CN110124761A - Water environment multi-parameter electrochemical detection device and its detection method based on micro-fluidic chip - Google Patents

Water environment multi-parameter electrochemical detection device and its detection method based on micro-fluidic chip Download PDF

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Publication number
CN110124761A
CN110124761A CN201910420014.1A CN201910420014A CN110124761A CN 110124761 A CN110124761 A CN 110124761A CN 201910420014 A CN201910420014 A CN 201910420014A CN 110124761 A CN110124761 A CN 110124761A
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valve
micro
peristaltic pump
fluidic chip
reagent bottle
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王鑫
孙立宁
冯侨华
施云波
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Harbin University of Science and Technology
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Harbin University of Science and Technology
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Priority to CN201910420014.1A priority Critical patent/CN110124761A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/50273Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the means or forces applied to move the fluids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/06Fluid handling related problems
    • B01L2200/0621Control of the sequence of chambers filled or emptied
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/06Auxiliary integrated devices, integrated components
    • B01L2300/0627Sensor or part of a sensor is integrated
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/08Geometry, shape and general structure
    • B01L2300/0861Configuration of multiple channels and/or chambers in a single devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00Moving or stopping fluids
    • B01L2400/04Moving fluids with specific forces or mechanical means
    • B01L2400/0403Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0415Moving fluids with specific forces or mechanical means specific forces electrical forces, e.g. electrokinetic

Abstract

Water environment multi-parameter electrochemical detection device and its detection method based on micro-fluidic chip, belong to water environment pollution detection technique field, bigger to solve existing water environment parameter measurement device, not portable, and the problem that test-types are single.Device for storing liquid of the present invention includes the reagent bottle of the different reagents of five storages, it is connected between reagent bottle and the inlet of micro-fluidic chip by pipeline, a valve is provided on the pipeline of each connection reagent bottle, there are two peristaltic pumps for setting on pipeline between valve and micro-fluidic chip, there are four micro reaction pools to detect four kinds of water quality parameters for setting in micro-fluidic chip, the detected data of micro-fluidic chip are exported to signal acquisition circuit, signal acquisition circuit will test after data amplify filtering processing and be sent to microcontroller, microcontroller will test after data carry out calculation process and be sent to display module and be shown, the liquid outlet of micro-fluidic chip is connected to waste collecting device by pipeline.The present invention is detected for water environment parameter.

Description

Water environment multi-parameter electrochemical detection device and its detection based on micro-fluidic chip Method
Technical field
The present invention relates to a kind of water environment multi-parameter electrochemical detection device and its detection methods, belong to water environment pollution inspection Survey technology field.
Background technique
With industrial development, urbanization speed-raising and the expansion of the size of population, demand of the China to water resource is growing; At the same time, the discharge wantonly of a large amount of industrial wastewater and exhausting sewage, causes surface water and groundwater water quality to be disliked increasingly Change, rivers and lakes water pollution and drinking water safety problem happen occasionally, and seriously restrict the sustainable development of economy and society. Real-time detection, analysis and prediction water quality parameter situation and changing rule are the important hands for carrying out water environment pollution control with administering Section.Therefore, quick accurately water environment detection device is just particularly important.
Currently, the method for measurement water environment parameter mainly includes chemical analysis, segregation analysis, spectra methods, electricity Chemical analysis and various detection means joint technology etc..Electrochemical methods are the electricity and electrochemistry using test substance Matter measures the quantitative and qualitative analysis method of its property.This method and other subject have it is close contact, in water environment detection side Face, electrochemical methods are a kind of generally acknowledged sensitive, fast and accurately micro and trace analysis methods, and its instrument is simple, It is at low cost, it is suitable for miniaturization.
Currently, the device of measurement water environment parameter and is being tested mainly by large scale equipments such as mass spectrograph, liquid chromatographs It carries out, is needed by many more manipulations such as pretreatment, separation, enrichment, detections under the conditions of room, detection time is long, real-time is poor.
Therefore, compel the be essential miniaturization that detecting instrument is unfolded, integrated, portability research, be the quick of water environment parameter Detection provides sound assurance, provides accurate, timely, comprehensive data for prevention and cure of pollution.
