CN107014807A - A kind of sea water COD determines device and method - Google Patents
A kind of sea water COD determines device and method Download PDFInfo
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- CN107014807A CN107014807A CN201710445840.2A CN201710445840A CN107014807A CN 107014807 A CN107014807 A CN 107014807A CN 201710445840 A CN201710445840 A CN 201710445840A CN 107014807 A CN107014807 A CN 107014807A
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- G—PHYSICS
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G01—MEASURING; TESTING
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- G01N1/00—Sampling; Preparing specimens for investigation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
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- G01—MEASURING; TESTING
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Abstract
The present invention provides a kind of sea water COD and determines apparatus and method, determining device includes sample injection unit, clears up unit, condensing unit and titration unit, also include color judgment means, the color judgment means include being arranged on the area source and color sensor of the titration tank both sides of the titration unit, the light that the area source is sent is received through the liquid in container by the color sensor, when color sensor reads color for white, judge that blueness is just taken off, titration terminates；Assay method, including sample preparation, clear up, and condense, titration, in addition to：Blank correction.High the beneficial effects of the invention are as follows the efficiency of heating surface, condensation rate is fast, is realized by blank correction and the color intensity of sea water with higher turbidity is accurately judged.
Description
Technical field
Device and method is determined the present invention relates to seawater quality detection field, more particularly to a kind of sea water COD.
Background technology
COD, English full name Chemical Oxygen Demand, i.e. COD, are chemically to measure water sample
It is middle to need the amount of oxidized reducing substances, represented with the mg/ L of oxygen, commonly used to weigh the relative of organic matter in water body
Content, is the measurement to the organic matter in water and inorganic oxide concentration, reflects the degree that water body is polluted by reducing substances,
It is the important indicator of water quality assessment, is one of seawater routine monitoring project.
The characteristics of for seawater quality, China uses basic potassium permanganate method（GB17378.4-2007）It is used as measure seawater
The national standard method of middle COD.Its cardinal principle is：Under alkaline heating condition, with known quantity and excessive permanganic acid
Aerobic material in potassium oxidation seawater, then under the conditions of sulfuric acid, excessive potassium permanganate and dioxy is reduced with KI
Change manganese, the free-iodine of generation is simultaneously titrated with sodium thiosulfate standard solution.This method is manual analytical methods, matched
Detecting instrument belong to non-automatic analytical instrument, due to by lab assistant according to national standard method test COD human errors compared with
Greatly, influence factor is numerous, such as clears up the heat time and differs, and heating-up temperature and solution each several part are heated the not first-class factor of situation all
Certain influence will be brought to experimental result, automation and on-line monitoring are the trend of marine monitoring in recent years.
For example, a kind of automatic analyzer of chemical oxygen demand in seawater is just refer in patent CN2645084Y, including
Electric control gear, optical detection apparatus, optical-electrical converter, amplifier, digital display, computer data processing unit and liquid flow
Road, the electric control gear is made up of control circuit and controlling switch and power supply, and the optical detection apparatus is main by light source, optics
Flow cell is constituted, and light source is light emitting diode, and the optical-electrical converter is made up of photoelectric tube machine support circuit, the liquid flow
It route sample flow path, oxidation solution stream, acidifying solution stream, reduction nitrite ion stream and analysis detection stream composition.It is such a automatic
Analytical instrument realizes automation in sample introduction, heating and analysis, can be easily and fast to the COD in seawater
Carry out online automatic detection.But there are still certain defect for above-mentioned COD detectors：Have a variety of anti-in analysis detection stream
Device, blender are answered, operating procedure is more and cumbersome, stream is complicated；In addition, the principle of the optical detection apparatus of detection is light splitting
Photometry, this method is when being applied to the high seawater of turbidity, and detection error is larger.
