CN102879091B - Echelle grating spectrometer, atomic emission spectrometer and spectrum testing method - Google Patents
Echelle grating spectrometer, atomic emission spectrometer and spectrum testing method Download PDFInfo
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Abstract
The invention relates to an echelle grating spectrometer, an atomic emission spectrometer based on the echelle grating spectrometer, and a spectrum testing method by virtue of the atomic emission spectrometer. According to the invention, an echelle grating is adopted as a main dispersion element; light rays emitted by a light source are focused at an incident pinhole by a collecting lens, outgoing beams at the incident pinhole are collimated by a collimating lens and then enter the echelle grating for main chromatic dispersion, then enter a cross dispersing prism for crosswise chromatic dispersion, and are finally imaged onto an image surface of a CCD (Charge Coupled Device) by a focus lens after crosswise chromatic dispersion; through changing the incident angle of the cross dispersing prism, rapid measurement of wave bands within 200 nm and 900 nm can be realized, and the advantages of wide wave band, high resolution, high sensitivity, low noise and small size can be achieved. As shown in the testing results, the test is simple and convenient, the sensitivity is high, the sample consumption is low, and the rapid measurement of multiple elements of the wide wave bands can be realized.
Description
Technical field
The invention belongs to spectral technique field, relate to a kind of echelle spectrometer, particularly a kind of echelle grating based on sectional type, the Atomic Emission Spectrometer AES based on echelle spectrometer and spectrum test method.
Background technology
Inductively coupled plasma atomic emission spectrum analytical technology is one of elemental analysis method being most widely used in Material Field.(Jilin University's Master's thesis " design and research of the ICP-AES spectrometer spectra collection scheme based on CCD " in 2002, University Of Tianjin's Master's thesis " development of ICP scanning spectrometer " in 2007) reported about inductively coupled plasma atomic emission spectrometer (ICP-AES), it utilizes the information that atomic emissions characteristic spectral line provides to carry out ultimate analysis, there is multielement while, quick, direct mensuration, in the commercial production such as metallurgy, petrochemical complex, machine-building, metal processing, bringing into play great function.
Atomic Emission Spectrometer AES has experienced a longer evolution.According to beam splitting system architectural feature, inductively coupled plasma atomic emission spectrometer is divided into: multiple tracks ICP Atomic Emission Spectrometer AES, ICP atomic emissions monochromator, sequential scanning ICP Atomic Emission Spectrometer AES, echelle grating ICP Atomic Emission Spectrometer AES (ICP-Echelle AES).Due to the demand of producing, the just continuous future development to full spectrum direct-reading, intellectuality, miniaturization, harmonic analysis cost of Atomic Emission Spectrometer AES.Beam splitting system is as the core of Atomic Emission Spectrometer AES, directly affect the performance level of instrument, the ICP-AES that the echelle spectrometer of take is spectral module, has the advantages that wavelength band is wide, resolution is high, highly sensitive, has become the emphasis of Atomic Emission Spectral Analysis technical research.At present, both at home and abroad Duo Jia scientific research institution is just making great efforts to develop the ICP-Echelle AES of superior performance.U.S. power & light company (Thermo Scientific), Jena, Germany company (analytikjena), U.S. Li Man-Lai Baisi company (Leeman Labs Inc), U.S. platinum Ai Ermo instrument company (PerkinElmer) develops in succession take the ICP-AES that echelle spectrometer is spectral module, but the restriction due to detection system, and the strict demand of wavelength band, spectral resolution, spectral analysis module-echelle spectrometer still exists more gordian technique to need further research.At present, the ICP-AES of domestic independent development mainly adopts the monochromator of scanning form as its spectral module, and the ICP-AES of this version is not only bulky, and the test duration is long, and test sample consumption is large.
The light channel structure of a kind of echelle spectrometer of application, comprises casing, condenser, incident pin hole, collimating mirror, echelle grating, crossed dispersion prism, focus lamp and planar array detector at present; Described collimating mirror and focus lamp all adopt parabolic lens; Condenser focuses on incident pin hole by incident beam, light beam irradiates collimating mirror from the outgoing of incident pin hole, the directional light of collimating mirror reflection is directly incident on echelle grating surface, the light beam of echelle grating diffraction shines on focus lamp after the reflection of crossed dispersion prism surface, and the light that converges of focus lamp reflection is received by planar array detector.But due to the restriction of detector development level, the spectral range of the echelle spectrometer of this version test is only 400nm-800nm, and its performance still can not meet the test request of ICP-AES.