Summary of the invention
It is bigger the invention aims to solve existing water environment parameter measurement device, it is not portable, and test-types list One the problem of, provides a kind of water environment multi-parameter electrochemical detection device and its detection method based on micro-fluidic chip.
Water environment multi-parameter electrochemical detection device of the present invention based on micro-fluidic chip, it include device for storing liquid, Valve controling circuit, peristaltic pump driving circuit, micro-fluidic chip, potentiostatic circuit, signal acquisition circuit, microcontroller, waste liquid Collection device and display module;It include the reagent bottle of the different reagents of five storages, reagent bottle and micro-fluidic chip in device for storing liquid Inlet between be connected by pipeline, be provided with a valve on the pipeline of each connection reagent bottle, valve and micro-fluidic core Setting is there are two peristaltic pump on pipeline between piece, and there are four micro reaction pools to detect four kinds of water quality ginsengs for setting in micro-fluidic chip It counts, potentiostatic circuit provides reference potential for the detecting electrode of micro-fluidic chip in detection process, and micro-fluidic chip detection obtains Data export to signal acquisition circuit, signal acquisition circuit will test data amplify filtering processing after be sent to microcontroller Device, microcontroller will test after data carry out calculation process and be sent to display module and shown, the liquid outlet of micro-fluidic chip It is connected to waste collecting device by pipeline, connects and is provided with a valve, valve on the pipeline of the liquid outlet of micro-fluidic chip Peristaltic pump is provided on pipeline between waste collecting device, for valve by valve controling circuit control switch, peristaltic pump is logical Peristaltic pump driving circuit control switch is crossed, microcontroller provides control signal for valve controling circuit and peristaltic pump driving circuit.
Preferably, five reagent bottles that the device for storing liquid includes are respectively that electrolyte storing reagent bottle, mark-on water sample are deposited Store up reagent bottle, cleaning solution storing reagent bottle, water sample storing reagent bottle to be measured and deionized water storing reagent bottle, electrolyte storage examination Agent bottle is connected with the first valve, and mark-on water sample storing reagent bottle is connected with the second valve, cleaning solution storing reagent bottle and third valve Door is connected, and water sample storing reagent bottle to be measured is connected with the 4th valve, and deionized water storing reagent bottle is connected with the 5th valve.
Preferably, the first valve is connected with the first peristaltic pump, the second valve, third valve, the 4th valve and the 5th valve It is connected with the second peristaltic pump, the 6th valve being arranged on liquid outlet pipeline is connected with third peristaltic pump.
Preferably, micro-fluidic chip includes test chamber upper cover, the first microsensor, the second microsensor, third micro sensing Device, the 4th microsensor and substrate are provided with inlet, the first micro reaction pool, the second micro reaction pool, third on lid on test chamber Micro reaction pool, the 4th micro reaction pool, liquid outlet and fluid channel, inlet are micro- by the first micro reaction pool of fluid channel connection, third Reaction tank and the 4th micro reaction pool, the 4th micro reaction pool are connected to the second micro reaction pool by fluid channel, and liquid outlet passes through fluid channel It is connected to the first micro reaction pool, third micro reaction pool and the second micro reaction pool, the first microsensor, the second microsensor, third are micro- It is micro- anti-that sensor and the 4th microsensor are located at the first micro reaction pool, the second micro reaction pool, third micro reaction pool and the 4th The lower section of Ying Chi, test chamber upper cover is bonded with substrate to be integrated.
Preferably, the first microsensor is concentration of heavy metal ion detection sensor, and the second microsensor is pH value detection Sensor, third microsensor are ammonium concentration detection sensor, and the 4th microsensor is temperature detection sensor.
