CN107966430A - A kind of method for being used to quickly detect fertilizer nutrient content - Google Patents
A kind of method for being used to quickly detect fertilizer nutrient content Download PDFInfo
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- CN107966430A CN107966430A CN201710972126.9A CN201710972126A CN107966430A CN 107966430 A CN107966430 A CN 107966430A CN 201710972126 A CN201710972126 A CN 201710972126A CN 107966430 A CN107966430 A CN 107966430A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a kind of method for being used to quickly detect fertilizer nutrient content, the described method includes prepare test sample, collection spectroscopic data, selected characteristic spectral line, establish calibration model with test of quantitative analysis sample into five steps.Laser induced breakdown spectroscopy is applied to the measure of fertilizer nutrient content by the method for the present invention; the workload of fertilizer nutrient test pre-treatment can be greatly reduced; and test speed can be improved; use manpower and material resources sparingly; fertilizer analysis cost is reduced, so as to all have great importance to promoting fertilizer Fast Detection Technique and specification agricultural materials market, the protection peasants' lawful rights and interests.
Description
Technical field
The invention belongs to fertilizer Quality Detection field, and in particular to a kind of side for being used to quickly detect fertilizer nutrient content
Method.
Background technology
Agricultural is the mankind's " mother's industry ", and the mankind resist nature threaten and depend on for existence it is basic.Social production
Development first start at agricultural, just have on the basis of agricultural industry production and development, only agricultural and industrial development
On the basis of, just have the development of the tertiary industry.In other words, agricultural is the basic of the national economic development.Wherein, the fertilizer of high quality
One of an important factor for material is agriculture fast-developing.
With developing rapidly for China's fertilizer industry, either there is considerable progress in terms of quantity or kind.Fertilizer
Whether material component and content are rationally the key factors for determining fertilizer quality quality, and various fertilizer have country or enterprise's rule
Calibration is accurate, so, it is not usually required to the content of nutrient in detection fertilizer.However, fertilizer may be deposited during transport or storage
In rotten phenomenon, and there is part of the manufacturer can not to be carried out because of the limitation of raw material sources and technical equipment to the content of fertilizer nutrient
It is precisely controlled.Therefore, it is the interests of protection peasant, fertilizer is detected, monitors the component content of fertilizer in real time to ensure fertilizer
The quality of material is necessary.
Suitable detection method is to measure the key technology of fertilizer nutrient content, and the detection of fertilizer nutrient at present is typically to adopt
With chemical detection method, and mostly using national standard or portion's mark method, but all it is that every kind of nutrient individually extracts, independent measure, leaching
Time length is put forward, it is complicated, take a lot of work, is time-consuming, expense medicine, testing cost is very high, and efficiency is very low.So how to realize that fertilizer is supported
Quantifying for dividing quickly detects and realizes that low cost is the research emphasis of presently relevant field research staff.
Spectral method of detection is also applied in the detection of compound fertilizer elemental composition now, such as atomic absorption spectrography (AAS), electricity
Feel coupled plasma optical emission spectroscopic methodology (ICP-AES).The analyze speed of the relatively traditional laboratory analysis methodologies of this kind of method
Increase, but need the complicated pretreatment process such as molten sample and dilution, then need to carry out for the higher potassium element of content
Multi-stage dilution, not only increases whole measurement period, and is readily incorporated multiple error, and unfavorable shadow is produced to measurement accuracy
Ring, and can not meet production process fast and accurately quality control requirements.
102426128 A of CN disclose a kind of rapid detection method for fertilizer nutrients, it adds the concentrated sulfuric acid in sample digestion
With perchloric acid as digestive pharmaceutical, N P and K in postdigestive prepare liquid is then detected at the same time by colorimetric method or turbidimetry
Amount, although the method achieve while detect, has strong oxidizing property and strong corruption due to the use of the concentrated sulfuric acid and perchloric acid this measurer
The material of corrosion and be not suitable for large-scale promotion application.
In conclusion it is quick to be badly in need of offer fertilizer content a kind of of low cost and can detecting N-P-K content at the same time
Detection method.
