CN109596679A - A kind of detection device of field quick detection heavy metal content in soil - Google Patents
A kind of detection device of field quick detection heavy metal content in soil Download PDFInfo
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- CN109596679A CN109596679A CN201811478017.2A CN201811478017A CN109596679A CN 109596679 A CN109596679 A CN 109596679A CN 201811478017 A CN201811478017 A CN 201811478017A CN 109596679 A CN109596679 A CN 109596679A
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
Abstract
The present invention provides a kind of and entirely different field quick detection heavy metal content in soil of prior art principle detection devices, detection device includes: sensor, programmable signal generator, current sampler, voltage sample device, instrumentation amplifier, A/D converter, interface circuit, MCU, input equipment, temperature control modules, power module；The sensor is also built-in with electric heater and thermocouple；When detecting, the soil pattern collected is filled in sensor.The shape of the Cp-f curve of the soil pattern obtained by measurement, Tan (Delta)-f curve, can be finally inversed by heavy metal content in soil.
Description
Technical field
The present invention relates to a kind of detection devices of field quick detection heavy metal content in soil.
Background technique
Heavy metal pollution of soil refers to due to natural or heavy metal is brought into soil by mankind's activity, causes soil
Content of beary metal is apparently higher than background value and causes existing or potential assessing index, Environmental deterioration in earth
The phenomenon that.Heavy metal-polluted soil is from a wealth of sources, mainly includes the improper heap of atmospheric falling dust, sewage irrigation, industrial solid castoff
It sets, mining activities, pesticide and chemical fertilizer etc..All materials using heavy metal and containing heavy metal are being produced as the industry of raw materials for production
Heavy metal may be discharged in the process, if mishandling, will result in environmental pollution.
Heavy metal pollution in soil seriously endangers human health.The heavy metals such as lead, cadmium, mercury, arsenic, due to industrial activity
Development, causes the enrichment in mankind's ambient enviroment, enters human body by big gas and water, food etc., in the certain organ inner products of human body
It is tired, slow poisoning is caused, is detrimental to health.
During prevention, monitoring, administering heavy metal pollution of soil, detection heavy metal content in soil is one extremely important
Link.The quantitative detecting analysis technology of heavy metal usually has: it is ultraviolet can spectrophotometry (UV), atomic absorption method (AAS), former
Sub- fluorescence method (AFS), inductively coupled plasma body method (ICP), X fluorescence spectrum (XRF), Inductively coupled plasma-mass spectrometry
(ICP-MS).In addition to the above methods, there are also spectroscopic methodology detections.Also some is analyzed using X fluorescence spectrum (XRF).
Atomic absorption spectrography (AAS) be the 1950s found a kind of new instrument analysis method, it and be mainly used for nothing
The atomic emission spectrometry of machine qualitative elementary analysis complements each other, it has also become the master of quantitative elementary analysis is carried out to inorganic compound
Want means.
Atomic absorption analysis process is as follows: solution (while doing blank) is made in sample；Prepare a series of known concentrations
The calibration solution (standard specimen) of analytical element；Successively measure the analog value of blank and standard specimen；It is bent that correction is drawn according to above-mentioned analog value
Line；Measure the analog value of unknown sample；Analog value according to calibration curve and unknown sample obtains the concentration value of sample.
Ultraviolet-visible spectrophotometry (UV) testing principle is: heavy metal is usually organic compound with color developing agent one, can
Complex reaction occurs in heavy metal, generates coloured molecule group, the solution colour depth is directly proportional to concentration.At a particular wavelength, than
Color detection.There are two types of spectrophotometric analyses, and one is be measured using substance itself to ultraviolet and visible light absorption；It is another
Kind is to generate colored compound, i.e., " develops the color ", then measure.
Atomic fluorescence spectrometry (AFS) is by measuring the atomic vapour of element to be measured below specific frequency radiation energy swashs
Generated fluorescent emission intensity, with this come the method that measures constituent content to be measured.Atomic fluorescence spectrometry is a kind of transmitting light
Spectrometry, but it is closely related with atomic absorption spectrography (AAS), the advantages of having two kinds of analysis methods of atomic emissions and Atomic absorption concurrently.
Electrochemical process is to rely on classical direct current polarography, derives oscillographic polarography, anodic stripping voltammetry again on this basis
The methods of.Anodic stripping voltammetry is that potentiostatic deposition is enriched with a kind of electrochemical analysis side combined with voltammetric determination
Method.Anodic Stripping Voltammetry Determination is in two steps.The first step is " electrolysis ", i.e., under a constant potential, by tested ion-conductance
Solution deposition, enrichment generate amalgam with mercury on electrode on the working electrode (s.Second step is " dissolution ", i.e., after enrichment, generally
After static 30s or 60s, applies a backward voltage on the working electrode (s, just scanned by negative sense, metal in amalgam is reoxidized
It is returned in solution for ion, generates oxidation current, recording voltage-current curve, i.e. volt-ampere curve.Curve is in peak shape, peak value electricity
Flow to be tested in solution from concentration it is directly proportional, can be used as the foundation of quantitative analysis, spike potential can be used as qualitative analysis
Foundation.
