CN104764892A - Water quality heavy metal multi-parameter online monitoring instrument - Google Patents
Water quality heavy metal multi-parameter online monitoring instrument Download PDFInfo
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- CN104764892A CN104764892A CN201510162911.9A CN201510162911A CN104764892A CN 104764892 A CN104764892 A CN 104764892A CN 201510162911 A CN201510162911 A CN 201510162911A CN 104764892 A CN104764892 A CN 104764892A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 69
- 238000012544 monitoring process Methods 0.000 title claims abstract description 56
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- 238000007405 data analysis Methods 0.000 claims description 2
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052785 arsenic Inorganic materials 0.000 abstract description 15
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052793 cadmium Inorganic materials 0.000 abstract description 15
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052804 chromium Inorganic materials 0.000 abstract description 15
- 239000011651 chromium Substances 0.000 abstract description 15
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052753 mercury Inorganic materials 0.000 abstract description 14
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Classifications
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
-
- 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
-
- 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
-
- 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
- G01N35/00584—Control arrangements for automatic analysers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/12—Circuits of general importance; Signal processing
- G01N2201/126—Microprocessor processing
Abstract
The invention discloses a water quality heavy metal multi-parameter online monitoring instrument which comprises an online sample digestion system, an online sample detection system and a measurement and control system. The water quality heavy metal multi-parameter online monitoring instrument disclosed by the invention can realize automatic online monitoring of content of heavy metals such as mercury, lead, cadmium, chromium and arsenic in water, can be widely applied to the fields of surface water quality pollution monitoring, seawater pollution monitoring, up-to-standard release monitoring of industrial wastewater treatment and municipal sewage treatment and the like and has the advantages of high functional expansibility, wide measurement range and low cost.
Description
Technical field
A kind of water quality heavy metal of the present invention multiparameter on-line monitoring instrument, relates to water quality monitoring instrument
science and technologyfield.
Background technology
Heavy metal is to the pollution of environment water, especially mercury, plumbous, cadmium, chromium, this five kind of class heavy metal pollution of arsenic, directly will affect water ecological environment safety and drinking water source safety, make hydrobiont dead, or be enriched in aquatic organism, eventually through food chain serious harm health, thus heavy metal is the water quality parameter needing strict monitoring, in recent years, water quality heavy metal pollution event takes place frequently, be subject to the great attention of the Chinese government, Chinese Ministry of Environmental Protection minister Zhou Shengxian once mentioned when acceptance " Chinese environmental report " is interviewed, the target of " 12 " Heavy Metal Pollution sets up fairly perfect Heavy Metal Pollution system, accident emergency system and environment and health risk evaluation system, and water quality monitoring heavy metal pollution is this system important prerequisite and basis, be badly in need of advanced water quality monitoring instrument science and technology to support, for the assessment of water pollutions, early warning provides important science and technology support with control.
Along with the development of science and technology, the detection method of water quality heavy metal pollution achieves very large achievement, conventional detection method has mass spectroscopy, atomic spectrometry determination, spectrophotometric method, inductively coupled plasma method etc., in addition, some emerging detection methods also develop to some extent, as hexavalent chrome bio-removal, inhibiting AChE, microfluidic analysis method etc., but these methods or operation steps redundant and complicated, or disturbing factor is more, or need to use large-sized analytic instrument costly, and have very high professional skill requirement to operating personnel, thus, mostly can only complete in laboratory, scene can not be met, the technical requirement of quick online detection.
Comparatively speaking, colorimetric analysis and electrochemical methods, detect fast, simple to operate, is easy to develop water quality monitoring instrument, realizes the scene of heavy metal, quick online detection.But heavy metal pollution is a lot, as mercury, plumbous, chromium, cadmium, arsenic, copper, manganese, iron etc., at present, environmental protection, the departments such as water conservancy, in order to comprehensive monitoring heavy metal pollution and Comprehensive Assessment of Water Quality change, have to adopt many electrochemical sensor probe integrated-type instrument, many colorimetric analysiss module integration type instrument, even these three kinds of technological approaches of combination of multiple stage one-parameter water quality monitoring instrument realize the multi-parameters real-time monitoring of water quality heavy metal, but, above technological approaches is difficult to meet important user's request and technical requirement in dirigibility these two that water quality monitoring technology promptly uses at extendability and the scene of multi-parameter monitoring, and use cost is higher, a maximum integrated 3-4 module as many colorimetric analysiss module integration type instrument, otherwise instrument cost is too high (is generally many detections water quality parameter, often increase a colorimetric analysis modularized instrument price and will increase 7-10 ten thousand yuan) and make user be difficult to accept, and also often an increase colorimetric analysis modularized instrument volume also can become large.Although multinomial heavy metal parameter can be detected based on the water quality heavy metal monitoring instrument of anodic stripping voltammetry, but, because sensing electrode contacts with water, for ensureing that electrode is not extended the serviceable life of instrument by corrosion in water, this quasi-instrument upper limit of detection is not high, and measurement range is little, generally can only monitor earth's surface one class and two class water pollutions, and the emission monitoring of Industrial Wastewater Treatment and municipal sewage treatment can not be used for, the sudden monitoring heavy metal pollution of surface water quality can not be used for.