The content of the invention
To solve the above-mentioned problems, inventor specifically researchs and analyses existing detection technique, finds to swash
Photoinduction breakdown spectral (Laser-induced breakdown spectroscopy, abbreviation LIBS) technology is supported applied to fertilizer
Divide the measure of content, the workload of fertilizer nutrient test pre-treatment can be greatly reduced, and test speed can be improved, save
Manpower and materials, reduce fertilizer analysis cost, so as to be closed to promoting fertilizer Fast Detection Technique and specification agricultural materials market, protection peasant
Right Yidu has great importance.
For this reason, the present invention provides a kind of method for being used to quickly detect fertilizer nutrient content, it is characterised in that the method
Comprise the following steps：
(1) test sample is prepared：Weigh chemical fertilizer sample and be ground, then using tabletting machine, obtain test specimens
This；
(2) spectroscopic data is gathered：Data acquisition is carried out to test sample using laser induced breakdown spectroscopy system, is surveyed
The laser induced breakdown spectroscopy data of sample sheet；
(3) selected characteristic spectral line：With reference to NIST (National Institute of Standards and
Technology Atomic Spectra Database) the characteristic spectral line letter of nitrogen, P elements and potassium element in database
Breath, qualitative analysis is carried out to fertilizer component, and the characteristic spectral line for picking out the nitrogen in test sample, P elements and potassium element is believed
Breath；
(4) calibration model is established：Several fertilizer samples known to selected nitrogen, P elements and Determination of Potassium simultaneously carry out
Grinding, then using tabletting machine, obtains calibration sample, afterwards using laser induced breakdown spectroscopy system to every kind of calibration sample
Product are detected to obtain the laser induced breakdown spectroscopy data of every kind of calibration sample, then respectively with nitrogen, P elements and
Determination of Potassium is dependent variable, using the laser induced breakdown spectroscopy intensity of measured respective element as independent variable, with fitting
Method establishes functional relation i.e. nitrogen model, phosphorus element content and the phosphorus between nitrogen element content and the intensity of spectral line of nitrogen
Between functional relation, that is, P elements model and Determination of Potassium and the intensity of spectral line of potassium element between the intensity of spectral line of element
Functional relation, that is, potassium element model；
(5) component in test of quantitative analysis sample：Extract nitrogen in the test sample in the step (3), phosphorus
The intensity of the characteristic spectral line of element and potassium element, and the calibration for the respective element established is entered into the step (4)
In model, i.e., the intensity of the characteristic spectral line of the nitrogen in test sample is input to the nitrogen established in the step (4)
In model, the intensity of the characteristic spectral line of the P elements in test sample is input to the P elements mould established in the step (4)
In type, the intensity of the characteristic spectral line of the potassium element in test sample is input to the potassium element model established in the step (4)
In, you can the content of the quick nitrogen obtained in test sample, P elements and potassium element.
The method of the present invention using the intensity of spectral line in Atomic Emission Spectral Analysis can directly reflect the change of concentration of element come
Carry out the test of fertilizer value：According to Sai Bai-Roman gold formula I=aCb, the surveyed intensity of spectral lines of wherein I expressions；a
It is two constants with b, the value of a depends on shooting condition, as analytical element enters the influence of the quantity, interference element of lasing region
Deng b is self-priming coefficient；C is the concentration of analytical element, therefore, can be with after establishing calibration model with reference to Sai Bai-Roman gold formula
By directly measuring the intensity of spectral line of each element in sample come calculating elements content.
The detection method of the present invention is compared to conventional chemical processing method complex pretreatment, of high cost, efficiency is low, operation is multiple
It is miscellaneous, the shortcomings that taking a lot of work, is time-consuming, there is achievable on-line checking can simultaneously detect the nitrogen in fertilizer, P elements and potassium member at the same time
The advantages of content of element.In addition, pushing away this and that, detection method of the invention can also detect the other elements in fertilizer at the same time
Content.
Preferably, it is not tight in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the order of the step (4)
Lattice requirement, can arrange its order according to actual conditions.As long as before step (5).
Preferably, nitrogen, phosphorus member in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (4)
The species of fertilizer sample known to element and Determination of Potassium is 10 kinds or more than 10 kinds.
Preferably, the chemical fertilizer sample weighed in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (1)
Product weight is 2g.
Preferably, chemical fertilizer sample is ground in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (1)
Particle diameter afterwards is 20-100 μm.