X ray fluorescence spectrometry (XRF) be using sample to the absorption of X-ray in sample ingredient and its how many variations
And change to qualitatively or quantitatively determine a kind of method of ingredient in sample.When sample is by x-ray, energetic particle beam, ultraviolet light
When Deng irradiating, due to high energy particle or photon and sample atomic collision, atom inner electron being evicted to form hole, is made at atom
In excitation state, this excited state ion service life is very short, and when outer-shell electron inner layer hole transition, extra energy is penetrated with x
The form of line is released, and is generated new hole in religion outer layer and generated new x-ray emission, just generates a series of feature in this way
X-ray.Signature x-ray is that various elements are intrinsic, it is related with the atomic of element.As long as being penetrated so having measured feature x
The wavelength X of line, so that it may find out the element for generating the wavelength.
Inductively coupled plasma mass spectrometry (ICP-MS) is by as ion source ICP torch, interface arrangement and as detection
The mass spectrograph three parts of device form.Ionization source used in ICP-MS is inductively coupled plasma (ICP), and main body is one by three
The torch pipe of layer quartz socket tube composition, torch pipe upper end are wound with loading coil, and three-layer pipe leads to carrier gas respectively from the inside to surface, assist gas and cold
But gas, loading coil are coupled by high frequency electric source and are powered, and generate the magnetic field perpendicular to coil plane.If making argon by high-frequency device
Pneumoelectric from, then argon ion and electronics can collide again with other ar atmos under electromagnetic field effect and generate more ions and electronics,
Form vortex.Powerful electric current generates high temperature, and moment makes argon gas formation temperature up to the plasma torch of 10000k.Analyzed sample
Product are usually introduced into argon gas stream with the aerosol form of aqueous solution, are under atmospheric pressure subsequently into what is excited by RF energy
Argon plasma center, the high temperature of plasma make sample desolvation, vaporization dissociation and ionization.Part plasma passes through
Different pressure areas enter vacuum system, and in vacuum system, cation is drawn out and separates according to its mass-to-charge ratio.
In these above-mentioned detection methods, used instrument and equipment is all more accurate, expensive, and volume is larger, and need to be
It is fixed after the installation and debugging of laboratory to use, it can not go out to carry use, when detecting heavy metal content in soil, require existing
After quarry sampling, pretreatment and dystopy detection and analysis that laboratory carries out later period complexity are delivered, it is not only time-consuming but also inconvenient, it is impossible to be used in
Field quick detection.
Need quickly detection, analysis heavy metal pollution of soil situation when, be badly in need of it is a kind of can be used in on-site test, side
Portable belt, inexpensive detecting instrument and detection method.
Summary of the invention
It is of the existing technology in order to solve the problems, such as, the purpose of the present invention is to provide it is a kind of completely new, be totally different from
The detecting instrument and measurement method of the heavy metal content in soil of the prior art.
Realizing the specific technical solution of the object of the invention is:
A kind of detection device of field quick detection heavy metal content in soil, comprising:
Sensor, programmable signal generator, current sampler, voltage sample device, instrumentation amplifier I, instrumentation amplifier
V, A/D converter I (i.e. ADC-I), A/D converter V (i.e. ADC-V), interface circuit, MCU (micro-control unit,
MicroController Unit；MCU, also known as one chip microcomputer), input equipment, temperature control modules, power supply mould
Block；The sensor is also built-in with electric heater and thermocouple；When detecting, the soil examination collected is filled in sensor
Sample；
The input equipment is electrically connected to MCU, and the controlled input end of programmable signal generator is electrically connected to MCU,
The signal output end of programmable signal generator is electrically connected to sensor, current sampler, voltage sample device respectively with sensing
Device is electrically connected, and the signal input part of current sampler and instrumentation amplifier I are electrically connected, voltage sample device and instrumentation amplifier
The signal input part of V is electrically connected, and the signal output end of instrumentation amplifier I is electrically connected to A/D converter I's (i.e. ADC-I)
Input end of analog signal, the signal output end of instrumentation amplifier V are electrically connected to the analog signal of A/D converter V (i.e. ADC-V)
Input terminal, the digital signal output end of A/D converter I and the digital signal output end of A/D converter V pass through interface circuit electricity
Property is connected to MCU；
Current sampler is usually made of the small resistance of one and sensor series；Voltage sample device is usually taken out by a band
The big resistance composition with sensor parallel of head；Wherein, the resistance value of the small resistance is less than the resistance of soil pattern significantly
Value, the resistance value of the big resistance are greater than the resistance value of soil pattern significantly；The resistance value of the small resistance and big resistance by
Depending on the accuracy of measurement；
The sensor includes the metal plate of a pair of parallel disc-shaped, is respectively connected with ac signal per a piece of metal plate
Input terminal, for being connected to the signal output end of programmable signal generator；Electric heating is also equipped with inside per a piece of metal plate