Summary of the invention
The technical matters that the present invention will solve is to provide a kind of echelle spectrometer that can realize multielement Quick Measurement in 200nm-900nm wavelength band.
In order to solve the problems of the technologies described above, echelle spectrometer of the present invention comprises condenser 1, incident pin hole 2, collimating mirror 3, echelle grating 4, crossed dispersion prism 5, focus lamp 6, casing 7 and planar array detector 8; Characterized by further comprising rotary drive mechanism 13, the turning axle of described rotary drive mechanism 13 is fixedly connected with crossed dispersion prism 5.
The inside surface blacking of described casing 7.
The inside surface of described casing 7 is done coarse processing.
The first diaphragm 10 and the second diaphragm 9 are set respectively before the light entrance face of described echelle grating 4 and crossed dispersion prism 5.
Second technical matters that the present invention will solve is to provide more than one and states the Atomic Emission Spectrometer AES that echelle spectrometer is spectral module.
The 3rd technical matters that the present invention will solve is to provide a kind of method of utilizing above-mentioned Atomic Emission Spectrometer AES to carry out spectrum test.
In order to solve the problems of the technologies described above, the method for utilizing above-mentioned Atomic Emission Spectrometer AES to carry out chemical example spectrum test of the present invention comprises the steps:
One, in echelle spectrometer casing 7, be filled with argon gas;
Two, open the solid state ICP light source 12 of Atomic Emission Spectrometer AES, the angle of utilizing rotary drive mechanism 13 to change crossed dispersion prism 5 makes incident angle within the scope of 27.56 ° ± 0.05 °;
Three, utilize the characteristic spectral line of Ar accurately to locate crossed dispersion prism angle, realize the spectral line of 200nm-400nm wavelength band and demarcate;
Four, chemical example is positioned in sample cell 11, the spectral line of chemical example 200nm-400nm is tested;
Five, the angle of utilizing rotary drive mechanism 13 to change crossed dispersion prism 5 makes incident angle within the scope of 27.10 ° ± 0.02 °;
Six, utilize the characteristic spectral line of Ar accurately to locate the angle of crossed dispersion prism 5, realize the spectral line of 400nm-900nm wavelength band and demarcate;
Seven,, the 400nm-900nm spectral line of chemical example is tested.
Echelle spectrometer is a kind of high resolving power, the novel spectral instrument of high precision, and it adopts echelle grating as principal dispersion element, after the horizontal dispersion of crossed dispersion prism, forms Two-dimensional Overlapping spectrum in image planes.The light that light source sends focuses on incident pin hole through condenser, incident pin hole outgoing beam incides echelle grating and carries out principal dispersion after collimating mirror collimation, then incide crossed dispersion prism and carry out horizontal dispersion, crossed dispersion is imaged in the image planes of CCD by focus lamp.
While carrying out sample test due to ICP-AES, realize several Ten microelements and measure simultaneously, so ICP-AES requires its beam splitting system will have the feature of broadband scope, high spectral resolution concurrently simultaneously, and can avoid the interference of characteristic spectral line between different elements.Echelle spectrometer adopts the version of echelle grating and crossed dispersion prism can meet preferably the demand of ICP-AES to system wavelength band and resolution, and has lower detection limit, can meet the test request of atomic emission spectrum.
Due to the demand of ICP-AES test performance and echelle spectrometer optical property, require system should there is higher signal to noise ratio (S/N ratio), so must effectively suppress system background noise.In system design process, box house adopts even blacking and carries out uneven surface processing.Meanwhile, according to optical texture feature, in internal system echelle grating and crossed dispersion prism place, increase diaphragm, thereby effectively suppressed system parasitic light, reduction system detection limit, raising system signal noise ratio are had to positive effect.