Preferably, tablet press machine is pressed in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (1)
Piece is that the tabletting of chemical fertilizer sample is more preferably circle into circular, square, rectangle or other shapes.
Preferably, tablet press machine is pressed in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (1)
Piece is into circular and its a diameter of 6-16mm by the tabletting of chemical fertilizer sample.
Preferably, in the above-mentioned method for being used to quickly detect fertilizer nutrient content, tablet press machine during tabletting in the step (1)
Pressure be 1-50N.
Preferably, in the above-mentioned method for being used to quickly detect fertilizer nutrient content, test specimens after tabletting in the step (1)
This thickness is 2-8mm.
Preferably, induced with laser is utilized in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (2)
The test condition of breakdown spectral system acquisition spectroscopic data is under vacuum atmosphere, and time delay is set as 2-8 μ s, laser energy
Scope is 50-100mJ, and the time of integration is 10-20 μ s, detector gain 2000, depth of focus 2mm, laser and test sample
Angle is 90 °.
It is highly preferred that lured in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (2) using laser
The test condition for leading breakdown spectral system acquisition spectroscopic data is under vacuum atmosphere, and time delay is set as 3 μ s, laser energy
Scope is 50-100mJ, and the time of integration is 15 μ s, detector gain 2000, depth of focus 2mm, the angle of laser and test sample
For 90 °.
The test condition selection vacuum environment of laser induced breakdown spectroscopy system acquisition spectroscopic data of the present invention is due to sky
The accuracy of nitrogen test result in disturbed specimen is understood in the presence of nitrogen in gas.
The line wavelength for the nitrogen that the laser induced breakdown spectroscopy system is surveyed is concentrated mainly on 746.64nm；Phosphorus member
The line wavelength of element is concentrated mainly on 213.51nm, 214.77nm, 253.48nm and 255.20nm；And the line wavelength of potassium element
It is concentrated mainly on 404.21nm, 404.61nm, 766.45nm and 769.67nm；
However, since potassium atom energy level is low and easy excitated, so stronger K spectrums can be also inspired even if poor sample
Line, and energy level is lower in the excitation of wavelength 766.45nm and 769.67nm, transition probability higher, and compound fertilizer collects potassium and supports in addition
Divide content high, it is contemplated that the spontaneous imbibition phenomena of element, the line wavelength of nitrogen choose 404.21nm and 404.61nm.
For P elements and nitrogen, both belong to nonmetalloid, its excitation level is higher, in plasma
Excitation in its spectral line influenced by self-absorption it is smaller, so be not in spectral peak deformation phenomenon.
Significantly interfered with according to nothing between selection principle, that is, spectral peak of common analysis spectral line in spectrum analysis, is overlapping, can
Adjacent spectral peaks are clearly distinguished, in the method that the present invention is used to quickly detect fertilizer nutrient content, the characteristic spectral line of nitrogen
Wavelength be 746.64nm, the wavelength of the characteristic spectral line of P elements is 213.51nm and 253.48nm, the characteristic spectral line of potassium element
Wavelength be 404.21nm and 404.61nm.
Linearly related degree between two groups of data is shown with related coefficient and fitting degree, shows two groups closer to 1
Linear dependence between data is better.Wherein related coefficient
Fitting degree is R2.According to variable analysis and as a result, related coefficient is between nitrogen the intensity of spectral line intensity and nitrogen element content
0.9557, fitting degree is 0.9133 therebetween；Phase relation between the intensity of spectral line intensity and phosphorus element content of P elements
Number is 0.9812, and fitting degree is 0.9627 therebetween；Phase relation between potassium element the intensity of spectral line intensity and Determination of Potassium
Number is 0.9375, and fitting degree is 0.8789 therebetween.
Preferably, induced with laser is utilized in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (2)
The test condition of breakdown spectral system acquisition spectroscopic data is with utilizing laser induced breakdown spectroscopy system acquisition in the step (4)
The test condition of spectroscopic data is consistent.
Preferably, in the above-mentioned method for being used to quickly detect fertilizer nutrient content, calibration sample in the step (4)
Preparation process is consistent with the process that test sample is prepared in the step (4).