Refer to a kind of COD detectors in patent CN106290353A, including the heating unit of setting, condensing unit,
Catching unit and titration unit, described heating unit include electric appliance control box, heating plate, reflection quilt, fluid reservoir, and described adds
Liquid unit includes liquid feeding mechanical arm, liquid feeding support, fluid filling pump, liquid-feeding tube, drive mechanism A, and described condensing unit includes condensation
Support, condensation water tower, condenser fan, holding support, the titration unit include gripping mechanical arm, mechanical tong, drive mechanism B
Driving, described self-test unit includes self-inspection support, gauge line.Automaticity of the present invention is high, with self-checking unit, it is ensured that real
Test data validity.But, above-mentioned COD analyzers are heated by the way of heating plate, and the efficiency of heating surface is not high；Condensing unit
Sample is easily stained with the condensed water tower wall of setting, experimental result is influenceed；In titration unit, video camera is to muddy water
Quality detection difficulty is larger, in the water quality of high concentrtion, and video camera is difficult to judge color correctness.
A kind of sea water COD automatic detection method is refer in patent CN101231237A, this method is potassium permanganate oxygen
Change method, its process detected includes the measure of the extra large Organic substance in water of potassium permanganate oxidation under alkalescence condition, acidifying and shading value.This
Invention have detect that accurate, easy to operate, detection cycle is short, analysis efficiency is high, data reproduction type is good, automatic inspiration or quick etc.
Advantage.But the oxidizing temperature of potassium permanganate does not reach alkalinity potassium permanganate oxidizing process under alkalescence condition（GB17378.4-2007）
Standard；The method that shading value detection is used in continuous mode, can be applied in the relatively low seawater of turbidity,
In the case that turbidity is high, the measurement result of shading value and the difference of actual measured value are larger.
The content of the invention
Apparatus and method are determined it is an object of the invention to provide a kind of sea water COD.
The technical scheme is that：
First aspect：A kind of sea water COD determines device, including sample injection unit, clears up unit, condensing unit and titration unit, institute
State sample injection unit by pipeline respectively with it is described clear up unit and titration unit be connected, it is described to disappear for conveying water sample and reagent
Solution unit is connected by pipeline with the condensing unit, is heated for mixed sample and reagent, and to mixed water sample
Clear up, the condensing unit is connected by pipeline with the titration unit, it is described for cooling down the mixed sample after heating is cleared up
Unit is titrated, for judging the titration to the mixed sample of cooling, in addition to color judgment means, the color judgment means bag
The area source and color sensor for the titration tank both sides for being arranged on the titration unit are included, the light that the area source is sent, which is passed through, to be held
Liquid in device is received by the color sensor, when color sensor reads color for white, judges that blueness just takes off
Go, titration terminates.
Further, the sample injection unit includes a syringe pump and ten passage switching valves, the passage of switching valve ten switching
Valve includes ten passage switchings and a central passage, and central passage is connected with syringe pump injection port, and the access of the tenth passage is empty
Gas, first passage accesses total sample intake passage, and each reagent is delivered to and clears up unit and titration unit, second channel access waste liquid
Mouthful, other eight passages are respectively connecting to various reagents.
Further, it is described to clear up counteracting tank, lid and counteracting tank base on counteracting tank that unit includes being fixed as one, it is described
The bottom of counteracting tank, which is provided with magnetic stirring apparatus, the outer wall of the counteracting tank, is provided with heater, on the counteracting tank
Cover and be provided with temp probe, and offer and clear up sample holes, clear up steam vent, air-blowing hole, it is described clear up sample holes with it is described
Sample injection unit is connected by pipeline, described to clear up steam vent and be connected with clearing up air bleeding valve by pipeline, the air-blowing hole with
Air-blowing device is connected by pipeline, is provided with the counteracting tank base and is cleared up outage, and the outage of clearing up is with clearing up
Tapping valve is connected by pipeline.
Further, the condensing unit includes the drainer containing cooling water, the drainer Shang Gai and cold being fixed as one
Solidifying ttom of pipe seat, the bottom of the drainer, which is provided with magnetic stirring apparatus, the drainer, is provided with helix tube, described cold
Condensation sample holes and condensation air-vent are offered on solidifying tank on lid, the condensation sample holes pass through pipeline phase with the unit of clearing up
Connection, the condensation air-vent is communicated with air, and condensation outage, the one of the helix tube are provided with the drainer base
End is connected with the condensation sample holes, and the other end is connected with the condensation outage.
