CN104122211A - Real-time calibration method of full-spectrum direct-reading spectrometer - Google Patents
Real-time calibration method of full-spectrum direct-reading spectrometer Download PDFInfo
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Abstract
The invention relates to a method for calibrating a spectral position of a full-spectrum direct-reading spectrometer and in particular relates to a real-time calibration method of a full-spectrum direct-reading spectrometer. The real-time calibration method of the full-spectrum direct-reading spectrometer comprises the following steps: (1) customizing data of the full-spectrum direct-reading spectrometer according to the requirement; (2) building analysis curves and saving data according to different analysis stages which comprise a first analysis stage and other analysis stages; (3) carrying out site preparation of the full-spectrum direct-reading spectrometer; (4) analyzing a sample by using the full-spectrum direct-reading spectrometer. With the adoption of the real-time calibration method of the full-spectrum direct-reading spectrometer, the full-spectrum direct-reading spectrometer does not need to come into a special software function module for calibration operation when the full-spectrum direct-reading spectrometer is used, so that the use of the full-spectrum direct-reading spectrometer is simplified; an optical chamber of the full-spectrum direct-reading spectrometer does not need constant temperature; the full-spectrum direct-reading spectrometer can be normally used under the room temperature condition, so that the use of the full-spectrum direct-reading spectrometer is greatly facilitated.
Description
Technical field
The present invention relates to the spectral position bearing calibration that a kind of full spectrum formula direct reading spectrometry adopts, relate in particular to a kind of real-time correction method of full spectrum direct-reading spectrometer.
Background technology
Direct-reading spectrometer is a kind of optical instrument of precision, its optical texture is placed in the light chamber interior of sealing, the light signal that excited sample produces in the use procedure of instrument enters light chamber, project and on line array sensor, be converted to electric signal by optical texture, then being converted to digital signal by electronic module is stored in single-chip microcomputer, operation analysis software on computers reads digital signal from single-chip microcomputer, carries out analysis and calculation, obtains the content of each chemical element in sample.
According to detector, direct-reading spectrometer can be divided into channel-type and two kinds of full spectrum formulas, and it is detector that channel-type direct-reading spectrometer adopts photomultiplier transit light pipe PMT, and each photomultiplier transit light pipe PMT, corresponding to a passage, measures an analytical element; Full spectrum formula direct-reading spectrometer adopts electric charge coupling original paper CCD as detector, and electric charge coupling original paper CCD is a kind of linear array detector, and every electric charge coupling original paper CCD can gather the spectral signal of certain limit, can measure multiple analytical elements.
Full spectrum direct-reading spectrometer adopts linear array detector that light signal is converted to electric signal.In the use procedure of full spectrum direct-reading spectrometer, the variation of light room temperature and vacuum tightness can affect light channel structure, cause the subtle change of spectrum and linear array detector relative position, show as specific wavelength and be offset corresponding to the pixel on linear array detector, spectral position changes.
At present, the spectral position bearing calibration that full spectrum formula direct-reading spectrometer adopts is spectral matching, its operating process is: after spectrometer has been calibrated, enter spectrum correction software module, set shooting parameter, excitation spectrum is proofreaied and correct sample, setting the spectrum gathering is reference spectra REFS, in instrument use procedure, at set intervals or carry out optical lens cleaning safeguard after, enter spectrum correction software module, excitation spectrum is proofreaied and correct sample, the spectrum gathering is designated as current spectrum CURS, the reference spectra of n sheet CCD and current spectrum mate and are designated as respectively REFS_n and CURS_n, taking pixel as step-length translation CURS_n, remember that the k time translation is CURS_n_k,
Calculate the related coefficient of CURS_n_k and REFS_n, if the scope of k is-L<=k<=L, can obtain 2L+1 related coefficient, the maximum of points of related coefficient, represent the skew that this sheet CCD spectrum occurs, when calculating position of spectral line, add this side-play amount and can obtain real position of spectral line.