Summary of the invention
For solving the problem, the invention provides a kind of water quality heavy metal multiparameter on-line monitoring instrument, can realize monitoring the automatic on-line of the content of beary metal such as water quality mercury, lead, cadmium, chromium, arsenic, the field such as qualified discharge monitoring of surface water quality pollution monitoring, seawater pollution monitoring and Industrial Wastewater Treatment and municipal sewage treatment can be widely used in.Possess that Multi-function extension promptly to use flexibly by force, on-the-spot, measurement range is wide and the advantage of low cost.
The technical scheme that the present invention takes is:
A kind of water quality heavy metal multiparameter on-line monitoring instrument, comprises online Specimen eliminating system, on-line sample detection system, measurement and control system.
Described in-line digestion system comprises clears up reaction tank, clears up reaction tank and connects the first miniature peristaltic pump, the second miniature peristaltic pump respectively; Clear up the liquid outlet connecting tee reversing solenoid valve of reaction tank, triplet commutation solenoid valve connects straightway pump; Described first miniature peristaltic pump is used for connecting through the pretreated online water sample of physics, and described second miniature peristaltic pump connects concatermer solenoid valve; Described reaction tank of clearing up connects the first digital temperature sensor, clears up reaction tank and is around with the first heating wire, and clearing up gummed bottom reaction tank has the first ultrasound wave generation systems.
On-line sample detection system comprises sample detection stream, sample detection room, micro spectrometer, described sample detection stream comprises multi-position valve, liquid storage ring, syringe pump, multi-position valve connects liquid storage ring one end by pipeline, the liquid storage ring other end connects syringe pump one end by pipeline, the syringe pump other end connects ultrapure water by pipeline, and multi-position valve connects sample detection room by pipeline;
Light source send detect light beam enter sample detection room, outgoing beam through lens focus laggard enter micro spectrometer, micro spectrometer connect measurement and control system.
Described sample detection room comprises stainless steel trough, circulation detecting pool is provided with in stainless steel trough, circulation detecting pool is communicated to sample detection room, described circulation detecting pool connects multi-position valve by pipeline, described circulation detecting pool connects waste liquid pool, described circulation detecting pool connects the 3rd miniature peristaltic pump, and the 3rd miniature peristaltic pump connects ultrapure water; Side, described sample detection room is mounted with the second ultrasound wave generation systems.
Described measurement and control system comprises power module, embedded system, peripheral control circuits system, embedded system is connected with man-machine interactive system by serial ports, man-machine interactive system comprises storer, touch-screen and gprs system, gprs system is connected with host computer by wireless transmission, and embedded system connects micro spectrometer; Embedded system is connected with peripheral control circuits system, and peripheral control circuits system connects sample on-line sample digestion system and on-line sample detection system.
Described reaction tank of clearing up is that stainless steel material processes, and clears up reaction tank and connects the first miniature peristaltic pump, the second miniature peristaltic pump respectively by silicone tube; The described common port of liquid outlet by silicone tube connecting tee reversing solenoid valve clearing up reaction tank; Described second miniature peristaltic pump connects the public outlet of concatermer solenoid valve by silicone tube; The normal opening of described triplet commutation solenoid valve connects straightway pump one end by silicone tube, and the straightway pump other end connects waste liquid pool by silicone tube.
Described first digital temperature sensor comprises being arranged on clears up thermosensitive resistor film in reaction tank, glass-encapsulated.
Described concatermer solenoid valve is six conjuncted electromagnetic valves, and the entrance of six conjuncted electromagnetic valves connects respectively by silicone tube clears up reagent, ultrapure water, air.
Described first heating wire connects the first relay; Described ultrasonic generator connects the second relay.
Described first miniature peristaltic pump, the second miniature peristaltic pump are micro-step motor peristaltic pump, and described straightway pump is DC micromotor peristaltic pump.
Described circulation detecting pool is provided with interface, overflow vent, stainless steel trough is provided with water inlet, described interface, water inlet, overflow vent are all communicated to sample detection room, described interface connects multi-position valve by pipeline, described overflow vent connects waste liquid pool, described water inlet connects the 3rd miniature peristaltic pump, and the 3rd miniature peristaltic pump connects ultrapure water; Side, described sample detection room is mounted with the second ultrasound wave generation systems.
The sidewall of described sample detection room is provided with thermoelectric control module, in circulation detecting pool, thermistor is installed, thermistor connects digital temperature sensor, and digital temperature sensor outputs signal measurement and control system, and measurement and control system connects thermoelectric control module.
Bottom, described sample detection room is provided with optical window, detects light beam through optical window and through circulation detecting pool.
Be provided with tank waste discharge mouth, detection cell waste discharge mouth bottom described sample detection room, tank waste discharge mouth connects first DC micromotor peristaltic pump one end, the first DC micromotor peristaltic pump other end connects waste liquid pool; The common port of described detection cell waste discharge mouth connecting tee reversing solenoid valve, the normal opening of described triplet commutation solenoid valve connects micro-step motor peristaltic pump, the normally closed port of described triplet commutation solenoid valve connects the second DC micromotor peristaltic pump, and the second DC micromotor peristaltic pump is connected to waste liquid pool.
