CN103592225A - Soil infrared photoacoustic spectrum rapid determinator and soil physical and chemical property determination method - Google Patents

Soil infrared photoacoustic spectrum rapid determinator and soil physical and chemical property determination method Download PDF

Info

Publication number
CN103592225A
CN103592225A CN201310529607.4A CN201310529607A CN103592225A CN 103592225 A CN103592225 A CN 103592225A CN 201310529607 A CN201310529607 A CN 201310529607A CN 103592225 A CN103592225 A CN 103592225A
Authority
CN
China
Prior art keywords
soil
annex
photoacoustic
infrared
light
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201310529607.4A
Other languages
Chinese (zh)
Other versions
CN103592225B (en
Inventor
杜昌文
王娇
周健民
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Soil Science of CAS
Original Assignee
Institute of Soil Science of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Soil Science of CAS filed Critical Institute of Soil Science of CAS
Priority to CN201310529607.4A priority Critical patent/CN103592225B/en
Publication of CN103592225A publication Critical patent/CN103592225A/en
Application granted granted Critical
Publication of CN103592225B publication Critical patent/CN103592225B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention discloses a soil infrared photoacoustic spectrum rapid determinator and a soil physical and chemical property determination method. The soil infrared photoacoustic spectrum rapid determinator is provided with a light source generator, a raster, a monochromator and an optical chopper; the soil infrared photoacoustic spectrum rapid determinator is characterized by also being provided with a photoacoustic attachment or a reflective optical fiber attachment, the photoacoustic attachment or the reflective optical fiber attachment is connected with a high-purity helium tank through a hard rubber hose, a light inlet of the photoacoustic attachment and a light outlet of the monochromator are located on a same optical axis; and the output of the photoacoustic attachment or the reflective optical fiber attachment and the output of the optical chopper are connected to a phase-locking amplifier, and the phase-locking amplifier is connected to a computer. The soil physical and chemical property determination method is as follows: putting a soil sample into a photoacoustic cell, putting the photoacoustic cell into the photoacoustic attachment, turning to a purging mode, turning on a high-purity helium valve, after purging, sealing the photoacoustic cell, when parameter setting is completed, starting to collect a soil spectrum. Compared with a traditional soil analysis method, the soil physical and chemical property determination method has the advantages of simultaneous qualitative and quantitative analysis on multiple components in soil, greatly improved soil analysis efficiency, no damage on soil samples, simple operation, high sensitivity, low detection limit, no pollution to the environment and good determination result reproducibility.