Preferably, the nitrogen member established in the above-mentioned method for being used to quickly detect fertilizer nutrient content, the step (4)
Prime model is Y=0.003791 × a-1.579, and wherein a is wavelength for the energy value at 746.64nm；P elements model is Y=-
0.02995 × a+0.01631 × b-0.8496, a be wavelength be 213.51nm place energy value, b be wavelength be 253.48nm at
Energy value；Potassium element model is Y=0.006376 × a-0.004192 × b-2.145, and wherein a is wavelength at 404.21nm
Energy value, b is wavelength for the energy value at 404.61nm.
Compared with prior art, the present invention has the following advantages and beneficial effect：
(1) the method for the present invention realizes quick detection fertilizer nutrient content, and realizes while detect a variety of nutrients and contain
Amount；
(2) the method for the present invention make use of laser induced breakdown spectroscopy, before it can greatly reduce fertilizer nutrient test
The workload of processing, avoids pollution of the chemical reagent to sample, and can improve test speed, uses manpower and material resources sparingly, drop
Low fertilizer analysis cost, effectively overcomes the shortcomings that traditional detection method detection time is long and operation is responsible for；
(3) the method for the present invention testing result error is small, can be controlled within 10%, and accuracy is high, and applicable at the same time
Fertilizer type is wide, applicable to various fertilizer.
Brief description of the drawings
Fig. 1 is the principle that the present invention is applied to fertilizer nutrient assay using laser induced breakdown spectroscopy systems technology
Figure；
Fig. 2 is the calibration model figure of the nitrogen in the calibration sample in embodiment 1；
Fig. 3 is the calibration model figure of the P elements in the calibration sample in embodiment 1；
Fig. 4 is the calibration model figure of the potassium element in the calibration sample in embodiment 1；
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, the present invention is done below in conjunction with the accompanying drawings into one
It is described in detail on step ground.
Referring to attached drawing 1, laser induced breakdown spectroscopy system of the present invention includes Laser Power Devices 1, laser 2, anti-
Penetrate mirror 3, perforation speculum 4, lens 51 and 52, rotating platform 6, high resolution spectrometer 9, time-delay trigger 8,10 and of computer
Optical fiber 12.Specific workflow is：Ready fertilizer sample 11 is placed on rotating platform 6, the light beam water that laser 2 is launched
On the speculum 3 of the flat plated film for inciding 45 ° of placements, after reflection perpendicular through plated film perforation speculum 4 hole and lens
51, high energy density laser beam is focused in the fertilizer sample 11 on rotating platform 6, and by its surface portion material ablation into etc.
Gas ions, emission spectrum signal obtains a branch of directional light by lens 51 when plasma cools down, and directional light is reflected by perforation
After mirror 4 reflects, by lens 52, it is transferred in high resolution spectrometer 9 and is handled through optical fiber 12 after focusing, and change into number
Word signal input computer 10 treats subsequent treatment.
In the present invention, the quick detection for fertilizer nutrient content be primarily referred to as nitrogen, P elements and potassium element this
The quick detection of three kinds of elements, certainly, the method for the present invention can also detect other elements content.
In order to make objects and advantages of the present invention more concise, the present invention will be explained with specific examples below
It is bright, but the present invention is only limitted to absolutely not these embodiments.Following embodiments are only more preferably embodiment, and be only used for explaining of the invention
State the present invention, it is impossible to be interpreted as limiting the scope of the present invention.It should be pointed out that it is all the present invention essence and principle it
Interior done all any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention.Therefore, it is of the invention
The protection domain of patent should be determined by the appended claims.
Calibration embodiment establishes nitrogen, P elements and potassium element calibration model
20 kinds of fertilizer samples known to 2g nitrogens, P elements and Determination of Potassium are weighed respectively and are ground, its grain
Footpath is 50 μm, then the circle with tabletting machine into a diameter of 10mm, and wherein tablet press machine pressure is 45N, obtains calibration sample.
