CN103592225B - Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof - Google Patents
Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof Download PDFInfo
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- CN103592225B CN103592225B CN201310529607.4A CN201310529607A CN103592225B CN 103592225 B CN103592225 B CN 103592225B CN 201310529607 A CN201310529607 A CN 201310529607A CN 103592225 B CN103592225 B CN 103592225B
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Abstract
Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property rapid assay methods thereof, be provided with light source generator, grating, monochromator and optical chopper；Feature is to be additionally provided with optoacoustic adnexa or mirror based fiber optica adnexa, connects high-pure helium gas tank by rigid rubber pipe, and the light inlet of optoacoustic adnexa and monochromator light-emitting window are positioned on same optical axis；Its output all connects lock-in amplifier with the output of described optical chopper, and lock-in amplifier connects computer.Loading pedotheque in photoacoustic cell, put in optoacoustic adnexa, be adjusted to purge mode, open high-pure helium air valve, seal photoacoustic cell after purging, parameter can start to gather soil spectrum after having set.Compared with the present invention analyzes method with conventional soil, have an advantage in that and can various ingredients in soil be carried out qualitative and quantitative analysis simultaneously, increase substantially the efficiency of soil analysis, pedotheque is not produced any destruction, simple to operate, highly sensitive, detection limit is low, environmentally safe, measurement result favorable reproducibility.
Description
Technical field
The invention belongs to measuring instrument technical field, be specifically related to a kind of soil infrared photoacoustic spectra Quick testing instrument.The invention still further relates to the soil physico-chemical property rapid assay methods of this soil infrared photoacoustic spectra Quick testing instrument.
Background technology
Soil investigation is that one important but the work of complexity, traditional Analysis On Physical And Chemical Property is all to utilize chemical method, not only waste time and energy, and destroy pedotheque to a certain extent, have ignored soil to interact as its internal complexity of an entirety, thus cause between measurement result and actual value, there is certain deviation.In order to preferably recognize and utilize soil resource, needing application with the analysis method of soil generally object of study, the soil investigation that appears as of infrared spectrum technology provides powerful support.Infrared spectrum technology is capable of the absorption to the mensuration of soil constitution being functional group based on different material to specific wavelength, resolves spectrum in conjunction with the most isoplastic fundamental vibration frequency, carries out qualitative and quantitative analysis soil different component.
The appearance of infrared transmission spectra the earliest, and is gradually widely used, the ratio of infrared absorption intensity of its direct measuring samples, is preferably applied to soil qualitative analysis.But owing to the transmission of soil is the lowest, this method is difficult to the quantitative analysis to soil, and therefore infrared reflectance spectroscopy is entered again soil investigation field.Infrared Reflective Spectra can be divided into again the different technologies such as direct reflection spectrum, diffuse-reflectance spectrum and attenuated total reflectance spectrum, use different infrared reflectance spectroscopies to achieve according to object of study to research and analyse soil fertility, organic matter and chemism etc. are many, although Infrared Reflective Spectra is widely used in agrology, still suffer from a lot of problem, such as sensitivity is the highest, and accuracy is relatively low.
The appearance of infrared photoacoustic spectra overcomes the many difficulties in infrared transmission spectra and infrared reflectance spectroscopy, measure without sample pre-treatments, sample is not produced any loss, and measure highly sensitive, spectrum stability is good, many kinds of substance can be analyzed simultaneously, have huge application potential in agrology research field.
Infrared spectral region can be divided into far infrared, mid-infrared and near-infrared zones of different according to wavelength, and wherein the spectral energy of near infrared band is high, has preferable excitation to characteristic group, is therefore widely used in soil fertility and structural property are studied.
Utilize near-infrared photoacoustic spectroscopy technology, it is possible to obtain accurate soil near-infrared photoacoustic spectroscopy figure, in conjunction with Mathematical Method, thus realize qualitative and quantitative analysis multi-component to soil, be quick, accurate a, technological means for environmental protection in soil investigation.
