CN102879091A - 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 the spectral technique field, relate to a kind of echelle spectrometer, particularly a kind of echelle grating based on sectional type is based on Atomic Emission Spectrometer AES and the spectrum test method of echelle spectrometer.
Background technology
The inductively coupled plasma atomic emission spectrum analytical technology is one of elemental analysis method that is most widely used in the Material Field.(Jilin University's Master's thesis in 2002 " based on the design and research of the ICP-AES spectrometer spectra collection scheme of CCD ", University Of Tianjin's Master's thesis " development of ICP scanning spectrometer " in 2007) reported about inductively coupled plasma atomic emission spectrometer (ICP-AES), the information that it utilizes the atomic emissions characteristic spectral line to provide is carried out ultimate analysis, have multielement while, advantage quick, that directly measure, in the commercial production such as metallurgy, petrochemical complex, machine-building, metal processing, bringing into play great function.
Atomic Emission Spectrometer AES has experienced long evolution.According to the 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).Because the just continuous future development to full spectrum direct-reading, intellectuality, miniaturization, harmonic analysis cost of the demand of producing, Atomic Emission Spectrometer AES.Beam splitting system is as the core of Atomic Emission Spectrometer AES, directly affect the performance level of instrument, ICP-AES take echelle spectrometer as 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, domestic and international many scientific research institutions are 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-come Bai Si company (Leeman Labs Inc), U.S. platinum Ai Ermo instrument company (PerkinElmer) develops the ICP-AES take echelle spectrometer as spectral module in succession, but because the restriction of detection system, and the strict demand of wavelength band, spectral resolution, spectral analysis module-echelle spectrometer still exists more gordian technique to remain 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 the specimen consumption is large.
The light channel structure of a kind of echelle spectrometer of using at present comprises casing, condenser, incident pin hole, collimating mirror, echelle grating, crossed dispersion prism, focus lamp and planar array detector; Described collimating mirror and focus lamp all adopt parabolic lens; Condenser focuses on the incident pin hole with 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 the echelle grating surface, the light beam of echelle grating diffraction shines on the 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 because the restriction of detector development level, the spectral range of the echelle spectrometer test of this version only is 400nm-800nm, and its performance still can not satisfy the test request of ICP-AES.
Summary of the invention
The technical matters that the present invention will solve provides a kind of echelle spectrometer that can realize multielement Quick Measurement in the 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 provides 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 provides 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 the chemical example spectrum test of the present invention comprises the steps:
One, in echelle spectrometer casing 7, is 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 in 27.56 ° ± 0.05 ° scope;
Three, utilize the characteristic spectral line of Ar that crossed dispersion prism angle is accurately located, realize that the spectral line of 200nm-400nm wavelength band is demarcated;
Four, chemical example is positioned in the 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 in 27.10 ° ± 0.02 ° scope;
Six, utilize the characteristic spectral line of Ar that the angle of crossed dispersion prism 5 is accurately located, realize that the spectral line of 400nm-900nm wavelength band is demarcated;
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 the 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 the incident pin hole through condenser, incident pin hole outgoing beam incides echelle grating and carries out principal dispersion behind the collimating mirror collimation, then incide the crossed dispersion prism and carry out horizontal dispersion, crossed dispersion is imaged on the image planes of CCD by focus lamp.
Because ICP-AES when carrying out sample test, realize tens kinds of trace elements and measure simultaneously, so ICP-AES requires its beam splitting system will have simultaneously the characteristics of broadband scope, high spectral resolution concurrently, 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 satisfy preferably ICP-AES to the demand of system's wavelength band and resolution, and has lower detection limit, can satisfy the test request of atomic emission spectrum.
Because the demand of ICP-AES test performance and echelle spectrometer optical property requires system should have higher signal to noise ratio (S/N ratio), so must effectively suppress the system background noise.In the system design process, box house adopts even blacking and carries out uneven surface and process.Simultaneously, according to the optical texture characteristics, increase diaphragm in internal system echelle grating and crossed dispersion prism place, thereby effectively suppressed system's parasitic light, reduction system detection limit, raising system signal noise ratio are had positive effect.
Areal survey formula echelle spectrometer of the present invention, by changing the incident angle of crossed dispersion prism, finish respectively 200nm-400nm, the measurement of 400nm-900nm, in existing detection level situation, realized the Quick Measurement in the 200nm-900nm wavelength band.Advantage with broadband, high resolving power, high sensitivity, low noise, small size satisfies the application demand of ICP Atomic Emission Spectrometer AES.With areal survey formula echelle spectrometer and solid state ICP combination of light sources, develop echelle grating ICP Atomic Emission Spectrometer AES.After system debug is finished, carried out the test analysis of chemical sample, experimental result shows that the sectional type echelle spectrometer satisfies 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, measure when can realize multielement, accurate each elemental composition of interpretation, the 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's integral time and the quantum efficiency.