Device and thermocouple, i.e., the described sensor is built-in, and there are two electric heater and two thermocouples；Electric heater and thermocouple are by drawing
Line extends outside metal plate, and electric heater and lead are electrically insulated with metal plate, i.e., electric heater and lead are equipped with insulation
Casing；Electric heater and thermocouple are connected to temperature control modules by lead, so that the temperature of soil pattern is protected when detecting
It holds by the preset temperature value of MCU；
Input equipment is used to input preset measurement parameter and detection instruction to MCU；
Programmable signal generator can receive the instruction that MCU is issued, according to the instruction that MCU is issued generate frequency and amplitude by
The preset ac signal of MCU；When detecting, presetting the ac signal generated is that t variation, amplitude are kept frequency f at any time
Constant ac signal；
Programmable signal generator exports the ac signal to sensor, detects to soil pattern；
When detecting, MCU is also issued to temperature controller and is instructed, and the electric heater built in sensor is made to work, and controls institute
The temperature value for stating sensor maintains preset value；
It exports after current sampler to instrumentation amplifier I and amplifies by the ac current signal of sensor, then
Amplified analog signal is converted into digital signal by A/D converter I, obtains the number of the ac current signal by sensor
Word value；The ac voltage signal at sensor both ends is exported to instrumentation amplifier V after voltage sample device and is amplified, then by A/
Amplified analog signal is converted to digital signal by D converter V, obtains the number of the ac voltage signal at sensor both ends
Value；Digital value, the digital value of the ac voltage signal at sensor both ends of the ac current signal by sensor pass through
Interface circuit is transmitted to MCU in real time, is stored in real time by MCU, and MCU is also according to the ac current signal and biography by sensor
Amplitude, the phase calculation of both ac voltage signals at sensor both ends obtain the apparent capacity real part Cp, apparent of soil pattern
Capacitor imaginary part Cp ', loss tangent Tan (Delta), while calculated result being stored in real time；
When detecting the content of beary metal of soil pattern, by the apparent capacity real part-of the MCU soil pattern that will test
Frequency curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (Delta)-f curve make normalized, to process
Normalized curve carries out the identification of curvilinear characteristic degree, then in MCU in song in the Standard Curve Database that prestores in the memory that sets
Line makees Auto-matching operation, and the numerical value in reference standard curve library obtains the content of beary metal of soil pattern collected, described
Standard Curve Database record has the process normalizing of multiple pre- standard soil samples for first passing through content of beary metal that measurement obtains, different
Apparent capacity real part-frequency curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (the Delta)-f for changing processing are bent
Line.
Each curve in Standard Curve Database, in routine work: use is ultraviolet can spectrophotometry (UV), atom
Absorption process (AAS), atomic fluorescence method (AFS), inductively coupled plasma body method (ICP), X fluorescence spectrum (XRF), inductive coupling etc.
When any method of ion mass spectrometry (ICP-MS) detects heavy metal in soil content, while being surveyed using technical solution of the present invention
Measure apparent capacity real part-frequency curve i.e. Cp-f curve, the loss tangent-frequency curve i.e. Tan of the soil pattern
(Delta)-f curve, Cp-f curve, Tan (Delta)-f curve and the corresponding heavy metal of the soil pattern that measurement is obtained
Type, content are recorded into Standard Curve Database.
Preferably, the sensor includes a pair of of parallel metal sheet, and a pair of of parallel metal sheet is thin discs shape；
Preferably, the size of the thin discs shape metal plate is Centimeter Level, with a thickness of grade；
Preferably, input equipment includes keyboard, button, touch screen etc.；
Two electric heaters can be electrically connected in series to temperature control modules, can also be electrically connected to temperature control in parallel
Molding block；
Micro-control unit (MicroController Unit；MCU), also known as one chip microcomputer (Single Chip
It Microcomputer) or single-chip microcontroller, is central processing unit (Central Process Unit；CPU frequency and specification)
Do appropriate reduction, and by the perimeter interfaces such as memory (memory), counter (Timer), USB, A/D conversion, UART, PLC, DMA,
Even LCD driving circuit all integrates the computer for forming chip-scale on a single chip, does different groups for different applications
Close control.
Measuring principle of the invention is described below:
Solid dielectric is in the effect by external electrical field, it may occur that electric polarization effect is not overlapped with positive and negative charge centroid
Electric polarization mode show electricity role and influence；Wherein play a major role be bound charge (in solid matter just
Anion, the electron outside nucleus fettered by atomic nucleus).Electrode law of bound charge under the action of electric field inside solid dielectric
There are substantial connections with medium microstructure.
There are three electropolarized basic processes: the 1. distortion polarization of extranuclear electron cloud；2. positive and negative ion in molecule
(opposite) displacement polarization；3. the steering of the intrinsic electric moment of molecule polarizes.Under extraneous electric field action, the permittivity ε of medium is comprehensive
Close the macroscopic physical quantity that ground reflects these three microprocess；It is the function of ε (f) of frequency f.
