CN104764696A - Water quality heavy metal online sample detection system - Google Patents
Water quality heavy metal online sample detection system Download PDFInfo
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- CN104764696A CN104764696A CN201510162654.9A CN201510162654A CN104764696A CN 104764696 A CN104764696 A CN 104764696A CN 201510162654 A CN201510162654 A CN 201510162654A CN 104764696 A CN104764696 A CN 104764696A
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Abstract
The invention discloses a water quality heavy metal online sample detection system which comprises a sample detection flow path, a sample detection chamber and a micro spectrometer, wherein the sample detection flow path comprises a multi-position valve, a liquid storage ring and an injection pump; the multi-position valve is connected with one end of the liquid storage ring by virtue of a pipeline; the other end of the liquid storage ring is connected with one end of the injection pump by virtue of a pipeline; the other end of the injection pump is connected with ultra-pure water by virtue of a pipeline; and the multi-position valve is connected with the sample detection chamber. The detection light beams emitted by a light source enter the sample detection chamber, the emergent light beams are focused by a lens and enter the micro spectrometer, and the micro spectrometer is connected with a measurement and control system. The water quality heavy metal online sample detection system disclosed by the invention has the functions of switching flow paths, accurately extracting samples and reagents and automatically cleaning the flow paths; and meanwhile, the functions of optical detection, automatic temperature preservation, stirring and cleaning are integrated into a whole based on the ultrasonic technology and water bath constant temperature principle under the condition that the detection light path is not influenced.
Description
Technical field
A kind of water quality heavy metal of the present invention on-line sample detection system, relates to water quality on-line checkingi field.
Background technology
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, lead, chromium, cadmium, arsenic, copper, manganese, iron etc.At present, environmental protection, the departments such as water conservancy are 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, above technological approaches be difficult to meet the dirigibility that water quality monitoring technology promptly uses at extendability and the scene of multi-parameter monitoring in technical requirement, and use cost is higher, as: a maximum integrated 3-4 module many colorimetric analysiss module integration type instrument, otherwise instrument cost is too high (generally often increases a colorimetric analysis module, instrument price will increase 7-10 ten thousand yuan, increase) and make user be difficult to accept, and also can become large as increased a colorimetric analysis modularized instrument volume.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 problems of the technologies described above, the invention provides a kind of water quality heavy metal on-line sample detection system.Can sequence detection multinomial water quality heavy metal parameter (as mercury, lead, chromium, cadmium, arsenic etc.) online, meanwhile, this system possesses that stream switches, the accurate extraction of sample and reagent, and the automatic cleaning function of stream; And not affecting under the prerequisite detecting light path, based on ultrasonic technique and constant temperature water bath principle, integrate the functions such as optical detection, automatic constant-temperature, stirring and cleaning.
The technical scheme that the present invention takes is:
A kind of water quality heavy metal 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, and the syringe pump other end connects ultrapure water by pipeline, and multi-position valve connects sample detection room.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 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, and described interface connects multi-position valve by pipeline, and described overflow vent connects waste liquid pool, described water inlet connects miniature peristaltic pump, and miniature peristaltic pump connects ultrapure water.Side, described sample detection room is mounted with ultrasonic transducer, and ultrasonic transducer connects ultrasonic generator.
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.Described first DC micromotor peristaltic pump, the second DC micromotor peristaltic pump, micro-step motor peristaltic pump, triplet commutation solenoid valve all connect measurement and control system.
The normal opening of described triplet commutation solenoid valve connects micro-step motor peristaltic pump by silicone tube, the normally closed port of described triplet commutation solenoid valve connects the second DC micromotor peristaltic pump by silicone tube, and the second DC micromotor peristaltic pump is connected to waste liquid pool by silicone tube.
Described water inlet connects miniature peristaltic pump by silicone tube, and miniature peristaltic pump is communicated with ultrapure water by silicone tube.
Described stainless steel trough is provided with cover plate.
Described multi-position valve is 24 multi-position valves.
Described pipeline is PEEK pipe.
A kind of water quality heavy metal of the present invention on-line sample detection system, technique effect is as follows:
1), take micro spectrometer as core, multinomial water quality heavy metal parameter can be detected in wide spectral range, compared with water quality heavy metal multi-parameter monitoring technology described in background technology, the extendability that native system has that cost is low, volume is little, water quality heavy metal multiparameter detects and the stronger technical advantage of dirigibility;
2), on the basis of micro spectrometer continuous wide spectral analysis, the research of online water quality monitoring signal transacting is more easily launched, to eliminate turbidity, the colourity background interference of detected water sample, thus the accuracy of heavy metal on-line checkingi of increasing water quality;
3), there is autoabstract, automatic stirring, automatic constant-temperature, automatically cleaning and the integrated technical advantage of the multifunction system that automatically detects, can the Stability and dependability of effective guarantee system.
Accompanying drawing explanation
Fig. 1 is present system connection diagram;
Fig. 2 is the spectral detection system schematic diagram of present system;
Fig. 3 is the sample detection cell structure schematic diagram one of present system;
Fig. 4 is the sample detection cell structure schematic diagram two of present system.