Summary of the invention
It is an object of the invention to provide one and measure quick, highly sensitive, detection limit soil infrared photoacoustic spectra Quick testing instrument low, nondestructive to sample, problem traditional chemical analysis method operation complexity can be overcome, sample being damaged analysis.The invention still further relates to the soil physico-chemical property rapid assay methods of this soil infrared photoacoustic spectra Quick testing instrument.
The technical scheme completing foregoing invention task is, a kind of soil near-infrared photoacoustic spectroscopy Quick testing instrument, is provided with light source generator, grating, monochromator and optical chopper；It is characterized in that, apply optoacoustic adnexa (or mirror based fiber optica adnexa), this optoacoustic adnexa (or mirror based fiber optica adnexa) connects high-pure helium gas tank by rigid rubber pipe, and meanwhile, the light inlet of this optoacoustic adnexa (or mirror based fiber optica adnexa) and described monochromator light-emitting window are positioned on same level optical axis；The output of this optoacoustic adnexa (or mirror based fiber optica adnexa) is all connected with lock-in amplifier with the output of described optical chopper, lock-in amplifier connects computer, and then by the modulating frequency of chopper regulation incident illumination, and combine the selection and optimization of lambda1-wavelength, it is achieved the quick mensuration of different soils physicochemical property.
In other words, a kind of soil near-infrared photoacoustic spectroscopy Quick testing instrument that the present invention proposes, mainly including light source generator, optical chopper, monochromator, optoacoustic adnexa, hand-operated lifting platform, computer, lock-in amplifier, light source generator connects stabilized current supply, is fixed on pedestal with monochromator；Optoacoustic adnexa (or mirror based fiber optica adnexa) light inlet and monochromator light-emitting window are positioned at same level, connect high-pure helium gas tank by rigid rubber pipe, and are connected with lock-in amplifier and computer；Lock-in amplifier connects computer.
In the present invention, optical chopper includes grating and impulse controller, and grating is positioned at the light-emitting window of light source generator, and the light inlet of alignment monochromator, impulse controller is connected with grating and lock-in amplifier respectively.
In the present invention, optoacoustic adnexa (or mirror based fiber optica adnexa) is fixed on above hand-operated lifting platform.
The technical scheme completing second invention task of the application is, the soil rapid assay methods of above-mentioned soil near-infrared photoacoustic spectroscopy Quick testing instrument, it is characterised in that step is as follows:
(1). appropriate pedotheque puts into photoacoustic cell (loading the pedotheque bottom less than 2/3 height and covering in photoacoustic cell)；
If (2). adnexa is optoacoustic adnexa, and optoacoustic adnexa is adjusted to purge mode, opens high-pure helium air valve, uses high-purity helium purge, removes the steam in photoacoustic cell and carbon dioxide；
If adnexa is fiber reflection adnexa, then purges with High Purity Nitrogen, remove the water in light path and carbon dioxide；
(3). immediately seal photoacoustic cell；
(4). opening light source, its white light sent becomes modulated near infrared light under the effect of optical chopper and grating；
(5). the pedotheque in photoacoustic cell absorbs the near infrared light of specific wavelength and produces heat, and the helium being conducted to around sample causes periodic pressure oscillation；
. this periodic pressure oscillation after lock-in amplifier is shown as pressure signal value in a computer form with spectrum show.
Compared with the present invention analyzes method with conventional soil, have an advantage in that and can various ingredients in soil be carried out qualitative and quantitative analysis simultaneously, soil sample to high-selenium corn, accuracy and sensitivity significantly improve, and increase substantially soil analysis efficiency, pedotheque is not produced any destruction, simple to operate, highly sensitive, detection limit is low, environmentally safe, measurement result favorable reproducibility.
Accompanying drawing explanation
Fig. 1 is the design drawing of this light.Complete equipment is shown by light source module, reference path module, detection module (photo-acoustic detection adnexa and reflection detection accessory) and spectrum and is analyzed module.By spectrum analysis by software soil infrared spectrum information system.
Fig. 2 is the structural representation of the present invention.