The execution of spectral matching is to be undertaken by independent software module, conventionally can certain interval of time between twice operation, require optical system constant temperature and light chamber vacustat in during this period of time.If proofreaied and correct in the interval time of carrying out at twice spectral position, temperature or the vacuum of optical system fluctuate, and spectral position is offset the data variation causing and cannot automatically eliminates.Particularly in the time that light room temperature changes because of reasons such as power down, light chamber arrives design temperature stable again, need the long period, temperature variation must be brought spectral line shift, analyze data fluctuations, consequently user need to wait for the long period, and instrument is proofreaied and correct after again stablizing, and then analyzes.For environments for use such as stokehold application, very inconvenient.
Summary of the invention
The technical problem to be solved in the present invention is: in order to reduce to change because of light room temperature and vacuum tightness the impact of the analysis data on full spectrum formula direct-reading spectrometer, the real-time correction method that the invention provides a kind of full spectrum direct-reading spectrometer solves the problems referred to above.
The technical solution adopted for the present invention to solve the technical problems is: a kind of real-time correction method of full spectrum direct-reading spectrometer, the real-time correction method of described full spectrum direct-reading spectrometer comprises the steps:
1) according to demand full spectrum direct-reading spectrometer is carried out to data customization, described data customization comprises:
1.1) full spectrum direct-reading spectrometer is carried out to scale operation;
1.2) in spectrum correction module, set shooting parameter, excitation spectrum is proofreaied and correct sample, and the spectrum collecting is set as to reference spectra REFS, sets Spectral matching parameter save data;
2) set up analytic curve according to the different analysis phases, save data, the described analysis phase comprises the first analysis phase and other analysis phases;
3) full spectrum direct-reading spectrometer is carried out to scene and prepare, described on-the-spot preparation comprises:
3.1) after full spectrum direct-reading spectrometer arrives use scene, described full spectrum direct-reading spectrometer is installed and powered on;
3.2) open full spectrum direct-reading spectrometer, wait for that the vacuum tightness of spectrometer light chamber arrives setting value;
4) use full spectrum direct-reading spectrometer to analyze sample, comprising:
4.1) call analytic curve, excited sample;
4.2) gather spectrum;
4.3) the first analysis phase spectrum mates with reference spectra REFS, the skew of calculating detector position, every spectrum corresponding to electric charge coupling original paper CCD is mated, calculate spectral position and proofread and correct polynomial expression, the correction polynomial expression that n piece CCD is corresponding is designated as POL_n, and wherein electric charge coupling original paper CCD is as the detector of full spectrum formula direct-reading spectrometer, and electric charge coupling original paper CCD is a kind of linear array detector, every electric charge coupling original paper CCD can gather spectral signal, can Measurement and analysis element;
4.4) obtain position of spectral line according to wavelength and calibration mapping table, bring corresponding position correction polynomial expression POL_n into, calculate the current tram of spectral line;
4.5) spectral line peak value is carried out to integration, obtain line strength, bring analytic curve into, and through interference correction operation, calculate the content of element.
Further, described step 2) in, it is identical with the shooting parameter in spectrum correction module that the first analysis phase was set shooting parameter, and the shooting parameter of all the other analysis phases is set as requested.
In order to improve counting yield, described step 4.3) in, the computing method of POL_n are that spectrum corresponding to n piece electric charge coupling original paper CCD is carried out to segmentation according to fixed width w, hop count is designated as K, while carrying out matching operation, carry out piecemeal, can obtain K matched position, p position is designated as (x_p, y_p), and x_p is the center of the p section in reference spectra, y_p is the center of the p section on current spectrum, K matched position carries out least square fitting, obtains y=f (x), and this polynomial expression is POL_n.
The invention has the beneficial effects as follows, the each measurement of full spectrum direct-reading spectrometer can be carried out spectral position correction, because the full time of composing direct-reading spectrometer analytic sample is conventionally between 20 to 40 seconds, carry out position of spectral line correction institute spended time and be conventionally less than 2 seconds, therefore real time correction can not bring obvious impact to the use of full spectrum direct-reading spectrometer, can effectively eliminate the environmental factors such as temperature and change the impact on spectrometer, promote the convenience of use and the stability of data.When use, do not need to enter special software function module and carry out correct operation, simplify the use of full spectrum direct-reading spectrometer.Full spectrum direct-reading spectrometer light chamber does not need to carry out constant temperature, and at ambient temperature, entirely composing direct-reading spectrometer can normally use, thereby greatly facilitates the use of full spectrum direct-reading spectrometer.
