provided with the helical blade brush 10,11 that can clean optical window.Be respectively equipped with two relatively also permanent magnetic iron blocks 12,13 of sealing at the inner housing center of both sides, above-mentioned water sample chamber, and both magnetic poles are opposite.Belong to the through hole that is respectively equipped with two coaxial cables on vertical two side bodies in addition of face in the water sample chamber with permanent magnet; One side is equipped with transparent optical window and is incident optical window 14 and outgoing optical window 15 each through hole towards the water sample chamber; Distance between two optical windows is the transmission light path; Be provided with the photoelectricity chamber housing that is connected as a single entity and seals with the water sample chamber in incident optical window 14 outsides, establish collimating optics module and spectroscope 16 on the incident optical window in it, spectroscope becomes 45 ° with input path; On the indoor spectroscopical reflected light path of photoelectricity, be provided with photoelectric switching circuit 17, light path is the transmission light path.It is convex lens 18 that emergent light is provided with the light convergence module in the hole of side outside window, and these convex lens are provided with photoelectric switching circuit 19 at the back, and above-mentioned two photoelectric switching circuits all link to each other with data processing module 20.At the indoor ultraviolet source 21 that is provided with of photoelectricity, this ultraviolet source (deuterium lamp) links to each other with light source driver module 22, and this light source driver module comprises power supply and driving circuit.All on a line, output port is 23 at the center of above-mentioned ultraviolet source, collimating optics module, incident optical window and outgoing optical window and light convergence module.In measuring cell, be provided with electric wire in addition and walk pipe 24.
In the course of work block diagram of the device for detecting chemical oxygen demand of the embodiment of the invention shown in Figure 3; This COD pick-up unit is when work; It is luminous that light source driver module orders about ultraviolet source, and this ultraviolet light respectively through the water sample of reference path and measuring cell, shines directly on the photodetector through the reflected light of reference path behind collimating optics module and spectroscope; And shine on the photodetector through the light convergence module through the transmitted light of measuring cell water sample; This photodetector converts the light signal of receiving into electric signal, passes to data processing module again, and the final COD value that will obtain then sends.The water sample chamber of measuring cell is provided with the optical window cleaning mechanism.The water sample chamber of measuring cell is provided with two permanent magnetic iron blocks that magnetic pole is opposite; The static magnetic field that they produce changes the distribution of seawater hydrone and configuration state; Can adsorb some short grained outstanding absurd creatures on the one hand; Reduce the turbidity factor that measurement has the greatest impact to COD, and can pollute in the processing helpful at water; On the other hand because in aqueous water; Behind strong magnetic field action, changed polarization characteristic through hydrogen bonded multi-form moisture subchain together; Thereby the distribution and the gathering of hydrone have also been changed; The change of this polarization and state of aggregation influenced the energy level transition characteristic of electronics in the molecule, thereby caused its increase to the absorption intensity of ultraviolet light, and then had influence on the COD value of seawater.Along with the increase of magnetizing time, photon absorbing intensity obviously increases in the shortwave ultraviolet region, but after the magnetic field radiation long enough time, its photon absorbing intensity no longer increases and increases along with the time, and we just utilize this saturation effect to measure the concentration of COD in the seawater.