Description

Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof
Technical field
The invention belongs to surveying 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 an important but complicated job, traditional Analysis On Physical And Chemical Property is all to utilize chemical method, not only waste time and energy, and destroyed to a certain extent pedotheque, ignore soil and made the complexity of as a whole its inside and interact, thereby caused existing between measurement result and actual value certain deviation.In order to be better familiar with and to utilize soil resource, need application to take the analytical approach that soil integral body is research object, the soil investigation that appears as of infrared spectrum technology provides powerful support.It is the absorption to specific wavelength of functional group based on different material that infrared spectrum technology can be realized the mensuration of soil constitution, in conjunction with not isoplastic fundamental vibration frequency, resolves spectrum, and soil different component is carried out qualitative and quantitative analysis.
The appearance of infrared transmission spectra the earliest, and is widely used gradually, and it directly measures the ratio of infrared absorption intensity of sample, is applied to preferably soil qualitative analysis.But because the transmission of soil is very low, this method is difficult to realize the quantitative test to soil, so infrared reflectance spectroscopy is entered into again soil investigation field.Infrared Reflective Spectra can be divided into again the different technologies such as mirror-reflection spectrum, diffuse reflection spectrum and attenuated total reflection spectrum, according to research object, adopt different infrared reflectance spectroscopies to realize many-sided researching and analysing such as soil fertility, organic matter and chemisms, although Infrared Reflective Spectra is widely used in pedology, still there are a lot of problems, for example sensitivity is not high, and accuracy is relatively low etc.
The appearance of infrared photoacoustic spectra has overcome the many difficulties in infrared transmission spectra and infrared reflectance spectroscopy, mensuration is without sample pre-treatments, sample is not produced to any loss, and measure highly sensitive, spectrum stability is good, can analyze many kinds of substance simultaneously, in pedology research field, have huge application potential.
Infrared spectral region according to wavelength can be divided into far infrared, in infrared and near infrared zones of different, therefore wherein the spectral energy of near infrared band is high, and characteristic group is had to good excitation, is widely used in soil fertility and structural property research.
Utilize near-infrared photoacoustic spectroscopy technology, can obtain accurate soil near-infrared photoacoustic spectroscopy figure, in conjunction with Mathematical Method, thereby realize the multi-component qualitative and quantitative analysis of soil, be in soil investigation one fast, accurately, the technological means of environmental protection.
Summary of the invention
The object of the present invention is to provide that a kind of measurement is quick, highly sensitive, detectability is low, to the nondestructive soil infrared photoacoustic spectra of sample Quick testing instrument, can overcome traditional chemical analytical approach complicated operation, sample be diminished to the problem of 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 that completes foregoing invention task is that 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, applied optoacoustic annex (or mirror based fiber optica annex), this optoacoustic annex (or mirror based fiber optica annex) connects high-pure helium gas tank by rigid rubber pipe, meanwhile, the light inlet of this optoacoustic annex (or mirror based fiber optica annex) and described monochromator light-emitting window are positioned on same level optical axis; The output of this optoacoustic annex (or mirror based fiber optica annex) is all connected lock-in amplifier with the output of described optical chopper, lock-in amplifier connects computing machine, and then by chopper, regulate the modulating frequency of incident light, and in conjunction with the selection and optimization of lambda1-wavelength, realize the Fast Measurement 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 comprise light source generator, optical chopper, monochromator, optoacoustic annex, hand-operated lifting platform, computing machine, lock-in amplifier, light source generator connects stabilized current supply, is fixed on pedestal with monochromator; Optoacoustic annex (or mirror based fiber optica annex) light inlet and monochromator light-emitting window are positioned at same level, by rigid rubber pipe, connect high-pure helium gas tank, and are connected with computing machine with lock-in amplifier; Lock-in amplifier connects computing machine.
In the present invention, optical chopper comprises grating and impulse controller, and grating is positioned at the light-emitting window of light source generator, aims at the light inlet of monochromator, and impulse controller is connected with lock-in amplifier with grating respectively.
In the present invention, optoacoustic annex (or mirror based fiber optica annex) is fixed on above hand-operated lifting platform.
The technical scheme that completes second invention task of the application is, the soil rapid assay methods of above-mentioned soil near-infrared photoacoustic spectroscopy Quick testing instrument, is characterized in that, step is as follows:
(1). appropriate pedotheque is put into photoacoustic cell (photoacoustic cell packs the pedotheque that is no more than 2/3 height and covers bottom into);
(2). if annex is optoacoustic annex, and optoacoustic annex is adjusted to purge mode, opens high-pure helium air valve, uses high-purity helium purge, removes water vapor and carbon dioxide in photoacoustic cell;
If annex is fiber reflection annex, with High Purity Nitrogen, purge, remove water and carbon dioxide in light path;
(3). immediately seal photoacoustic cell;
(4). open light source, its white light sending becomes the near infrared light that can modulate 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 conduction causes periodic pressure surge to sample helium around;
. this periodic pressure surge after lock-in amplifier is shown as pressure signal value in computing machine the form with spectrum show.
The present invention compares with traditional soil analysis method, its advantage is to various ingredients in soil, to carry out qualitative and quantitative analysis simultaneously, the soil sample that height is absorbed, accuracy and sensitivity significantly improve, and increase substantially soil analysis efficiency, pedotheque is not produced to any destruction, simple to operate, highly sensitive, detectability is low, environmentally safe, measurement result favorable reproducibility.
Accompanying drawing explanation
Fig. 1 is this bright design drawing.Equipment set is shown and analysis module by light source module, reference path module, detection module (photo-acoustic detection annex and reflection detection accessory) and spectrum.By spectral analysis by software soil infrared spectrum infosystem.
Fig. 2 is structural representation of the present invention.
Embodiment
Embodiment 1, soil near-infrared photoacoustic spectroscopy Quick testing instrument, as shown in Figure 1 and Figure 2, the present invention includes number in the figure is respectively: light source generator 1, grating 2, monochromator 3, hand-operated lifting platform 4, optoacoustic annex or mirror based fiber optica 5, computing machine 6, lock-in amplifier 7, optical chopper 8, stabilized current supply 9, high-pure helium gas tank 10.
Light source adopts bromine tungsten filament lamp light source (or tunable laser source), bromine tungsten filament lamp light source low price, the model adopting is Beijing Chinese light LHT150 QTH that stands upright, 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 adopts 30/25 slit specification, the optical chopper that connection model is SR540, and modulating frequency can 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, and its light inlet is aimed at the light-emitting window of bromine tungsten filament lamp light source, and connects computing machine by USB port.Optoacoustic annex model is the Model 300 that U.S. METC company produces, be fixed on hand-operated lifting platform, adjusting highly makes optoacoustic annex light inlet and monochromator light-emitting window be positioned at same plane, guarantee that near infrared light enters optoacoustic annex, optoacoustic annex purging air intake opening connects high-pure helium gas tank by flowmeter simultaneously.Lock-in amplifier adopts SR810, connects respectively optical chopper, computing machine and optoacoustic annex, and in photoacoustic cell, pressure change signal converts electric signal according to optoacoustic transfer principle to 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: in photoacoustic cell, pack the pedotheque that is no more than 2/3 height and covers bottom into, put into optoacoustic annex, optoacoustic annex is adjusted to purge mode, open high-pure helium air valve, after purging 10 s with the flow of 0.5-2 mL/s, seal photoacoustic cell, setting respectively modulating frequency is 20-100 Hz, and resolution is 4-8 nm, wavelength coverage 400-2500 nm, can start to gather soil spectrum after setting parameter completes.
The main performance of present device is as follows:
(1) wavelength coverage 800-2500 nm, minimum 0.3 nm that reaches of bandwidth;
(2) input passage: 1 reflected light passage 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 is 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 μ s to 30 ks.
 