When just thinking that frequency is zero or frequency very low (such as 200Hz), three kinds of microprocess are involved in effect, dielectric at this moment
Constant ε (0) is constant for certain dielectric, is commonly referred to as dielectric constant, this namely static permittivity ε s or
Low-frequency dielectric constant.With the increase of frequency, the steering polarization of the intrinsic electric moment of molecule gradually lags behind the variation in outfield, at this moment,
Dielectric constant takes plural form ε (ω)=ε ' (f)-j ε " (f), and wherein imaginary part ε " (ω) represents dielectric loss；Although (dielectric
Capacitor changing with frequency, " dielectric constant " be not be a constant, but usually still use that " dielectric is normal in this field
Count " this term)；It is since electric polarization course is not followed caused by the variation in outfield.Real part with frequency increase
And be remarkably decreased, there is peak value in imaginary part.Frequency is further added by, and real part ε ' (f) is down to new value, and (f) becomes zero imaginary part ε ", this indicates to divide
The steering polarization of sub intrinsic electric moment cannot respond.When frequency enters infrared region, the vibration of positive and negative ion electric moment in molecule
When frequency and outfield are resonated, real part ε ' (f) first increase suddenly suddenly declines, ε that " (f) peak value occurs again immediately；Cross this with
Afterwards, the displacement polarization of positive and negative ion no longer works.
It is always defective in solid state medium for hard-packed solid state medium, under the action of an external electric field, charged defects
As soon as jumping to another equilbrium position or ion in certain local from equilbrium position to vibrate back and forth, effect phase
When in the steering of electric moment.Some solids with strong ionic (key), their static permittivity ε s are always bigger than the numerical value of n2
Much, outside the contribution of deionization displacement polarization, difference is exactly caused by the jump of charged defects under the action of an external electric field.
Study dielectric constant with frequency variation i.e. research dielectric constant frequency dispersion (dispersion) relationship, research dielectric loss,
Absorption of Medium and dielectric relaxation, rotation, ion for the structure of analyzing molecules and solid, the property of chemical bond and molecule
Vibration etc. it is clearly highly important.
For the solid dielectric of existing defects (especially foreign ion), under the action of an external electric field, not only exist
Electric polarization course, there is also conductance processes, show macroscopic view conduction current effect.
For the soil pattern by heavy metal pollution, since the quality of heavy metal ion is greater than other elements significantly
Ions/atoms, frequency response process of the ion of different quality in alternating electric field is there is apparent difference, in alternation electricity
During the frequency of field gradually rises, heavy metal ion becomes increasingly difficult to keep up with first the steering of applied alternating field, matter
It is such to measure bigger ion；And since heavy metal ion exists in the form of foreign ion in soil pattern, so that native
Earth sample, there is also being lost as caused by conduction electric current, shows electricresistance effect, soil pattern institute when by extra electric field
Impure ion is more, and leakage current is bigger, in test, shows as apparent capacity imaginary part Cp ', loss tangent Tan
(Delta) increase.
In the soil pattern by heavy metal pollution, type, the content of heavy metal significantly affect apparent capacity reality
Portion-frequency curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (Delta)-f curve shape, curve shape
Distortion degree, distortion occur position, embody the weight of the substance of heterogeneity in soil.
By the apparent capacity real part-frequency curve i.e. Cp-f curve, loss angle tangent for the soil pattern that experiment measurement obtains
Value-frequency curve, that is, Tan (Delta)-f curve shape, can be finally inversed by heavy metal content in soil.In inverting, soil weight
The order of accuarcy of tenor depends on the sample-rich degree of established Standard Curve Database.
The content that this specification is not described in detail belongs to the prior art well known to professional and technical personnel in the field.
Beneficial effects of the present invention:
Using technical solution of the present invention, compared with the existing technology, have the advantages that following significant:
Since detecting instrument can be made small in size, Portable belt, and test device there is no it is such as ultraviolet can spectrophotometric
Method (UV), atomic absorption method (AAS), atomic fluorescence method (AFS), inductively coupled plasma body method (ICP), X fluorescence spectrum
(XRF), accurate, the enervated component in Inductively coupled plasma-mass spectrometry (ICP-MS), is quite suitable for field condition and quickly examines
It surveys.
Due to taking to the normalized processing of test data, so that in front in step, without substituting into parallel metal sheet
Area, spacing come the dielectric constant that converts, also, even if when soil sample compresses between parallel metal sheet, no matter soil sample
The whether really completely dense space filled up between parallel metal sheet, even if apparent capacity can be brought there are some perforations, missing
The measured deviation of real part Cp, apparent capacity imaginary part Cp ', but after normalized, these influence all disappear, in subsequent number
According in processing, without considering the absolute size of these measured values, but the shape for the curve that measurement obtains need to be only considered.This point
Bring the convenience of measurement.
And it is ultraviolet can spectrophotometry (UV), atomic absorption method (AAS), atomic fluorescence method (AFS), inductive coupling etc. from
Daughter method (ICP), X fluorescence spectrum (XRF), in Inductively coupled plasma-mass spectrometry (ICP-MS) measuring technique, none is not needed
Accurate, careful pre-treatment work is carried out to sample, is also had in measurement work meticulous.