Further, titration unit include be fixed as one titration tank, titration tank on lid and buret base, the titration
The bottom of tank, which is provided with magnetic stirring apparatus, the titration tank on lid, offers titration sample holes, titration steam vent, titration
Hole, the titration sample holes are connected with the condensing unit by pipeline, and the titration steam vent passes through with titration air bleeding valve
Pipeline is connected, and the titration hole is connected with the sample injection unit by pipeline, and titration is provided with the titration tank bottom seat
Outage, the titration outage is connected with titration tapping valve by pipeline.
Second aspect：A kind of sea water COD assay method, comprises the following steps：
（1）Sample preparation, water sample, sodium hydroxide solution and liquor potassic permanganate are mixed, and are made and are determined solution；
（2）Clear up, solution will be determined and be stirred heating；
（3）Condensation, the measure solution after clearing up is cooled to room temperature；
（4）Titration, will clear up condensed measure solution, sulfuric acid and liquor kalii iodide mixing, after stirring is stood, and be made preliminary molten
Liquid；Preliminary solution and starch solution are mixed, solution to be titrated is made；Hypo solution is slowly titrated to be titrated molten
In liquid, drop to it is blue just take off untill, when color sensor reads color for white, judge that blueness is just taken off, titration is tied
Beam；
Before judging whether blueness just takes off, in addition to：
Blank correction, water sample is placed into container, is adjusted the brightness of the area source, is when color sensor reads color
When white, area source brightness no longer changes, and air-conditioning correction terminates, in titration step, using the face light in blank correction step
Source brightness.
Further, according to National Standard of the People's Republic of China GB17378.4-2007, Part IV：In sea water analysis
Basic potassium permanganate method carries out reagent preparation and preparation, and the liquor kalii iodide is 0.5g/ml.
Further, the mode of heating cleared up in step is when will determine solution to be heated to 100 DEG C, persistently to boil 10
Minute.
The present invention has the advantages and positive effects of：
1st, infrared heating device, is cleared up by the way of far-infrared thermal radiation to the progress heating of former seawater；
2nd, polytetrafluoro spiral cold-finger and inner panel, polytetrafluoro spiral cold-finger are wrapped on inner panel, realize the boiling to clearing up unit
Water is quickly cooled down；
3rd, color sensor, area source and blank correction, were titrated by the control to color sensor and area source to recognize
The change of color in journey, is realized by blank correction and the color intensity of sea water with higher turbidity is accurately judged；
4th, liquid is provided successively by clearing up unit, condensing unit and the mobilization dynamic for titrating unit by air-blowing device；
5th, counteracting tank, drainer and the stirring for titrating pot liquid are realized, the mixing of each solution is realized respectively；
6th, automaticity is high, simple in construction, dependable performance, system automatic detection, cleaned automatically with instrument, temperature control from
Dynamicization, the instruction of long-range receiving activity, remote transmission data.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to do one simply to introduce, it should be apparent that, drawings in the following description are this hairs
Some bright embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can be with root
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the structural representation that a kind of sea water COD that the embodiment of the present invention one is provided determines device
Fig. 2 is the structural representation for clearing up unit that the embodiment of the present invention one is provided；
Fig. 3 is the structural representation for the condensing unit that the embodiment of the present invention one is provided；
Fig. 4 is the structural representation for the titration unit that the embodiment of the present invention one is provided.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, hereinafter with reference to attached in the embodiment of the present invention
Figure, technical scheme is clearly and completely described by embodiment, it is clear that described embodiment is the present invention one
Section Example, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
Go out the every other embodiment obtained under the premise of creative work, belong to the scope of protection of the invention.