The soil physico-chemical property that this equipment can detect is as following table:
Soil property parameter Detect error RMSE Linear dependence R 2
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 fast, the advantages such as high sensitivity, do not produce any destruction to pedotheque in mensuration process, and can to the various ingredients in soil, analyze simultaneously, in addition, inapplicable any chemical substance in spectra collection process, and do not produce any pollutant, be one efficient, accurately, the soil analysis means of environmental protection.

Claims (10)

1. a soil near-infrared photoacoustic spectroscopy Quick testing instrument, is provided with light source generator, grating, monochromator and optical chopper; It is characterized in that, also be provided with optoacoustic annex or mirror based fiber optica annex, this optoacoustic annex or mirror based fiber optica annex connect high-pure helium gas tank by rigid rubber pipe, and meanwhile, the light inlet of this optoacoustic annex or mirror based fiber optica annex and described monochromator light-emitting window are positioned on same optical axis; This optoacoustic annex or the output of mirror based fiber optica annex and the output of described optical chopper all connect lock-in amplifier, and this lock-in amplifier connects computing machine.
2. soil near-infrared photoacoustic spectroscopy Quick testing instrument according to claim 1, is characterized in that, described light source generator connects stabilized current supply.
3. soil near-infrared photoacoustic spectroscopy Quick testing instrument according to claim 1, is characterized in that, described light source generator and monochromator are fixed on pedestal.
4. soil near-infrared photoacoustic spectroscopy Quick testing instrument according to claim 1, is characterized in that, described optical chopper comprises grating and impulse controller, and grating is wherein positioned at the light-emitting window of light source generator, aims at the light inlet of monochromator; Described impulse controller is connected with lock-in amplifier with grating respectively.
5. soil near-infrared photoacoustic spectroscopy Quick testing instrument according to claim 1, is characterized in that, described optoacoustic annex or mirror based fiber optica annex are fixed on above hand-operated lifting platform.
6. according to the soil near-infrared photoacoustic spectroscopy Quick testing instrument one of claim 1-5 Suo Shu, it is characterized in that, described light source generator adopts bromine tungsten filament lamp light source or tunable laser source.
7. the soil rapid assay methods of soil near-infrared photoacoustic spectroscopy Quick testing instrument claimed in claim 1, is characterized in that, step is as follows:
(1). appropriate pedotheque is put into photoacoustic cell;
(2). if annex is optoacoustic annex, and optoacoustic annex is adjusted to purge mode, opens high-pure helium air valve, uses high-purity helium purge, removes water vapor and carbon dioxide in photoacoustic cell;
If annex is fiber reflection annex, with High Purity Nitrogen, purge, remove water and carbon dioxide in light path;
(3). immediately seal photoacoustic cell;
(4). open light source, its white light sending becomes the near infrared light that can modulate 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 conduction causes periodic pressure surge to sample helium around;
. this periodic pressure surge after lock-in amplifier is shown as pressure signal value in computing machine the form with spectrum show.
8. the soil rapid assay methods of soil near-infrared photoacoustic spectroscopy Quick testing instrument according to claim 7, it is characterized in that, step (1) described appropriate pedotheque is put into photoacoustic cell, refers to: in photoacoustic cell, pack the pedotheque that is no more than 1/2 height and covers bottom into.
9. the soil rapid assay methods of soil near-infrared photoacoustic spectroscopy Quick testing instrument according to claim 7, is characterized in that, step is (2) described uses high-purity helium purge, is that the flow with 0.5-2 mL/s purges 10 s.
10. according to the soil rapid assay methods of the soil near-infrared photoacoustic spectroscopy Quick testing instrument one of claim 7-9 Suo Shu, it is characterized in that, step (4), (5) described operation is: setting respectively modulating frequency is 20-100 Hz, resolution is 4-8 nm, wavelength coverage 400-2500 nm, can start to gather soil spectrum after setting parameter completes.
CN201310529607.4A 2013-10-31 2013-10-31 Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof Active CN103592225B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310529607.4A CN103592225B (en) 2013-10-31 2013-10-31 Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310529607.4A CN103592225B (en) 2013-10-31 2013-10-31 Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof

Publications (2)

Publication Number Publication Date
CN103592225A true CN103592225A (en) 2014-02-19
CN103592225B CN103592225B (en) 2016-08-17

Family

ID=50082452

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310529607.4A Active CN103592225B (en) 2013-10-31 2013-10-31 Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof

Country Status (1)

Country Link
CN (1) CN103592225B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105445218A (en) * 2015-11-25 2016-03-30 中国科学院南京土壤研究所 Establishing method of self-adaptive model for detection of content of protein of rapeseeds on basis of mid-infrared spectrum
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
CN107884358A (en) * 2017-11-07 2018-04-06 成都恒力达科技有限公司 A kind of portable soil nutrient detection means
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

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008045938A (en) * 2006-08-11 2008-02-28 Toshiba Medical Systems Corp Photoacoustic analysis and photoacoustic analyzer for concentration measurement of analysis object in specimen tissue
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008045938A (en) * 2006-08-11 2008-02-28 Toshiba Medical Systems Corp Photoacoustic analysis and photoacoustic analyzer for concentration measurement of analysis object in specimen tissue
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

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
杜昌文等: "土壤的中红外光声光谱研究", 《光谱学与光谱分析》, vol. 28, no. 6, 30 June 2008 (2008-06-30) *
马赵扬等: "土壤碳酸钙中红外光声光谱特征及其应用", 《光谱学与光谱分析》, vol. 32, no. 5, 31 May 2012 (2012-05-31) *
马赵扬等: "黄土的红外反射光谱与红外光声光谱特征及其差异研究", 《土壤》, vol. 44, no. 5, 15 October 2012 (2012-10-15) *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105445218A (en) * 2015-11-25 2016-03-30 中国科学院南京土壤研究所 Establishing method of self-adaptive model for detection of content of protein of rapeseeds on basis of mid-infrared spectrum
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
CN107884358A (en) * 2017-11-07 2018-04-06 成都恒力达科技有限公司 A kind of portable soil nutrient detection means
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

Also Published As

Publication number Publication date
CN103592225B (en) 2016-08-17

Similar Documents

Publication Publication Date Title
CN205374298U (en) Trace gas concentration detection apparatus based on TDLAS
CN102539338B (en) Online monitoring system for gas content in transformer oil by using photoacoustic spectrum
CN202404070U (en) System for monitoring content of gas in transformer oil in online manner
CN103115894B (en) Stable isotopic abundance ratio real-time online monitoring device and method
CN109991189B (en) Fixed point wavelength modulation gas concentration measuring device based on wave number drift correction and measuring method thereof
CN109085133B (en) Off-axis integral cavity atmosphere CH based on real-time reflectivity correction4Concentration measuring device and measuring method thereof
CN104020114A (en) Method for analyzing trace concentration of ammonia gas
CN105158206A (en) Laser detection system for oxygen concentration in tail gas of vehicle-mounted type motor vehicle
Werle et al. Fast chemical sensor for eddy-correlation measurements of methane emissions from rice paddy fields
CN102706831B (en) Frequency-domain Tera Hertz device and method for monitoring CO concentration in coal spontaneous combustion gas
CN103592225B (en) Soil infrared photoacoustic spectra Quick testing instrument and soil physico-chemical property assay method thereof
CN101178153A (en) Locating method and system for city gas pipeline leakage test
CN1928531A (en) Method for detecting methane gas concentration with opto-acoustic spectroscopic method
CN105319183A (en) Detector and detection method for real-time on-line detection of emission smoke intensity of diesel engine
CN201402257Y (en) Gas content on-line monitoring system in transformer oil
CN102288574A (en) Device and method for quantitatively analyzing concentration of multi-component oil fume
CN2426148Y (en) Infrared sulfur dioxide analysis instrument
CN104777145A (en) Raman spectrum system aiming at industrial gas multi-component analysis
CN110907398A (en) Gas concentration measuring method and measuring device
CN104833660B (en) A kind of quartz tuning-fork formula laser breakdown detection means
CN211347925U (en) Gas concentration measuring device
CN112697747A (en) Device and method for detecting decomposer, moisture and purity in sulfur hexafluoride gas
CN204374087U (en) A kind of Raman spectrum test macro based on liquid core waveguide
CN110261349A (en) Gas concentration measuring method and device based on TDLAS
CN108181261A (en) Device based on terahertz time-domain spectroscopy detection mixed gas each component content

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant