CN106198700A - The thread three electrode sensing systems of data self-tolerant of detection submarine hydrothermal solution - Google Patents
The thread three electrode sensing systems of data self-tolerant of detection submarine hydrothermal solution Download PDFInfo
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Abstract
The invention discloses a kind of thread three electrode sensing systems of data self-tolerant detecting submarine hydrothermal solution, realize the concentration of metal ions abnormality detection in submarine hydrothermal solution plume, it is simultaneously introduced temperature sensing, complete different sensors data fusion and calibration, improve detection accuracy and the capacity of resisting disturbance of sensor in extreme environment.This sensing system is made up of the pressure cavity of titanium alloy and the data self-tolerant metal ion detection instrument being fixed in cavity, wherein metal ion detection instrument includes power module, analog module, digital circuit blocks and sensor, store with data with the detection automatically of completion system, realize, to seabed concentration of metal ions and the long term monitoring of temperature, for submarine hydrothermal solution detection, there is great reference value and application prospect.
Description
Technical field
The present invention relates to electrochemical sensor field, particularly relate to a kind of concentration of metal ions for sea bottom complex environment
Thread three electrode sensing systems with temperature anomaly long term monitoring.
Background technology
Submarine hydrothermal activity generally occurs at big midocean active plate border and intraplate volcanism center.Submarine hydrothermal solution
For the activity of human knowledge's earth depths, the exploration of submarine hydrothermal solution mineral products, extreme environment biological evolution mode and origin of life
Have great significance Deng the research of problem in science.Submarine hydrothermal solution is rich in various metals composition, and seabed concentration of metal ions is abnormal
Detect the discovery to submarine hydrothermal solution and sea floor hydrothermal polymetallic deposit to have great significance.
Seabed is special due to circumstance complication, and common metal ion detecting device is difficult to on-the-spot in situ detection, traditional
The mode of the sampling of first deep-sea, again test in laboratory, not only workload is greatly, time-consumingly for a long time, and technical difficulty is big, expends a large amount of manpower
Material resources.By contrast, stripping voltammetry passes through heavy metal ion preenrichment under constant potential, and working electrode table is greatly improved
The concentration of face heavy metal, with after-applied by bearing to positive scanning voltage, make the heavy metal of enrichment reoxidized for ionic state, passes through
Heavy metal characteristic of correspondence peak carries out quantitative analysis.Stripping voltammetry has the lowest Monitoring lower-cut, can detect multiple heavy simultaneously
Metal, the time of measuring is short, highly sensitive, simple to operate, can be as quick long term monitoring means.
Tradition large electrode size is relatively big, and structure does not have the material package such as toughness, and many employing politef, it is difficult to ensure that
Normal use under the environment under high pressure of seabed, micro-nano electrode is owing to using silicon base or substrate of glass, material brittle simultaneously, it is also difficult to
Complicated environments such as subsea uses.Thread metal electrode size is little, has metal toughness and intensity, adapts to seabed environment under high pressure
In.At present, there is not yet, about domestic and international researcher, thread three electrodes are used for the relevant of submarine hydrothermal solution concentration of metal ions detection
Report.
Along with the development of habitata demand, metal ion long-term in-situ monitoring in seabed is the most important.The present invention uses silk
Thread three combination of electrodes of the thread silver electrode of shape gold electrode, thread platinum electrode and plating silver chloride, introduce temperature sensing number
According to concentration of metal ions model calibration, it is simultaneously used for revising submarine hydrothermal solution forecast model, many to solve ocean bottom currents temperature etc.
The impact of the factor of kind, improves the capacity of resisting disturbance of submarine hydrothermal solution sensor.This pressure cavity of system titanium alloy includes polymer simultaneously
Lithium battery and serial flash, can meet seabed long term power source supply and the demand of data storage, at aspect tools such as deep-sea detectings
There is great application prospect.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of data self-tolerant detecting submarine hydrothermal solution
Thread three electrode sensing systems, the present invention may be used for the long term monitoring of seabed concentration of metal ions and temperature, reaches seabed heat
The application requirement of liquid detection.