Areal survey formula echelle spectrometer of the present invention, by changing the incident angle of crossed dispersion prism, complete respectively 200nm-400nm, the measurement of 400nm-900nm, in existing detection level situation, realized the Quick Measurement in 200nm-900nm wavelength band.There is broadband, high resolving power, high sensitivity, low noise, small size, meet the application demand of ICP Atomic Emission Spectrometer AES.By areal survey formula echelle spectrometer and solid state ICP combination of light sources, develop echelle grating ICP Atomic Emission Spectrometer AES.After system debug completes, carried out the test analysis of chemical sample, experimental result shows that sectional type echelle spectrometer meets ICP Atomic Emission Spectrometer AES performance requirement, test easy, highly sensitive, sample consumption is few, can realize the Quick Measurement of broadband multielement.
Good effect of the present invention: for the testing requirement of ICP-AES, by Optical Properties, designed a kind of sectional type test type echelle spectrometer.It is combined with solid state ICP light source, design inductively coupled plasma echelle grating Atomic Emission Spectrometer AES (ICP-Echelle AES), and carried out actual test analysis, when can realize multielement, measure, accurate each elemental composition of interpretation, wavelength measurement error is less than 0.01nm.This version has reduced between level time preferably to be disturbed, and has solved the contradictory relation between system integral time and quantum efficiency.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is echelle spectrometer structural representation of the present invention.
Fig. 2 (a), 2 (b) are respectively echelle spectrometer of the present invention two-dimension spectrum images in 200nm-400nm, 400nm-900nm wave band.
Fig. 3 is CCD quantum efficiency curve in the present invention.
Fig. 4 (a), 4 (b) are respectively that ICP-Echelle AES is at the test spectrogram of 200nm-400nm, 400nm-900nm wave band.
Embodiment
As shown in Figure 1, echelle spectrometer of the present invention comprises condenser 1, incident pin hole 2, collimating mirror 3, echelle grating 4, crossed dispersion prism 5, focus lamp 6, casing 7, planar array detector 8 and rotary drive mechanism 13; Described collimating mirror 3 and focus lamp 6 all adopt parabolic lens; Condenser 1 focuses on incident pin hole 2 by incident beam, light beam irradiates collimating mirror 3 from 2 outgoing of incident pin hole, the directional light of collimating mirror 3 reflections is directly incident on the surface of echelle grating 4, the light beam of echelle grating 4 diffraction shines on focus lamp 6 after crossed dispersion prism 5 surface reflections, and the light that converges of focus lamp 6 reflections is received by planar array detector 8; The turning axle of rotary drive mechanism 13 is fixedly connected with crossed dispersion prism 5.Described rotary drive mechanism 13 can adopt any one rotary drive mechanism in prior art, such as motor, motor etc.
The light beam that light source sends enters optical system through incident pin hole 2, along incident pin hole 2 emergent ray directions, apart from f place, place reflection parabolic lens as collimating mirror 3, in collimating mirror 3 reflected light directions, place echelle grating 4, crossed dispersion prism 5 is positioned in echelle grating 4 diffraction light directions, the reflection parabolic lens that the light beam reflecting through crossed dispersion prism 5 shines the place ahead is focus lamp 6, focus lamp 6 focuses on emergent light on planar array detector 8, all minute surfaces (comprise collimating mirror 3, echelle grating 4, crossed dispersion prism 5, the center of centre-height focus lamp 6) and incident pin hole 2 is contour.
Laterally the effect of dispersion is that the spectral order overlaping after echelle grating 4 dispersions is separated, and its dispersive power has no significant effect the spectrally resolved ability of system.But consider that spectral range, level time are disturbed, the problems such as utilization factor of detector, need to carry out accurate Calculation to horizontal dispersion parameters.Because crossed dispersion prism 5 is stronger in shortwave scope internal dispersion ability, long-wave limit internal dispersion ability a little less than, so the in the situation that of identical incident angle, short-wave band level minor tick is larger, and at different levels spacings of long-wave band are nearer, easily produce level time and disturb.Analyze as calculated, knownly under two angles, can cover spectral range 200nm-900nm.First wavelength band is 200nm-400nm, and the incident angle of crossed dispersion prism 5 is 27.56 °; Second wavelength band is 400nm-900nm, and the incident angle of crossed dispersion prism 5 is 27.10 °.Fig. 2 (a) is two-dimension spectrum image distribution in 200nm-400nm wavelength band; Fig. 2 (b) is two-dimension spectrum image distribution in 400nm-900nm wavelength band.