Description of drawings
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 among 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 with 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 the focus lamp 6 behind 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 the prior art, such as motor, motor etc.
The light beam that light source sends enters optical system through incident pin hole 2, place the reflection parabolic lens as collimating mirror 3 along incident pin hole 2 emergent ray directions apart from the f place, place echelle grating 4 in collimating mirror 3 reflected light directions, crossed dispersion prism 5 is positioned on the echelle grating 4 diffraction light directions, the reflection parabolic lens that shines the place ahead through the light beam of crossed dispersion prism 5 reflection is focus lamp 6, focus lamp 6 focuses on emergent light on the planar array detector 8, and 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 that will overlap after echelle grating 4 dispersions separates, and its dispersive power has no significant effect the spectrally resolved ability of system.But consider the problems such as utilization factor of spectral range, level time interference, 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 in the situation of identical incident angle, short-wave band level minor tick is larger, and close together between at different levels times of long-wave band, produces easily level and time disturb.Analyze as calculated, under two angles, can cover spectral range 200nm-900nm as can be known.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 the 200nm-400nm wavelength band; Fig. 2 (b) is two-dimension spectrum image distribution in the 400nm-900nm wavelength band.
Because ICP-AES has high sensitivity and low detection limit, so having relatively high expectations to detection system.By to the echelle spectrometer performance evaluation, native system selects highly sensitive ultraviolet enhancement area array CCD camera as the planar array detector 8 of system, the CCD chip is in the 200nm-850nm scope, has more uniform quantum efficiency, its efficiency curve is shown in curve III among Fig. 3 (among the 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).Simultaneously, this CCD has lower dark current noise and reads noise, can freeze during work to-70 ℃, and by are set different integral time, this detection system can satisfy 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 finish spectral line measurement in the 200nm-900nm scope.For the accuracy that guarantees to test, in each test process, need the spectrogram position is demarcated.In the spectrogram calibration process, the echelle spectrometer applying argon gas is to finish the measurement of ultraviolet band.Characteristic spectral line by analyzing Ar as can be known its characteristic spectral line is distributed between 300nm-520nm, can be used for realizing 200nm-400nm, and the spectral line of two wavelength band of 400nm-900nm is demarcated.The present invention utilizes the characteristic spectral line of Ar that the angle of crossed dispersion prism 5 is accurately located, and the completion system parameter is determined and adjustment.The present invention carries out test analysis to chemical sample, and the two-dimension spectrum information of taking in the experiment is such as Fig. 4 (a), 4(b) shown in.
Calculate by two-dimentional spectrogram reductive agent, with the characteristic wavelength of Ar element system is demarcated.Demarcation is rear to Se in the solution, Zn, and Mn, Cu, Ba, Mg, Ca, Si, C, K, the Na element is tested, and its test result is as shown in table 1.Every kind of unit have the various features spectral line, but it detects the larger difference of existence, this experiment only provide the characteristic spectral line energy more by force, the characteristic spectral line calibration result distinguished comparatively easily.From experimental result can find out instrument whole wavelength band all have less wavelength measurement error (＜0.01nm), can satisfy the demand of Atomic Emission Spectral Analysis.
In test process, the echelle spectrometer applying argon gas is to finish the measurement of ultraviolet band, characteristic spectral line by analyzing Ar as can be known its characteristic spectral line is distributed between 300nm-520nm, can be used for realizing 200nm-400nm, and the spectral line of two wavelength band of 400nm-900nm is demarcated.The present invention utilizes the characteristic spectral line of Ar that the angle of crossed dispersion prism 5 is accurately located, and the completion system parameter is determined and adjustment.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, is filled with argon gas;
Two, open the solid state ICP light source 12 of Atomic Emission Spectrometer AES, utilizing rotary drive mechanism 13 to drive crossed dispersion prism 5 rotates, judge the incident angle of crossed dispersion prism 5 by the facula position on the planar array detector 8, make its incident angle in 27.56 ° ± 0.05 ° scope, crossed dispersion prism 5 is carried out coarse positioning;
Three, utilize the characteristic spectral line of Ar that the angle of crossed dispersion prism 5 is accurately located, realize that the spectral line of 200nm-400nm wavelength band is demarcated;
Four, the spectral line of chemical example 200nm-400nm is tested;
Five, utilize rotary drive mechanism 13 to drive crossed dispersion prism 5 and make its rotation, judge the incident angle of crossed dispersion prism 5 by the facula position on the planar array detector 8, make its incident angle in 27.10 ° ± 0.02 ° scope, crossed dispersion prism 5 is carried out coarse positioning;
Six, utilize the characteristic spectral line of Ar that the angle of crossed dispersion prism 5 is accurately located, realize that the spectral line of 400nm-900nm wavelength band is demarcated;
Seven, the 400nm-900nm spectral line of chemical example is tested.