Brief description of the drawings
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the operational flowchart that the present invention composes direct-reading spectrometer real-time correction method entirely.
Embodiment
In conjunction with the accompanying drawings, the present invention is further detailed explanation.These accompanying drawings are the schematic diagram of simplification, and basic structure of the present invention is only described in a schematic way, and therefore it only shows the formation relevant with the present invention.
As shown in Figure 1, the real-time correction method of a kind of full spectrum direct-reading spectrometer of the present invention, the real-time correction method of described full spectrum direct-reading spectrometer comprises the steps:
1) according to demand full spectrum direct-reading spectrometer is carried out to data customization, described data customization comprises:
1.1) full spectrum direct-reading spectrometer is carried out to scale operation;
1.2) in spectrum correction module, set shooting parameter, excitation spectrum is proofreaied and correct sample, and the spectrum collecting is set as to reference spectra REFS, sets Spectral matching parameter save data;
2) set up analytic curve according to the different analysis phases, save data, the described analysis phase comprises the first analysis phase and other analysis phases;
3) full spectrum direct-reading spectrometer is carried out to scene and prepare, described on-the-spot preparation comprises:
3.1) after full spectrum direct-reading spectrometer arrives use scene, described full spectrum direct-reading spectrometer is installed and powered on;
3.2) open full spectrum direct-reading spectrometer, wait for that the vacuum tightness of spectrometer light chamber arrives setting value;
4) use full spectrum direct-reading spectrometer to analyze sample, comprising:
4.1) call analytic curve, excited sample;
4.2) collection spectrum;
4.3) the first analysis phase spectrum mates with reference spectra REFS, the skew of calculating detector position, every spectrum corresponding to electric charge coupling original paper CCD is mated, calculate spectral position and proofread and correct polynomial expression, the correction polynomial expression that n piece CCD is corresponding is designated as POL_n, and wherein electric charge coupling original paper CCD is as the detector of full spectrum formula direct-reading spectrometer, and electric charge coupling original paper CCD is a kind of linear array detector, every electric charge coupling original paper CCD can gather spectral signal, can Measurement and analysis element;
4.4) obtain position of spectral line according to wavelength and calibration mapping table, bring corresponding position correction polynomial expression POL_n into, calculate the current tram of spectral line;
4.5) spectral line peak value is carried out to integration, obtain line strength, bring analytic curve into, and through interference correction operation, calculate the content of element.
Further, described step 2) in, it is identical with the shooting parameter in spectrum correction module that the first analysis phase was set shooting parameter, and the shooting parameter of all the other analysis phases is set as requested.
In order to improve counting yield, described step 4.3) in, the computing method of POL_n are that spectrum corresponding to n piece electric charge coupling original paper CCD is carried out to segmentation according to fixed width w, hop count is designated as K, while carrying out matching operation, carry out piecemeal, can obtain K matched position, p position is designated as (x_p, y_p), and x_p is the center of the p section in reference spectra, y_p is the center of the p section on current spectrum, K matched position carries out least square fitting, obtains y=f (x), and this polynomial expression is POL_n.
The time of full spectrum direct-reading spectrometer analytic sample is between 20 to 40 seconds, carry out position of spectral line correction institute spended time and be less than 2 seconds, therefore real time correction can not bring obvious impact to the use of spectrometer, can effectively eliminate the environmental factors such as temperature and change the impact on spectrometer, promote the convenience of use and the stability of data.
Taking above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, relevant staff can, not departing from the scope of this invention technological thought, carry out various change and amendment completely.The technical scope of this invention is not limited to the content on instructions, must determine its technical scope according to claim scope.