The detection method of water environment multi-parameter electrochemical detection device of the present invention based on micro-fluidic chip, the detection The detailed process of method are as follows:
S1, the second peristaltic pump and the 4th valve are opened, cleaning solution is extracted into micro-fluidic chip, fill four micro- reactions Pond is then shut off the second peristaltic pump and the 4th valve, opens third peristaltic pump and the 6th valve, and cleaning solution is expelled to waste liquid and is received Acquisition means;
S2, the second peristaltic pump and the 4th valve are opened, cleaning solution is extracted into micro-fluidic chip, fill four micro- reactions The electrode in pond, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60-120s is then shut off Second peristaltic pump and the 4th valve, open third peristaltic pump and the 6th valve, and cleaning solution is expelled to waste collecting device;
S3, the first peristaltic pump and the first valve are opened, electrolyte is extracted into micro-fluidic chip, fill four micro- reactions Pond is then shut off the first peristaltic pump and the first valve, opens third peristaltic pump and the 6th valve, and electrolyte is expelled to waste liquid and is received Acquisition means;
S4, the first peristaltic pump and the first valve are opened, with flow velocity 1ml/min extract electrolyte, open the second peristaltic pump and 5th valve extracts ionized water with flow velocity 0.5ml/min, the mixed liquor of electrolyte and ionized water is extracted to micro-fluidic chip, Four micro reaction pools are filled, the electrode of four microsensors applies 0-0.45V voltage, and time of measuring 60-120s obtains background Electric current closes the first peristaltic pump, the first valve, the second peristaltic pump and the 5th valve, opens third peristaltic pump and the 6th valve, will Liquid is expelled to waste collecting device;
S5, the second peristaltic pump and the 4th valve are opened, cleaning solution is extracted into micro-fluidic chip, fill four micro- reactions The electrode in pond, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60-120s is then shut off Second peristaltic pump and the 4th valve, open third peristaltic pump and the 6th valve, and cleaning solution is expelled to waste collecting device;
S6, the first peristaltic pump and the first valve are opened, with flow velocity 1ml/min extract electrolyte, open the second peristaltic pump and Third valve is extracted the mixed liquor of electrolyte and standard water sample to micro-fluidic core with flow velocity 0.5ml/min draw standard water sample Piece fills four micro reaction pools, and the electrode of four microsensors applies 0-0.5V voltage, and time of measuring 60-120s is marked The response current of quasi- water sample closes the first peristaltic pump, the first valve, the second peristaltic pump and third valve, opens third peristaltic pump With the 6th valve, liquid is expelled to waste collecting device;
S7, the concentration for changing standard water sample, repeat S6, obtain the response current of the standard water sample of various concentration, root Standard curve is established according to the various concentration and corresponding standard water sample response current of water sample;
S8, the second peristaltic pump and the 4th valve are opened, cleaning solution is extracted into micro-fluidic chip, fill four micro- reactions The electrode in pond, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60-120s is then shut off Second peristaltic pump and the 4th valve, open third peristaltic pump and the 6th valve, and cleaning solution is expelled to waste collecting device;
S9, the first peristaltic pump and the first valve are opened, with flow velocity 1ml/min extract electrolyte, open the second peristaltic pump and Second valve extracts water sample to be measured with flow velocity 0.5ml/min, the mixed liquor of electrolyte and water sample to be measured is extracted to micro-fluidic core Piece, fills four micro reaction pools, and the electrode of four microsensors applies 0-0.5V voltage, time of measuring 60-120s, obtain to The response current of water sample is surveyed, the first peristaltic pump, the first valve, the second peristaltic pump and the second valve is closed, opens third peristaltic pump With the 6th valve, liquid is expelled to waste collecting device;
S10, it is compared according to the standard curve that the response current and S7 of water sample to be measured obtain, obtains the water quality ginseng of water sample to be measured Particle density value.
Advantages of the present invention: it is set in the micro-fluidic test chamber of water environment multi-parameter electrochemical detection device proposed by the present invention Four micro reaction pools have been set, four water quality parameters can be measured simultaneously, using microflow control technique there is test device small-sized Change, integrated, portability advantage.Also, detection cycle can be shortened using device measurement water quality, using less sample The quick precise measurement of water quality parameter can be realized with reaction reagent.
Detailed description of the invention
Fig. 1 is the structural representation of the water environment multi-parameter electrochemical detection device of the present invention based on micro-fluidic chip Figure;
Fig. 2 is the structural schematic diagram of device for storing liquid;
Fig. 3 is the structural schematic diagram of test chamber upper cover;
Fig. 4 is the top view of test chamber upper cover;
Fig. 5 is the structural schematic diagram of micro-fluidic chip.