It is an object of the invention to be achieved through the following technical solutions: a kind of data self-tolerant silk detecting submarine hydrothermal solution
Shape three electrode sensing system, this system is made up of the pressure cavity of titanium alloy and data self-tolerant metal ion detection instrument；Described
Metal ion detection instrument includes power module, analog module, digital circuit blocks and sensor；Described sensor includes
Thread gold electrode, thread platinum electrode, thread silver electrode and temperature sensor；Thread silver electrode passes through plating mode at electroplating surface
One layer of chlorination silverskin；It is pressure that described thread gold electrode, thread platinum electrode, thread silver electrode and temperature sensor are fixed on titanium alloy
The titanium alloy of cavity seals and covers, and one end is exposed to containment portion；Described power module, analog module and digital circuit mould
Block is fixed in the pressure cavity body of titanium alloy by copper post, and analog module is electric with thread gold respectively by coaxial shielding line
Pole, thread platinum electrode, thread silver electrode are connected with temperature sensor；Described digital circuit blocks and analog module are by electricity
Source line is connected with power module.Being stored by timing detection and testing result self-tolerant, native system may be used for heavy metal ion
Long-term detection.
Further, described thread gold electrode is as working electrode, and be diameter 0.5mm, the spun gold of long 10mm；Described silk
Shape platinum electrode is as to electrode, and be diameter 0.5mm, the platinum filament of long 10mm；Described thread silver electrode is as reference electrode, and is
Diameter 0.5mm, the filamentary silver of long 10mm.
Further, described analog module includes I/V translation circuit, filters, returns to zero and amplifying circuit, analog digital conversion
Circuit, operational amplifier, D/A converting circuit, temperature sensor modulate circuit and screened circuit of having chance with；Described digital circuit mould
Block includes microprocessor, real-time timepiece chip, storage chip and serial line interface；Described power module include poly-lithium battery and
Electric power management circuit；
Described analog module carries out LC in front end to the output signal of thread three electrodes and tentatively filters, and uses coaxial electrical
Cable transmits, and the screen layer to thread gold electrode and thread silver electrode uses active shielding circuit to improve shield effectiveness simultaneously；
Described D/A converting circuit, analog to digital conversion circuit, temperature sensor modulate circuit, real-time timepiece chip, storage chip and serial
Interface is all connected with micro-process；Microprocessor by real-time timepiece chip obtain real-time time, thus reach timing detect and to
The purpose that testing result adds timestamp；Microprocessor utilizes serial line interface and upper machine communication, receives instruction, or will store core
Testing result in sheet passes to host computer；The output of D/A converting circuit is connected to source screened circuit and operational amplifier
In-phase input end, be used for the bias required for have chance with screened circuit voltage and electrochemical reaction is provided；Thread silver electrode connects
The inverting input of operational amplifier, the outfan of operational amplifier connects thread platinum electrode；Thread gold electrode, I/V convert electricity
Road, filter, return to zero and amplifying circuit, analog to digital conversion circuit are sequentially connected with, by I/V translation circuit by faint electrochemical signals
(current signal) is converted into stronger voltage signal, the voltage signal simultaneously changed out after filtering, zeroing and amplifying circuit enter
After row signal condition, it is transferred to microprocessor through analog to digital conversion circuit；Described temperature sensor and temperature sensor modulate circuit
Connect, the resistance signal of temperature sensor by temperature sensor modulate circuit conditioning produce corresponding voltage signal, then by
Microprocessor internal AD conversion unit gathers.
Further, the signal condition process of described filtering, zeroing and amplifying circuit is particularly as follows: utilize four different one
Rank passive RC filter carries out low-pass filtering to voltage signal, the high-frequency noise that may introduce in removing circuit；Introduce zeroing
Circuit carries out pretreatment, DC-offset correction to the signal sending into analog to digital conversion circuit, makes full use of the amount of analog to digital conversion circuit
Journey；Signal carries out a homophase amplify, make full use of the range of analog to digital conversion circuit, it is achieved High Resolution is changed.
Further, this system utilizes the difference of feature oxidation-reduction potential of each heavy metal species to detect；First enter
Row voltage is enriched with: thread gold electrode, as working electrode, applies constant potential on thread gold electrode, and heavy metal ion is reduced
For atomic state, it is deposited on thread gold electrode surfaces；Next carries out being electrolysed dissolution: use Differential Pulse Stripping Voltammetry, i.e. at silk
On the basis of applying the dc sweeps voltage of linear change on shape gold electrode, the rectangular pulse current potential of the little amplitude of superposition, every time
Before superimposed pulse, before a certain sampling time and pulse termination, a certain sampling time gathers current signal, records the electric current of twice collection
Signal difference, obtains differential pulse Stripping Voltammetry curve；Differential Pulse Stripping Voltammetry substantially eliminates the shadow of background current
Ringing, make detection limit decline, sensitivity greatly improves.