A kind of water quality heavy metal multiparameter on-line monitoring method, online water sample with clear up reagent and enter clear up reaction tank by clearing up stream, realize online high temperature and ultrasonic assistant is cleared up clearing up in reaction tank, the heavy metal in water sample is made to be oxidized to ionic state, after clearing up, the rear water sample of clearing up of certain volume enters on-line sample detection system again, described on-line sample detection system makes to clear up rear water sample and detection reagent corresponding to tested heavy metal, sample detection room is accurately entered by certain volume, online chromogenic reaction and spectral analysis is completed in sample detection indoor, simultaneously, control to detect stream, realize the online sequence detection of water quality heavy metal multiparameter, the embedded system of described measurement and control system is given an order, by in-line digestion process and the on-line checkingi process of peripheral control circuits Systematical control sample, embedded system connects micro spectrometer to obtain the output data of micro spectrometer, the content of tested heavy metal in water sample is detected by Digital Signal Analysis and Processing, and by GPRS, measurement result is sent to host computer, measurement and control system controls the running of whole instrument system and Data Analysis Services, and carry out signal and communication by GPRS and host computer, realize the remote monitoring of host computer to instrument work.
A kind of water quality heavy metal of the present invention multiparameter on-line monitoring instrument, technique effect is as follows:
1, ultrasonic wave added is adopted to clear up technology, utilize the hyperacoustic cavitation of higher-wattage, with the nonionic state heavy metal that the overwhelming majority in pulverizing, emulsification, dissolving test environment water sample exists with molecule form, accelerate the process of in-line digestion reaction, improve and clear up efficiency, the accuracy for instrument provides technology and ensures;
2, take micro spectrometer as core detection means, in its continuous wide spectral range, be easy to launch based on the online water quality monitoring spectroscopy signal process of spectral analysis, dynamically to eliminate the systematic error of spectroscopy signal, noise and background interference, the accuracy of monitoring of increasing water quality;
3, the water quality heavy metal monitoring instrument analyzed continuously based on wide spectral can realize the on-line monitoring to a class heavy metal pollution (mercury, lead, cadmium, chromium, arsenic), the on-line monitoring of multiple stage instrument realization to multinomial water quality heavy metal parameter can be replaced, greatly reduce the use cost of user;
4, only need to change corresponding detection reagent and spectral detection wavelength, remaining water quality heavy metal parameter can be detected, thus this instrument has the dirigibility of very strong function expansibility and on-the-spot Emergency use, it is a water quality heavy metal multiparameter on-line monitoring technique platform in essence, can meet the in-line digestion to 20 heavy metal species such as water quality mercury, lead, cadmium, chromium, arsenic, copper, manganese, iron and detection;
5, there is automatic Calibration and calibration function, earth's surface one class can be applied to and two class Water Pollution Monitoring, seawater pollution are monitored and multiple field such as the qualified discharge monitoring of Industrial Wastewater Treatment and municipal sewage treatment, wide application, applicability is strong, therefore, this instrument as network node applies in modern water quality monitoring Internet of Things, can realize the network monitoring to water pollution monitoring and early warning.
Accompanying drawing explanation
Fig. 1 is general structure schematic diagram of the present invention.
Fig. 2 is on-line sample digestion system schematic diagram of the present invention.
Fig. 3 is on-line sample detection system schematic diagram of the present invention.
Fig. 4 is instrument spectral detection system schematic diagram of the present invention.
Fig. 5 (a), Fig. 5 (b) are example reaction sensing chamber of the present invention structural representations.
Fig. 6 is apparatus measures of the present invention and control system schematic diagram.
Fig. 7 is Specimen eliminating temperature of reaction system control system figure of the present invention.
Fig. 8 is sample detection temperature of reaction system control system figure of the present invention.
Fig. 9 is instrument workflow diagram of the present invention.
Figure 10 is water quality cadmium of the present invention, lead, arsenic three parameter detecting process flow diagram.
Figure 11 is water quality chromium overhaul flow chart of the present invention.
Figure 12 is water quality mercury overhaul flow chart of the present invention.
Embodiment
A kind of water quality heavy metal multiparameter on-line monitoring instrument, by on-line sample digestion system A, on-line sample detection system B, measurement and control system C forms, (namely pulverize through physics pre-service, emulsification, filter) after online detected water sample under the effect of control system, be introduced into on-line sample digestion system A, make the mercury in water sample, plumbous, cadmium, chromium, arsenic is all oxidized to be cleared up for after corresponding ionic state, enter on-line sample detection system B detects tested heavy metal content by " chromogenic reaction " and " spectral analysis " again, instrument integration national standard detection method, due to mercury, plumbous, cadmium, characteristic absorption wavelength closely (the mercury: 485nm of chromium and each self-corresponding tested substance that show color of arsenic, plumbous: 535nm, cadmium: 518nm, chromium: 540nm, arsenic: 530nm), therefore, for reducing the difficulty of spectral signal process and ensureing the degree of accuracy of detection, instrument adopts the method for multiparameter sequence detection.
On-line sample digestion system A clears up technology in conjunction with ultrasonic assistant with reference to national environmental protection protecting standard (clearing up of HJ 678-2013 water quality, total metal content) innovation and designs, and clears up reaction tank, heating constant-temperature equipment, ultrasound wave generation systems (ultrasonic transducer, ultrasonic generator) composition primarily of Specimen eliminating stream, stainless steel.Online water sample and clear up reaction reagent and entered by flow path system under the effect of control system by certain volume and volume ratio and clear up reaction tank, reaction system is cleared up in formation, under high temperature and ul-trasonic irradiation, the oxidation accelerating heavy metal is cleared up, after fully reacting, controlled by stream, the reaction solution extracting certain volume enters on-line sample detection system B, is detected the content of tested heavy metal by online chromogenic reaction and spectral analysis.