Embodiment one：
As shown in figure 1, a kind of sea water COD of the invention determines device, including sample injection unit 100, clear up unit 200, condensing unit
300 and titration unit 400, the sample injection unit 100 by pipeline respectively with it is described clear up unit 200 and titrate unit 400 connect
Connect, for conveying water sample and reagent, the unit 200 of clearing up is connected by pipeline with the condensing unit 300, for mixing water
Sample and reagent, and the progress heating of mixed water sample is cleared up, the condensing unit 300 passes through pipeline and the titration unit
400 connections, for cooling down the mixed sample after heating is cleared up, the titration unit 400, for judging the mixed sample to cooling
Titration, in addition to color judgment means, the color judgment means include being arranged on the titration tank both sides of the titration unit
Area source and color sensor, the light that the area source is sent receives through the liquid in container by the color sensor
Arrive, when color sensor reads color for white, judge that blueness is just taken off, titration terminates.
The sample injection unit 100 is ten passage switching valves, and eight kinds of reagent bottles connect eight in ten passage switching valves respectively
Passage, ten passages switching valve outlet connects injection pump intake, and the passage of switching valve the 9th connects injection pump discharge, will by the tenth passage
Each reagent, which is delivered to, clears up unit 200 and titration unit 400.
As shown in Fig. 2 the unit 200 of clearing up includes lid 202 and counteracting tank base 203 on counteracting tank 201, counteracting tank,
Lid 202 and the counteracting tank base 203 are strained and fixed by trip bolt 10 between the two on the counteracting tank disappears described
Solve on tank 201, be provided with infrared heating device 204, the counteracting tank on lid 202 and set on the outer wall of the counteracting tank 201
There is temp probe 205, and offer and clear up sample holes 206, clear up steam vent 207, air-blowing hole 208, it is described to clear up sample holes 206
It is connected with the sample intake passage of ten passage switching valves by pipeline, it is described to clear up steam vent 207 and clear up air bleeding valve 210 by pipe
Road is connected, and the air-blowing hole 208 is connected with air-blowing device 211 by pipeline, is provided with and disappears on the counteracting tank base 203
Solve outage 209, the outage 209 of clearing up with clearing up being connected by pipeline for tapping valve 212, the counteracting tank 201
Bottom is provided with magnetic stirring apparatus 20, and the magnetic force that the magnetic stirring apparatus 20 includes being arranged in the counteracting tank 201 is stirred
Mix son 21 and the rotary magnet 22 being arranged on outside the counteracting tank 201.
The infrared heating device 204 is wound in the outer wall of counteracting tank 201, using Heated by Far-Infrared Radiation, heating effect
Rate is high, and sealing ring is provided between lid 202 and the counteracting tank base 203 on the counteracting tank 201 and the counteracting tank（In figure
Not depending on going out）, the counteracting tank 201 is made of quartz glass material, lid 202, the counteracting tank base 203 on the counteracting tank
It is made with pipeline of polytetrafluoroethylmaterial material, the sealing ring uses the resistant to elevated temperatures fluorine cushion rubber of acid and alkali-resistance.
Clear up flow：
Sample injection unit conveying 100ml water samples, 1ml sodium hydroxide solutions, 10ml liquor potassic permanganates to counteracting tank, each solution according to
National Standard of the People's Republic of China GB17378.4-2007, Part IV：Basic potassium permanganate method in sea water analysis is carried out
Prepare and prepare, open infrared heating device 204, magnetic stirring apparatus 20, temp probe 205, clear up air bleeding valve 210, treat temperature
When degree is increased to 100 degrees Celsius, persistently boil after 10 minutes, 10 minutes, close infrared heating device 204, magnetic stirring apparatus
20th, temp probe 205, clear up air bleeding valve 210, water sample clears up completion.Counteracting tank fan is opened to be radiated.