Because ICP-AES has high sensitivity and low detection limit, so having relatively high expectations to detection system.By to echelle spectrometer performance evaluation, native system selects highly sensitive ultraviolet enhancement area array CCD camera as the planar array detector 8 of system, CCD chip is within the scope of 200nm-850nm, there is more uniform quantum efficiency, its efficiency curve is as shown in curve III in Fig. 3 (in figure: I-medium wave segment type efficiency curve, II-broadband type efficiency curve, III-ultraviolet type efficiency curve, IV-non-film-coating type efficiency curve).Meanwhile, this CCD has lower dark current noise and reads noise, can freeze to-70 ℃ during work, and by are set different integral time, this detection system can meet the test of feeble signal.
Owing to the invention belongs to non-solid-state measurement, in test process, need to rotate crossed dispersion prism 5 and complete the spectral line measurement within the scope of 200nm-900nm.In order to guarantee the accuracy of test, in each test process, need spectrogram position to demarcate.In spectrogram calibration process, echelle spectrometer applying argon gas is to complete the measurement of ultraviolet band.By analyzing known its characteristic spectral line of characteristic spectral line of Ar, be distributed between 300nm-520nm, can be used for realizing 200nm-400nm, the spectral line of two wavelength band of 400nm-900nm is demarcated.The present invention utilizes the characteristic spectral line of Ar accurately to locate the angle of crossed dispersion prism 5, and completion system parameter is determined and adjusts.The present invention carries out test analysis to chemical sample, and the two-dimension spectrum information of taking in experiment is as Fig. 4 (a), 4(b) as shown in.
By two-dimentional spectrogram reductive agent, calculate, with the characteristic wavelength of Ar element, system is demarcated.After demarcation to Se in solution, Zn, Mn, Cu, Ba, Mg, Ca, Si, C, K, Na element is tested, its test result is as shown in table 1.Every kind of unit have various features spectral line, but it detects the difference that existence is larger, this experiment only provide characteristic spectral line energy more by force, the characteristic spectral line calibration result comparatively easily distinguished.From experimental result, can find out that instrument all has less wavelength measurement error (<0.01nm) in whole wavelength band, can meet the demand of Atomic Emission Spectral Analysis.
In test process, echelle spectrometer applying argon gas is to complete the measurement of ultraviolet band, by analyzing known its characteristic spectral line of characteristic spectral line of Ar, be distributed between 300nm-520nm, can be used for realizing 200nm-400nm, the spectral line of two wavelength band of 400nm-900nm is demarcated.The present invention utilizes the characteristic spectral line of Ar accurately to locate the angle of crossed dispersion prism 5, and completion system parameter is determined and adjusts.Then to Se, Zn, Mn, Cu, Ba, Mg, Ca, Si, C, K, the mixed solution of Na element is tested.Adopt different integral time, respectively to 200nm-400nm, two wavelength band of 400nm-900nm are tested.Concrete testing procedure is as follows:
One, in echelle spectrometer casing 7, be filled with argon gas;
Two, open the solid state ICP light source 12 of Atomic Emission Spectrometer AES, utilize rotary drive mechanism 13 to drive crossed dispersion prism 5 to rotate, by the incident angle of the facula position judgement crossed dispersion prism 5 on planar array detector 8, make its incident angle within the scope of 27.56 ° ± 0.05 °, crossed dispersion prism 5 is carried out to coarse positioning;
Three, utilize the characteristic spectral line of Ar accurately to locate the angle of crossed dispersion prism 5, realize the spectral line of 200nm-400nm wavelength band and demarcate;
Four, the spectral line of chemical example 200nm-400nm is tested;
Five, utilize rotary drive mechanism 13 to drive crossed dispersion prism 5 to make its rotation, by the incident angle of the facula position judgement crossed dispersion prism 5 on planar array detector 8, make its incident angle within the scope of 27.10 ° ± 0.02 °, crossed dispersion prism 5 is carried out to coarse positioning;
Six, utilize the characteristic spectral line of Ar accurately to locate the angle of crossed dispersion prism 5, realize the spectral line of 400nm-900nm wavelength band and demarcate;
Seven, the 400nm-900nm spectral line of chemical example is tested.