On-line sample detection system B designs based on sequential injection principle and continuous spectrum analysis, and primarily of sample detection stream, spectral detection system composition, described spectral detection system is made up of collimated light source d, sample detection room b and micro spectrometer c.Under control system effect, detect stream order extract certain volume clear up rear water sample and detection reagent corresponding to tested heavy metal (i.e. chromogenic reaction detection reagent) enters sample detection room b, in the b of sample detection room, complete chromogenic reaction, detected the content of tested heavy metal in water sample by spectral analysis.
Described measurement and control system C is made up of power module, peripheral control circuits and embedded system.Preferably, in embedded system, master controller is SAMSUNGS3C6410 microprocessor, it adopts linux kernel technology, embedded system is given an order, by in-line digestion process and the on-line checkingi process of peripheral control circuits Systematical control sample, embedded system obtains the output data of spectrometer in on-line sample detection system by parallel port, is detected the content of tested heavy metal in sample by Digital Signal Analysis and Processing.
Fig. 1 shows the general structure of invention, this monitor comprises online Specimen eliminating system A, on-line sample detection system B, measurement and control system C, the function of described Specimen eliminating system A is that the tested heavy metal oxidation in water sample is become ionic state, the function of described specimen inspection system is reacted with heavy metal ion with detecting reagent (or claiming " chromogenic reagent "), generate substance that show color, and pass through the content of tested heavy metal in the characteristic absorption spectrum analysis water-like of this substance that show color, the function of described measurement and control system is the in-line digestion and the testing process that control water sample, and detect tested content of beary metal in water sample by spectral analysis, thus realize full-automatic online water quality monitoring.
Fig. 2 shows on-line sample digestion system A structural principle, and this system mainly comprises Specimen eliminating stream, stainlessly clears up reaction tank 1, heating constant-temperature equipment and the first ultrasound wave generation systems 9.
Described clear up stream by clearing up reaction tank 1, first miniature peristaltic pump 2, second miniature peristaltic pump 3, concatermer solenoid valve 4: six conjuncted electromagnetic valve, triplet commutation solenoid valve 5, straightway pump 6 form.Described reaction tank 1 of clearing up processes for stainless steel, is the core of flow path system, connects the first miniature peristaltic pump 2 and the second miniature peristaltic pump 3 by silicone tube 7, and its liquid outlet 8 is by the common port 9 of silicone tube 7 connecting tee reversing solenoid valve 5; Described first miniature peristaltic pump 2 other end is connected through the pretreated online water sample of physics.Described second miniature peristaltic pump 3 other end connects the public outlet 10 of six conjuncted electromagnetic valves by silicone tube, six conjuncted electromagnetic valves process by six miniature electromagnetic valves are integrated, by each solenoid valve of control circui switch (under usual state each solenoid valve be close, pass to the conducting of 12V high level rear electromagnetic valve), the entrance (i.e. the entrance of each solenoid valve) of six conjuncted electromagnetic valves clears up reagent, ultrapure water w and air respectively by silicone tube link, the normal opening 11 of described triplet commutation solenoid valve connects straightway pump 6 by silicone tube, the other end of straightway pump 6 connects waste liquid pool 6.1 by silicone tube, the normally closed port 12 of described triplet commutation solenoid valve connects online specimen inspection system by silicone tube, under usual state, normal opening 11 and the common port 9 of described triplet commutation solenoid valve is that (but straightway pump 6 does not work in conducting, still guarantee that the liquid outlet of digestion pool is in external closed condition), when described triplet commutation solenoid valve passes to 12V high level, then normally closed port 12 is opened and common port conducting, the rear water sample of process is cleared up for on-line detecting system provides.To sum up, described Specimen eliminating stream has three zones: the extraction of water sample and reagent, water sample after in-line digestion process is provided, cleaning reaction pond, be specified as: the online water sample accurately being extracted certain volume by peristaltic pump enters reaction tank, reaction tank is entered with the reagent extracting certain volume that mates of six conjuncted electromagnetic valves by the first miniature peristaltic pump 2, water sample is cleared up after completion of the reaction, the normally closed port opening triplet commutation solenoid valve 5 clears up rear water sample for on-line detecting system provides, triplet commutation solenoid valve 5 is finally made to work in normality (no power), straightway pump 6 works, to drain unnecessary waste liquid in reaction tank, and open the valve 5# of six conjuncted electromagnetic valves 4, with the first miniature peristaltic pump 2 collaborative work, complete the cleaning of reaction tank.
