CN106290952B - Total nitrogen, total phosphorus monitoring system and monitoring method in a kind of water body - Google Patents
Total nitrogen, total phosphorus monitoring system and monitoring method in a kind of water body Download PDFInfo
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- CN106290952B CN106290952B CN201610614968.2A CN201610614968A CN106290952B CN 106290952 B CN106290952 B CN 106290952B CN 201610614968 A CN201610614968 A CN 201610614968A CN 106290952 B CN106290952 B CN 106290952B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/08—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a stream of discrete samples flowing along a tube system, e.g. flow injection analysis
- G01N35/085—Flow Injection Analysis
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention discloses total nitrogen in a kind of water body, total phosphorus monitoring system and monitoring method, which includes automatic sampling control device, digestion instrument, total nitrogen, total phosphorus colour developing flow path, wherein：Automatic sampling control device is connected with digestion instrument, and providing power by syringe pump drives solution to flow；Each channel of eight channel selector valves is connected respectively with digestion instrument, phosphorus color developing agent, total nitrogen, total phosphorus colour developing flow path and spectrometer；Total nitrogen, total phosphorus colour developing flow path are made of liquid storage pipe and syringe pump；It using this method, after the completion of resolution, sucks successively in a certain amount of digestion solution to liquid storage pipe, is sequentially completed total nitrogen, total phosphorus yield, pipeline and digestion instrument are cleaned automatically after the completion of measuring.By the achievable total nitrogen of the present invention, the online while resolution of total phosphorus and on-line determination, there is easy to operate, dependable performance, high sensitivity, the advantages such as selectivity is good, reagent consumption is low.
Description
Technical field
The present invention relates to the online auto monitoring system of total nitrogen, total phosphorus in a kind of water body, suitable for surface water, seawater,
And the quick on-line automatic measure of Determination of Total Nitrogen in Waste Water, total phosphorus, belong to water quality monitoring technical field.
Background technology
At present, nitrogen, phosphorus are one of main nutrient elements in water body, and excessive nitrogen phosphorus can lead to the eutrophication of water body.It is right
In total nitrogen, total phosphorus yield, artificial sample is time-consuming and laborious.And existing total phosphorus, total nitrogen on-line determination instrument are to flow note mostly
Analysis is penetrated as principle, sequential injection is a kind of powerful single channel Flow Technique, that eliminates flow injection using peristaltic pump as power
The shortcomings that, using precise injection pump as power.There is higher reproducibility, stability and the consumption of low reagent simultaneously, two will not be generated
Secondary pollution.Therefore, it is more and more urgent to grope a kind of total nitrogen, total phosphorus online auto monitoring system on the basis of sequential injection.
Invention content
The technical problem to be solved in the present invention is to provide total nitrogen, total phosphorus on-line monitoring system and monitoring sides in a kind of water body
Method, to realize quick, accurate, low consumed monitoring.
The technical solution used in the present invention is to solve above-mentioned technical problem：Total nitrogen, total phosphorus monitoring system in a kind of water body
System, key technology are：It includes automatic sampling control device, digestion instrument and total nitrogen, total phosphorus colour developing flow path；
The automatic sampling control device include syringe pump, described mono- channel of syringe pump S1 respectively with the load of provided with electromagnetic valve
Liquid, sample to be tested are connected with the inlet pipe of digestion solution sample；
The digestion instrument includes counteracting tank, and the band connected with syringe pump S1 another channel is equipped with above the counteracting tank
Electromagnetic heating is arranged below in the sample feeding pipe of solenoid valve, the exhaust pipe of provided with electromagnetic valve and temperature and pressure transmitter, the counteracting tank
Device, the sewer pipe of provided with electromagnetic valve, provided with electromagnetic valve drain pipe；
The total nitrogen, total phosphorus colour developing flow path include liquid storage pipe HC and the syringe pump S2 connected with liquid storage pipe HC one end, with storing up
Eight channel selector valves of liquid pipe HC other ends connection, phosphorus color developing agent A, the phosphorus connected with eight channel selector valve two of which channels are shown
Toner B and spectrometer, eight channel selector valve are made of a public passage C and 8 subchannels, wherein public passage C
It can be connected respectively with 8 channels, the spectrometer is connected with one of channel of eight channel selector valve.
