CN102706828B - Chemical oxygen demand detecting device and detecting method - Google Patents
Chemical oxygen demand detecting device and detecting method Download PDFInfo
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- CN102706828B CN102706828B CN201210171889.0A CN201210171889A CN102706828B CN 102706828 B CN102706828 B CN 102706828B CN 201210171889 A CN201210171889 A CN 201210171889A CN 102706828 B CN102706828 B CN 102706828B
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000126 substance Substances 0.000 title claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 20
- 239000001301 oxygen Substances 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 230000003287 optical effect Effects 0.000 claims abstract description 36
- 238000012545 processing Methods 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 230000005622 photoelectricity Effects 0.000 claims description 12
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- 238000004140 cleaning Methods 0.000 claims description 9
- 241000237983 Trochidae Species 0.000 claims description 6
- 238000010561 standard procedure Methods 0.000 claims description 6
- 230000007246 mechanism Effects 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
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- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000000523 sample Substances 0.000 description 59
- 239000013535 sea water Substances 0.000 description 11
- 238000005259 measurement Methods 0.000 description 7
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 4
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- 238000004497 NIR spectroscopy Methods 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
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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 chemical oxygen demand (COD).
Background technology chemical oxygen demand (COD) (Chemical Oxygen Demand, be called for short COD) is the amount of the oxygenant that reducing substances consumed that is easily oxidized by strong oxidizer in water, and is converted into the mass concentration of oxygen, in mg/L.In water, reducing substances has organism, nitrite, ferrous salt and sulfide etc., and chemical oxygen demand (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, owing to clearing up sample, need the regular hour, and in digestion agent, contain the heavy metal ion such as chromium ion, silver ion, when not focusing on, easily environment is caused to secondary pollution; Meanwhile, chemical method COD on-line monitoring instrument has the shortcomings such as test data time delay is long, failure rate is high, experimental cost is high, the COD analyser that for example U.S.'s Hash company develops, 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 without using chemical reagent, 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 larger to water-quality constituents restriction; Near-Infrared Absorption Method, because hydrone is seriously restricted infrared light scattering, only limits to the laboratory study stage, can not generally use.
Summary of the invention the object of the present invention is to provide that detection speed is fast, pick-up unit and the detection method of non-secondary pollution, cost is low, usable range is wide online detection chemical oxygen demand (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 connected closure casings, and one is water sample chamber, and another is 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 sample introduction through hole is provided with screen pack; Its water sample chamber lower case is provided with out sample 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 contrary.The through hole that is respectively equipped with two coaxial cables on another two side bodies vertical with permanent magnet place face of water sample chamber, it is incident and outgoing optical window that the side of through hole towards water sample chamber is provided with transparent optical window, the distance between two optical windows is transmission light path.Incident light outside window side be provided with the photoelectricity chamber housing that is connected as a single entity with water sample chamber and seals, incident optical window in it is provided with collimating optics module and spectroscope, spectroscope and input path are at 45 °, at the indoor ultraviolet source that is provided with of photoelectricity as deuterium lamp, this ultraviolet source is connected with light source driver module, and this light source driver module comprises power supply and driving circuit.The light that ultraviolet source sends after the light splitting of collimating optics module, through the transmissive portion of sample cell as flashlight, be irradiated to emergent light outside window in side opening set light convergence module as convex lens, after collimation, be irradiated on the photodetector of photoelectric switching circuit; Reflected light is irradiated on the photodetector of photoelectric switching circuit in reference path, and light path is transmission light path.Above-mentioned two photoelectric switching circuits are all connected with data processing module.The effect of this data processing module is electric signal that the photoelectric switching circuit on reflected light path is obtained and through the electric signal that water sample chamber photoelectric switching circuit obtains, processes the then output port through being connected 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.Separately, 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.Wherein, motor is the clockwise and anticlockwise motor being connected with photoelectricity driver module, is arranged on the top shell body of water sample chamber, and motor outside is provided with the under shed flute profile outer cover of its containing, and outer cover lower ending opening is connected with the housing seal of water sample chamber.Above-mentioned motor output shaft is connected with drive link upper end, and this drive link is connected with driving gear through the through hole lower end on top shell body, and this driving gear meshes with a follower gear again.Because motor output shaft turns half cycle, oppositely turn, therefore two gears only have half intermeshing, and each is connected second half of the non-engagement of two gears with a connecting rod, and the other end of these two connecting rods is respectively provided with the helical blade brush that can clean optical window.
Detection method of the present invention is as follows:
1, by the water sample chamber sample holes valve open of above-mentioned COD pick-up unit, be then placed in underwater, gather detected water sample.
