CN109781660A - Oil pollution object detecting method in soil based on multi-photon electron extraction spectrum - Google Patents
Oil pollution object detecting method in soil based on multi-photon electron extraction spectrum Download PDFInfo
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Abstract
The invention belongs to environmental pollution analyte detection correlative technology fields, it discloses oil pollution object detecting methods in a kind of soil based on multi-photon electron extraction spectrum, method includes the following steps: (1) carries out length scanning to the sample to be tested in electric field using Wavelength tunable laser, detection obtains the corresponding photo-signal curve of sample to be tested when different wave length laser action simultaneously, then it determines the spectrogram of the sample to be tested, and determines optimum resonance excitation wavelength；(2) Wavelength tunable laser issues the laser that wavelength is the optimum resonance excitation wavelength be scanned to the sample to be tested of different petroleum pollution concentration to obtain corresponding photo-current intensity data, and the photo-current intensity data are handled to obtain the calibration curve of petroleum pollution ingredient in the sample to be tested, thus complete the detection of petroleum pollution in soil.This invention simplifies process, accuracy is improved, and easy to implement.
Description
Technical field
The invention belongs to environmental pollution analyte detection correlative technology fields, are based on multi-photon electronics more particularly, to one kind
Extract oil pollution object detecting method in the soil of spectrum.
Background technique
Petroleum plays an important role in the development of national economy, however, pollution problem of the petroleum to environment
It is on the rise.Petroleum pollution is complicated organic matter, is mainly made of compounds such as various alkane, cycloalkane, aromatic hydrocarbon, such as
Fruit petroleum pollution penetrates into soil, it is easy to and underground water pollution is caused, plant absorption moisture and nutrient are hindered, it is serious to destroy
Ecological environment.Currently, in soil the traditional detection method of petroleum pollution mainly include detect organic matter oil bath clear up-weigh chromium
Sour potassium capacity method, gas chromatography-mass spectrometry (being commonly called as GC-MS) and ftir Analysis spectra methods (being commonly called as TG-IR)
Deng.Wherein, it be easy to cause the organic matter on oil bath surface seriously to volatilize using oil bath resolution-potassium bichromate titrimetric method, and clears up
The greasy dirt of tube outer surface attachment being difficult to clean may make measurement result higher.Therefore, this method has pollution air, accurate
The disadvantages of degree difference.GC-MS is related to complicated ingredient separation, nonreactive gas auxiliary, particle mass spectral analysis, it is seen then that
GC-MS method for combined use needs to introduce gas auxiliary, and the program of detection is excessively cumbersome, and there is a degree of errors.TG-IR
Combination method needs complicated extraction process, and organic solvent used in extraction not only has high volatile and high pollution, but also
Extraction agent is affected to experimental result, therefore, this method have time-consuming, it is at high cost, be excessively used toxic chemical,
The disadvantages of error is big.How to be realized by new material, new technology, new method and quick, the accurate detection of petroleum pollution is had become
For the key subjects in environment protection field.
In conclusion there is program complexity, secondary pollution, error are larger for the detection method of petroleum pollution at this stage
The deficiencies of, this field needs to make further perfect and improve, and correspondingly, this field is a kind of easy and accurate there is developing
The technical need of oil pollution object detecting method in soil of the property preferably based on multi-photon electron extraction spectrum.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides one kind to be based on multi-photon electron extraction light
Oil pollution object detecting method in the soil of spectrum, based on the detection feature of petroleum pollution in existing soil, research and design
Oil pollution object detecting method in a kind of easy and soil of the accuracy preferably based on multi-photon electron extraction spectrum.It is described
Detection method does not need to introduce additional gas auxiliary, does not need complicated extraction process yet, but uses novel laser light
Detection mode is composed, thus solves that program complexity present in detection pedotheque petroleum components, secondary pollution, error are larger etc. to ask
Topic.