Embodiment 1
The characteristic wavelength 203.985nm of Se element in mixed solution (take characteristic spectral line energy more by force, what more easily distinguish is example, lower same), between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (69,213), actual measurement wavelength 203.986nm, wavelength accuracy error 0.001nm.
Embodiment 2
The characteristic wavelength 213.856nm of Zn element in mixed solution, between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (132,222), actual measurement wavelength 213.861nm, wavelength accuracy error 0.005nm.
Embodiment 3
The characteristic wavelength 257.610nm of Mn element in mixed solution, between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (315,250), actual measurement wavelength 257.614nm, wavelength accuracy error 0.004nm.
Embodiment 4
The characteristic wavelength 324.754nm of Cu element in mixed solution, between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (446,222), actual measurement wavelength 324.752nm, wavelength accuracy error 0.002nm.
Embodiment 5
The characteristic wavelength 279.079nm of Mg element in mixed solution, between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (369,293), actual measurement wavelength 279.080nm, wavelength accuracy error 0.001nm.
Embodiment 6
The characteristic wavelength 315.889nm of Ca element in mixed solution, between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (434,307), actual measurement wavelength 315.894nm, wavelength accuracy error 0.005nm.
Embodiment 7
The characteristic wavelength 288.158nm of Si element in mixed solution, between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (388,304), actual measurement wavelength 251.157nm, wavelength accuracy error 0.001nm.
Embodiment 8
The characteristic wavelength 247.856nm of C element in mixed solution, between wavelength band 200nm-400nm, the incident angle of crossed dispersion prism 5 is 27.56 °, actual measurement position of spectral line (284,253), actual measurement wavelength 247.855nm, wavelength accuracy error 0.001nm.
Embodiment 9
The characteristic wavelength 455.403nm of Ba element in mixed solution, between wavelength band 400nm-900nm, the incident angle of crossed dispersion prism 5 is 27.10 °, actual measurement position of spectral line (350,114), actual measurement wavelength 455.415nm, wavelength accuracy error 0.008nm.
Embodiment 10
The characteristic wavelength 766.490nm of K element in mixed solution, between wavelength band 400nm-900nm, the incident angle of crossed dispersion prism 5 is 27.10 °, actual measurement position of spectral line (409,460), actual measurement wavelength 766.498nm, wavelength accuracy error 0.008nm.
Embodiment 11
The characteristic wavelength 588.995nm of Na element in mixed solution, between wavelength band 400nm-900nm, the incident angle of crossed dispersion prism 5 is 27.10 °, actual measurement position of spectral line (387,23), actual measurement wavelength 589.004nm, wavelength accuracy error 0.009nm.
Claims (1)
1. utilize Atomic Emission Spectrometer AES to carry out a method for spectrum test, it is characterized in that comprising the steps:
One, in echelle spectrometer casing (7), be filled with argon gas;
Two, open the solid state ICP light source (12) of Atomic Emission Spectrometer AES, the angle of utilizing rotary drive mechanism (13) to change crossed dispersion prism (5) makes incident angle within the scope of 27.56 ° ± 0.05 °;
Three, utilize the characteristic spectral line of Ar accurately to locate crossed dispersion prism angle, realize the spectral line of 200nm-400nm wavelength band and demarcate;
Four, chemical example is positioned in sample cell (11), the spectral line of chemical example 200nm-400nm is tested;
Five, the angle of utilizing rotary drive mechanism (13) to change crossed dispersion prism (5) makes incident angle within the scope of 27.10 ° ± 0.02 °;
Six, utilize the characteristic spectral line of Ar accurately to locate the angle of crossed dispersion prism (5), realize the spectral line of 400nm-900nm wavelength band and demarcate;
Seven, the 400nm-900nm spectral line of chemical example is tested.
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| CN104914075A (en) * | 2015-05-22 | 2015-09-16 | 湖北省地质实验测试中心 | CCD sensor-based element detection system and detection method |
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