The invention has the beneficial effects as follows, the present invention uses thread three electrodes and temperature sensor as detecting element, passes through
The data fusion of multiple sensors and calibration, improve accuracy and the capacity of resisting disturbance of the detection submarine hydrothermal solution of system.Design
Sensor-based system, for subsea use environment, uses high strength titanium alloy to make and seals pressure cavity, and by timing automatic detection
Store with testing result self-tolerant, it is achieved this system is long term monitoring concentration of heavy metal ion and temperature under sea bottom complex environment
Demand, provides data and model reference for submarine hydrothermal solution detection.
Accompanying drawing explanation
Fig. 1 is the structured flowchart of sensor-based system of the present invention；
Fig. 2 is the circuit structure diagram of data self-tolerant metal ion detection instrument of the present invention；
In figure, thread silver electrode 1, thread gold electrode 2, thread platinum electrode 3, temperature sensor 4, titanium alloy is pressure cavity 5,
Titanium alloy seal lid 6, digital circuit blocks 7, analog module 8, power module 9, I/V translation circuit 10, filter, return to zero and
Amplifying circuit 11, analog to digital conversion circuit 12, operational amplifier 13, D/A converting circuit 14, temperature sensor modulate circuit 15, have
Edge screened circuit 16, microprocessor 17, real-time timepiece chip 18, storage chip 19, serial line interface 20, poly-lithium battery 21,
Electric power management circuit 22.
Detailed description of the invention
With specific embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings.
As it is shown in figure 1, the present invention detects for submarine hydrothermal solution, sensor-based system is held certainly by the pressure cavity of titanium alloy 5 and data
Formula metal ion detection instrument forms；Described metal ion detection instrument includes power module 9, analog module 8, numeral electricity
Road module 7 and sensor；Described sensor includes thread gold electrode 2, thread platinum electrode 3, thread silver electrode 1 and temperature sensor
4；Thread silver electrode 1 passes through plating mode at one layer of chlorination silverskin of electroplating surface；Described thread gold electrode 2, thread platinum electrode 1,
Thread silver electrode 3 and temperature sensor 4 are fixed on the titanium alloy of the pressure cavity of titanium alloy 5 and seal on lid 6, and one end is exposed to cavity
Outside；Described power module 9, analog module 8 and digital circuit blocks 7 are fixed on the pressure cavity body of titanium alloy by copper post
In 5, analog module 8 by coaxial shielding line respectively with thread gold electrode 2, thread platinum electrode 1, thread silver electrode 3 and temperature
Degree sensor 4 is connected；Described digital circuit blocks 7 is connected with power module 9 by power line with analog module 8.
As in figure 2 it is shown, described analog module 8 includes I/V translation circuit 10, filter, return to zero and amplifying circuit 11, mould
Number conversion circuit 12, operational amplifier 13, D/A converting circuit 14, temperature sensor modulate circuit 15 and screened circuit of having chance with
16；Described digital circuit blocks 7 includes microprocessor 17, real-time timepiece chip 18, storage chip 19 and serial line interface 20；Described
Power module 9 includes poly-lithium battery 21 and electric power management circuit 22；Data self-tolerant metal ion detection instrument uses poly-
Compound lithium battery 21 is powered, and provides corresponding power supply by electric power management circuit 22 for modules.
Described analog module 8 carries out LC in front end to the output signal of thread three electrodes and tentatively filters, and uses coaxial
Cable transmits, and the screen layer to thread gold electrode 2 and thread silver electrode 1 uses active shielding circuit to improve shielding effect simultaneously
Really；The form of short-circuited conducting sleeve is also taken to improve signal to noise ratio for the signal lead on pcb board.
Described D/A converting circuit 14, analog to digital conversion circuit 12, temperature sensor modulate circuit 15, real-time timepiece chip
18, storage chip 19 and serial line interface 20 are all connected with micro-process 17；This system can use 16 super low-power consumptions, have and simplify finger
The mixed-signal processor MSP430F5438A of order collection is as micro-process 17, it is achieved the control to whole system detection process.Micro-
Processor 17 obtains real-time time by real-time timepiece chip 18, thus reaches what timing detected and added timestamp to testing result
Purpose；Microprocessor 17 utilizes serial line interface 20 and upper machine communication, receives instruction, or the detection in storage chip 19 is tied
Fruit passes to host computer；Real-time timepiece chip 18 uses DS1302, storage chip 19 to use high speed Flash chip
SST25VF032B, it is ensured that the application requirement of about 5000 testing result storages.
The output of D/A converting circuit 14 is connected to source screened circuit 16 and the in-phase input end of operational amplifier 13,
It is used for providing the bias required for have chance with screened circuit voltage 16 and electrochemical reaction；D/A converting circuit 14 uses TI company
DAC8831 chip, for 16 figure place weighted-voltage D/A converters of SPI interface.