To achieve the above object, the present invention provides oil pollutions in a kind of soil based on multi-photon electron extraction spectrum
Object detecting method, the detection method mainly comprise the steps that
(1) length scanning is carried out using sample to be tested of the Wavelength tunable laser to the soil in electric field, simultaneously
Detection obtains the corresponding photo-signal curve of sample to be tested when different wave length laser action, then determines the sample to be tested
Spectrogram, and determine the optimum resonance excitation wavelength for detecting petroleum pollution in the sample to be tested；
(2) laser that the Wavelength tunable laser issues that wavelength is the optimum resonance excitation wavelength comes to different stones
The sample to be tested of oil contaminants concentration is scanned to obtain corresponding photo-current intensity data, and uses linear fit or interior
Standardization is handled the photo-current intensity data to obtain the calibration of petroleum pollution ingredient in sample to be tested song
Thus line completes the detection of petroleum pollution in soil.
It further, further include using soil of the pressed disc method preparation containing petroleum pollution before step (1) to test sample
The step of product.
Further, the soil containing petroleum pollution is mixed with poly (vinyl alcohol) binder to obtain mixture,
The mixture is pressed into using fully automatic powder tablet press machine by discoid sample to be tested again.
Further, the wavelength of the laser is 286nm~341nm.
Further, select sample to be tested in spectral signal most by force without include petroleum pollution sample in spectrum letter
Optical maser wavelength when number most weak is as the optimum resonance excitation wavelength.
Further, the optimum resonance excitation wavelength is 326nm.
Further, the content of petroleum pollution is positively correlated with corresponding photo-signal intensity in the sample to be tested
Relationship.
Further, the detection method is realized using detection device, and the detection device includes data line, meter
Calculation machine, the first synchronous transmission of signal BNC line, the second synchronous transmission of signal BNC line, the Wavelength tunable laser, reflecting mirror,
Condenser lens, DC high-voltage power supply, digitizing oscilloscope, galvo-preamplifier, positive plate, faraday cup and negative plate, institute
It states computer and the Wavelength tunable laser is connected to by the data line；The reflecting mirror is arranged in the laser
Exit direction on, be used for the laser reflection to the condenser lens；The condenser lens is arranged in the reflection
The lower section of mirror is used to act on the sample to be tested after focusing the laser；The positive plate and the negative plate phase
Mutual parallel interval setting, the sample to be tested are set between the positive plate and the negative plate；The positive plate, it is described to
Sample and the negative plate are all set in the faraday cup；The positive plate is connected to the DC high-voltage power supply；Institute
It states negative plate and is connected to the galvo-preamplifier；The galvo-preamplifier passes through first synchronous transmission of signal
BNC line is connected to the digitizing oscilloscope；The digitizing oscilloscope is connected by the second synchronous transmission of signal BNC line
In the Wavelength tunable laser.
Further, the computer is used to control the laser that the Wavelength tunable laser issues tunable wave length；
The laser action when surface of the sample to be tested, petroleum pollution ingredient in the sample to be tested occur ionization and
Negative ions are generated, the negative ions occur displacement between the positive plate and the negative plate and generate photoelectricity
Stream；The galvo-preamplifier amplifies processing to the photoelectric current formed between the positive plate and the negative plate, and
The signal of processing is transferred to the digitizing oscilloscope.
Further, the data line is USB data transmission line；The Wavelength tunable laser is Wavelength tunable
Humorous OPO laser.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, base provided by the invention
Oil pollution object detecting method mainly has the advantages that in the soil of multi-photon electron extraction spectrum
1. the detection method does not cause secondary pollution to environment without using the organic reagent seriously to volatilize without high temperature；
Without complicated sample pretreatment means, it is not necessarily to extraction process, without introducing additional gas auxiliary, there will not be depositing because of gas
And bring the error of detection, improve accuracy.
2. the detection method has the detection of petroleum pollution in soil sensitivity with higher and accuracy
Rapidly and efficiently, the advantages such as easy to operate, low in cost have very strong applicability.
3. the detection method is based on multi-photon electron extraction spectrum, the interference of bias light, promotion side can be effectively avoided
The sensitivity of method, flexibility is higher, and accuracy is preferable, and application range is wider.