Preferably, the syringe pump is pumped using 10mL precise injections.
Preferably, the liquid storage pipe HC be diameter 0.76mm, the polyfluortetraethylene pipe of length 1m.
The monitoring method of above-mentioned automatic monitoring system, includes the following steps：
A, the resolution of water sample：
Carrier fluid, digestion solution, sample to be tested are injected into digestion instrument by a certain percentage by the control of solenoid valve, close
120 DEG C are warming up in the counteracting tank closed in 180s, clears up 300S at such a temperature, cool 300S after the completion of resolution；B, it is total
The detection process of nitrogen and total phosphorus
The measure of B-1 total nitrogens
Total nitrogen is completely converted into nitrate nitrogen in sample to be tested after the completion of resolution, solenoid valve V4 and V6 is opened, by multichannel
Switching valve public passage C is connected with channel 8a, and by syringe pump S2, sample is to liquid storage pipe HC after drawing 300 μ L resolutions, then incites somebody to action
Public passage C is connected with channel 3a where detecting system, by syringe pump S2 that the sample after resolution is direct by liquid storage pipe HC
It pushes in spectrometer, absorbance measurement is carried out under 220nm and 275nm；
The total phosphorus yields of B-2
Total phosphorus is completely converted into orthophosphates in sample to be tested after the completion of resolution, opens solenoid valve V6, multichannel is converted
Valve public passage C is connected with channel 8a, and by syringe pump S2, liquid, then will be public to storage tube HC after drawing 300 μ L resolutions
Channel C is connected respectively with channel 1a and channel 3a, draws color developing agent A and color developing agent B respectively to storage tube, stops 15s, make to treat
Sample and color developing agent A and B carry out hybrid concurrency life reaction generation blue complex in liquid storage pipe, then by public passage C
It is connected with channel 3a where detecting system, the sample after developing the color in liquid storage pipe is pushed into spectrometer, is inhaled under 710nm
The measure of luminosity.
It is using advantageous effect caused by above-mentioned technical proposal：
This monitoring system is using Sequential Injection Analysis as principle, and sequentical injection analysis precision is high, reproducible, and this is
System provides power by syringe pump, and syringe pump has the characteristics that precision is high, long-play stability is good, therefore the system pair
Total nitrogen, measurement result accuracy higher, the stability of total phosphorus are more preferable.Sequential Injection Analysis reagent consumption is in micro updating simultaneously
Not, reagent consumption is low, extends period of equipment maintenance while saving reagent, and the system is by can be real by computer
It now automatically controls, realizes and total nitrogen, the automatic of total phosphorus are cleared up and automatically determine.Convenient for water bodys such as river, river, lake and seawater
Automatic on-line monitoring, to monitor water quality, prevention body eutrophication be of great significance.
The achievable total nitrogen of the present invention, the online while resolution of total phosphorus and on-line determination, have easy to operate, dependable performance,
High sensitivity, the advantages such as selectivity is good, reagent consumption is low.
Description of the drawings
Fig. 1 is automatic monitoring system flow diagram of the present invention；
Fig. 2 is the schematic diagram of digestion instrument in the present invention；
In figure：1-1, solenoid valve V1,1-2, solenoid valve V2,1-3, solenoid valve V3,1-4, solenoid valve V4,1-5, solenoid valve
V5,1-6, solenoid valve V6,1-7, solenoid valve V7,1-8, solenoid valve V8,2-1, syringe pump S1,2-2, syringe pump S2,3, liquid storage pipe
HC, 4, counteracting tank, 4-1, sample feeding pipe, 4-2, air hose, 4-3, sewer pipe, 4-4, drain pipe, 4-5, solenoid valve, the choosing of 5, eight channels
Select valve, 6, spectrometer, 7, temperature and pressure transmitter, 8, electromagnetic heater, 9, phosphorus color developing agent A, 10, phosphorus color developing agent B, 11, carry
Liquid, 12, sample to be tested, 13, digestion solution, 14, waste liquid, the 15, second carrier fluid, a, detector, b, third waste liquid, c, light source.
Specific embodiment
The present invention will be described in detail in the following with reference to the drawings and specific embodiments.
Shown in Fig. 1, which includes automatic sampling control device, digestion instrument, total nitrogen, total phosphorus colour developing flow path etc..
The present invention is based on Sequential Injection Analysis method, using the polyfluortetraethylene pipe of a diameter of 0.76mm, sample and various reagents
It injects in certain sequence, is mutually mixed and reacts in liquid storage pipe HC.
Wherein：There are two channels by syringe pump S1 in automatic sampling control device, and a channel is connected with inlet pipe, another
A channel is connected with counteracting tank 4.The pipeline connection of inlet pipe and carrier fluid, sample to be tested and digestion agent has on each pipeline
One solenoid valve controls the type of sample introduction by the switch of solenoid valve.Syringe pump S1 is connected first with sample feeding pipe 4-1, sucking
It connects, injects a sample into counteracting tank 4 with counteracting tank 4 again after sample.Automatic sampling control device passes through pipeline and digestion instrument
It is connected, the sample after resolution is drawn into liquid storage pipe HC by eight channel selector valves 5 after the completion of resolution, then successively to total nitrogen
And total phosphorus is measured.Automatic sampling control device by 10mL precise injections pump S1 provide power, solenoid valve V1, solenoid valve V2 and
Solenoid valve V3 controls each inlet pipe respectively.The total nitrogen, total phosphorus colour developing flow path include liquid storage pipe HC and with liquid storage pipe HC one end
The syringe pump S2 of connection, eight channel selector valves 5 connected with the liquid storage pipe HC other ends lead to eight channel selector valves, 5 two of which
Phosphorus color developing agent A, phosphorus color developing agent B and the spectrometer of road connection, eight channel selector valve 5 is by a public passage C and 8 points
Channel forms, and wherein public passage C can connect with 8 channels respectively, the spectrometer 6 and eight channel selector valve 5 its
In the connection of channel.The storage tube HC be diameter 0.76mm, the polyfluortetraethylene pipe of length 1m.The spectrometer 6,
Measurement range is ultraviolet visible light, can measure the absorbance under different wave length simultaneously automatically under software control.
Eight channel selector valves 5 are made of eight individual channels and a public passage, public passage can successively with eight
Channel（Eight channels are respectively 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a）Connection.Wherein, channel 1a, 2a respectively with phosphorus color developing agent
A, phosphorus color developing agent B is connected, channel 3a and flow cell（That is spectrometer）Connection, channel 8a connects with digestion instrument, public passage and
Liquid storage pipe HC is connected.The liquid storage pipe HC other ends are connected with a channel of syringe pump S2, and another channel of syringe pump S2 is with carrying
Liquid phase connects.
Total nitrogen is measured first after the completion of Specimen eliminating：Syringe pump S2 suck a certain amount of carrier fluid then with liquid storage pipe HC
Connection, solenoid valve V6 are opened, and the public passage 5a of eight channel selector valves 5 is connected with channel 8a, are sucked by syringe pump S2 a certain amount of
In sample to HC after resolution, then the public passage of eight channel selector valves 5 is connected with channel 3a, by syringe pump S2 by liquid storage pipe
Solution in HC pushes to spectrometer 6, measures absorbance at 220nm and 275nm respectively.After the completion of determination of total nitrogen content to total phosphorus into
Row measures：Syringe pump S2 sucks a certain amount of carrier fluid and then is connected with liquid storage pipe HC, and solenoid valve V6 is opened, and passes through eight channel selector valves
5 switching draws the solution after a certain amount of phosphorus color developing agent A, resolution, in phosphorus color developing agent B to liquid storage pipe HC, waits to have reacted successively
Spectrometer 6 is pushed to by syringe pump S2 after, absorbance is measured at 710nm.
Shown in Fig. 2, digestion instrument includes a closed polytetrafluoroethylene (PTFE) counteracting tank 4, and sample is carried out using electromagnetic wave
Sample feeding pipe 4-1, air hose 4-2 and temperature and pressure transmitter 7 are arranged at heating, 4 top of counteracting tank, and electromagnetic heating is arranged at 4 bottom of counteracting tank
Device 8 is used for heating, and drain pipe 4-4 and sewer pipe 4-3, each pipeline is by a solenoid valve control.During resolution, it is first turned on
Sample and digestion solution are injected into through sample feeding pipe 4-1 in counteracting tank 4 by solenoid valve 4-5, are then shut off all solenoid valves, open electricity
Magnetic heater 8 monitors the temperature and pressure in digestion pool in real time, by solution under air-proof condition by temperature and pressure transmitter 7
120 DEG C are heated to, 700S is cleared up, closes electromagnetic heater 8 after the completion of resolution, cool.After cooling, air hose electromagnetism is opened
Valve and drain pipe solenoid valve carry out total nitrogen, total phosphorus yield successively.After the completion of measure, remaining digestion solution is arranged by sewer pipe 4-3
Go out.Then it opens the injection of inlet tube solenoid valve and cleans counteracting tank 4 without ammonium hydroxide, discharged after the completion of cleaning by sewer pipe 4-3.
Foregoing description is only carried as total nitrogen of the present invention, total phosphorus online auto monitoring system and the enforceable technical solution of method
Go out, not as the single restrictive condition to its structure in itself.
Claims (3)
1. a kind of total nitrogen, total phosphorus monitor the monitoring method of system, it is characterised in that：It is by total nitrogen, total phosphorus monitoring system in water body
System is completed, and the monitoring system includes automatic sampling control device, digestion instrument and total nitrogen, total phosphorus colour developing flow path；
The automatic sampling control device includes syringe pump S1（2-1）, the syringe pump S1（2-1）A channel respectively with band
The carrier fluid of solenoid valve（11）, sample to be tested（12）With digestion solution sample（13）Inlet pipe connection；
The digestion instrument includes counteracting tank（4）, the counteracting tank（4）It is equipped with and syringe pump S1 above（2-1）Another is logical
The sample feeding pipe of the provided with electromagnetic valve of road connection（4-1）, provided with electromagnetic valve exhaust pipe（4-2）And temperature and pressure transmitter（7）, it is described
Counteracting tank（4）Electromagnetic heater is arranged below（8）, provided with electromagnetic valve sewer pipe（4-3）With the drain pipe of provided with electromagnetic valve（4-4）；
The total nitrogen, total phosphorus colour developing flow path include liquid storage pipe HC（3）With with liquid storage pipe HC（3）The syringe pump S2 of one end connection（2-
2）And liquid storage pipe HC（3）Eight channel selector valves of other end connection（5）And eight channel selector valves（5）Two of which channel connects
Phosphorus color developing agent A（9）, phosphorus color developing agent B（10）And spectrometer（6）, eight channel selector valve（5）By a public passage C
It is formed with 8 subchannels, wherein public passage C can be connected with 8 channels respectively, the spectrometer（6）It is selected with eight channel
Select valve（5）One of channel connection；
The monitoring method includes the following steps：
A, the resolution of water sample：
Carrier fluid, digestion solution, sample to be tested are injected into digestion instrument by a certain percentage by the control of solenoid valve, closed
Counteracting tank（4）120 DEG C are warming up in middle 180s, clears up 300S at such a temperature, cool 300S after the completion of resolution；
B, the detection process of total nitrogen and total phosphorus
The measure of B-1 total nitrogens
Total nitrogen is completely converted into nitrate nitrogen in sample to be tested after the completion of resolution, opens solenoid valve V4 and V6, multichannel is converted
Valve（5）Public passage C be connected with channel 8a, pass through syringe pump S2（2-2）, sample is to liquid storage pipe after drawing 300 μ L resolutions
HC（3）, then channel 3a where public passage C and detecting system is connected, pass through syringe pump S2（2-2）By the sample after resolution
By liquid storage pipe HC（3）It directly pushes in spectrometer, absorbance measurement is carried out under 220nm and 275nm；
The total phosphorus yields of B-2
Total phosphorus is completely converted into orthophosphates in sample to be tested after the completion of resolution, opens solenoid valve V4 and V6, multichannel is converted
Valve public passage C is connected with channel 8a, passes through syringe pump S2（2-2）, liquid is to storage tube HC after drawing 300 μ L resolutions（3）,
Public passage C with channel 1a and channel 3a is connected respectively again, draws phosphorus color developing agent A and phosphorus color developing agent B respectively to storage tube
HC（3）, 15s is stopped, makes sample to be tested and phosphorus color developing agent A, phosphorus color developing agent B in storage tube HC（3）Interior progress hybrid concurrency life is anti-
Blue complex should be generated, then public passage C is connected with channel 3a where detecting system, by storage tube HC（3）In show
Sample after color pushes to spectrometer（6）, the measure of progress absorbance under 710nm.