The inverting input of thread silver electrode 1 concatenation operation amplifier 13, the outfan of operational amplifier 13 connects thread
Platinum electrode 3；Thread gold electrode 1, I/V translation circuit 10, filter, return to zero and amplifying circuit 11, analog to digital conversion circuit 12 connect successively
Connect, convert 10 circuit by I/V and faint electrochemical signals (current signal) is converted into stronger voltage signal, change simultaneously
The voltage signal gone out after filtering, zeroing and after amplifying circuit 11 carries out signal condition, be transferred to micro-through analog to digital conversion circuit 12
Processor 17；Analog to digital conversion circuit 12 uses the ADS8509 chip of TI company, and this chip is 16 250kHzCMOS analog digital conversion
Device, has SPI interface, is used for the electrochemical signals to producing and is acquired.Described filtering, zeroing and the signal of amplifying circuit 11
Conditioning process is particularly as follows: utilize four different single order passive RC filters that voltage signal is carried out low-pass filtering, removing circuit
In may introduce high-frequency noise；Introduce zeroing circuit and the signal sending into analog to digital conversion circuit is carried out pretreatment, eliminate straight
Stream biasing, makes full use of the range of analog to digital conversion circuit；Signal carries out a homophase amplify, make full use of analog to digital conversion circuit
The range of 12, it is achieved High Resolution is changed.
Described temperature sensor 4 is connected with temperature sensor modulate circuit 15, and the resistance signal of temperature sensor 4 is by temperature
Degree Conditioning Circuits of Sensor 15 conditioning produces corresponding voltage signal, is then adopted by the internal AD conversion unit of microprocessor 17
Collection.Recording temperature value while Voltammetric detection, carry out the data fusion of electrochemical signals and temperature signal, calibration is by environment temperature
The electrochemical signals of degree impact, can improve detection accuracy and the capacity of resisting disturbance of sensor in extreme environment.
Further, described thread gold electrode 2 is as working electrode, and be diameter 0.5mm, the spun gold of long 10mm；Described
Thread platinum electrode 3 is as to electrode, and be diameter 0.5mm, the platinum filament of long 10mm；Described thread silver electrode 1 as reference electrode,
And be diameter 0.5mm, the filamentary silver of long 10mm.
The Cleaning Principle of native system is as follows: this system utilizes the difference of the feature oxidation-reduction potential of each heavy metal species to carry out
Detection；First voltage enrichment is carried out: thread gold electrode 1, as working electrode, applies constant potential, weight on thread gold electrode 1
Metal ion is reduced to atomic state, is deposited on thread gold electrode 1 surface；Next carries out being electrolysed dissolution: use differential pulse molten
Go out voltammetry, on the basis of i.e. applying the dc sweeps voltage of linear change on thread gold electrode 1, the rectangle of the little amplitude of superposition
Pulse potential, before each superimposed pulse, before a certain sampling time and pulse termination, a certain sampling time gathers current signal, note
Record the current signal difference of twice collection, obtain differential pulse Stripping Voltammetry curve.Different heavy metals is specific by it
Oxidizing potential makes a distinction, and the amplitude of oxidation peak current is linear with sample heavy metal concentration, determining for heavy metal
Component analysis.
The workflow that the present invention is complete is: host computer sends detection instruction to microprocessor 17 by serial line interface 20,
Arrange including parameter, regularly detection etc..When real-time timepiece chip 18 arrives timing, microprocessor 17 controls instrument and starts
Concentration of heavy metal ion and temperature detection, and testing result is stored in storage chip 19.Host computer passes through serial line interface 20
Sending result to microprocessor 17 and read instruction, microprocessor 17 reads storage chip 19 accordingly result, and passes through serial line interface
20 return host computer.
Claims (5)
1. the thread three electrode sensing systems of data self-tolerant detecting submarine hydrothermal solution, it is characterised in that this system is closed by titanium
The pressure cavity of gold and data self-tolerant metal ion detection instrument composition；Described metal ion detection instrument include power module,
Analog module, digital circuit blocks and sensor；Described sensor includes thread gold electrode, thread platinum electrode, thread silver
Electrode and temperature sensor；Thread silver electrode passes through plating mode at one layer of chlorination silverskin of electroplating surface；Described thread gold electrode,
Thread platinum electrode, thread silver electrode and temperature sensor are fixed on the titanium alloy sealing of the pressure cavity of titanium alloy and cover, and one end is sudden and violent
It is exposed at containment portion；It is pressure that described power module, analog module and digital circuit blocks are fixed on titanium alloy by copper post
In cavity body, analog module by coaxial shielding line respectively with thread gold electrode, thread platinum electrode, thread silver electrode and temperature
Degree sensor is connected；Described digital circuit blocks is connected with power module by power line with analog module.