It quickly being detected in addition, being suitable for field condition just because of technical solution of the present invention, operation very simple is convenient,
So that monitoring efficiency greatly improves in efforts at environmental protection.
Detailed description of the invention
Fig. 1: the structure chart of the detection device of field quick detection heavy metal content in soil of the invention.
Fig. 2: the sensor in detection device of the invention, dotted line indicates two electric heaters built in sensor in figure.
The insulating sleeve that electric heater and lead are equipped with is not drawn into figure, temperature sensor is also not drawn into.
Fig. 3: the structure chart of the power module in detection device of the invention.
Fig. 4: the AT89C51 single chip computer architecture figure that programmable signal generator uses in one embodiment of the present of invention.
Specific embodiment
It is of the invention for ease of understanding, come specifically to introduce technical solution of the present invention below with reference to example.
As shown in Figure 1, a kind of detection device of field quick detection heavy metal content in soil, comprising:
Sensor, programmable signal generator, current sampler, voltage sample device, instrumentation amplifier I, instrumentation amplifier
V, A/D converter I (i.e. ADC-I), A/D converter V (i.e. ADC-V), interface circuit, MCU (micro-control unit,
MicroControHer Unit；MCU, also known as one chip microcomputer), input equipment, temperature control modules, power module；
The sensor is also built-in with electric heater；When detecting, the soil pattern collected is filled in sensor；
The input equipment is electrically connected to MCU, and the controlled input end of programmable signal generator is electrically connected to MCU,
The signal output end of programmable signal generator is electrically connected to sensor, current sampler, voltage sample device respectively with sensing
Device is electrically connected, and the signal input part of current sampler and instrumentation amplifier I are electrically connected, voltage sample device and instrumentation amplifier
The signal input part of V is electrically connected, and the signal output end of instrumentation amplifier I is electrically connected to A/D converter I's (i.e. ADC-I)
Input end of analog signal, the signal output end of instrumentation amplifier V are electrically connected to the analog signal of A/D converter V (i.e. ADC-V)
Input terminal, the digital signal output end of A/D converter I and the digital signal output end of A/D converter V pass through interface circuit electricity
Property is connected to MCU；
Input equipment is used to input preset measurement parameter and detection instruction to MCU；
Programmable signal generator can receive the instruction that MCU is issued, according to the instruction that MCU is issued generate frequency and amplitude by
The preset ac signal of MCU；When detecting, presetting the ac signal generated is that t variation, amplitude are kept frequency f at any time
Constant ac signal；
Programmable signal generator exports the ac signal to sensor, detects to soil pattern；
When detecting, MCU is also issued to temperature controller and is instructed, and the electric heater built in sensor is made to work, and controls institute
The temperature value for stating sensor maintains preset value；
It exports after current sampler to instrumentation amplifier I and amplifies by the ac current signal of sensor, then
Amplified analog signal is converted into digital signal by A/D converter I, obtains the number of the ac current signal by sensor
Word value；The ac voltage signal at sensor both ends is exported to instrumentation amplifier V after voltage sample device and is amplified, then by A/
Amplified analog signal is converted to digital signal by D converter V, obtains the number of the ac voltage signal at sensor both ends
Value；Digital value, the digital value of the ac voltage signal at sensor both ends of the ac current signal by sensor pass through
Interface circuit is transmitted to MCU in real time, is stored in real time by MCU, and MCU is also according to the ac current signal and biography by sensor
Amplitude, the phase calculation of both ac voltage signals at sensor both ends obtain the apparent capacity real part Cp, apparent of soil pattern
Capacitor imaginary part Cp ', loss tangent Tan (Delta), while calculated result being stored in real time；
When detecting the content of beary metal of soil pattern, by the apparent capacity real part-of the MCU soil pattern that will test
Frequency curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (Delta)-f curve make normalized, to process
Normalized curve carries out the identification of curvilinear characteristic degree, then in MCU in song in the Standard Curve Database that prestores in the memory that sets
Line makees Auto-matching operation, and the numerical value in reference standard curve library obtains the content of beary metal of soil pattern collected, described
Standard Curve Database record has the process normalizing of multiple pre- standard soil samples for first passing through content of beary metal that measurement obtains, different
Apparent capacity real part-frequency curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (the Delta)-f for changing processing are bent
Line.
As shown in Fig. 2, the sensor includes the metal plate of a pair of parallel disc-shaped, it is respectively connected with per a piece of metal plate
Ac signal input terminal, respectively AC1 and AC2, for being connected to the signal output end of programmable signal generator；Per a piece of
Electric heater is also equipped with inside metal plate, i.e., the described sensor is built-in, and there are two electric heaters；Electric heater is prolonged by lead
It stretches out outside metal plate, electric heater and lead are electrically insulated with metal plate, i.e. electric heater and lead is equipped with insulating sleeve；
Electric heater is connected to temperature control modules by lead, so that the temperature of soil pattern is maintained at is preset by MCU when detecting
Temperature value；Described two electric heaters are respectively provided with lead end Heater1 and Heater1-1, Heater2 and Heater2-2,
Lead end Heater1-1 and Heater2-2 are electrically connected, and the conducting wire between Heater1-1 and Heater2-2 is using pine
Soft conducting wire, Heater1 and Heater2 are for being electrically connected to temperature controller.