Specific embodiment
Specific embodiment 1: illustrating present embodiment below with reference to Fig. 1, micro-fluidic chip is based on described in present embodiment Water environment multi-parameter electrochemical detection device, it includes device for storing liquid 1, valve controling circuit 2, peristaltic pump driving circuit 3, micro- Fluidic chip 4, potentiostatic circuit 5, signal acquisition circuit 6, microcontroller 7, waste collecting device 8 and display module 9;Liquid storage dress Setting in 1 includes five reagent bottles for storing different reagents, passes through pipeline phase between reagent bottle and the inlet of micro-fluidic chip 4 Even, it is provided with a valve on the pipeline of each connection reagent bottle, is provided with two on the pipeline between valve and micro-fluidic chip 4 A peristaltic pump, there are four micro reaction pools to detect four kinds of water quality parameters, potentiostatic circuit in detection process for setting in micro-fluidic chip 4 5 provide reference potential for the detecting electrode of micro-fluidic chip 4, and the detected data of micro-fluidic chip 4 are exported to signal acquisition Circuit 6, signal acquisition circuit 6 will test after data amplify filtering processing and be sent to microcontroller 7, and microcontroller 7 will be examined It is sent to display module 9 after measured data progress calculation process to be shown, the liquid outlet of micro-fluidic chip 4 is connected to by pipeline Waste collecting device 8 connects and is provided with a valve on the pipeline of the liquid outlet of micro-fluidic chip 4, and valve and waste collection fill It sets and is provided with peristaltic pump on the pipeline between 8, valve is driven by 2 control switch of valve controling circuit, peristaltic pump by peristaltic pump Dynamic 3 control switch of circuit, microcontroller 7 are that valve controling circuit 2 and peristaltic pump driving circuit 3 provide control signal.
In present embodiment, valve controling circuit 2 controls certain valve opening all the way by microcontroller 7 when work, by compacted Dynamic pump driving circuit 3 drives corresponding peristaltic pump, by the reagent aspiration in reagent bottle to micro-fluidic chip 4, after the reaction was completed, Waste liquid is expelled in waste collecting device 8 by driving valve and peristaltic pump.
Specific embodiment 2: illustrating that present embodiment, present embodiment make into one embodiment one below with reference to Fig. 2 Step explanation, five reagent bottles that the device for storing liquid 1 includes are respectively electrolyte storing reagent bottle 1-1, the storage examination of mark-on water sample Agent bottle 1-2, cleaning solution storing reagent bottle 1-3, water sample storing reagent bottle 1-4 to be measured and deionized water storing reagent bottle 1-5, electrolysis Liquid storing reagent bottle 1-1 is connected with the first valve 2-1, and mark-on water sample storing reagent bottle 1-2 is connected with the second valve 2-2, cleaning Liquid storing reagent bottle 1-3 is connected with third valve 2-3, and water sample storing reagent bottle 1-4 to be measured is connected with the 4th valve 2-4, go from Sub- water storing reagent bottle 1-5 is connected with the 5th valve 2-5.
Specific embodiment 3: illustrating that present embodiment, present embodiment make into one embodiment two below with reference to Fig. 1 Step explanation, the first valve 2-1 is connected with the first peristaltic pump 3-1, the second valve 2-2, third valve 2-3, the 4th valve 2-4 and the Five valve 2-5 are connected with the second peristaltic pump 3-2, the 6th valve 2-6 being arranged on liquid outlet 4-1-6 pipeline and third peristaltic pump 3-3 is connected.
Specific embodiment 4: illustrating present embodiment below with reference to Fig. 3, Fig. 4 and Fig. 5, present embodiment is to embodiment party Formula one, two or three is described further, and micro-fluidic chip 4 includes test chamber upper cover 4-1, the first microsensor 4-2, second micro- biography Sensor 4-3, third microsensor 4-4, the 4th microsensor 4-5 and substrate 4-6,
Be provided on test chamber upper cover 4-1 inlet 4-1-1, the first micro reaction pool 4-1-2, the second micro reaction pool 4-1-3, Third micro reaction pool 4-1-4, the 4th micro reaction pool 4-1-5, liquid outlet 4-1-6 and fluid channel 4-1-7, inlet 4-1-1 pass through Fluid channel 4-1-7 is connected to the first micro reaction pool 4-1-2, third micro reaction pool 4-1-4 and the 4th micro reaction pool 4-1-5, and the 4th is micro- Reaction tank 4-1-5 is connected to the second micro reaction pool 4-1-3 by fluid channel 4-1-7, and liquid outlet 4-1-6 is connected by fluid channel 4-1-7 Logical first micro reaction pool 4-1-2, third micro reaction pool 4-1-4 and the second micro reaction pool 4-1-3,
First microsensor 4-2, the second microsensor 4-3, third microsensor 4-4 and the 4th microsensor 4-5 difference Positioned at the first micro reaction pool 4-1-2, the second micro reaction pool 4-1-3, third micro reaction pool 4-1-4 and the 4th micro reaction pool 4-1-5 Lower section,
Test chamber upper cover 4-1 is bonded with substrate 4-6 and is integrated.