A kind of thread three electrode sensing systems of data self-tolerant detecting submarine hydrothermal solution the most according to claim 1, it is special
Levying and be, described thread gold electrode is as working electrode, and be diameter 0.5mm, the spun gold of long 10mm；Described thread platinum electrode is made
For to electrode, and be diameter 0.5mm, the platinum filament of long 10mm；Described thread silver electrode as reference electrode, and be diameter 0.5mm,
The filamentary silver of long 10mm.
Thread three electrodes of data self-tolerant of a kind of seabed concentration of metal ions the most according to claim 1 and temperature monitoring
Sensor-based system, it is characterised in that described analog module includes I/V translation circuit, filters, returns to zero and amplifying circuit, modulus
Change-over circuit, operational amplifier, D/A converting circuit, temperature sensor modulate circuit and screened circuit of having chance with；Described numeral electricity
Road module includes microprocessor, real-time timepiece chip, storage chip and serial line interface；Described power module includes polymer lithium electricity
Pond and electric power management circuit；
Described analog module carries out LC in front end to the output signal of thread three electrodes and tentatively filters, and uses coaxial wire
Transmitting, the screen layer to thread gold electrode and thread silver electrode uses active shielding circuit to improve shield effectiveness simultaneously；Described
D/A converting circuit, analog to digital conversion circuit, temperature sensor modulate circuit, real-time timepiece chip, storage chip and serial line interface
All it is connected with micro-process；Microprocessor obtains real-time time by real-time timepiece chip, thus reaches timing and detect and to detection
The purpose that result adds timestamp；Microprocessor utilizes serial line interface and upper machine communication, receives instruction, or by storage chip
Testing result pass to host computer；The output of D/A converting circuit is connected to the same of source screened circuit and operational amplifier
Phase input, is used for providing the bias required for have chance with screened circuit voltage and electrochemical reaction；Thread silver electrode concatenation operation
The inverting input of amplifier, the outfan of operational amplifier connects thread platinum electrode；Thread gold electrode, I/V translation circuit, filter
Ripple, zeroing and amplifying circuit, analog to digital conversion circuit are sequentially connected with, by I/V translation circuit by faint electrochemical signals (electric current
Signal) be converted into stronger voltage signal, the voltage signal simultaneously changed out after filtering, zeroing and amplifying circuit carry out signal
After conditioning, it is transferred to microprocessor through analog to digital conversion circuit；Described temperature sensor is connected with temperature sensor modulate circuit, temperature
The resistance signal of degree sensor produces corresponding voltage signal, then by microprocessor by the conditioning of temperature sensor modulate circuit
Internal AD conversion unit collection.
A kind of thread three electrode sensing systems of data self-tolerant detecting submarine hydrothermal solution the most according to claim 1, it is special
Levying and be, the signal condition process of described filtering, zeroing and amplifying circuit is particularly as follows: utilize four different single orders passive RC filters
Ripple device carries out low-pass filtering to voltage signal, the high-frequency noise that may introduce in removing circuit；Introduce zeroing circuit to feeding
The signal of analog to digital conversion circuit carries out pretreatment, DC-offset correction, makes full use of the range of analog to digital conversion circuit；Signal is entered
Homophase of row amplifies, and makes full use of the range of analog to digital conversion circuit, it is achieved High Resolution is changed.
A kind of thread three electrode sensing systems of data self-tolerant detecting submarine hydrothermal solution the most according to claim 1, it is special
Levying and be, this system utilizes the difference of the feature oxidation-reduction potential of each heavy metal species to detect；First voltage enrichment is carried out:
Thread gold electrode, as working electrode, applies constant potential on thread gold electrode, and heavy metal ion is reduced to atomic state, heavy
Amass in thread gold electrode surfaces；Next carries out being electrolysed dissolution: uses Differential Pulse Stripping Voltammetry, i.e. executes on thread gold electrode
On the basis of adding the dc sweeps voltage of linear change, the rectangular pulse current potential of the little amplitude of superposition, before each superimposed pulse certain
Before one sampling time and pulse termination, a certain sampling time gathers current signal, records the current signal difference of twice collection,
To differential pulse Stripping Voltammetry curve.
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| Publication number | Publication date |
|---|---|
| CN106198700B (en) | 2018-09-28 |
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