Then calibration sample is placed on the rotating platform of laser induced breakdown spectrograph device respectively, laser is opened, to every kind of calibration
Sample is detected to obtain the laser induced breakdown spectroscopy data of every kind of calibration sample, wherein laser induced breakdown spectrograph device
Parameter be vacuum atmosphere, time delay is set as 3 μ s, range of laser energy 50-100mJ, and the time of integration is 15 μ s, detection
Device gain is 2000, depth of focus 2mm, and the angle of laser and test sample is 90 °.Then respectively with nitrogen, P elements and potassium
Constituent content is dependent variable, with the characteristic spectral line of the laser induced breakdown spectroscopy of measured respective element (wherein nitrogen
The wavelength of characteristic spectral line is 746.64nm, and the wavelength of the characteristic spectral line of P elements is 213.51nm and 253.48nm, potassium element
The wavelength of characteristic spectral line is 404.21nm and 404.61nm) intensity be independent variable, establish nitrogen element content with the method for fitting
Between the intensity of spectral line of functional relation, that is, nitrogen model, phosphorus element content and P elements between the intensity of spectral line of nitrogen
Functional relation, that is, P elements model and Determination of Potassium and the intensity of spectral line of potassium element between functional relation, that is, potassium element mould
Type, specific calibration model are shown in attached drawing 2-4,.
Testing example
Testing example 1
Weighing 2g fertilizer samples, (nitrogen element content 16.32%, phosphorus element content 16.36%, Determination of Potassium are
15.86%) and it is ground, its particle diameter is 50 μm, then the circle with tabletting machine into a diameter of 10mm, wherein tablet press machine
Pressure is 45N, obtains test sample.Test sample is then placed in the rotating platform of laser induced breakdown spectrograph device respectively
On, laser is opened, test sample is detected to obtain the laser induced breakdown spectroscopy data of test sample, wherein laser
The parameter of induced breakdown spectrograph device is vacuum atmosphere, and time delay is set as 3 μ s, range of laser energy 50-100mJ, product
It is 15 μ s between timesharing, detector gain 2000, depth of focus 2mm, the angle of laser and test sample is 90 °.Then pick out
The characteristic spectral line information of nitrogen, P elements and potassium element in test sample, the wavelength of the wherein characteristic spectral line of nitrogen are
746.64nm, the wavelength of the characteristic spectral line of P elements is 213.51nm and 253.48nm, and the wavelength of the characteristic spectral line of potassium element is
404.21nm and 404.61nm.By the intensity of the characteristic spectral line of nitrogen, P elements and potassium element, it is input to calmly respectively afterwards
In the calibration model for the respective element established in mark embodiment, i.e. the intensity of the characteristic spectral line of nitrogen is input to calibration and implements
In the nitrogen model established in example, the intensity of the characteristic spectral line of P elements is input to the phosphorus member established in calibration embodiment
In prime model, the intensity of the characteristic spectral line of potassium element is input in the potassium element model established in calibration embodiment, and is obtained
The content of nitrogen, P elements and potassium element in test sample.The fertilizer sample carries out 3 repetitions and detects, and takes it averagely to tie
Fruit and the results are shown in table 1 below.
Testing example 2
Retest embodiment 1, difference is, nitrogen, P elements and Determination of Potassium are different in fertilizer sample,
Nitrogen element content is 16.04% wherein in the fertilizer sample of the present embodiment, phosphorus element content 6.79%, and Determination of Potassium is
9.98%.
Testing example 3
Retest embodiment 1, difference is, nitrogen, P elements and Determination of Potassium are different in fertilizer sample,
Nitrogen element content is 20.05% wherein in the fertilizer sample of the present embodiment, phosphorus element content 13.55%, and Determination of Potassium is
15.52%.
Fertilizer sample nutrient content test result in 1 testing example 1-3 of table
As seen from the above table, the present invention, which is used for the quick method for detecting fertilizer nutrient content, can detect nitrogen in fertilizer sample at the same time
The content of element, P elements and potassium element, and relative error is small, is held in less than 10%, particularly the opposite of P elements is missed
Difference is less than 5%, so that a variety of nutrient contents in fertilizer can effectively and quickly be detected by demonstrating the method for the present invention.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula make a change and modification.Therefore, the invention is not limited in embodiment disclosed and described above, to the one of invention
A little modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, although used in this specification
Some specific terms, but these terms are merely for convenience of description, do not limit the present invention in any way.