As shown in figure 3, the condensing unit 300 includes the drainer 301 containing cooling water, lid 302 and cold on drainer
Lid 302 and the drainer base 303 are tensed by trip bolt 10 between the two on solidifying tank bottom seat 303, the drainer
It is fixed on the drainer 301, is provided with helix tube 304, the drainer 301 and is opened up on lid in the drainer 301
There are condensation sample holes 305, the condensation sample holes 305 are connected with the outage 212 of clearing up by pipeline, the drainer
Condensation outage 306 is provided with base 303, one end of the helix tube 304 is connected with the condensation sample holes 305, another
End is connected with the condensation outage 306, and the bottom of the drainer 303 is provided with magnetic stirring apparatus 20, and the magnetic force is stirred
Mixing device 20 includes the magnetic stir bar 21 being arranged in the drainer 303 and the rotation being arranged on outside the drainer 303
Electromagnet 22.
The helix tube 305 passes through inner panel（Not depending on going out in figure）It is arranged in the drainer 301, the drainer 301
Sealing ring is provided between lid 302 on the drainer and the drainer base 303（Not depending on going out in figure）, the drainer
301 are made of quartz glass material, lid 302, the drainer base 303, the helix tube 304 on the drainer
It is made with pipeline of polytetrafluoroethylmaterial material, the sealing ring uses the resistant to elevated temperatures fluorine cushion rubber of acid and alkali-resistance.Good cooling results,
Liquid after clearing up after condensing unit by that, without stagnation, can flow directly in titration unit.
Condense flow：
After the completion of water sample is cleared up, the air-blowing device 211 for clearing up unit 200 is opened, the water sample in counteracting tank 201 is delivered to condensation
Tank 301, opens condenser fan and magnetic stirring apparatus is used as auxiliary heat dissipation, it is ensured that water sample is sufficiently cooled to room temperature, and water sample is complete
After cooling, it is delivered in titration tank.
As shown in figure 4, the titration unit 400 includes titration tank 401, titrates lid 402 and titration tank bottom seat 403 on tank,
Lid 402 and the titration tank bottom seat 403 are strained and fixed in the drop by trip bolt 10 between the two on the titration tank
Determine on tank 401, offer titration sample holes 404, titration steam vent 405, titration hole 406, institute on the titration tank on lid 401
State titration sample holes 404 with the condensation outage 306 of the condensing unit 300 by pipeline to be connected, the titration row
Stomata 405 is connected with titration air bleeding valve 407 by pipeline, and the titration passage of the passage switching valve of titration hole 406 and ten leads to
Cross pipeline to be connected, be provided with titration outage 408 on the titration tank bottom seat 403, the titration outage 408 is arranged with titration
Liquid valve 409 is connected by pipeline, and the bottom of the titration tank 403 is provided with magnetic stirring apparatus 20, the magnetic agitation dress
Putting 20 includes the magnetic stir bar 21 being arranged in the titration tank 401 and the rotating electromagnetic being arranged on outside the titration tank 401
Iron 22.
On the titration tank 401 and the titration tank sealing ring is provided between lid 402 and the titration tank bottom seat 403
（Not depending on going out in figure）, the titration tank 401 is made of quartz glass material, described to titrate lid 402, the titration on tank
Tank bottom seat 403 and pipeline are made of polytetrafluoroethylmaterial material, and the sealing ring uses the resistant to elevated temperatures fluorine cushion rubber of acid and alkali-resistance.
Also include color judgment means 500, the color judgment means 500 include being arranged on the titration unit 400
The area source 501 and color sensor 502 of the both sides of tank 504 are titrated, the light that the area source 501 is sent passes through the liquid in container
Received by the color sensor 502, when color sensor 502 reads color for white, judge that blueness is just taken off, drip
Terminate calmly.
There is no the interference of chloride ion interference, only turbidity in titration process, but add blank correction this setting, it is real
The accurate titration of existing seawater.
Titrate flow：
The conveying 5ml of sample injection unit 100 sulfuric acid, 1ml liquor kalii iodides, each solution is according to National Standard of the People's Republic of China
GB17378.4-2007, Part IV：Basic potassium permanganate method in sea water analysis is prepared and prepared, and the KI is molten
Liquid is 0.5g/ml, opens agitating device 20, reagent is mixed, after standing 5 minutes.Sample injection unit 100 conveys 1ml starch
To titration tank 401, agitating device 20, area source 501, color sensor 502 are opened, sample injection unit 100 extracts the thio sulphur of 10ml
Sour sodium is titrated, control injection pump speed, titration is slowly carried out, and it is white to treat that color sensor 502 reads color value
When, titration terminates.