Describedly clear up the core that reaction tank 1 is whole in-line digestion system, its upper surface has bleeder vent 13 and ambient atmosphere conducting, glass packaged thermosensitive resistor 14 is equipped with to clear up the temperature detection of reaction system 15 in detection reaction pond in it, external first digital temperature sensor 16 of thermistor, temperature sensor output signal send measurement and control system C.Described stainless steel clear up outside reaction tank around heating with the first heating wire 17, the heating to clearing up reaction system in reaction tank can be realized by the conducting of relay 18.Described stainless steel is cleared up reaction tank outer bottom and is coupled with the first ultrasonic generator 19 by gluing technique, first ultrasound wave generation systems 19 is entered by the ultrasound wave 20 that the first ultrasonic transducer sends clears up reaction tank to accelerate the carrying out of in-line digestion reaction, can realize the ultrasonic assistant effect to clearing up reaction system in reaction tank by the second relay 21 conducting.To sum up, described stainless steel is cleared up reaction tank and is had the function that high-temperature heating and ultrasonic assistant clear up reaction.
First miniature peristaltic pump 2, second miniature peristaltic pump 3, six conjuncted electromagnetic valve of described on-line sample digestion system A, triplet commutation solenoid valve 5, straightway pump 6, first relay 18 are all connected measurement and control system C with the second relay 21, control its duty or the course of work by measurement and control system C.
Fig. 3 shows on-line sample detection system B structural principle, and this system mainly comprises sample detection stream a and spectral detection system, and described spectral detection system comprises light source e, sample detection room b and micro spectrometer c.
Described sample detection stream is made up of 24 multi-position valve a1, liquid storage ring a2 and syringe pump a3, mainly design based on sequential injection principle, described 24 multi-position valve a1 have multi-channel flow passage handoff functionality, its valve position 13# is by PEEK(polyetheretherketone) pipe connects online Specimen eliminating system stream, its common port connects liquid storage ring by PEEK pipe, and its valve position 1# is connected to the sample detection room b in line spectrum detection system by PEEK pipe.The described liquid storage ring a2 other end connects syringe pump a3 by PEEK pipe, and ultrapure water w is connected by PEEK pipe in the another port of syringe pump a3.Sample detection stream a has stream switching, sample and the accurate extraction of reagent and the automatic cleaning function of stream, be specified as: control multi-position valve rotor (its inner rotary pipeline) and common port and connection standard sample, the stream conducting detecting reagent, the online valve position such as water sample, ultrapure water can be made, thus realize stream switching; When detecting a certain heavy metal parameter, control syringe pump and multi-position valve, the sample of certain volume (standard model or clear up rear online water sample) with in corresponding detection reagent successively suction liquid storage ring, then multi-position valve rotor forwards valve position 1# to, syringe pump a3 is counter to be pushed away, example reaction system sample detection room b be can be pushed and online chromogenic reaction and spectral detection carried out, after detection, control straightway pump emptying sample detection room b, and control multi-position valve and syringe pump a3 collaborative work, complete the automatic cleaning of sample detection room.
Fig. 4 shows spectral detection system principle, comprises light source e, sample detection room b and micro spectrometer c.Described light source e is instrument halogen tungsten lamp, after collimation, form parallel detection beam 9.1 enter sample detection room b, outgoing beam focuses into into micro spectrometer c through lens e, micro spectrometer c exports data and carries out Treatment Analysis by parallel port feeding measurement and control system C, and measurement and control system C is also powered to micro spectrometer c by parallel port.Described micro spectrometer c wavelength coverage is: 200-1100nm, and wavelength resolution is 1nm.
Fig. 5 shows the structural representation of sample detection room b, described microminiature multifunctional sample sensing chamber not only considers the optical detection of water sample reaction system in design concept, but also for the online chromogenic reaction of sample to stirring, the technical requirement of constant temperature and cleaning, as intersecting of systems axiol-ogy light path and sample stream, do not affecting under the prerequisite detecting light path, based on ultrasonic technique and constant temperature water bath principle, devise a kind of multi-functional microminiature sample detection room integrating the functions such as optical detection, automatic constant-temperature, stirring and high-efficiency washing.
As shown in Fig. 5 (a) He Fig. 5 (b), the main body of described microminiature sample detection room is stainless steel trough 1.1, is provided with circulation detecting pool 2.1 in it, and described circulation detecting pool 2.1 is provided with interface 3.1, overflow vent 4.1; Described stainless steel trough 1.1 is provided with water inlet 5.1; Described interface 3.1, water inlet 5.1, overflow vent 4.1 are all communicated to sample detection room b, and stretch out sample chamber outer wall; Described interface 3.1 is communicated with multi-position valve valve position 1#(by PEEK pipe and namely connects detection stream), described overflow vent 4.1 is connected to waste liquid pool 6.1 by pipeline, described water inlet 5.1 connects the 3rd miniature peristaltic pump the 7.1, three miniature peristaltic pump 7.1 by silicone tube and connects ultrapure water w by silicone tube.Described 3rd miniature peristaltic pump 7.1 is micro-step motor peristaltic pump, and connection control system controls its duty and process.
Described sample detection room b lower sides is provided with optical window 8.1, detects light beam 9.1 by optical window 8.1 and through circulation detecting pool 2.1.B side, described sample detection room outer wall gummed has the second ultrasonic transducer 10.1, second ultrasonic transducer 10.1 to connect the second ultrasonic generator, produces ultrasound wave 12.1, stirs for ultrasound wave.Described second ultrasound wave generation systems 11.1 connects measurement and control system C, controls its duty and process.