Above-mentioned COD pick-up unit is placed the seawater in marine site, Qinhuangdao,, place 50cm place, underwater to gather detected water sample water sample chamber sample holes valve open.The Single-chip Controlling automatic cleaning system will be gone into before measurement, the outgoing optical window cleans up through helical blade brush.Pack up two brushes through corresponding control circuit and mechanical hook-up after cleaning 20s, to guarantee that ultraviolet light can pass through the water sample chamber smoothly.Treat to open ultraviolet source through triggering light source driver module after the water sample chamber is full of water sample; This ultraviolet source (deuterium lamp) sends ultraviolet light, its wave band be 200nm ~ 400nm after the spectroscope beam split, water sample is crossed in one tunnel transmittance; Be delivered to photoelectric switching circuit through the optics convergence module again; Another road is directly delivered on the photodetection module after reflection, and two-way light converts the light signal of receiving to electric signal and sends into data processing module, obtains electric signal through after the signal Processing; Transfer out through antenna radiation pattern, receive, show and analyze by the base station.Then power-off is waited for the beginning of next time measuring.The COD value of this water sample adopts following formula to calculate: COD=k
BA
B=k
BLn (V
0/ V)/(1-ζ), incite somebody to action wherein k
B, V
0, V and each parameter of ζ concrete numerical value substitution following formula, promptly get the COD value of this place's seawater, wherein k
BFor response sensitivity is the slope of matched curve, V can be obtained by National Standard Method (GB 11892-1989) (basic potassium permanganate method) match
0For reference voltage, V are that measuring voltage, ζ handle back COD reduction amplitude (for the sample of concentration range 5 ~ 25mg/L for magnetization; Apply different magnetic field intensitys (0.1T ~ 0.5T); Treat to note when COD concentration is constant the reduction amplitude ζ of this moment, match obtains the relation of magnetic field intensity B and the amplitude of reduction ζ; Prediction is during sample, B=0.35T for example, this moment, ζ was about 0.15).
Adopt identical method, the seawater to 4 different locations detects again, and its result as follows.
Table 1 is to adopt the result's contrast to 5 water sample detection of the inventive method and National Standard Method respectively
Can find out that by last table the testing result error of result that employing apparatus of the present invention and detection method draw and National Standard Method (adopting the GB11892-1989 basic potassium permanganate method) is very little, is convenient to realize online detection.
Claims (6)
1. device for detecting chemical oxygen demand, it is characterized in that: measuring cell is two continuous closure casings, one is the water sample chamber; Another is the photoelectricity chamber, and its water sample chamber upper body is provided with sample introduction through hole and the sample holes valve supporting with it, and the sample introduction through hole is provided with screen pack; Its water sample chamber lower case is provided with out kind through hole and sample outlet hole valve and the screen pack supporting with it, on the inner housing of both sides, above-mentioned water sample chamber, be respectively equipped with two relatively also permanent magnetic iron blocks of sealing, and both magnetic poles is opposite; Belong to the through hole that is respectively equipped with two coaxial cables on vertical two side bodies in addition of face in the water sample chamber with permanent magnet, the side of through hole towards the water sample chamber is provided with incident optical window and outgoing optical window, and the distance between two optical windows is the transmission light path; Incident light outside window side be provided with the photoelectricity chamber housing that is connected as a single entity and seals with the water sample chamber; Incident optical window in it is provided with collimating optics module and spectroscope, and spectroscope becomes 45 ° with input path, at the indoor ultraviolet source that is provided with of photoelectricity; This ultraviolet source links to each other with light source driver module; On photoelectricity indoor reflection light path, be provided with photoelectric switching circuit, light path is the transmission light path, and emergent light is provided with the light convergence module in the side opening outside window; This light convergence module is provided with photoelectric switching circuit at the back; Above-mentioned two photoelectric switching circuits all link to each other with data processing module, and this data processing module links to each other with output port, and the center of above-mentioned ultraviolet source, collimating optics module, incident optical window and outgoing optical window and light convergence module all point-blank.
2. device for detecting chemical oxygen demand according to claim 1; It is characterized in that: at the indoor optical window cleaning mechanism that is provided with of water sample; Its motor is the clockwise and anticlockwise motor that links to each other with the photoelectricity driver module, is arranged on the housing of top, water sample chamber, and the motor outside is provided with the under shed flute profile outer cover with its containing; The outer cover lower ending opening is connected with the housing seal of water sample chamber; Above-mentioned motor output shaft links to each other with the drive link upper end, and the through hole lower end that this drive link passes on the housing of top links to each other with driving gear, and this driving gear meshes with a follower gear again; Each links to each other second half of the non-engagement of two gears with a connecting rod, and the other end of these two connecting rods respectively is provided with the helical blade brush that can clean optical window.
3. device for detecting chemical oxygen demand according to claim 1 and 2 is characterized in that: water sample chamber sample introduction through hole with go out on kind through hole to be equipped with screen pack.