Claims (8)
- A kind of 1. method for being used to quickly detect fertilizer nutrient content, it is characterised in that the described method comprises the following steps：(1) test sample is prepared：Weigh chemical fertilizer sample and be ground, then using tabletting machine, obtain test sample；(2) spectroscopic data is gathered：Data acquisition is carried out to test sample using laser induced breakdown spectroscopy system, obtains test specimens This laser induced breakdown spectroscopy data；(3) selected characteristic spectral line：With reference to NIST (National Institute of Standards and Technology Atomic Spectra Database) the characteristic spectral line information of nitrogen, P elements and potassium element in database, to fertilizer into Point qualitative analysis is carried out, pick out the characteristic spectral line information of nitrogen in test sample, P elements and potassium element；(4) calibration model is established：Several fertilizer samples known to selected nitrogen, P elements and Determination of Potassium are simultaneously ground Mill, then using tabletting machine, obtains calibration sample, afterwards using laser induced breakdown spectroscopy system to every kind of calibration sample It is detected to obtain the laser induced breakdown spectroscopy data of every kind of calibration sample, then respectively with nitrogen, P elements and potassium Constituent content is dependent variable, using the laser induced breakdown spectroscopy intensity of measured respective element as independent variable, with the side of fitting Method establishes functional relation i.e. nitrogen model, phosphorus element content and the phosphorus member between nitrogen element content and the intensity of spectral line of nitrogen The letter between functional relation, that is, P elements model and Determination of Potassium and the intensity of spectral line of potassium element between the intensity of spectral line of element Number relation, that is, potassium element model；(5) component in test of quantitative analysis sample：Extract nitrogen in the test sample in the step (3), P elements With the intensity of the characteristic spectral line of potassium element, and the calibration model for the respective element established is entered into the step (4) In, i.e., the intensity of the characteristic spectral line of the nitrogen in test sample is input to the nitrogen model established in the step (4) In, the intensity of the characteristic spectral line of the P elements in test sample is input in the P elements model established in the step (4), The intensity of the characteristic spectral line of potassium element in test sample is input in the potassium element model established in the step (4), i.e., The content of nitrogen in test sample, P elements and potassium element can quickly be obtained.
- 2. according to the method described in claim 1, it is characterized in that, the particle diameter in the step (1) after the grinding of chemical fertilizer sample is 20-100μm。
- 3. according to the method described in claim 1, it is characterized in that, it is by chemical fertilizer that tablet press machine, which carries out tabletting, in the step (1) Sample tabletting is more preferably circular into circular, square, rectangle or other shapes.
- 4. according to the method described in claim 1, it is characterized in that, it is by chemical fertilizer that tablet press machine, which carries out tabletting, in the step (1) Sample tabletting is into circular and its a diameter of 6-16mm.
- 5. according to the method described in claim 1, it is characterized in that, the thickness of test sample is after tabletting in the step (1) 2-8mm。
- 6. according to the method described in claim 1, it is characterized in that, laser induced breakdown spectroscopy system is utilized in the step (2) The test condition of system collection spectroscopic data is under vacuum atmosphere, and time delay is set as 2-8 μ s, range of laser energy 50- 100mJ, the time of integration are 10-20 μ s, detector gain 2000, depth of focus 2mm, and the angle of laser and test sample is 90 °.
- 7. according to the method described in claim 6, it is characterized in that, the wavelength of the characteristic spectral line of the nitrogen is 746.64nm, the wavelength of the characteristic spectral line of the P elements are 213.51nm and 253.48nm, the characteristic spectral line of the potassium element Wavelength be 404.21nm and 404.61nm.
- 8. according to the method described in claim 1, it is characterized in that, the nitrogen model established in the step (4) is Y= 0.003791 × a-0.436, wherein a are wavelength for the energy value at 746.64nm；P elements model is Y=-0.02995 × a+ 0.01631 × b-0.8496, a be wavelength be 213.51nm place energy value, b be wavelength be 253.48nm at energy value；Potassium Element model is Y=0.006376 × a-0.004192 × b-0.145, and wherein a is wavelength for the energy value at 404.21nm, b It is wavelength for the energy value at 404.61nm.