Detailed description of the invention
Embodiment 1, soil near-infrared photoacoustic spectroscopy Quick testing instrument, as shown in Figure 1 and Figure 2, the present invention includes that in figure, label is respectively as follows: light source generator 1, grating 2, monochromator 3, hand-operated lifting platform 4, optoacoustic adnexa or mirror based fiber optica 5, computer 6, lock-in amplifier 7, optical chopper 8, stabilized current supply 9, high-pure helium gas tank 10.
Light source uses bromine tungsten filament lamp light source (or tunable laser source), bromine tungsten filament lamp light source low price, the model used is to stand upright Chinese light LHT150 QTH in Beijing, built-in 150W bromine tungsten filament lamp bulb, this light source stability is good, life-span is long, is the perfect light source of Visible-to-Near InfaRed wave band, connects supporting LPT150 stabilized current supply.Grating is fixed on the light-emitting window of bromine tungsten filament lamp light source, and chopper wheel uses 30/25 slit specification, and connecting model is the optical chopper of SR540, and modulating frequency may be up to 3.7 kHz.Monochromator uses the Chinese light Omni-λ 150 that stands upright, and is fixed on same pedestal with bromine tungsten filament lamp light source, the light-emitting window of its light inlet alignment bromine tungsten filament lamp light source, and connects computer by USB port.Optoacoustic adnexa model is the Model 300 that METC company of the U.S. produces, it is fixed on hand-operated lifting platform, adjusting highly makes optoacoustic adnexa light inlet be generally aligned in the same plane with monochromator light-emitting window, ensureing that near infrared light enters optoacoustic adnexa, optoacoustic adnexa is purged into QI KOU by effusion meter connection high-pure helium gas tank simultaneously.Lock-in amplifier uses SR810, connects optical chopper, computer and optoacoustic adnexa respectively, and in photoacoustic cell, pressure change signal is converted into the signal of telecommunication according to optoacoustic transfer principle by lock-in amplifier, and is shown as spectrum on computers.
The principle that the present invention gathers soil near-infrared photoacoustic spectroscopy is as follows: load the pedotheque bottom less than 2/3 height and covering in photoacoustic cell, put in optoacoustic adnexa, optoacoustic adnexa is adjusted to purge mode, open high-pure helium air valve, purging with the flow of 0.5-2 mL/s and seal photoacoustic cell after 10 s, set modulating frequency respectively as 20-100 Hz, resolution is 4-8 nm, wave-length coverage 400-2500 nm, parameter can start to gather soil spectrum after having set.
The main performance of present device is as follows:
(1) wave-length coverage 800-2500 nm, bandwidth is minimum up to 0.3 nm；
(2) signal detection passage: 1 reflection optical channel and 1 optoacoustic passage；
(3) reflectance spectrum investigative range: 400-1700 nm, minimum detection accuracy reaches 0.1 nm, optical fiber probe and fiberoptic connection；
Fully digitalization electronic processing system, resolution reaches 262,144 roads；
(4) photo-acoustic detection sensitivity be 65 mV/Pa, 5 Hz to 20 kHz, 12 times of gains；
(5) phase-locked amplification frequency adjustable extent contains 1 mHz-102.4 kHz, and time constant contains 10 s to 30 ks.
The soil physico-chemical property such as following table that this equipment can detect:
| Soil property parameter | Detection error RMSE | Linear dependence R2 |
| Organic (g kg-1) | <2.00 | >0.80 |
| pH | <0.25 | >0.80 |
| Mineral (%) | <5.0 | >0.75 |
| Full nitrogen (g kg-1) | <0.20 | >0.80 |
| Full phosphorus (g kg-1) | <0.15 | >0.75 |
In sum, this equipment has simple to operate, measure quickly, the advantages such as high sensitivity, do not produce any destruction, it is possible to be analyzed the various ingredients in soil to pedotheque simultaneously during mensuration, in addition, inapplicable any chemical substance during spectra collection, and do not produce any pollutant, it is efficient, accurate, soil analysis means for environmental protection.