Blank correction：Before being condensed to former seawater, sample injection unit 100 first extracts former seawater into titration tank 401, right
It carries out the gamma correction of area source 501, and with the brightness increase of area source, the light sent from area source is perforated through face after seawater
Color is continually changing, and when the color value that color sensor 502 is received is white, area source brightness is not further added by, blank
Correction terminates, when being titrated after former seawater condensing, using area source brightness during blank correction as background, is titrated.
Embodiment two：
A kind of sea water COD assay method, comprises the following steps：
（1）Sample preparation, water sample, sodium hydroxide solution and liquor potassic permanganate are mixed, and are made and are determined solution；
（2）Clear up, solution will be determined and be stirred heating；
（3）Condensation, the measure solution after clearing up is cooled to room temperature；
（4）Titration, will clear up condensed measure solution, sulfuric acid and liquor kalii iodide mixing, after stirring is stood, and be made preliminary molten
Liquid；Preliminary solution and starch solution are mixed, solution to be titrated is made；Hypo solution is slowly titrated to be titrated molten
In liquid, drop to it is blue just take off untill, when color sensor reads color for white, judge that blueness is just taken off, titration is tied
Beam；
Before judging whether blueness just takes off, in addition to：
Blank correction, water sample is placed into container, is adjusted the brightness of the area source, is when color sensor reads color
When white, area source brightness no longer changes, and air-conditioning correction terminates, in titration step, using the face light in blank correction step
Source brightness.
According to National Standard of the People's Republic of China GB17378.4-2007, Part IV：Alkalescence in sea water analysis is high
Potassium manganate method carries out reagent preparation and preparation, and the liquor kalii iodide is 0.5g/ml.
The mode of heating cleared up in step is when will determine solution to be heated to 100 DEG C, persistently to boil 10 minutes.
Note, above are only presently preferred embodiments of the present invention and institute's application technology principle.It will be appreciated by those skilled in the art that
The invention is not restricted to specific embodiment described here, can carry out for a person skilled in the art it is various it is obvious change,
Readjust and substitute without departing from protection scope of the present invention.Therefore, although the present invention is carried out by above example
It is described in further detail, but the present invention is not limited only to above example, without departing from the inventive concept, also
Other more equivalent embodiments can be included, and the scope of the present invention is determined by scope of the appended claims.
Claims (8)
1. a kind of sea water COD determines device, it is characterised in that：Including sample injection unit, clear up unit, condensing unit and titration list
Member, the sample injection unit by pipeline respectively with it is described clear up unit and titration unit be connected, for conveying water sample and reagent, institute
State and clear up unit and be connected by pipeline with the condensing unit, carried out for mixed sample and reagent, and to mixed water sample
Heating is cleared up, and the condensing unit is connected by pipeline with the titration unit, for cooling down the mixed sample after heating is cleared up,
The titration unit, for judging the titration to the mixed sample of cooling, in addition to color judgment means, the color judges dress
The area source and color sensor of the titration tank both sides including being arranged on the titration unit are put, the light that the area source is sent is worn
The liquid crossed in container is received by the color sensor, when color sensor reads color for white, judges blueness
Just take off, titration terminates.
2. measure device according to claim 1, it is characterised in that：The sample injection unit includes a syringe pump and ten and led to
Road switching valve, the passage switching valve of switching valve ten includes ten passage switchings and a central passage, central passage and note
The connection of pump injection port is penetrated, the tenth passage access air, first passage accesses total sample intake passage, each reagent is delivered to and clears up list
Member and titration unit, second channel access waste liquid port, other eight passages are respectively connecting to various reagents.