4. the detection method simplifies process, simple easy to implement, with strong applicability, be conducive to promote and apply.
Detailed description of the invention
Fig. 1 is the stream of oil pollution object detecting method in the soil provided by the invention based on multi-photon electron extraction spectrum
Journey schematic diagram.
Fig. 2 is the inspection that oil pollution object detecting method is related in the soil based on multi-photon electron extraction spectrum in Fig. 1
Survey the schematic diagram of device.
Fig. 3 is oil pollution in the soil based on multi-photon electron extraction spectrum provided using first embodiment of the invention
The MEES spectrum comparison diagram for the pedotheque and blank pedotheque containing petroleum pollution that object detecting method obtains.
Fig. 4 is oil pollution in the soil based on multi-photon electron extraction spectrum provided using first embodiment of the invention
Object detecting method obtain under optimum resonance excitation wavelength in pedotheque petroleum pollution concentration gradient photocurrent curve
Figure.
Fig. 5 is oil pollution quality testing in the soil based on multi-photon electron extraction spectrum of first embodiment of the invention offer
The calibration curve figure of petroleum pollution ingredient in the pedotheque obtained by linear fit that survey method is related to.
Fig. 6 is oil pollution quality testing in the soil based on multi-photon electron extraction spectrum of first embodiment of the invention offer
The calibration curve figure of petroleum pollution ingredient in the pedotheque obtained by internal standard method that survey method is related to.
In all the appended drawings, identical appended drawing reference is used to denote the same element or structure, in which: the transmission of 1- data
Line, 2- computer, 3- the first synchronous transmission of signal BNC line, 4- sample, 5- the second synchronous transmission of signal BNC line, 6- Wavelength tunable
Humorous laser, 7- reflecting mirror, 8- condenser lens, 9- DC high-voltage power supply, 10- digitizing oscilloscope, the preposition amplification of 11- electric current
Device, 12- positive plate, 13- faraday cup, 14- negative plate.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
Please refer to Fig. 1 and Fig. 2, oil pollution quality testing in the soil provided by the invention based on multi-photon electron extraction spectrum
Survey method mainly comprises the steps that
Step 1 prepares the sample to be tested of the soil containing petroleum pollution by pressed disc method.
Specifically, the soil containing petroleum pollution and poly (vinyl alcohol) binder are mixed into wet shape according to a certain percentage
Pedotheque prevent soil to be difficult to blocking to increase viscosity, and using fully automatic powder tablet press machine by damp soil sample
It is pressed into circular sample to be tested.
Step 2 carries out length scanning to sample to be tested using Wavelength tunable laser, while detection obtains photoelectric current
Signal curve, and then determine the spectrogram of the sample to be tested, and determine oil pollution analyte detection in the sample to be tested
Optimum resonance excitation wavelength.
Specifically, detection device is provided, the detection device carries out spectral scan and signal acquisition for sample to be tested.Institute
Stating detection device includes data line 1, computer 2, the first synchronous transmission of signal BNC line 3, the second synchronous transmission of signal BNC
Line 5, Wavelength tunable laser 6, reflecting mirror 7, condenser lens 8, DC high-voltage power supply 9, digitizing oscilloscope 10, electric current are preposition
Amplifier 11, positive plate 12, faraday cup 13 and negative plate 14.The computer 2 is connected to institute by the data line 1
Wavelength tunable laser 6 is stated, the computer 2 is for controlling the Wavelength tunable laser 6.In present embodiment, institute
Stating data line 1 is USB data transmission line；The Wavelength tunable laser 6 is tunable wave length OPO laser.It is described
Wavelength tunable laser 6 is used to issue the laser beam of tunable wave length with ablation sample.