2, water sample chamber until this device is full of after water sample, by triggering light source driver module, open ultraviolet source, this ultraviolet source (deuterium lamp) sends ultraviolet light, available band is 200nm ~ 400nm, after spectroscope light splitting, one road light transmission is crossed water sample and after converging, is transmitted arrival photoelectric switching circuit, another road is directly delivered in photodetection module after reflection, two-way light converts the light signal of receiving to electric signal and sends into data processing module, after processing, signal obtains electric signal V, output terminal transfers out by antenna radiation pattern, by base station, received, show and analyze.
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 obtain absorbance
wherein A is the absorbance of sample solution, I
0be with reference to light intensity value, I is the transmitted intensity after sample absorbs, and K is absorption coefficient, and C is the concentration of sample solution, and L is the length of optical propagation direction sample cell.Magnetized Seawater sample is diluted to n different concentration, measure the absorbance of Magnetized Seawater in the full spectrum of ultraviolet and by National Standard Method (GB 11892-1989) (basic potassium permanganate method), measure the COD of the Seawater Samples of variable concentrations, after modeling, be used for predicting the COD of Seawater Samples to be measured, 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, in additional magnetic field B, is within the scope of 0.1T ~ 0.5T, obtains respectively the ultraviolet absorptivity A at the every 10nm of 200 ~ 400nm place by spectrometer
200+10*i, i=0,1,2 ..., 20.Due to the COD under same case, adopt magnetization to process rear reduction amplitude consistent.Magnetization process after COD to reduce amplitude ζ relevant with magnetic field intensity, when outside magnetic field is 0.35T, the COD measurement upper limit is compared and when not adding magnetic field, has been become large approximately 17.6%.After opto-electronic conversion, photoelectricity flow valuve be can obtain, then through current-to-voltage convertor, corresponding measuring voltage V and reference voltage V are transformed into
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 be obtained by National Standard Method (GB11892-1989) (basic potassium permanganate method) matching.
For guaranteeing measuring accuracy, be preferably in before detecting the entrance window of water sample chamber and exit window are cleaned, i.e. actuating motor, motor cleans incident optical window and outgoing optical window by drive link, gear and connecting rod drive brush.After cleaning, by corresponding control circuit and mechanical hook-up, two brushes are packed up, to guarantee that ultraviolet light can pass through water sample chamber smoothly.
The present invention compared with prior art tool has the following advantages: 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 testing cost, do not increase secondary pollution; 4, introduce strong magnetic field action, expanded measurement range; Be widely used in the natural water samples such as seawater, river, lake water.
Accompanying drawing explanation
Fig. 1 is that the master of the device for detecting chemical oxygen demand of the embodiment of the present invention looks 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 present invention.
Fig. 3 is the course of work block diagram of the device for detecting chemical oxygen demand of the embodiment of the present invention.
Embodiment
In the simplified schematic diagram of the device for detecting chemical oxygen demand of the embodiment of the present invention shown in Fig. 1 and Fig. 2, measuring cell is two connected 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 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.Separately at the indoor optical window cleaning mechanism that is provided with of water sample, the turn clockwise and anticlockwise motor that half cycle oppositely turn of its motor 6 for being connected with light source driver module, be arranged on the top shell body of water sample chamber, motor outside is provided with the under shed flute profile outer cover of its containing, and outer cover lower ending opening is connected with the housing seal of water sample chamber.Above-mentioned motor output shaft is connected with drive link 7 upper ends, this drive link is connected with driving gear 8 through the through hole lower end on top shell body, this driving gear meshes with a follower gear again, each is connected second half of the non-engagement of two gears with a connecting rod 9, and the other end of these two connecting rods is respectively provided with the helical blade brush 10,11 that can clean optical window.At the inner housing center of both sides, above-mentioned water sample chamber, be respectively equipped with two relatively also permanent magnetic iron blocks 12,13 of sealing, and both magnetic poles are contrary.On another two side bodies vertical with permanent magnet place face of water sample chamber, be respectively equipped with the through hole of two coaxial cables, each through hole is equipped with transparent optical window towards water sample chamber one side and is incident optical window 14 and outgoing optical window 15, distance between two optical windows is transmission light path, in incident optical window 14 outsides, be provided with the photoelectricity chamber housing that is connected as a single entity with water sample chamber and seals, on incident optical window in it, establish collimating optics module and spectroscope 16, spectroscope and input path are at 45 °, on the indoor spectroscopical reflected light path of photoelectricity, be provided with photoelectric switching circuit 17, light path is transmission light path.It is convex lens 18 that emergent light is provided with light convergence module in the hole of side outside window, is provided with photoelectric switching circuit 19 after these convex lens, and above-mentioned two photoelectric switching circuits are all connected with data processing module 20.At the indoor ultraviolet source 21 that is provided with of photoelectricity, this ultraviolet source (deuterium lamp) is connected with light source driver module 22, and this light source driver module comprises power supply and driving circuit.The center of above-mentioned ultraviolet source, collimating optics module, incident optical window and outgoing optical window and light convergence module is all on a line, and output port is 23.Separately in measuring cell, be provided with electric wire and walk pipe 24.