3. measure device according to claim 1, it is characterised in that：The unit of clearing up includes clearing up for being fixed as one
Lid and counteracting tank base on tank, counteracting tank, the bottom of the counteracting tank is provided with magnetic stirring apparatus, the outer wall of the counteracting tank
On be provided with heater, the counteracting tank on lid and be provided with temp probe, and offer and clear up sample holes, clear up exhaust
Hole, air-blowing hole, the sample holes of clearing up are connected with the sample injection unit by pipeline, described to clear up steam vent and clear up exhaust
Valve is connected by pipeline, and the air-blowing hole is connected with air-blowing device by pipeline,
It is provided with the counteracting tank base and clears up outage, the outage of clearing up is with clearing up being connected by pipeline for tapping valve
Connect.
4. measure device according to claim 1, it is characterised in that：It is characterized in that：The condensing unit includes fixing
The drainer containing cooling water, lid and the condenser pipe base on drainer being integrated, the bottom of the drainer is provided with magnetic force
It is provided with agitating device, the drainer on helix tube, the drainer on lid and offers condensation sample holes and condense ventilative
Hole, the condensation sample holes are connected with the unit of clearing up by pipeline, and the condensation air-vent is communicated with air, described cold
Condensation outage is provided with solidifying tank bottom seat, one end of the helix tube is connected with the sample holes that condense, the other end with it is described
Condense outage connection.
5. measure device according to claim 1, it is characterised in that：Titration unit include be fixed as one titration tank,
Lid and buret base on tank are titrated, the bottom of the titration tank is provided with magnetic stirring apparatus, the titration tank opens on lid
Provided with titration sample holes, titration steam vent, titration hole, the titration sample holes are connected with the condensing unit by pipeline,
The titration steam vent is connected with titration air bleeding valve by pipeline, and the titration hole is connected with the sample injection unit by pipeline
Connect, titration outage is provided with the titration tank bottom seat, the titration outage is connected with titration tapping valve by pipeline.
6. a kind of sea water COD assay method of the device described in utilization claim 1, comprises the following steps：
（1）Sample preparation, water sample, sodium hydroxide solution and liquor potassic permanganate are mixed, and are made and are determined solution；
（2）Clear up, solution will be determined and be stirred heating；
（3）Condensation, the measure solution after clearing up is cooled to room temperature；
（4）Titration, will clear up condensed measure solution, sulfuric acid and liquor kalii iodide mixing, after stirring is stood, and be made preliminary molten
Liquid；Preliminary solution and starch solution are mixed, solution to be titrated is made；Hypo solution is slowly titrated to be titrated molten
In liquid, drop to it is blue just take off untill, when color sensor reads color for white, judge that blueness is just taken off, titration is tied
Beam；
Before judging whether blueness just takes off, in addition to：
Blank correction, water sample is placed into container, is adjusted the brightness of the area source, is when color sensor reads color
When white, area source brightness no longer changes, and air-conditioning correction terminates, in titration step, using the face light in blank correction step
Source brightness.
7. assay method according to claim 6, it is characterised in that：According to National Standard of the People's Republic of China
GB17378.4-2007, Part IV：Basic potassium permanganate method in sea water analysis carries out reagent preparation and preparation, the iodate
Potassium solution is 0.5g/ml.
8. assay method according to claim 6, it is characterised in that：The mode of heating cleared up in step is to survey
When determining solution and being heated to 100 DEG C, persistently boil 10 minutes.
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| CN201710445840.2A CN107014807A (en) | 2017-06-14 | 2017-06-14 | A kind of sea water COD determines device and method |
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| CN201710445840.2A CN107014807A (en) | 2017-06-14 | 2017-06-14 | A kind of sea water COD determines device and method |
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| CN108918443A (en) * | 2018-07-14 | 2018-11-30 | 浙江迪特西科技有限公司 | A kind of integrated portable water-quality COD detection device |
| CN109444244A (en) * | 2018-12-14 | 2019-03-08 | 力合科技（湖南）股份有限公司 | Seawater permanganate index analysis system and method |
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| CN115389492A (en) * | 2022-08-19 | 2022-11-25 | 重庆长安新能源汽车科技有限公司 | Determination method and determination device for detecting content of free acid in electrolyte |
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