The reflecting mirror 7 is arranged in the exit direction of the laser, is used to for the laser beam being reflected into described poly-
On focus lens 8.The lower section of the reflecting mirror 7 is arranged in the condenser lens 8, is used to act on after the laser beam focus
On sample 4.The positive plate 12 is parallel to each other with the negative plate 14 is spaced setting, and the sample 4 is set to the positive plate
Between 12 and the negative plate 14.The positive plate 12, the sample 4 and the negative plate 14 are all set in the faraday cup
In 13.The positive plate 12 is connected to the DC high-voltage power supply 9, and the DC high-voltage power supply 9 is for providing voltage.It is described negative
Pole plate 14 is connected to the galvo-preamplifier 11, and the galvo-preamplifier 11 is used to collecting and amplifying photoelectric current, and
Amplified photoelectric current is transferred to the digitizing oscilloscope 10.Wherein, the galvo-preamplifier 11 passes through described the
One synchronous transmission of signal BNC line 3 is connected to the digitizing oscilloscope 10, and the digitizing oscilloscope 10 is used for receiving
Photoelectric current carries out digitized processing, and data are shown by treated.The digitizing oscilloscope 10 passes through described second
Synchronous transmission of signal BNC line 5 is connected to the Wavelength tunable laser 6, so that acquisition and the laser beam of photo-signal
Transmitting synchronize.The digitizing oscilloscope 10 to photo-signal carry out digitized processing come obtain under each wavelength to
The photocurrent curve of sample.
Output wavelength tunable laser after the Wavelength tunable laser 6 is switched on, the wavelength of the laser be 286nm~
341nm, the Wavelength tunable laser 6 issues the laser of multiple wavelength, and the wavelength of multiple laser successively increases, phase
The wavelength of two adjacent laser beams differs 5nm.
By acting on the surface of sample after focusing, the petroleum pollution ingredient in sample occurs ionization and produces laser
Raw negative ions.The DC high-voltage power supply 9 and the positive plate 12 be formed by electronics that electric field generates sample surfaces into
Row is collected.Work as negative ions, especially electronics and meeting when displacement occurs between the positive plate 12 and the negative plate 14
Generate photoelectric current.The galvo-preamplifier 11 is to the faint light formed between the positive plate 12 and the negative plate 14
Electric current amplifies processing, and signal is transferred to the digitizing oscilloscope 10 by treated.
During laser irradiation sample, when laser energy density is more than the ionization threshold of test analyte in sample
When, ionization can occur and generate negative ions.Negative ions occur fixed between the positive plate 12 and the negative plate 14
To photoelectric current is generated when movement, in this process, because absorbing laser, photon electron energy level jump occurs for the organic molecule in sample
It moves.It is then " off-resonance " excitation when the energy needed for electron transition and photon energy mismatch, the photoelectric current letter detected at this time
Number intensity is weaker；When the energy needed for electron transition matches just with the energy of laser photon, then resonant excitation occurs, at this time
Degree of ionization is significantly promoted, and the photo-signal intensity detected will be greatly enhanced, and optical maser wavelength at this time is known as altogether
Vibration excitation wavelength.
The corresponding photo-signal intensity of wavelength each in 286nm~341nm, which is carried out drawing, can be obtained sample to be tested
MEES spectral results.By comparing the MEES spectrogram of pedotheque and blank sample containing petroleum pollution, contain petroleum wastewater
There are multiple resonant excitation wavelength within the scope of 286nm~341nm for the pedotheque of dye object, select the sample containing petroleum pollution
MEES signal is most strong and the optical maser wavelength in the most weak situation of blank sample signal as in soil oil pollution analyte detection it is best
Resonant excitation wavelength.
Step 3, the Wavelength tunable laser, which issues the laser beam that wavelength is the optimum resonance excitation wavelength, to be come pair
The sample to be tested of different petroleum pollution concentration is scanned to obtain corresponding photo-current intensity data, and uses linear fit
Or interior standardization is handled the photo-current intensity data to obtain petroleum pollution ingredient in the sample to be tested
Thus calibration curve completes the detection of petroleum pollution in soil.