In the connection type, two electric heaters are series system cut-in temperature controller.
As shown in figure 3, power module includes AC-DC converting unit, DC-DC converting unit, isolating transformer, rectification
Device, filter.This power module has effectively achieved the electric isolution between detection device and mains circuit, improves safety
Property.AC-DC converting unit generallys use full-bridge rectifier.
When using above-mentioned detection device to detect heavy metal content in soil, step approximately as:
Collection in worksite soil pattern；In acquisition, dead twigs and withered leaves, macroscopic gravel particle are removed；Soil pattern
Sampling quantity is several grams to ten grams, in this way, both measurement error will not be caused big because sample size is very little in measurement, it will not
Cause the electric energy of overlong time spent by heating, drying, consuming excessive because sample size is too big.Normally, to several grams to ten
Gram soil pattern amount for, in the state of compression carry out heating, drying to constant weight, generally require 3-5 minutes；
The soil pattern collected is pulverized, a pair that the soil pattern pulverized is placed directly in sensor is parallel
Apply pressure compaction between metal plate, scrapes off the redundance leaked out outside parallel metal sheet with scraping blade, be made and parallel metal sheet
Shape is identical, equal-sized laminar sample；
MCU issues heating instructions to temperature controller, and heating baking is carried out in the state of compression to the soil pattern of compacting
It does to constant weight；By soil pattern, drying to constant weight, is that the moisture in order to avoid containing in sample brings subsequent electrical measurement
Large error.The temperature of heating, drying is carried out in the state of compression between 110 DEG C -120 DEG C to the soil pattern of compacting.
Sweep check: at a constant temperature, using programmable signal generator on a pair of of parallel metal sheet of sensor
Apply the continually changing alternate electrical signal vt of a frequency to act on the soil pattern of drying, the output in the alternating signal source is handed over
The frequency f of varying electrical signals vt at any time t and change, signal amplitude then remains unchanged；Programmable signal generator is issued by MCU
Instruction controlled；In an example, the output alternate electrical signal v of programmable signal generatortFrequency f every 200ms
Variation is primary, and frequency increases from 100Hz, and 1.1 times are differed between every two frequency, until increasing to 1MHz or so, specific frequency
It is listed as follows:
100Hz, 110Hz, 121Hz, 133.1Hz ..., 777.88KHz, 855.67KHz, 941.23KHz, 1.035MHz,
98 Frequency points in total, 98 Frequency point tests are completed, and need time 49s in total.
Real-time detection simultaneously records the electrical parameter that the alternate electrical signal passes through above-mentioned a pair of of parallel metal sheet and soil pattern,
The electrical parameter includes the apparent capacity real part Cp of alternate electrical signal, apparent capacity imaginary part Cp ', loss tangent Tan
(Delta), frequency f；Wherein, loss tangent Tan (Delta) is equal to apparent capacity imaginary part Cp ' and apparent capacity real part Cp
Ratio；
MCU will test the obtained data of record, respectively export obtain apparent capacity real part-frequency curve i.e. Cp-f curve,
Loss tangent-frequency curve, that is, Tan (Delta)-f curve；It is bent in all apparent capacity real part-frequency curves, that is, Cp-f
In line, loss tangent-frequency curve, that is, Tan (Delta)-f curve, frequency takes logarithm, i.e. logf or lgf；It is described
The output alternate electrical signal v of programmable signal generatortFrequency f down to Hz magnitude, up to MHz magnitude；Alternating signal source
Export alternate electrical signal vtFrequency f t makees logarithmic parabola variation at any time；
Obtained apparent capacity real part-frequency curve is made normalized by MCU；Loss tangent Tan (Delta)-
Frequency f curve itself has been substantially nondimensional, normalized curve, without remaking normalized；
When detecting the content of beary metal of soil pattern, by the apparent capacity real part-of the MCU soil pattern that will test
Frequency curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (Delta)-f curve make normalized, to process
Normalized curve carries out the identification of curvilinear characteristic degree, then in MCU in song in the Standard Curve Database that prestores in the memory that sets
Line makees Auto-matching operation, and the numerical value in reference standard curve library obtains the content of beary metal of soil pattern collected, described
Standard Curve Database record has the process normalizing of multiple pre- standard soil samples for first passing through content of beary metal that measurement obtains, different
Apparent capacity real part-frequency curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (the Delta)-f for changing processing are bent
Line.In all apparent capacity real part-frequency curves, loss tangent-frequency curve, frequency takes logarithm, i.e. logf
Or lgf.In Standard Curve Database, each curve also has additional information, and the additional information includes: each by normalization
Apparent capacity real part-frequency curve of processing, all extreme points of loss tangent-frequency curve, first derivative curve
Zero point, the zero point of Second derivative curves；
Actual test temperature value is identical as the measurement temperature in Standard Curve Database.