In the course of work block diagram of the device for detecting chemical oxygen demand of the embodiment of the present invention shown in Fig. 3, this COD pick-up unit is when work, it is luminous that light source driver module orders about ultraviolet source, this ultraviolet light after collimating optics module and spectroscope respectively through the water sample of reference path and measuring cell, reflected light through reference path shines directly on photodetector, and be irradiated on photodetector through light convergence module through the transmitted light of measuring cell water sample, this photodetector is converted to electric signal by the light signal of receiving, pass to again data processing module, then the final COD value obtaining is sent.The water sample chamber of measuring cell is provided with optical window cleaning mechanism.The water sample chamber of measuring cell is provided with two permanent magnetic iron blocks that magnetic pole is contrary, the static magnetic field that they produce changes the distribution of seawater hydrone and configuration state, can adsorb some short grained things that are suspended on the one hand, reduce the turbidity factor that measurement has the greatest impact to COD, and can pollute in processing helpful at water; On the other hand due in aqueous water, by Hydrogenbond multi-form moisture subchain together, after strong magnetic field action, changed polarization characteristic, thereby distribution and the gathering of hydrone have also been changed, the change of this polarization and state of aggregation has affected the energy level transition characteristic of electronics in 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 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 the concentration of COD in this saturation effect measurement seawater.
Above-mentioned COD pick-up unit is placed in to the seawater in marine site, Qinhuangdao, by water sample chamber sample holes valve open, is placed in 50cm place, underwater and gathers detected water sample.Before measurement, Single-chip Controlling automatic cleaning system will enter, outgoing optical window brushed and cleaned up by helical blade.After cleaning 20s, by corresponding control circuit and mechanical hook-up, two brushes are packed up, to guarantee that ultraviolet light can pass through water sample chamber smoothly.After being full of water sample, water sample chamber opens ultraviolet source by triggering light source driver module, this ultraviolet source (deuterium lamp) sends ultraviolet light, its wave band is that 200nm ~ 400nm is after spectroscope light splitting, water sample is crossed in one road light transmission, through optics convergence module, be delivered to photoelectric switching circuit again, another road is directly delivered in photodetection module after reflection, two-way light converts the light signal of receiving to electric signal and sends into data processing module, after processing, signal obtains electric signal, by antenna radiation pattern, transfer out, by base station, receive, show and analyze.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), wherein k
b, V
0, V and each parameter of ζ concrete numerical value substitution above formula, obtain the COD value of this place's seawater, wherein k
bfor response sensitivity is the slope of matched curve, can be obtained by National Standard Method (GB 11892-1989) (basic potassium permanganate method) matching V
0for reference voltage, V are that measuring voltage, ζ are for the rear COD reduction of magnetization processing amplitude is (for the sample of concentration range 5 ~ 25mg/L, apply different magnetic field intensity (0.1T ~ 0.5T), when COD concentration is constant, record reduction amplitude ζ now, matching obtains the relation of magnetic field intensity B and the amplitude of reduction ζ; Prediction is during sample, B=0.35T for example, now ζ is about 0.15).
Adopt identical method, again the seawater of 4 different locations is detected, its result is as following table.
Table 1 is to adopt respectively the inventive method and the result contrast of National Standard Method to 5 water sample detection
As can be seen from the above table, the testing result error of the result that employing apparatus of the present invention and detection method draw and National Standard Method (adopting GB11892-1989 basic potassium permanganate method) is very little, is convenient to realize online detection.