Claims (4)
1. a soil rapid assay methods for soil near-infrared photoacoustic spectroscopy Quick testing instrument, described soil near-infrared photoacoustic spectroscopy Quick testing instrument, it is provided with light source generator, grating, monochromator and optical chopper；Being additionally provided with optoacoustic adnexa or mirror based fiber optica adnexa, this optoacoustic adnexa or mirror based fiber optica adnexa connect high-pure helium gas tank by rigid rubber pipe, and meanwhile, the light inlet of this optoacoustic adnexa or mirror based fiber optica adnexa and described monochromator light-emitting window are positioned on same optical axis；The output of this optoacoustic adnexa or mirror based fiber optica adnexa all connects lock-in amplifier with the output of described optical chopper, and this lock-in amplifier connects computer；
It is characterized in that, step is as follows:
(1). appropriate pedotheque puts into photoacoustic cell；
If (2). adnexa is optoacoustic adnexa, and optoacoustic adnexa is adjusted to purge mode, opens high-pure helium air valve, to the high-purity helium purge of optoacoustic adnexa, removes the steam in photoacoustic cell and carbon dioxide；
If adnexa is mirror based fiber optica adnexa, then purges with High Purity Nitrogen, remove the water in light path and carbon dioxide；
(3). immediately seal photoacoustic cell；
(4). opening light source, its white light sent becomes modulated near infrared light under the effect of optical chopper and grating；
(5). the pedotheque in photoacoustic cell absorbs the near infrared light of specific wavelength and produces heat, and the helium being conducted to around sample causes periodic pressure oscillation；
. this periodic pressure oscillation after lock-in amplifier is shown as pressure signal value in a computer form with spectrum show.
The soil rapid assay methods of soil near-infrared photoacoustic spectroscopy Quick testing instrument the most according to claim 1, it is characterized in that, the (1) described appropriate pedotheque of step puts into photoacoustic cell, refers to: load in photoacoustic cell less than 1/2 height and the pedotheque bottom covering.
The soil rapid assay methods of soil near-infrared photoacoustic spectroscopy Quick testing instrument the most according to claim 1, it is characterised in that step is (2) described to the high-purity helium purge of optoacoustic adnexa, is to purge 10 s with the flow of 0.5-2 mL/s.
4. according to the soil rapid assay methods of the soil near-infrared photoacoustic spectroscopy Quick testing instrument one of claim 1-3 Suo Shu, it is characterized in that, the (4) described operation of step is: set modulating frequency respectively as 20-100 Hz, resolution is 4-8 nm, wave-length coverage 400-2500 nm, parameter can start to gather soil spectrum after having set.
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| CN105445218B (en) * | 2015-11-25 | 2018-12-18 | 中国科学院南京土壤研究所 | The method for building up of middle infrared spectrum rapeseed protein content detection adaptive model |
| CN106269826A (en) * | 2016-09-26 | 2017-01-04 | 山东省科学院海洋仪器仪表研究所 | Automatization's Ecosystem restoration system of a kind of soil and method |
| CN107884358B (en) * | 2017-11-07 | 2020-04-21 | 重庆昆顶环保科技有限公司 | Portable soil nutrient detection device |
| CN110208195A (en) * | 2019-06-25 | 2019-09-06 | 南京无书化工有限公司 | A kind of optoacoustic spectroscopy single channel locking phase amplifying device and method for gas detection |
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| CN101153860A (en) * | 2006-09-27 | 2008-04-02 | Ir微系统股份有限公司 | Gas detection method and gas detection device |
| CN101441179A (en) * | 2008-12-11 | 2009-05-27 | 华南师范大学 | Light sound acidity-basicity imaging method and apparatus based on reagent colour development difference |
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| JP4751271B2 (en) * | 2006-08-11 | 2011-08-17 | 東芝メディカルシステムズ株式会社 | Photoacoustic analysis method and photoacoustic analysis apparatus for measuring the concentration of an analyte in a specimen tissue |
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| CN101153860A (en) * | 2006-09-27 | 2008-04-02 | Ir微系统股份有限公司 | Gas detection method and gas detection device |
| CN101441179A (en) * | 2008-12-11 | 2009-05-27 | 华南师范大学 | Light sound acidity-basicity imaging method and apparatus based on reagent colour development difference |
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