In present embodiment, test chamber upper cover 4-1 is made of PMMA, and substrate 4-6 is made up of silica or silicon.It is logical It crosses bonding techniques and is bonded test chamber upper cover 4-1 with substrate 4-6, guarantee that solution is contacted with the electrode of microsensor when detection, four A microsensor can be realized simultaneously the detection of four kinds of water quality parameters.
Specific embodiment 5: present embodiment is described further embodiment four, the first microsensor 4-2 attaches most importance to Concentration of metal ions detection sensor, the second microsensor 4-3 be pH value detection sensor, third microsensor 4-4 be ammonium from Sub- concentration detection sensor, the 4th microsensor 4-5 are temperature detection sensor.
Specific embodiment 6: present embodiment is described further embodiment five, temperature detection sensor is used Thermistor.
Specific embodiment 7: present embodiment is described further embodiment five, concentration of heavy metal ion detection Sensor, pH value detection sensor and ammonium concentration detection sensor are all made of three electrode measurement devices, and three electrodes are respectively Working electrode, to electrode and reference electrode.
In the present invention, when work, valve controling circuit 2 controls certain valve opening all the way by microcontroller 7, passes through peristaltic pump Driving circuit 3 drives corresponding peristaltic pump, and by the reagent aspiration in reagent bottle to micro-fluidic chip 4, peristaltic pump is adjustable stream Speed pump, flow velocity adjustable range are 0.5-20ml/min, flow velocity can be arranged according to actual test demand.
Specific embodiment 8: the water environment multi-parameter Electrochemical Detection described in present embodiment based on micro-fluidic chip fills The detection method set, the detailed process of the detection method are as follows:
S1, the second peristaltic pump 3-2 and the 4th valve 2-4 is opened, cleaning solution is extracted into micro-fluidic chip 4, fills four A micro reaction pool is then shut off the second peristaltic pump 3-2 and the 4th valve 2-4, opens third peristaltic pump 3-3 and the 6th valve 2-6, Cleaning solution is expelled to waste collecting device 8;
S2, the second peristaltic pump 3-2 and the 4th valve 2-4 is opened, cleaning solution is extracted into micro-fluidic chip 4, fills four The electrode of a micro reaction pool, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60-120s, It is then shut off the second peristaltic pump 3-2 and the 4th valve 2-4, third peristaltic pump 3-3 and the 6th valve 2-6 is opened, cleaning solution is arranged Out to waste collecting device 8;
S3, the first peristaltic pump 3-1 and the first valve 2-1 are opened, electrolyte is extracted into micro-fluidic chip 4, fills four A micro reaction pool is then shut off the first peristaltic pump 3-1 and the first valve 2-1, opens third peristaltic pump 3-3 and the 6th valve 2-6, Electrolyte is expelled to waste collecting device 8;
S4, the first peristaltic pump 3-1 and the first valve 2-1 are opened, electrolyte is extracted with flow velocity 1ml/min, it is compacted to open second Dynamic pump 3-2 and the 5th valve 2-5, extracts ionized water with flow velocity 0.5ml/min, by the mixed liquor of electrolyte and ionized water extract to Micro-fluidic chip 4, fills four micro reaction pools, and the electrode of four microsensors applies 0-0.45V voltage, time of measuring 60- 120s obtains background current, closes the first peristaltic pump 3-1, the first valve 2-1, the second peristaltic pump 3-2 and the 5th valve 2-5, opens Logical third peristaltic pump 3-3 and the 6th valve 2-6, is expelled to waste collecting device 8 for liquid;
S5, the second peristaltic pump 3-2 and the 4th valve 2-4 is opened, cleaning solution is extracted into micro-fluidic chip 4, fills four The electrode of a micro reaction pool, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60-120s, It is then shut off the second peristaltic pump 3-2 and the 4th valve 2-4, third peristaltic pump 3-3 and the 6th valve 2-6 is opened, cleaning solution is arranged Out to waste collecting device 8;