Claims (3)
1. a real-time correction method for full spectrum direct-reading spectrometer, is characterized in that: the real-time correction method of described full spectrum direct-reading spectrometer comprises the steps:
1) according to demand full spectrum direct-reading spectrometer is carried out to data customization, described data customization comprises:
1.1) full spectrum direct-reading spectrometer is carried out to scale operation;
1.2) in spectrum correction module, set shooting parameter, excitation spectrum is proofreaied and correct sample, and the spectrum collecting is set as to reference spectra REFS, sets Spectral matching parameter save data;
2) set up analytic curve according to the different analysis phases, save data, the described analysis phase comprises the first analysis phase and other analysis phases;
3) full spectrum direct-reading spectrometer is carried out to scene and prepare, described on-the-spot preparation comprises:
3.1) after full spectrum direct-reading spectrometer arrives use scene, described full spectrum direct-reading spectrometer is installed and powered on;
3.2) open full spectrum direct-reading spectrometer, wait for that the vacuum tightness of spectrometer light chamber arrives setting value;
4) use full spectrum direct-reading spectrometer to analyze sample, comprising:
4.1) call analytic curve, excited sample;
4.2) gather spectrum;
4.3) the first analysis phase spectrum mates with reference spectra REFS, the skew of calculating detector position, every spectrum corresponding to electric charge coupling original paper CCD is mated, calculate spectral position and proofread and correct polynomial expression, the correction polynomial expression that n piece CCD is corresponding is designated as POL_n, and wherein electric charge coupling original paper CCD is as the detector of full spectrum formula direct-reading spectrometer, and electric charge coupling original paper CCD is a kind of linear array detector, every electric charge coupling original paper CCD can gather spectral signal, can Measurement and analysis element;
4.4) obtain position of spectral line according to wavelength and calibration mapping table, bring corresponding position correction polynomial expression POL_n into, calculate the current tram of spectral line;
4.5) spectral line peak value is carried out to integration, obtain line strength, bring analytic curve into, and through interference correction operation, calculate the content of element.
2. the real-time correction method of full spectrum direct-reading spectrometer according to claim 1, it is characterized in that: described step 2) in, it is identical with the shooting parameter in spectrum correction module that the first analysis phase was set shooting parameter, and the shooting parameter of all the other analysis phases is set as requested.
3. the real-time correction method of full spectrum direct-reading spectrometer according to claim 1, it is characterized in that: described step 4.3) in, the computing method of POL_n are that spectrum corresponding to n piece electric charge coupling original paper CCD is carried out to segmentation according to fixed width w, hop count is designated as K, while carrying out matching operation, carry out piecemeal, can obtain K matched position, p position is designated as (x_p, y_p), x_p is the center of the p section in reference spectra, y_p is the center of the p section on current spectrum, K matched position carries out least square fitting, obtain y=f (x), this polynomial expression is POL_n.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105021546A (en) * | 2015-07-09 | 2015-11-04 | 无锡创想分析仪器有限公司 | Method for measuring chemical elements by whole-spectrum direct-reading spectrometer |
| CN107167466A (en) * | 2017-05-09 | 2017-09-15 | 无锡创想分析仪器有限公司 | The method for improving Zn-ef ficiency measurement accuracy in brass |
| CN111344550A (en) * | 2017-10-09 | 2020-06-26 | Tsi有限公司 | Particle counter component calibration |
| CN112557306A (en) * | 2020-12-07 | 2021-03-26 | 无锡钱荣分析仪器有限公司 | Abnormal spectrum eliminating method of full-spectrum type straightness spectrometer |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021546A (en) * | 2015-07-09 | 2015-11-04 | 无锡创想分析仪器有限公司 | Method for measuring chemical elements by whole-spectrum direct-reading spectrometer |
| CN107167466A (en) * | 2017-05-09 | 2017-09-15 | 无锡创想分析仪器有限公司 | The method for improving Zn-ef ficiency measurement accuracy in brass |
| CN111344550A (en) * | 2017-10-09 | 2020-06-26 | Tsi有限公司 | Particle counter component calibration |
| CN112557306A (en) * | 2020-12-07 | 2021-03-26 | 无锡钱荣分析仪器有限公司 | Abnormal spectrum eliminating method of full-spectrum type straightness spectrometer |
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