Specifically, under the laser action of optimum resonance excitation wavelength, in the sample of soil the content of petroleum pollution with
Photo-signal intensity correlation.By the intensity of signal under analysis optimum resonance wavelength, the soil containing petroleum pollution
Organic matter in earth sample can be determined, and can not only whether there is petroleum-type organic matter in qualitative analysis soil, additionally it is possible to
Quantitative detection goes out the content situation of Hydrocarbon in Soil organic matter.
Embodiment 1
Fig. 3, Fig. 4, Fig. 5 and Fig. 6 are please referred to, the present invention is described in more detail with specific embodiment below.
First embodiment of the invention choose content containing petroleum pollution be respectively 0ppm, 100ppm, 300ppm, 500ppm, 800ppm,
The soil of 1200ppm, 1600ppm, 2000ppm carry out mixing sample preparation as adhesive using polyvinyl alcohol (analysis is pure).This hair
In the soil based on multi-photon electron extraction spectrum that bright first embodiment provides oil pollution object detecting method mainly include with
Lower step:
(1) pedotheque of the 8g containing petroleum hydrocarbons and 0.3g poly (vinyl alcohol) binder is taken to be mixed into wet shape.It is pressing
Under conditions of power 25t, duration 60s, wet sample is pressed into a thickness of 5mm or so, directly with fully automatic powder tablet press machine
Diameter is the circular sample of 30mm or so.During the experiment, the scanning range of optical maser wavelength is set as 286~341nm, every
The wavelength interval 5nm measures the photo-signal intensity of a sample, and polar plate voltage is set as 100V, and pole plate spacing is 4mm, passes through
Compare MEES (Multiphoton Electron Extraction Spectroscopy) spectrum of 0ppm and 2000ppm sample
It determines the resonant wavelength of Hydrocarbon in Soil pollutant sample, then selects the strongest wavelength of MEES signal as optimum resonance
Excitation wavelength.
(2) under optimum resonance excitation wavelength, respectively measure oil content be 100ppm, 300ppm, 500ppm,
The photo-signal intensity of the pedotheque of 800ppm, 1200ppm, 1600ppm, 2000ppm, and with normal linear fitting and it is interior
Mark method carries out quantitative analysis to sample.
As shown in figure 3, the MEES spectrogram of pedotheque and blank sample containing petroleum pollution has larger difference, and have
Have multiple resonance characteristics peaks, due to sample MEES signal corresponding at 326nm wavelength is most strong and blank sample signal is most weak, selection
Optimum resonance excitation wavelength of the 326nm as oil pollution analyte detection in soil.As shown in figure 4, in optimum resonance excitation wavelength
Under, the photocurrent curve figure of petroleum pollution concentration gradient in pedotheque, with the increase of petroleum pollution content, signal
Intensity is consequently increased.As shown in figure 5, in the pedotheque as made from linear fit petroleum pollution ingredient calibration curve
R2 is 0.9206, and detection limit LoD is 108.02ppm.As shown in fig. 6, oil pollution in the pedotheque as made from internal standard method
The calibration curve R2 of object ingredient is 0.9498, and detection limit LoD is 71.46ppm.In the above experiment, using made from internal standard method
Spectroscopic data is dominant.
Oil pollution object detecting method in soil provided by the invention based on multi-photon electron extraction spectrum, the detection
Method is based on multi-photon electron extraction spectrum, can effectively avoid the interference of bias light, the sensitivity of method for improving, and is not necessarily to multiple
Miscellaneous sample pretreatment means are not necessarily to extraction process, assist without introducing additional gas, simplify process, be easy to simply implement,
Accuracy and applicability are improved, flexibility is preferable, is conducive to promote and apply.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. oil pollution object detecting method in a kind of soil based on multi-photon electron extraction spectrum, which is characterized in that this method
The following steps are included:
(1) length scanning is carried out using sample to be tested of the Wavelength tunable laser to the soil in electric field, detected simultaneously
The corresponding photo-signal curve of sample to be tested when different wave length laser action is obtained, then determines the spectrum of the sample to be tested
Figure, and determine the optimum resonance excitation wavelength for detecting petroleum pollution in the sample to be tested；
(2) laser that the Wavelength tunable laser issues that wavelength is the optimum resonance excitation wavelength comes to different petroleum wastewaters
The sample to be tested of dye object concentration is scanned to obtain corresponding photo-current intensity data, and uses linear fit or interior calibration
Method handles to obtain the calibration curve of petroleum pollution ingredient in the sample to be tested photo-current intensity data, by
This completes the detection of petroleum pollution in soil.