S6, the first peristaltic pump 3-1 and the first valve 2-1 are opened, electrolyte is extracted with flow velocity 1ml/min, it is compacted to open second Dynamic pump 3-2 and third valve 2-3 is taken out the mixed liquor of electrolyte and standard water sample with flow velocity 0.5ml/min draw standard water sample It takes to micro-fluidic chip 4, fills four micro reaction pools, the electrode of four microsensors applies 0-0.5V voltage, and time of measuring is 60-120s, obtains the response current of standard water sample, close the first peristaltic pump 3-1, the first valve 2-1, the second peristaltic pump 3-2 and Third valve 2-3, opens third peristaltic pump 3-3 and the 6th valve 2-6, and liquid is expelled to waste collecting device 8;
S7, the concentration for changing standard water sample, repeat S6, obtain the response current of the standard water sample of various concentration, root Standard curve is established according to the various concentration and corresponding standard water sample response current of water sample;
S8, the second peristaltic pump 3-2 and the 4th valve 2-4 is opened, cleaning solution is extracted into micro-fluidic chip 4, fills four The electrode of a micro reaction pool, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60-120s, It is then shut off the second peristaltic pump 3-2 and the 4th valve 2-4, third peristaltic pump 3-3 and the 6th valve 2-6 is opened, cleaning solution is arranged Out to waste collecting device 8;
S9, the first peristaltic pump 3-1 and the first valve 2-1 are opened, electrolyte is extracted with flow velocity 1ml/min, it is compacted to open second Dynamic pump 3-2 and the second valve 2-2, extracts water sample to be measured with flow velocity 0.5ml/min, the mixed liquor of electrolyte and water sample to be measured is taken out It takes to micro-fluidic chip 4, fills four micro reaction pools, the electrode of four microsensors applies 0-0.5V voltage, and time of measuring is 60-120s, obtains the response current of water sample to be measured, close the first peristaltic pump 3-1, the first valve 2-1, the second peristaltic pump 3-2 and Second valve 2-2, opens third peristaltic pump 3-3 and the 6th valve 2-6, and liquid is expelled to waste collecting device 8;
S10, it is compared according to the standard curve that the response current and S7 of water sample to be measured obtain, obtains the water quality ginseng of water sample to be measured Particle density value.

Claims (8)

1. the water environment multi-parameter electrochemical detection device based on micro-fluidic chip, which is characterized in that it includes device for storing liquid (1), valve controling circuit (2), peristaltic pump driving circuit (3), micro-fluidic chip (4), potentiostatic circuit (5), signal acquisition electricity Road (6), microcontroller (7), waste collecting device (8) and display module (9);It include that five storages are different in device for storing liquid (1) The reagent bottle of reagent is connected between reagent bottle and the inlet of micro-fluidic chip (4) by pipeline, the pipe of each connection reagent bottle A valve is provided on road, there are two peristaltic pump, micro-fluidic chips for setting on the pipeline between valve and micro-fluidic chip (4) (4) there are four micro reaction pools to detect four kinds of water quality parameters for setting in, and potentiostatic circuit (5) is micro-fluidic chip in detection process (4) detecting electrode provides reference potential, and micro-fluidic chip (4) detected data are exported to signal acquisition circuit (6), letter Number Acquisition Circuit (6) will test after data amplify filtering processing and be sent to microcontroller (7), and microcontroller (7) will test It is sent to display module (9) after data progress calculation process to be shown, the liquid outlet of micro-fluidic chip (4) passes through pipeline and connects To waste collecting device (8), connects and be provided with a valve, valve and waste liquid on the pipeline of the liquid outlet of micro-fluidic chip (4) Peristaltic pump is provided on pipeline between collection device (8), for valve by valve controling circuit (2) control switch, peristaltic pump is logical Peristaltic pump driving circuit (3) control switch is crossed, microcontroller (7) is that valve controling circuit (2) and peristaltic pump driving circuit (3) mention For controlling signal.