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| CN109187498A (en) * | 2018-08-31 | 2019-01-11 | 浙江大学 | The rapid detection method of soil calcium constituent based on conllinear double-pulse laser induced breakdown spectrum |
| CN110455752A (en) * | 2019-08-14 | 2019-11-15 | 重庆科正花果苗木有限责任公司 | A kind of the fertilizer detection system and method for the citrus sapling multiplication based on Internet of Things |
| CN110646407A (en) * | 2019-11-20 | 2020-01-03 | 中国海洋大学 | Method for rapidly detecting content of phosphorus element in aquatic product based on laser-induced breakdown spectroscopy technology |
| CN111103279A (en) * | 2018-10-26 | 2020-05-05 | 深圳市芭田生态工程股份有限公司 | Preparation method of sample for LIBS detection and detection method of fertilizer nutrients |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661935A (en) * | 2012-05-15 | 2012-09-12 | 广东电网公司电力科学研究院 | LIBS (Laser-induced Breakdown Spectroscopy) belt type powdery material detector |
| CN103185708A (en) * | 2011-12-31 | 2013-07-03 | 中国农业机械化科学研究院 | Online detection apparatus and method for soil elements |
| CN205067178U (en) * | 2015-09-14 | 2016-03-02 | 国麒光电科技（天津）有限公司 | A automatic system appearance system for laser induction puncture spectrum appearance |
| CN106124482A (en) * | 2016-06-15 | 2016-11-16 | 安徽有果信息技术服务有限公司 | A kind of composite heat transfer N-P-K content online measuring technique |
-
2017
- 2017-10-18 CN CN201710972126.9A patent/CN107966430A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103185708A (en) * | 2011-12-31 | 2013-07-03 | 中国农业机械化科学研究院 | Online detection apparatus and method for soil elements |
| CN102661935A (en) * | 2012-05-15 | 2012-09-12 | 广东电网公司电力科学研究院 | LIBS (Laser-induced Breakdown Spectroscopy) belt type powdery material detector |
| CN205067178U (en) * | 2015-09-14 | 2016-03-02 | 国麒光电科技（天津）有限公司 | A automatic system appearance system for laser induction puncture spectrum appearance |
| CN106124482A (en) * | 2016-06-15 | 2016-11-16 | 安徽有果信息技术服务有限公司 | A kind of composite heat transfer N-P-K content online measuring technique |
Non-Patent Citations (3)
| Title |
|---|
| 余洋 等: "激光诱导击穿光谱单变量及多元线性回归方法研究", 《激光与光电子学进展》 * |
| 卢伟业 等: "复合肥氮磷钾元素含量的激光诱导击穿光谱同步测量", 《中国激光》 * |
| 陈凯: "基于激光诱导击穿光谱的复混肥成分分析研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108827942A (en) * | 2018-08-31 | 2018-11-16 | 浙江大学 | The rapid detection method of soil ferro element based on conllinear double-pulse laser induced breakdown spectrum |
| CN108872199A (en) * | 2018-08-31 | 2018-11-23 | 浙江大学 | The rapid detection method of soil magnesium elements based on conllinear double-pulse laser induced breakdown spectrum |
| CN109001186A (en) * | 2018-08-31 | 2018-12-14 | 浙江大学 | The rapid detection method of soil manganese element based on conllinear double-pulse laser induced breakdown spectrum |
| CN109030428A (en) * | 2018-08-31 | 2018-12-18 | 浙江大学 | The rapid detection method of soil potassium element based on conllinear double-pulse laser induced breakdown spectrum |
| CN109115733A (en) * | 2018-08-31 | 2019-01-01 | 浙江大学 | The rapid detection method of soil sodium element based on conllinear double-pulse laser induced breakdown spectrum |
| CN109187498A (en) * | 2018-08-31 | 2019-01-11 | 浙江大学 | The rapid detection method of soil calcium constituent based on conllinear double-pulse laser induced breakdown spectrum |
| CN111103279A (en) * | 2018-10-26 | 2020-05-05 | 深圳市芭田生态工程股份有限公司 | Preparation method of sample for LIBS detection and detection method of fertilizer nutrients |
| CN110455752A (en) * | 2019-08-14 | 2019-11-15 | 重庆科正花果苗木有限责任公司 | A kind of the fertilizer detection system and method for the citrus sapling multiplication based on Internet of Things |
| CN110646407A (en) * | 2019-11-20 | 2020-01-03 | 中国海洋大学 | Method for rapidly detecting content of phosphorus element in aquatic product based on laser-induced breakdown spectroscopy technology |
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