Tank waste discharge mouth 13.1 is provided with bottom described sample detection room b, detection cell waste discharge mouth 14.1, described tank waste discharge mouth 13.1 connects the first DC micromotor peristaltic pump 15.1 by silicone tube, the other end pipeline of the first DC micromotor peristaltic pump 15.1 connects waste liquid pool 6.1, described detection cell waste discharge mouth 14.1 is by the common port 17.1 of silicone tube connecting tee reversing solenoid valve 16.1, the normal opening 18.1 of described triplet commutation solenoid valve 16.1 connects micro-step motor peristaltic pump 19.1 by silicone tube, the normally closed port 20.1 of described triplet commutation solenoid valve 16.1 is by silicone tube connector second DC micromotor peristaltic pump 21.1, second DC micromotor peristaltic pump 21.1 is connected to waste liquid pool 6.1 by silicone tube.Described detection cell waste discharge mouth 13.1 is the import of air bubble stream.Described first DC micromotor peristaltic pump 15.1 is all connected measurement and control system C with the second DC micromotor peristaltic pump 21.1, described micro-step motor peristaltic pump 19.1, described triplet commutation solenoid valve 16, to control its duty or the course of work.
The sidewall of described sample detection room b is provided with thermoelectric control module 22.1, glass packaged thermosensitive resistor 23.1 is installed in flow cell, thermistor 23.1 connects digital temperature sensor 24.1 by wire, described digital temperature sensor 24.1 output signal send measurement and control system C, the mode of operation of thermoelectric control module 22.1 is controlled as feedback signal
To be controlled the temperature of example reaction system 25.1 in circulation detecting pool 2.1 by constant temperature water bath.
Cover plate 26.1 is fixed by physical construction, stainless steel trough 1.1 passes through water inlet 5.1 under master control system effect, the ultrapure water w of certain volume is injected in tank 1.1, the replacing of ultrapure water w is by entering waste liquid pool 6.1 by tank waste discharge mouth 13.1 and the first DC micromotor peristaltic pump 15.1 by waste liquid, overflow vent 4.1 stretches out example reaction sensing chamber by sealing fixed sturcture, being connected with waste liquid pool 6.1 by silicone tube, is safety assurance during stream sample introduction fault.Interface 3.1, for detecting stream interface, connects circulation detecting pool 2.1, the external detection stream in sample chamber in sample detection indoor.Under control system effect, sample can be injected and detect reagent in circulation detecting pool 2.1, forming online sample chemical pre-treatment reaction system 25.1.Control micro-step motor peristaltic pump 19.1 by control system can oppositely blow, bubble agitation 27.1 is formed to reaction system 25.1, after sample detection, the normally closed port 20.1 of triplet commutation solenoid valve 16.1 is opened by control system, control the second DC micromotor peristaltic pump 21.1, second ultrasound wave generation systems 11.1 and detect stream, four collaborative works, complete waste discharge and the cleaning of sample detection room.Flow path system, described ultrasonic generator, the equal connection control system C of thermoelectric control module are enclosed in described flow path system and sample detection outdoor, to control its course of work.
Fig. 6 shows the principle of work of apparatus measures and control system, described measurement and control system C comprises power module, embedded system and peripheral control circuits system, embedded system is connected with man-machine interactive system by serial ports, man-machine interactive system comprises storer, touch-screen and gprs system, gprs system is connected with host computer by wireless transmission, and embedded system connects data acquisition module in spectrometer by parallel port; Embedded system master controller SAMSUNGS3C6410 has pin to be connected with peripheral control circuits system, and peripheral control circuits system connects sample on-line sample digestion system A and on-line sample detection system B.Described core of embedded system is SAMSUNGS3C6410 microprocessor, adopt linux kernel technology, described power module is embedded system and peripheral control circuits system power supply, embedded system master controller SAMSUNG S3C6410 to the periphery control circuit system sends control command, realizes the control of on-line sample digestion system A and the on-line sample detection system B course of work.The control of the described on-line sample digestion system A course of work, comprises and clears up stream control and digestion condition control.
Described clear up stream control be: control online water sample and clear up reagent and under the effect of clearing up flow path system, enter Specimen eliminating reaction tank 1 by certain volume and volume ratio, clear up after completion of the reaction through certain hour, control is cleared up stream and is detected stream collaborative work, make to clear up rear water sample and enter on-line detecting system, in addition, the waste discharge of clearing up reaction tank 1 also needs control to clear up stream with cleaning to be achieved.
Fig. 7 shows described digestion condition stream control procedure and principle, because electric-heating-wire-heating and ul-trasonic irradiation can make temperature of reaction system rise, promote the carrying out of Specimen eliminating reaction, therefore temperature controls to include simultaneously and controls and ul-trasonic irradiation control electric-heating-wire-heating, can be realized by the duty of pilot relay 1 and 2, it is 400W that described ultrasound wave clears up power, and described temperature controlling range is: 95 ± 2 DEG C.
The control of the described on-line sample detection system B course of work, comprises and detects that stream controls, example reaction temperature controls, reaction system mixing control and stream cleaning control, and described stream cleaning control comprises and controlling the ultrasonic cleaning of sample detection room.The switching stream that detected water sample consists of 24 multi-position valve a1 and syringe pump a3 with detection reagent enters microminiature sample detection room by certain volume ratio high-precision quantitative, example reaction system, under the effect of thermostatic control, mixing control, completes online chemical pre-treatment and the spectral analysis of sample in the b of sample detection room.It is the essential condition guaranteeing instrument repeatability that temperature of reaction system controls, Fig. 8 shows described example reaction system temperature control principle, namely realize temperature by the mode of operation of thermoelectric control module (Peltier) to control, described temperature controlling range is: 30 ± 0.1 DEG C.