2. the water environment multi-parameter electrochemical detection device according to claim 1 based on micro-fluidic chip, feature exist In five reagent bottles that the device for storing liquid (1) includes are respectively electrolyte storing reagent bottle (1-1), the storage examination of mark-on water sample Agent bottle (1-2), cleaning solution storing reagent bottle (1-3), water sample storing reagent bottle (1-4) to be measured and deionized water storing reagent bottle (1-5), electrolyte storing reagent bottle (1-1) are connected with the first valve (2-1), mark-on water sample storing reagent bottle (1-2) and second Valve (2-2) is connected, and cleaning solution storing reagent bottle (1-3) is connected with third valve (2-3), water sample storing reagent bottle (1- to be measured 4) it is connected with the 4th valve (2-4), deionized water storing reagent bottle (1-5) is connected with the 5th valve (2-5).
3. the water environment multi-parameter electrochemical detection device according to claim 2 based on micro-fluidic chip, feature exist In the first valve (2-1) is connected with the first peristaltic pump (3-1), the second valve (2-2), third valve (2-3), the 4th valve (2- 4) it is connected with the second peristaltic pump (3-2) with the 5th valve (2-5), the 6th valve (2- being arranged on liquid outlet (4-1-6) pipeline 6) it is connected with third peristaltic pump (3-3).
4. the water environment multi-parameter electrochemical detection device according to claim 1,2 or 3 based on micro-fluidic chip, special Sign is, micro-fluidic chip (4) include test chamber upper cover (4-1), the first microsensor (4-2), the second microsensor (4-3), Third microsensor (4-4), the 4th microsensor (4-5) and substrate (4-6),
Inlet (4-1-1), the first micro reaction pool (4-1-2), the second micro reaction pool (4- are provided in test chamber upper cover (4-1) 1-3), third micro reaction pool (4-1-4), the 4th micro reaction pool (4-1-5), liquid outlet (4-1-6) and fluid channel (4-1-7), into Liquid mouth (4-1-1) is connected to the first micro reaction pool (4-1-2), third micro reaction pool (4-1-4) and the 4th by fluid channel (4-1-7) Micro reaction pool (4-1-5), the 4th micro reaction pool (4-1-5) are connected to the second micro reaction pool (4-1-3) by fluid channel (4-1-7), Liquid outlet (4-1-6) passes through fluid channel (4-1-7) connection the first micro reaction pool (4-1-2), third micro reaction pool (4-1-4) and the Two micro reaction pools (4-1-3),
First microsensor (4-2), the second microsensor (4-3), third microsensor (4-4) and the 4th microsensor (4-5) It is micro- anti-to be located at the first micro reaction pool (4-1-2), the second micro reaction pool (4-1-3), third micro reaction pool (4-1-4) and the 4th The lower section of Ying Chi (4-1-5),
Test chamber upper cover (4-1) is bonded with substrate (4-6) and is integrated.
5. the water environment multi-parameter electrochemical detection device according to claim 4 based on micro-fluidic chip, feature exist In the first microsensor (4-2) is concentration of heavy metal ion detection sensor, and the second microsensor (4-3) is that pH value detection passes Sensor, third microsensor (4-4) are ammonium concentration detection sensor, and the 4th microsensor (4-5) is temperature detection sensing Device.
6. the water environment multi-parameter electrochemical detection device according to claim 5 based on micro-fluidic chip, feature exist In temperature detection sensor uses thermistor.
7. the water environment multi-parameter electrochemical detection device according to claim 5 based on micro-fluidic chip, feature exist In concentration of heavy metal ion detection sensor, pH value detection sensor and ammonium concentration detection sensor are all made of three electrodes Measuring device, three electrodes are respectively working electrode, to electrode and reference electrode.