Embodiment 1
The characteristic wavelength 203.985nm of Se element in the mixed solution (take the characteristic spectral line energy more by force, more easily distinguish as example, together lower), 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 the 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.
The characteristic wavelength 257.610nm of Mn element in the 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 the 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.
The characteristic wavelength 279.079nm of Mg element in the 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 the 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 the 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.
The characteristic wavelength 247.856nm of C element in the 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.
The characteristic wavelength 455.403nm of Ba element in the 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.
The characteristic wavelength 766.490nm of K element in the 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 the 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 (5)
1. an echelle spectrometer 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).
2. echelle spectrometer according to claim 1 is characterized in that the inside surface blacking of described casing (7).
3. echelle spectrometer according to claim 1 and 2 is characterized in that before the light entrance face of described echelle grating (4) and crossed dispersion prism (5) the first diaphragm (10) and the second diaphragm (9) being set respectively.
4. Atomic Emission Spectrometer AES take the described echelle spectrometer of claim 1 as spectral module.
5. a method of utilizing the described Atomic Emission Spectrometer AES of claim 4 to carry out spectrum test comprises the steps:
One, in echelle spectrometer casing (7), is 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 in 27.56 ° ± 0.05 ° scope;
Three, utilize the characteristic spectral line of Ar that crossed dispersion prism angle is accurately located, realize that the spectral line of 200nm-400nm wavelength band is demarcated;
Four, chemical example is positioned in the 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 in 27.10 ° ± 0.02 ° scope;
Six, utilize the characteristic spectral line of Ar that the angle of crossed dispersion prism (5) is accurately located, realize that the spectral line of 400nm-900nm wavelength band is demarcated;
Seven, the 400nm-900nm spectral line of chemical example is tested.
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Cited By (6)
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| CN103308167A (en) * | 2013-06-24 | 2013-09-18 | 中国科学院长春光学精密机械与物理研究所 | Ultraviolet, visible and ultraviolet prism chromatic dispersion imaging spectrometer |
| CN103487144A (en) * | 2013-08-29 | 2014-01-01 | 中国科学院长春光学精密机械与物理研究所 | Double-grating beam splitting system packaging structure stable in stray light eliminating ability |
| CN103575398A (en) * | 2013-11-26 | 2014-02-12 | 武进田 | Echelette-grating light splitting device of UV/VIS/NIR spectrophotometer |
| CN104121991A (en) * | 2014-07-03 | 2014-10-29 | 清华大学 | Plasma emission spectroscopy two-dimensional space distribution measuring system |
| CN107677368A (en) * | 2017-09-11 | 2018-02-09 | 上海理工大学 | Linear dispersion is adjustable optical filtering type spectrometer |
| CN114034386A (en) * | 2021-11-07 | 2022-02-11 | 天津大学 | Full-spectrum direct-reading atomic emission spectrometer combining electric arc excitation and echelle grating light splitting |
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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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| CN103308167A (en) * | 2013-06-24 | 2013-09-18 | 中国科学院长春光学精密机械与物理研究所 | Ultraviolet, visible and ultraviolet prism chromatic dispersion imaging spectrometer |
| CN103308167B (en) * | 2013-06-24 | 2015-11-25 | 中国科学院长春光学精密机械与物理研究所 | Ultraviolet, visible, near infrared prismatic colours astigmatic image spectrometer |
| CN103487144A (en) * | 2013-08-29 | 2014-01-01 | 中国科学院长春光学精密机械与物理研究所 | Double-grating beam splitting system packaging structure stable in stray light eliminating ability |
| CN103487144B (en) * | 2013-08-29 | 2016-01-13 | 中国科学院长春光学精密机械与物理研究所 | The double grating beam splitting system encapsulating structure that eliminate stray light ability is stable |
| CN103575398A (en) * | 2013-11-26 | 2014-02-12 | 武进田 | Echelette-grating light splitting device of UV/VIS/NIR spectrophotometer |
| CN104121991A (en) * | 2014-07-03 | 2014-10-29 | 清华大学 | Plasma emission spectroscopy two-dimensional space distribution measuring system |
| CN104121991B (en) * | 2014-07-03 | 2016-08-24 | 清华大学 | The measurement system of plasma emission spectroscopy two-dimensional space distribution |
| CN107677368A (en) * | 2017-09-11 | 2018-02-09 | 上海理工大学 | Linear dispersion is adjustable optical filtering type spectrometer |
| CN114034386A (en) * | 2021-11-07 | 2022-02-11 | 天津大学 | Full-spectrum direct-reading atomic emission spectrometer combining electric arc excitation and echelle grating light splitting |
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