Embodiment
Online detected water sample after physics pre-service (mainly the filtration of precipitation and certain precision) is introduced into on-line sample digestion system under the effect of monitoring instrument control system, make that the mercury in water sample, lead, cadmium, chromium, arsenic are all oxidized to be cleared up for after corresponding ionic state, enter a kind of water quality heavy metal of the present invention on-line sample detection system again, to detect the content of tested heavy metal in water sample.As shown in Figure 1, a kind of water quality heavy metal on-line sample detection system, this system mainly comprises sample detection stream a and spectral detection system, and described spectral detection system comprises light source d, sample detection room b and micro spectrometer c.
Described sample detection stream a 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 a2 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 24 multi-position valve a1 rotors (its inner a 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 a3 and 24 multi-position valve a1, the sample of certain volume (standard model or clear up rear online water sample) with in corresponding detection reagent successively suction liquid storage ring a2, then multi-position valve rotor forwards valve position 1# to, syringe pump a3 is counter to be pushed away, example reaction system can be pushed sample detection room b, carry out online chromogenic reaction and spectral detection, 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 b.To sum up: sample detection stream order extracts water sample and detection reagent corresponding to tested heavy metal enters sample detection room b, (this needs control 24 multi-position valve a1, syringe pump a3 and liquid storage ring a2 collaborative work, namely switched by the stream of 24 multi-position valve a1, syringe pump a3 order extracts the water sample of certain volume and detection reagent corresponding to tested heavy metal enters liquid storage ring a2, then, the common port of 24 multi-position valve a1 is switched to stream corresponding to spectral detection system again, sample detection room b is shifted onto counter for the reaction system in liquid storage ring a2 again by syringe pump a3, complete the detection to water quality parameter tested in water sample, after detection, automatic cleaning sample detection room b, and then extract the water sample of certain volume and detection reagent corresponding to the tested heavy metal of the next one enters sample detection room b, to complete the online sequence detection to multinomial water quality heavy metal.
Fig. 2 shows spectral detection system principle, comprises light source d, sample detection room b and micro spectrometer c.Described light source d is instrument halogen tungsten lamp, after collimation, form parallel detection light beam 9 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 f, and measurement and control system f 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. 3 shows the structural representation of sample detection room b, described sample detection room b is in design concept, not only consider the optical detection of water sample reaction system, 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 Figure 3, Figure 4, the main body of sample detection room b is stainless steel trough 1, is provided with circulation detecting pool 2 in it, and described circulation detecting pool 2 is provided with interface 3, overflow vent 4; Described tank 1 is provided with water inlet 5; Described interface 3, water inlet 5, overflow vent 4 are all communicated to sample detection room b, and stretch out sample chamber outer wall; Described interface 3 is communicated with multi-position valve valve position 1#(by PEEK pipe and namely connects detection stream), described overflow vent 4 is connected to waste liquid pool 6 by pipeline, and described water inlet 5 connects miniature peristaltic pump 7 by silicone tube, and miniature peristaltic pump 7 connects ultrapure water w by silicone tube.Described miniature peristaltic pump 7 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, detects light beam 9 by optical window 8 and through circulation detecting pool 2.B side, described sample detection room is mounted with ultrasonic transducer 10, and ultrasonic transducer 10 connects ultrasonic generator 11, produces ultrasound wave 12, stirs for ultrasound wave.Described excusing from death wave producer 11 connection control system, controls its duty and process.
Tank waste discharge mouth 13 is provided with bottom described sample detection room b, detection cell waste discharge mouth 14, described tank waste discharge mouth 13 connects the first DC micromotor peristaltic pump 15 by silicone tube, first DC micromotor peristaltic pump 15 other end pipeline connects waste liquid pool 6, described detection cell waste discharge mouth 14 is by the common port 17 of silicone tube connecting tee reversing solenoid valve 16, the normal opening 18 of described triplet commutation solenoid valve 16 connects micro-step motor peristaltic pump 19 by silicone tube, the normally closed port 20 of described triplet commutation solenoid valve 16 is by silicone tube connector second DC micromotor peristaltic pump 21, second DC micromotor peristaltic pump 21 is connected to waste liquid pool 6 by silicone tube.Described detection cell waste discharge mouth 13 is the import of air bubble stream.Described first DC micromotor peristaltic pump 15 and the second DC micromotor peristaltic pump 21, described micro-step motor peristaltic pump 19, described triplet commutation solenoid valve 16 all connection control system, to control its duty or the course of work.
The sidewall of described sample detection room b is provided with thermoelectric control module 22, glass packaged thermosensitive resistor 23 is installed in circulation detecting pool 2, thermistor 23 connects digital temperature sensor 24 by wire, described digital temperature sensor 24 output signal send measurement and control system f, the mode of operation of thermoelectric control module 22 is controlled, to be controlled the temperature of example reaction system 25 in circulation detecting pool 2 by constant temperature water bath as feedback signal.