2. total nitrogen according to claim 1, total phosphorus monitor the monitoring method of system, it is characterised in that：The syringe pump S1
（2-1）With syringe pump S2（2-2）It is pumped using 10mL precise injections.
3. total nitrogen according to claim 1, total phosphorus monitor the monitoring method of system, it is characterised in that：The liquid storage pipe HC
（3）For diameter 0.76mm, the polyfluortetraethylene pipe of length 1m.
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| CN201610614968.2A CN106290952B (en) | 2016-08-01 | 2016-08-01 | Total nitrogen, total phosphorus monitoring system and monitoring method in a kind of water body |
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| CN107024570A (en) * | 2017-03-20 | 2017-08-08 | 河北科技大学 | A kind of total nitrogen, phosphorus online automatic monitor and its cleaning method |
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| CN108168995A (en) * | 2017-12-25 | 2018-06-15 | 重庆市宇驰检测技术有限公司 | The formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality |
| CN108226075A (en) * | 2017-12-29 | 2018-06-29 | 江苏汇环环保科技有限公司 | A kind of total nitrogen analysis measuring apparatus |
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| CN109632452B (en) * | 2018-10-31 | 2021-03-26 | 江西索立德环保服务有限公司 | Total phosphorus and total nitrogen digestion instrument |
| CN110006882B (en) * | 2019-04-03 | 2021-06-25 | 山东职业学院 | Micro-fluidic chip for detecting nitrogen and phosphorus content in water body and detection method |
| CN109991182B (en) * | 2019-04-29 | 2023-09-01 | 上海柏中观澈智能科技有限公司 | Total phosphorus detection system and total phosphorus detection method |
| CN110208200A (en) * | 2019-06-04 | 2019-09-06 | 中国原子能科学研究院 | A kind of four, uranic while on-line measurement system |
| CN112098186A (en) * | 2019-06-17 | 2020-12-18 | 安洲源(上海)环境科技有限公司 | Total nitrogen and total phosphorus detection device in water sample |
| CN111751308A (en) * | 2020-06-24 | 2020-10-09 | 中国科学院西安光学精密机械研究所 | Seawater total nitrogen and total phosphorus data processing system and method based on embedded ARM platform |
| CN111982843A (en) * | 2020-08-24 | 2020-11-24 | 上海洗霸科技股份有限公司 | Online monitoring system and method for organic phosphonate in circulating water system |
| CN112378871A (en) * | 2020-11-04 | 2021-02-19 | 福建省吉龙德环保科技有限公司 | System and method for simultaneously measuring nitrite nitrogen, nitrate nitrogen and total nitrogen |
| CN115128063A (en) * | 2022-05-24 | 2022-09-30 | 天津大学青岛海洋技术研究院 | Automatic monitoring system and control method for total phosphorus and total nitrogen on ship |
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