4. the method for detecting chemical oxygen demand of claim 1 is characterized in that:
(1), with the water sample chamber sample holes valve open of above-mentioned COD pick-up unit, place the underwater then, gather detected water sample;
(2), after the water sample chamber of treating this device is full of water sample; Open ultraviolet source by triggering light source driver module; This ultraviolet source sends ultraviolet light; After the spectroscope beam split; One road light transmission is crossed water sample and after converging, is transmitted the arrival photoelectric switching circuit; Another road is directly delivered on the photodetection module after reflection; Two-way light converts the optical signal of receiving to the signal of telecommunication and sends into data processing module; Through obtaining signal of telecommunication V after the signal processing; Output port transfers out by antenna radiation pattern, is received, shows and analyzed by the base station;
(3), the COD value of this water sample adopts following formula to calculate: COD=k
BA
B=k
BLn (V
0/ V)/(1-ζ), incite somebody to action wherein k
B, V
0, V and each parameter of ζ concrete numerical value substitution following formula, promptly get the COD value of this place's seawater, wherein k
BFor response sensitivity is the slope of matched curve, V can be obtained by National Standard Method (GB 11892-1989) (basic potassium permanganate method) match
0For reference voltage, V are that measuring voltage, ζ handle back COD reduction amplitude for magnetization.
5. method for detecting chemical oxygen demand according to claim 4 is characterized in that: it is 200nm ~ 400nm that ultraviolet source sends the ultraviolet light available band.
6. according to claim 4 or 5 described method for detecting chemical oxygen demand; It is characterized in that: entrance window and exit window to the water sample chamber before detection clean; It is actuating motor; Motor drives brush through drive link, gear and connecting rod incident optical window and outgoing optical window is cleaned, and cleans the back that finishes and packs up two brushes through corresponding control circuit and mechanical hook-up.
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| CN103163053A (en) * | 2013-02-05 | 2013-06-19 | 中国矿业大学 | Infrared detection device and detection method of coal dust |
| CN105954192A (en) * | 2016-07-20 | 2016-09-21 | 中国科学院烟台海岸带研究所 | Online dual-light-path water environment measurement device based on spectral measurement technology |
| CN109374559A (en) * | 2018-12-24 | 2019-02-22 | 燕山大学 | A kind of water body COD value measuring method based on ultra-violet absorption spectrum |
| CN109459402A (en) * | 2018-12-26 | 2019-03-12 | 南京波思途智能科技股份有限公司 | A kind of spectroscopic methodology water-quality COD parameter prediction method |
| CN109923414A (en) * | 2016-08-25 | 2019-06-21 | Rs海卓有限公司 | Water quality sensing |
| CN111678869A (en) * | 2020-05-29 | 2020-09-18 | 山东省科学院海洋仪器仪表研究所 | Water quality ecological parameter detection device and detection method |
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| CN103163053A (en) * | 2013-02-05 | 2013-06-19 | 中国矿业大学 | Infrared detection device and detection method of coal dust |
| CN103163053B (en) * | 2013-02-05 | 2015-04-01 | 中国矿业大学 | Infrared detection device and detection method of coal dust |
| CN105954192A (en) * | 2016-07-20 | 2016-09-21 | 中国科学院烟台海岸带研究所 | Online dual-light-path water environment measurement device based on spectral measurement technology |
| CN105954192B (en) * | 2016-07-20 | 2019-07-30 | 中国科学院烟台海岸带研究所 | A kind of double light path water body environment on-line measurement device based on spectral measurement methods |
| CN109923414A (en) * | 2016-08-25 | 2019-06-21 | Rs海卓有限公司 | Water quality sensing |
| CN109374559A (en) * | 2018-12-24 | 2019-02-22 | 燕山大学 | A kind of water body COD value measuring method based on ultra-violet absorption spectrum |
| CN109374559B (en) * | 2018-12-24 | 2020-04-07 | 燕山大学 | Water body COD value determination method based on ultraviolet absorption spectrum |
| CN109459402A (en) * | 2018-12-26 | 2019-03-12 | 南京波思途智能科技股份有限公司 | A kind of spectroscopic methodology water-quality COD parameter prediction method |
| CN111678869A (en) * | 2020-05-29 | 2020-09-18 | 山东省科学院海洋仪器仪表研究所 | Water quality ecological parameter detection device and detection method |
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