According to our practical experience, in low-frequency range, the apparent capacity real part Cp- frequency f curve of sample, loss angle tangent
Value Tan (Delta)-frequency f curve usually changes more slowly, if t makees linear rule variation to frequency f at any time, from hundred Hz amounts
Grade will lead to time-consuming too long to million Hz magnitudes, be up to a few hours, and obtained data volume is too many, does not see obviously in low-frequency range
Variation；And select frequency f t makees logarithmic parabola variation at any time, then it takes only about 1 minute, change can be shown in each frequency band
Law.
In an example, programmable signal generator uses AT89C51 single-chip microcontroller for core composition.AT89C51 monolithic
The internal structure of machine includes CPU, memory, parallel interface, serial line interface, timing ga(u)ge/number device, system construction drawing such as Fig. 4 institute
Show.It is integrated with each component part of single-chip microcontroller on a single die, function is as follows: (1) eight central processing units
CPU, AIU unit, 8 bit accumulator ACC, register B and program state including 8 arithmetical operations and logical operation can be carried out
Register PSW etc..(2) data storage RAM (128B) in piece, can be with the data of read/write, such as the knot among operation for storing
Fruit, final result or data of pre-display etc..(3) piece internal program deposits several device ROM/EPROM, for storing initial data, program
And table.(4) four 8 ports parallel-by-bit I/O interface P0-P3, each connecing port can be used for inputting or exporting.
When the result of detection be reported out heavy metal in soil content it is significantly exceeded when, mark the soil of the sampling section by weight
Metallic pollution, and using it is ultraviolet can spectrophotometry (UV), atomic absorption method (AAS), atomic fluorescence method (AFS), inductive coupling
Plasma method (ICP), X fluorescence spectrum (XRF), any method in Inductively coupled plasma-mass spectrometry (ICP-MS) carry out
Further heavy metal type identifies, content accurately measures.
Certainly, described above is only that presently preferred embodiments of the present invention is answered the present invention is not limited to enumerate above-described embodiment
When explanation, anyone skilled in the art is all equivalent substitutes for being made, bright under the introduction of this specification
Aobvious variant, all falls within the essential scope of this specification, ought to be by protection of the invention.
The content that this specification is not described in detail belongs to the prior art well known to professional and technical personnel in the field.
Express one's thanks to: the invention patent project is by the 2017 Australian (2017Australian of research project magnificent
Studies in China Program) fund subsidy, express thanks herein.
Claims (10)
1. a kind of detection device of field quick detection heavy metal content in soil, which is characterized in that the detection device includes: to pass
Sensor, amplifier and one chip microcomputer.
2. a kind of detection device of field quick detection heavy metal content in soil, which is characterized in that the detection device includes:
Sensor, programmable signal generator, current sampler, voltage sample device, instrumentation amplifier I, instrumentation amplifier V, A/D
Converter I (i.e. ADC-I), A/D converter V (i.e. ADC-V), interface circuit, MCU (micro-control unit, MicroController
Unit；MCU, also known as one chip microcomputer), input equipment, temperature control modules, power module；The sensor is also interior
It is equipped with electric heater and thermocouple；When detecting, the soil pattern collected is filled in sensor；
The input equipment is electrically connected to MCU, and the controlled input end of programmable signal generator is electrically connected to MCU, can compile
The signal output end of journey signal generator is electrically connected to sensor, current sampler, voltage sample device respectively with sensor electricity
Property connection, the signal input part of current sampler and instrumentation amplifier I is electrically connected, voltage sample device and instrumentation amplifier V's
Signal input part is electrically connected, and the signal output end of instrumentation amplifier I is electrically connected to the simulation of A/D converter I (i.e. ADC-I)
Signal input part, the signal output end of instrumentation amplifier V are electrically connected to the analog signal input of A/D converter V (i.e. ADC-V)
End, the digital signal output end of A/D converter I and the digital signal output end of A/D converter V pass through interface circuit and electrically connect
It is connected to MCU；
The sensor includes the metal plate of a pair of parallel disc-shaped, and ac signal input is respectively connected with per a piece of metal plate
End, for being connected to the signal output end of programmable signal generator；Per be also equipped with inside a piece of metal plate electric heater and
Thermocouple, i.e., the described sensor is built-in, and there are two electric heater and two thermocouples；Electric heater and thermocouple are prolonged by lead
It stretches out outside metal plate, electric heater and lead are electrically insulated with metal plate, i.e. electric heater and lead is equipped with insulating sleeve；
Electric heater and thermocouple are connected to temperature control modules by lead so that the temperature of soil pattern be maintained at when detecting by
The preset temperature value of MCU；
Input equipment is used to input preset measurement parameter and detection instruction to MCU；
Programmable signal generator can receive the instruction that MCU is issued, and the instruction issued according to MCU generates frequency and amplitude by MCU