8. the detection method of the water environment multi-parameter electrochemical detection device based on micro-fluidic chip, which is characterized in that the detection The detailed process of method are as follows:
S1, the second peristaltic pump (3-2) and the 4th valve (2-4) are opened, cleaning solution is extracted into micro-fluidic chip (4), is filled Four micro reaction pools are then shut off the second peristaltic pump (3-2) and the 4th valve (2-4), open third peristaltic pump (3-3) and the 6th Cleaning solution is expelled to waste collecting device (8) by valve (2-6);
S2, the second peristaltic pump (3-2) and the 4th valve (2-4) are opened, cleaning solution is extracted into micro-fluidic chip (4), is filled The electrode of four micro reaction pools, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60- 120s is then shut off the second peristaltic pump (3-2) and the 4th valve (2-4), opens third peristaltic pump (3-3) and the 6th valve (2- 6) cleaning solution, is expelled to waste collecting device (8);
S3, the first peristaltic pump (3-1) and the first valve (2-1) are opened, electrolyte is extracted into micro-fluidic chip (4), is filled Four micro reaction pools are then shut off the first peristaltic pump (3-1) and the first valve (2-1), open third peristaltic pump (3-3) and the 6th Electrolyte is expelled to waste collecting device (8) by valve (2-6);
S4, the first peristaltic pump (3-1) and the first valve (2-1) are opened, electrolyte is extracted with flow velocity 1ml/min, it is compacted to open second Dynamic pump (3-2) and the 5th valve (2-5) extract ionized water with flow velocity 0.5ml/min, the mixed liquor of electrolyte and ionized water are taken out It takes to micro-fluidic chip (4), fills four micro reaction pools, the electrode of four microsensors applies 0-0.45V voltage, time of measuring For 60-120s, background current is obtained, closes the first peristaltic pump (3-1), the first valve (2-1), the second peristaltic pump (3-2) and the Five valves (2-5) open third peristaltic pump (3-3) and the 6th valve (2-6), and liquid is expelled to waste collecting device (8);
S5, the second peristaltic pump (3-2) and the 4th valve (2-4) are opened, cleaning solution is extracted into micro-fluidic chip (4), is filled The electrode of four micro reaction pools, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60- 120s is then shut off the second peristaltic pump (3-2) and the 4th valve (2-4), opens third peristaltic pump (3-3) and the 6th valve (2- 6) cleaning solution, is expelled to waste collecting device (8);
S6, the first peristaltic pump (3-1) and the first valve (2-1) are opened, electrolyte is extracted with flow velocity 1ml/min, it is compacted to open second Dynamic pump (3-2) and third valve (2-3), with flow velocity 0.5ml/min draw standard water sample, by the mixing of electrolyte and standard water sample Liquid is extracted to micro-fluidic chip (4), fills four micro reaction pools, and the electrode of four microsensors applies 0-0.5V voltage, measurement Time is 60-120s, obtains the response current of standard water sample, is closed the first peristaltic pump (3-1), the first valve (2-1), second compacted Dynamic pump (3-2) and third valve (2-3), open third peristaltic pump (3-3) and the 6th valve (2-6), liquid are expelled to waste liquid Collection device (8);
S7, the concentration for changing standard water sample, repeat S6, the response current of the standard water sample of various concentration are obtained, according to water The various concentration of sample and corresponding standard water sample response current establish standard curve;
S8, the second peristaltic pump (3-2) and the 4th valve (2-4) are opened, cleaning solution is extracted into micro-fluidic chip (4), is filled The electrode of four micro reaction pools, four microsensors applies 0-0.5V voltage, cleans to electrode, scavenging period 60- 120s is then shut off the second peristaltic pump (3-2) and the 4th valve (2-4), opens third peristaltic pump (3-3) and the 6th valve (2- 6) cleaning solution, is expelled to waste collecting device (8);
S9, the first peristaltic pump (3-1) and the first valve (2-1) are opened, electrolyte is extracted with flow velocity 1ml/min, it is compacted to open second Dynamic pump (3-2) and the second valve (2-2) extract water sample to be measured with flow velocity 0.5ml/min, by the mixing of electrolyte and water sample to be measured Liquid is extracted to micro-fluidic chip (4), fills four micro reaction pools, and the electrode of four microsensors applies 0-0.5V voltage, measurement Time is 60-120s, obtains the response current of water sample to be measured, is closed the first peristaltic pump (3-1), the first valve (2-1), second compacted Dynamic pump (3-2) and the second valve (2-2), open third peristaltic pump (3-3) and the 6th valve (2-6), liquid are expelled to waste liquid Collection device (8);
S10, it is compared according to the standard curve that the response current and S7 of water sample to be measured obtain, the water quality parameter for obtaining water sample to be measured is dense Angle value.
CN201910420014.1A 2019-05-20 2019-05-20 Water environment multi-parameter electrochemical detection device and its detection method based on micro-fluidic chip Pending CN110124761A (en)

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