Cover plate 26 is fixed by physical construction, tank 1 passes through water inlet 5 under master control system effect, the ultrapure water w of certain volume is injected in stainless steel trough 1, the replacing of ultrapure water w is by entering waste liquid pool 6 by tank waste discharge mouth 13 and the first DC micromotor peristaltic pump 15 by waste liquid, overflow vent 4 stretches out example reaction sensing chamber by sealing fixed sturcture, being connected with waste liquid pool 6 by silicone tube, is safety assurance during stream sample introduction fault.
Interface 3, for detecting stream interface, connects circulation detecting pool 2, at the external detection stream of sample detection room b in the b of sample detection room.Under control system effect, sample can be injected and detect reagent in circulation detecting pool 2, forming online sample chemical pre-treatment reaction system 25.Control micro-step motor peristaltic pump 19 by control system can oppositely blow, bubble agitation 27 is formed to reaction system 25, after sample detection, the normally closed port 20 of triplet commutation solenoid valve 16 is opened by control system, control the second DC micromotor peristaltic pump 21, ultrasonic generator 11 and detect stream, four collaborative works, complete waste discharge and the cleaning of sample detection room.
Flow path system, described ultrasonic generator 11, thermoelectric control module 22 all connection control system are enclosed in described flow path system and sample detection outdoor, to control its course of work.
Claims (10)
1. a water quality heavy metal 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) 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 (f);
Described sample detection room (b) comprises stainless steel trough (1), circulation detecting pool (2) is provided with in stainless steel trough (1), circulation detecting pool (2) is provided with interface (3), overflow vent (4), stainless steel trough (1) is provided with water inlet (5), described interface (3), water inlet (5), overflow vent (4) is all communicated to sample detection room (b), described interface (3) connects multi-position valve by pipeline, described overflow vent (4) connects waste liquid pool (6), described water inlet (5) connects miniature peristaltic pump (7), miniature peristaltic pump (7) connects ultrapure water (w),
Described sample detection room (b) side is mounted with ultrasonic transducer (10), and ultrasonic transducer (10) connects ultrasonic generator (11).
2. a kind of water quality heavy metal on-line sample detection system 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).
3. a kind of water quality heavy metal on-line sample detection system 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).
4. a kind of water quality heavy metal on-line sample detection system 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).
5. a kind of water quality heavy metal on-line sample detection system according to claim 4, it is characterized in that, described first DC micromotor peristaltic pump (15), the second DC micromotor peristaltic pump (21), micro-step motor peristaltic pump (19), triplet commutation solenoid valve (16) all connect measurement and control system (f).
6. a kind of water quality heavy metal on-line sample detection system according to claim 4, it is characterized in that, the normal opening (18) of described triplet commutation solenoid valve (16) connects micro-step motor peristaltic pump (19) by silicone tube, the normally closed port (20) of described triplet commutation solenoid valve (16) connects the second DC micromotor peristaltic pump (21) by silicone tube, and the second DC micromotor peristaltic pump (21) is connected to waste liquid pool (6) by silicone tube.
7. a kind of water quality heavy metal on-line sample detection system according to claim 1, it is characterized in that, described water inlet (5) connects miniature peristaltic pump (7) by silicone tube, and miniature peristaltic pump (7) is communicated with ultrapure water (w) by silicone tube.
8. a kind of water quality heavy metal on-line sample detection system according to claim 1, it is characterized in that, described stainless steel trough (1) is provided with cover plate (26).
9. a kind of water quality heavy metal on-line sample detection system according to claim 1, it is characterized in that, described multi-position valve is 24 multi-position valves.
10. a water quality heavy metal on-line sample detection method, it is characterized in that, sample detection stream order extracts water sample and detection reagent corresponding to tested heavy metal enters sample detection room (b), control 24 multi-position valves (a1), syringe pump (a3) and liquid storage ring a2 collaborative work, namely switched by the stream of 24 multi-position valves (a1), syringe pump (a3) order extracts the water sample of certain volume and detection reagent corresponding to tested heavy metal enters liquid storage ring (a2), then, the common port of 24 multi-position valves (a1) is switched to stream corresponding to spectral detection system again, sample detection room (b) is shifted onto counter for the reaction system in liquid storage ring (a2) again by syringe pump (a3), complete the detection to water quality parameter tested in water sample, after detection, automatic cleaning sample detection room (b), and then extract the water sample of certain volume and detection reagent corresponding to the tested heavy metal of the next one enters sample detection room (b), to complete the online sequence detection to multinomial water quality heavy metal.
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| CN105929124A (en) * | 2016-06-12 | 2016-09-07 | 深圳市清时捷科技有限公司 | On-line water quality analysis instrument and water quality analysis method thereof |
| CN106959350A (en) * | 2017-04-01 | 2017-07-18 | 三峡大学 | A kind of QPQ technologies base salt cyanic acid radical content fully-automated synthesis analytical instrument |
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| CN112903369A (en) * | 2021-01-15 | 2021-06-04 | 杭州绿洁环境科技股份有限公司 | Online wet settlement collection long-distance collection and sample separation system |
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| CN113495164B (en) * | 2020-04-02 | 2023-11-21 | 中国科学院深圳先进技术研究院 | Continuous liquid sample injection system and control method thereof |
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Application publication date: 20150708 |