Preset ac signal；When detecting, presetting the ac signal generated is that t variation, amplitude remain unchanged frequency f at any time
Ac signal；
Programmable signal generator exports the ac signal to sensor, detects to soil pattern；
When detecting, MCU is also issued to temperature controller and is instructed, and so that the electric heater built in sensor is worked, is controlled the biography
The temperature value of sensor maintains preset value；
It exports after current sampler to instrumentation amplifier I and amplifies by the ac current signal of sensor, then by A/D
Amplified analog signal is converted to digital signal by converter I, obtains the digital value of the ac current signal by sensor；
The ac voltage signal at sensor both ends is exported to instrumentation amplifier V after voltage sample device and is amplified, then is converted by A/D
Amplified analog signal is converted to digital signal by device V, obtains the digital value of the ac voltage signal at sensor both ends；It is described
Digital value by the digital value of the ac current signal of sensor, the ac voltage signal at sensor both ends passes through interface circuit
It is transmitted to MCU in real time, is stored in real time by MCU, MCU is also according to the ac current signal and sensor both ends for passing through sensor
Amplitude, the phase calculation of both ac voltage signals obtain the apparent capacity real part Cp of soil pattern, apparent capacity imaginary part
Cp ', loss tangent Tan (Delta), while calculated result being stored in real time；
When detecting the content of beary metal of soil pattern, by apparent capacity real part-frequency of the MCU soil pattern that will test
Curve, that is, Cp-f curve, loss tangent-frequency curve, that is, Tan (Delta)-f curve make normalized, to by normalizing
The curve of change carries out the identification of curvilinear characteristic degree, then in MCU in curve in the Standard Curve Database that prestores in the memory that sets make
Auto-matching operation, the numerical value in reference standard curve library, obtains the content of beary metal of soil pattern collected, the standard
Curve library record has at the process normalization of multiple pre- standard soil samples for first passing through content of beary metal that measurement obtains, different
Apparent capacity real part-frequency curve, that is, Cp-f curve, the loss tangent-frequency curve, that is, Tan (Delta)-f curve of reason.
3. a kind of detection device of field quick detection heavy metal content in soil as claimed in claim 2, it is characterised in that:
In the soil pattern by heavy metal pollution, type, the content of heavy metal affect apparent capacity real part-frequency curve
That is Cp-f curve, loss tangent-frequency curve, that is, Tan (Delta)-f curve shape, the distortion degree of curve shape,
The position that distortion occurs, embodies the weight of the substance of heterogeneity in soil.
4. a kind of detection device of field quick detection heavy metal content in soil as claimed in claim 2 or claim 3, feature exist
In: the output alternate electrical signal v in alternating signal sourcetFrequency f down to Hz magnitude, up to MHz magnitude；The output in alternating signal source
Alternate electrical signal vtFrequency f t makees logarithmic parabola variation at any time.
5. a kind of detection device of such as described in any item field quick detection heavy metal content in soil of claim 2-4, special
Sign is: the size of the disc-shaped metal plate of the sensor is Centimeter Level, with a thickness of grade.
6. a kind of detection device of such as described in any item field quick detection heavy metal content in soil of claim 2-5, special
Sign is: power module includes AC-DC converting unit, DC-DC converting unit, isolating transformer, rectifier, filter；Electricity
Source module realizes the electric isolution between detection device and mains circuit, improves safety；AC-DC converting unit is whole using full-bridge
Flow device.
7. a kind of detection device of such as described in any item field quick detection heavy metal content in soil of claim 2-6, special
Sign is: two electric heaters built in the sensor are electrically connected in series to temperature control modules.
8. a kind of detection device of such as described in any item field quick detection heavy metal content in soil of claim 2-7, special
Sign is: programmable signal generator uses AT89C51 single-chip microcontroller for core composition, the internal structure packet of AT89C51 single-chip microcontroller
Include CPU, memory, parallel interface, serial line interface, timing ga(u)ge/number device.
9. a kind of detection device of such as described in any item field quick detection heavy metal content in soil of claim 2-8, special
Sign is: in Standard Curve Database, each curve also has additional information, and the additional information includes: each by normalizing
Change apparent capacity real part-frequency curve, all extreme points of loss tangent-frequency curve, first derivative curve of processing
Zero point, the zero point of Second derivative curves.
10. a kind of such as detection device of the described in any item field quick detection heavy metal content in soil of claim 2-9 is answered
With, it is characterised in that: when the result of detection be reported out heavy metal in soil content it is significantly exceeded when, mark the soil of the sampling section
Earth by heavy metal pollution, and using it is ultraviolet can spectrophotometry (UV), atomic absorption method (AAS), atomic fluorescence method (AFS), electricity
Feel coupled plasma method (ICP), X fluorescence spectrum (XRF), any side in Inductively coupled plasma-mass spectrometry (ICP-MS)
Method, further progress heavy metal type identifies, content accurately measures.
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