2. oil pollution object detecting method in the soil as described in claim 1 based on multi-photon electron extraction spectrum, special
Sign is: further including the steps that the sample to be tested using soil of the pressed disc method preparation containing petroleum pollution before step (1).
3. oil pollution object detecting method in the soil as claimed in claim 2 based on multi-photon electron extraction spectrum, special
Sign is: the soil containing petroleum pollution being mixed with poly (vinyl alcohol) binder to obtain mixture, then is used entirely certainly
The mixture is pressed into discoid sample to be tested by dynamic powder compressing machine.
4. oil pollution object detecting method in the soil as described in claim 1 based on multi-photon electron extraction spectrum, special
Sign is: the wavelength of the laser is 286nm~341nm.
5. oil pollution object detecting method in the soil as described in claim 1 based on multi-photon electron extraction spectrum, special
Sign is: selection sample to be tested in spectral signal most by force without include petroleum pollution sample in spectral signal it is most weak when
Optical maser wavelength is as the optimum resonance excitation wavelength.
6. oil pollution object detecting method in the soil as described in claim 1 based on multi-photon electron extraction spectrum, special
Sign is: the optimum resonance excitation wavelength is 326nm.
7. oil pollution analyte detection side in the soil as claimed in any one of claims 1 to 6 based on multi-photon electron extraction spectrum
Method, it is characterised in that: the content of petroleum pollution and corresponding photo-signal intensity are positively correlated pass in the sample to be tested
System.
8. oil pollution analyte detection side in the soil as claimed in any one of claims 1 to 6 based on multi-photon electron extraction spectrum
Method, it is characterised in that: the detection method realizes that the detection device includes data line, calculates using detection device
Machine, the second synchronous transmission of signal BNC line, the Wavelength tunable laser, reflecting mirror, gathers the first synchronous transmission of signal BNC line
Focus lens, DC high-voltage power supply, digitizing oscilloscope, galvo-preamplifier, positive plate, faraday cup and negative plate, it is described
Computer is connected to the Wavelength tunable laser by the data line；The laser is arranged in the reflecting mirror
In exit direction, it is used for the laser reflection to the condenser lens；The condenser lens is arranged in the reflecting mirror
Lower section, be used for will the laser focus after act on the sample to be tested；The positive plate and the negative plate are mutual
Parallel interval setting, the sample to be tested are set between the positive plate and the negative plate；It is the positive plate, described to be measured
Sample and the negative plate are all set in the faraday cup；The positive plate is connected to the DC high-voltage power supply；It is described
Negative plate is connected to the galvo-preamplifier；The galvo-preamplifier passes through the first synchronous transmission of signal BNC
Line is connected to the digitizing oscilloscope；The digitizing oscilloscope is connected to by the second synchronous transmission of signal BNC line
The Wavelength tunable laser.
9. oil pollution object detecting method in the soil as claimed in claim 8 based on multi-photon electron extraction spectrum, special
Sign is: the computer is used to control the laser that the Wavelength tunable laser issues tunable wave length；The laser is made
When surface for the sample to be tested, the petroleum pollution ingredient in the sample to be tested ionization occurs and generate it is positive and negative from
Son, the negative ions occur displacement between the positive plate and the negative plate and generate photoelectric current；The electric current
Preamplifier amplifies processing to the photoelectric current formed between the positive plate and the negative plate, and by the signal of processing
It is transferred to the digitizing oscilloscope.
10. oil pollution object detecting method in the soil as claimed in claim 9 based on multi-photon electron extraction spectrum, special
Sign is: the data line is USB data transmission line；The Wavelength tunable laser is tunable wave length OPO laser
Device.
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Application publication date: 20190521 |