The spectrometer of on-line sample detection system B exports data and is transferred to embedded system by parallel port, pass through data process&analysis, detect tested content of beary metal in sample, and by gprs system, measurement result is sent to host computer, embedded Webserver controls the running of whole instrument system, and carry out signal and communication by wireless sending module and host computer, realize the remote monitoring of host computer to instrument work.
Fig. 6 shows surveying work schematic flow sheet of the present invention, operationally, sends instruction after powering on by host computer monitoring software, control system responds, after boot system self-inspection, after system initialization, start the content of tested heavy metal (mercury, lead, cadmium, chromium, arsenic) in on-line checkingi water sample.Because the national standard resolution principle of this five classes heavy metal is distinguished to some extent, (detection of these three heavy metal water quality parameters of cadmium, lead, arsenic needs high temperature to assist red fuming nitric acid (RFNA) to clear up; The detection of chromium needs high temperature to assist red fuming nitric acid (RFNA)-concentrated hydrochloric acid to clear up, and the concentration of red fuming nitric acid (RFNA) is different from the former, the detection of mercury needs high temperature to assist potassium permanganate-alkaline potassium per-sulfate digestion), therefore instrument adopt that parameters order is cleared up, the on-line checkingi flow process of sequence detection and method.
Figure 10 shows the online sequence detection flow process of water quality heavy metal cadmium, lead, arsenic.
Figure 11 shows the on-line checkingi flow process of water quality heavy metal chromium.
Figure 12 shows the on-line checkingi flow process of water quality heavy metal Hg.
The on-line checkingi of described water quality heavy metal (mercury, lead, cadmium, chromium, arsenic) is the on-line checkingi to total heavy metal in detected water sample (total mercury, always plumbous, total cadmium, always chromium and always arsenic) in fact.
Protection scope of the present invention is not limited to the above embodiments, and obviously, those skilled in the art can carry out various change and distortion to the present invention and not depart from the scope of the present invention and spirit.If these are changed and distortion belongs in the scope of the claims in the present invention and equivalent technologies thereof, then the intent of the present invention also comprises these changes and distortion.
Claims (10)
1. a water quality heavy metal multiparameter on-line monitoring instrument, comprises online Specimen eliminating system (A), on-line sample detection system (B), measurement and control system (C), it is characterized in that,
Described in-line digestion system (A) comprises clears up reaction tank (1), clears up reaction tank (1) and connects the first miniature peristaltic pump (2), the second miniature peristaltic pump (3) respectively; Clear up liquid outlet (8) the connecting tee reversing solenoid valve (5) of reaction tank (1), triplet commutation solenoid valve (5) connects straightway pump (6); Described first miniature peristaltic pump (2) is for connecting through the pretreated online water sample of physics, and described second miniature peristaltic pump (3) connects concatermer solenoid valve (4); Described reaction tank (1) of clearing up connects the first digital temperature sensor (16), clears up reaction tank (1) and is around with the first heating wire (17), and clearing up reaction tank (1) bottom gummed has the first ultrasound wave generation systems (19);
On-line sample detection system comprises sample detection stream (a), sample detection room (b), micro spectrometer (c); It is characterized in that, described sample detection stream (a) comprises multi-position valve, liquid storage ring (a2), syringe pump (a3), multi-position valve connects liquid storage ring (a2) one end by pipeline, liquid storage ring (a2) other end connects syringe pump (a3) one end by pipeline, syringe pump (a3) other end connects ultrapure water (w) by pipeline, and multi-position valve connects sample detection room (b);
Light source (d) send detect light beam (9.1) enter sample detection room (b), outgoing beam through lens (e) focus on laggard enter micro spectrometer (c), micro spectrometer (c) connects measurement and control system (C);
Described sample detection room (b) comprises stainless steel trough (1.1), circulation detecting pool (2.1) is provided with in stainless steel trough (1.1), circulation detecting pool (2.1) is communicated to sample detection room (b), described circulation detecting pool (2.1) connects multi-position valve (a1) by pipeline, described circulation detecting pool (2.1) connects waste liquid pool (6.1), described circulation detecting pool (2.1) connects the 3rd miniature peristaltic pump (7.1), and the 3rd miniature peristaltic pump (7.1) connects ultrapure water (w); Described sample detection room (b) side is mounted with the second ultrasound wave generation systems (11.1);
Described measurement and control system comprises power module, embedded system, peripheral control circuits system, embedded system is connected with man-machine interactive system by serial ports, man-machine interactive system comprises storer, touch-screen and gprs system, gprs system is connected with host computer by wireless transmission, and embedded system connects micro spectrometer (c); Embedded system is connected with peripheral control circuits system, and peripheral control circuits system connects sample on-line sample digestion system and on-line sample detection system.
2. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, described reaction tank (1) of clearing up processes for stainless steel material, clears up reaction tank (1) and connects the first miniature peristaltic pump (2), the second miniature peristaltic pump (3) respectively by silicone tube (7); The described common port (9) of liquid outlet (8) by silicone tube (7) connecting tee reversing solenoid valve (5) clearing up reaction tank (1); Described second miniature peristaltic pump (3) connects the public outlet (10) of concatermer solenoid valve (4) by silicone tube (7); The normal opening (11) of described triplet commutation solenoid valve (5) connects straightway pump (6) one end by silicone tube (7), and straightway pump (6) other end connects waste liquid pool (6.1) by silicone tube (7).
3. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, described first digital temperature sensor (16) comprises being arranged on clears up thermosensitive resistor film (14) in reaction tank (1), glass-encapsulated;
Described concatermer solenoid valve (4) is six conjuncted electromagnetic valves, and the entrance of six conjuncted electromagnetic valves connects respectively by silicone tube (7) clears up reagent, ultrapure water, air.
4. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, described first heating wire (17) connects the first relay (18); Described ultrasonic generator (19) connects the second relay (21).
5. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, described first miniature peristaltic pump (2), the second miniature peristaltic pump (3) are micro-step motor peristaltic pump, and described straightway pump (6) is DC micromotor peristaltic pump.
6. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, described circulation detecting pool (2.1) is provided with interface (3.1), overflow vent (4.1), stainless steel trough (1.1) is provided with water inlet (5.1), described interface (3.1), water inlet (5.1), overflow vent (4.1) is all communicated to sample detection room (b), described interface (3.1) connects multi-position valve (a1) by pipeline, described overflow vent (4.1) connects waste liquid pool (6.1), described water inlet (5.1) connects the 3rd miniature peristaltic pump (7.1), 3rd miniature peristaltic pump (7.1) connects ultrapure water (w), described sample detection room (b) side outer wall gummed has the second ultrasound wave generation systems (11.1).
7. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, the sidewall of described sample detection room (b) is provided with thermoelectric control module (22), thermistor (23) is installed in circulation detecting pool (2), thermistor (23) connects digital temperature sensor (24), digital temperature sensor (24) output signal is to measurement and control system (f), and measurement and control system (f) connects thermoelectric control module (22).
8. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, described sample detection room (b) bottom is provided with optical window (8), detects light beam (9) through optical window (8) and through circulation detecting pool (2).
9. a kind of water quality heavy metal multiparameter on-line monitoring instrument according to claim 1, it is characterized in that, described sample detection room (b) bottom is provided with tank waste discharge mouth (13), detection cell waste discharge mouth (14), and tank waste discharge mouth (13) connects first DC micromotor peristaltic pump (15) one end, first DC micromotor peristaltic pump (15) other end connects waste liquid pool (6); The common port (17) of described detection cell waste discharge mouth (14) connecting tee reversing solenoid valve (16), the normal opening (18) of described triplet commutation solenoid valve (16) connects micro-step motor peristaltic pump (19), the normally closed port (20) of described triplet commutation solenoid valve (16) connects the second DC micromotor peristaltic pump (21), and the second DC micromotor peristaltic pump (21) is connected to waste liquid pool (6).
10. a water quality heavy metal multiparameter on-line monitoring method, it is characterized in that, online water sample with clear up reagent and enter clear up reaction tank (1) by clearing up stream, realize online high temperature and ultrasonic assistant is cleared up clearing up in reaction tank (1), the heavy metal in water sample is made to be oxidized to ionic state, after clearing up, the rear water sample of clearing up of certain volume enters on-line sample detection system (B) again, described on-line sample detection system (B) makes to clear up rear water sample and detection reagent corresponding to tested heavy metal, accurately sample detection room (b) is entered by certain volume, online chromogenic reaction and spectral analysis is completed in sample detection room (b), simultaneously, control to detect stream, realize the online sequence detection of water quality heavy metal multiparameter, the embedded system of described measurement and control system (C) is given an order, by in-line digestion process and the on-line checkingi process of peripheral control circuits Systematical control sample, embedded system connects micro spectrometer (C) to obtain the output data of micro spectrometer, the content of tested heavy metal in water sample is detected by Digital Signal Analysis and Processing, and by GPRS, measurement result is sent to host computer, measurement and control system (C) controls the running of whole instrument system and Data Analysis Services, and carry out signal and communication by GPRS and host computer, realize the remote monitoring of host computer to instrument work.
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| CN201610203316.XA CN105866448B (en) | 2015-04-08 | 2015-04-08 | A kind of water quality heavy metal monitors instrument on-line |
| CN201610205602.XA CN105866449B (en) | 2015-04-08 | 2015-04-08 | A kind of water quality heavy metal multi-parameter on-line monitoring method |
| CN201510162911.9A CN104764892B (en) | 2015-04-08 | 2015-04-08 | A kind of water quality heavy metal multi-parameter on-line monitoring instrument |
| CN201610205576.0A CN105842467B (en) | 2015-04-08 | 2015-04-08 | A kind of multi-parameter water-quality monitors instrument on-line |
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| CN109557847A (en) * | 2018-11-26 | 2019-04-02 | 北京必创科技股份有限公司 | A kind of automatic cleaning control system and method |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN105866448A (en) | 2016-08-17 |
| CN105866449B (en) | 2017-06-30 |
| CN104764892B (en) | 2016-05-11 |
| CN105842467A (en) | 2016-08-10 |
| CN105866449A (en) | 2016-08-17 |
| CN105842467B (en) | 2017-06-06 |
| CN105866448B (en) | 2017-06-23 |
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