Claims (6)
1. a device for detecting chemical oxygen demand, measuring cell comprises water sample chamber and photoelectricity chamber, its water sample chamber lower case is provided with out sample through hole and sample outlet hole valve and the screen pack supporting with it, on two side bodies of water sample chamber, be respectively equipped with the through hole of two coaxial cables, the side of through hole towards water sample chamber is provided with incident optical window and outgoing optical window, incident light outside window side be provided with ultraviolet source, this ultraviolet source is connected with light source driver module, emergent light is provided with light convergence module in side opening outside window, after this light convergence module, be provided with photoelectric switching circuit, photoelectric switching circuit is connected with data processing module, this data processing module is connected with output port, it is characterized in that: water sample chamber upper body is provided with sample introduction through hole and the sample holes valve supporting with it, sample introduction through hole is provided with screen pack, 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 contrary, distance between two optical windows vertical with permanent magnet place face of water sample chamber is transmission light path, incident light outside window side be provided with the photoelectricity chamber housing that is connected as a single entity with water sample chamber and seals, incident optical window in it is provided with collimating optics module and spectroscope, spectroscope and input path are at 45 °, in photoelectricity indoor reflection light path, be provided with photoelectric switching circuit, light path is transmission light path, above-mentioned ultraviolet source, collimating optics module, the center of 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 being connected with photoelectricity driver module, be arranged on the top shell body of water sample chamber, motor outside is provided with the under shed flute profile outer cover of its containing, outer cover lower ending opening is connected with the housing seal of water sample chamber, above-mentioned motor output shaft is connected with drive link upper end, this drive link is connected with driving gear through the through hole lower end on top shell body, this driving gear meshes with a follower gear again, each is connected second half of the non-engagement of two gears with a connecting rod, the other end of these two connecting rods is respectively 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 and go out on sample through hole to be equipped with screen pack.
4. the method for detecting chemical oxygen demand of claim 1, is characterized in that:
(1), by the water sample chamber sample holes valve open of above-mentioned COD pick-up unit, be then placed in underwater, gather detected water sample;
(2), until the water sample chamber of this device, be full of after water sample, by triggering light source driver module, open ultraviolet source, this ultraviolet source sends ultraviolet light, after spectroscope light splitting, one road light transmission is crossed water sample and after converging, is transmitted arrival photoelectric switching circuit, another road is directly delivered in photodetection module after reflection, two-way light converts the light signal of receiving to electric signal and sends into data processing module, after processing, signal obtains electric signal V, output port transfers out by antenna radiation pattern, by base station, is received, is shown and analyze;
(3), the COD value of this water sample adopts following formula to calculate: COD=k
ba
b=k
bln (V
0/ V)/(1-ζ), wherein k
b, V
0, V and each parameter of ζ concrete numerical value substitution above formula, obtain the COD value of this water sample, wherein k
bfor response sensitivity is the slope of matched curve, can be obtained by the matching of National Standard Method GB11892-1989 basic potassium permanganate method V
0for reference voltage, V are that measuring voltage, ζ are the rear COD reduction of magnetization processing amplitude.
5. method for detecting chemical oxygen demand according to claim 4, is characterized in that: it is 200nm～400nm that ultraviolet source sends ultraviolet light available band.
6. according to the method for detecting chemical oxygen demand described in claim 4 or 5, it is characterized in that: before detection, the entrance window of water sample chamber and exit window are cleaned, it is actuating motor, motor drives brush to clean incident optical window and outgoing optical window by drive link, gear and connecting rod, after cleaning, by corresponding control circuit and mechanical hook-up, two brushes is packed up.
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| CN103163053B (en) * | 2013-02-05 | 2015-04-01 | 中国矿业大学 | Infrared detection device and detection method of coal dust |
| 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 |
| GB201614497D0 (en) * | 2016-08-25 | 2016-10-12 | Rs Hydro Ltd | Water quality sensing |
| CN109374559B (en) * | 2018-12-24 | 2020-04-07 | 燕山大学 | Water body COD value determination method based on ultraviolet absorption spectrum |
| CN109459402B (en) * | 2018-12-26 | 2021-02-23 | 南京波思途智能科技股份有限公司 | Method for predicting COD (chemical oxygen demand) parameter of water quality by spectrometry |
| 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 |
| CN117805046B (en) * | 2024-02-28 | 2024-06-04 | 三亚海慧海洋科技有限公司 | Method and device for detecting chemical oxygen demand based on turbidity compensation |
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| CN2735341Y (en) * | 2003-07-02 | 2005-10-19 | 江苏绿叶环保科技仪器有限公司 | Online automatic monitor for chemical oxygen demand |
| CN101329252B (en) * | 2007-06-18 | 2010-09-08 | 北京安控科技股份有限公司 | Method for detecting chemical oxygen demand |
| DE102009026453A1 (en) * | 2009-05-25 | 2010-12-09 | Endress + Hauser Conducta Gesellschaft für Mess- und Regeltechnik mbH + Co. KG | Method and device for determining a statement about the occurrence of ingredients of a liquid sample with oxygen requirement |
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