CN105021546A - Method for measuring chemical elements by whole-spectrum direct-reading spectrometer - Google Patents
Method for measuring chemical elements by whole-spectrum direct-reading spectrometer Download PDFInfo
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Abstract
The invention relates to a method for measuring chemical elements by a whole-spectrum direct-reading spectrometer. The method comprises the following steps: a sample is analyzed by the use of a whole-spectrum direct-reading spectrometer, and analysis of the sample contains calling an analytical curve and exciting the sample; a spectrum is collected; data pretreatment is carried out; calibration position of a reference spectral line and offset of spectral line peak value are calculated by a peak searching method, and the offset is used as offset of an analytical spectral line; and offset correction is carried out on the analytical spectral line according to the offset of the analytical spectral line; and spectral line intensity is calculated, and the spectral line intensity is substituted into the analytical curve to calculate element content. According to a value of the reference spectral line at the peak position during calibration when a test is conducted, offset between the peak position of the reference spectral line during testing and the peak position of the reference spectral line during calibration is calculated by the peak searching method. According to the offset, position of the analytical spectral line can be corrected at real time, the influence of spectral position offset on analytical data is minimized, and stability and accuracy of the analytical data are enhanced.
Description
Technical field
The present invention relates to a kind of method that full spectrum direct-reading spectrometer measures chemical element.
Background technology
Direct-reading spectrometer is a kind of instrument simultaneously can measuring different chemical constituent content in test sample block to be checked.Its measuring principle is, test sample block to be checked and electrode carry out effluve under the control of light source module, form stable plasma flame, light is introduced light room, adopt grating to carry out light splitting and form spectrum, different chemical element correspond to the characteristic spectral line of different wave length, spectrum projects above linear array detector, namely different spectral line drops on above different detection pixel, and light signal converts electric signal to, thus realizes the measurement of line strength.Constituent content and line strength positive correlation, adopt the standard substance of polylith known elements content, can set up the polynomial relation between content and line strength, when analyzing the sample of unknown content, according to line strength of different element, can calculate constituent content.
In the use procedure of reality, the environmental factor changes such as temperature, humidity, voltage, the stability of optical system in direct-reading spectrometer can be affected, the relative position between detector and spectrum is caused to offset, detector pixel can not correspond to all-the-time stable the peak of spectral line, when calculating light intensity according to pixel, the light intensity obtained is unstable, thus the stability of impact analysis data and accuracy.So will correct according to the position of spectral line of actual conditions to direct-reading spectrometer.
Direct-reading spectrometer can be divided into channel-type and full spectrum formula two kinds according to optical signal detector type.The position of spectral line bearing calibration that full spectrum formula spectrometer adopts is spectral matching, its operating process is: after spectrometer completes calibration, excite authentic specimen, gather spectrum and be set to reference to spectral line, after there is position skew in spectrometer spectrum, again excite authentic specimen, gather the standard reference of new spectrum as comparison, carry out mating with the reference spectra offset and contrast, calculate spectral shift amount, record it, when analyzing sample, with calculated spectral shift amount, offset correction is carried out to the analysis spectrum collected, and then carry out other and calculate constituent content.
The spectral matching of full spectrum formula spectrometer has evaded the movable part in light path system, effectively reduces the failure rate of instrument.The defect of spectral matching is can not real time correction, if spectral shift can not be there occurs by Timeliness coverage instrument when using, stability and the accuracy of so analyzing data will be affected, may cause having produced underproof product, or the material used in processing is underproof, causes economic loss.And find that the also higher to the requirement of technician of skew occurs full spectrum formula spectrometer spectrum.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of and the full spectrum direct-reading spectrometer of real time correction position of spectral line can measure the method for chemical element.
The technical solution adopted for the present invention to solve the technical problems is: a kind of full spectrum direct-reading spectrometer measures the method for chemical element, comprises the steps:
1) scale operation is carried out to full spectrum direct-reading spectrometer;
2) carry out data customization to full spectrum direct-reading spectrometer according to demand, described data customization comprises:
2.1) the scope selection analysis spectral line of the chemical element kind analyzed as required and Water demand,
2.2) arrange with reference to spectral line according to every bar analysis spectral line;
3) select complete standard substance, set up analytic curve according to the different analysis phases, preserve data;
4) analytical standard material, the repeatability of inspection full spectrum direct-reading spectrometer;
5) carry out scene to full spectrum direct-reading spectrometer to prepare, described scene prepares to comprise:
5.1) carry out installation to described full spectrum direct-reading spectrometer to power on;
5.2) detected state data;
6) use full spectrum direct-reading spectrometer to analyze sample, described sample analysis to be comprised:
6.1) analytic curve is called, excited sample;
6.2) spectrum is gathered;
6.3) data prediction is carried out;
6.4) by the calibration position of peak-seeking method computing reference spectral line and the side-play amount of spectral line peak value and using described side-play amount as the side-play amount of analysis spectral line;
6.5) according to the side-play amount of analysis spectral line, offset correction is carried out to analysis spectral line;
6.6) calculate line strength, bring analytic curve into, calculate the content of element.
Further, described step 6.3) described in data prediction comprise one or more processing modes in substrate deduction, filtering, interpolation and the correction of spectral singularity point.
The invention has the beneficial effects as follows, according to during test in the value at peak place of timing signal with reference to spectral line, with reference to the peak of spectral line and the side-play amount of the peak of timing signal reference spectral line when calculating test by peak-seeking method.Can the position of real time correction analysis spectral line according to described side-play amount, reduce spectral position skew to the impact analyzing data, improve the stability and accuracy of analyzing data, correctly can obtain the chemical element content in detected sample.Effectively eliminate the impact of the environmental factor changes such as temperature on spectrometer simultaneously, improve the environmental suitability of full spectrum direct-reading spectrometer.Spectrometer start can use, and shorten the preheating time of instrument, user does not need specially to carry out position of spectral line correction, facilitates the use of spectrometer, improves the stability of data.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the operational flowchart that the present invention composes that direct-reading spectrometer measures the method for chemical element entirely.
Fig. 2 is the spectral curve that spectrometer detects sample.
Embodiment
In conjunction with the accompanying drawings, the present invention is further detailed explanation.These accompanying drawings are the schematic diagram of simplification, only basic structure of the present invention are described in a schematic way, and therefore it only shows the formation relevant with the present invention.
As shown in Figure 1, a kind of full spectrum direct-reading spectrometer of the present invention measures the method for chemical element, comprises the steps:
1) scale operation is carried out to full spectrum direct-reading spectrometer;
2) carry out data customization to full spectrum direct-reading spectrometer according to demand, described data customization comprises:
2.1) the scope selection analysis spectral line of the chemical element kind analyzed as required and Water demand,
2.2) arrange with reference to spectral line according to every bar analysis spectral line;
3) select complete standard substance, set up analytic curve according to the different analysis phases, preserve data;
4) analytical standard material, the repeatability of inspection full spectrum direct-reading spectrometer;
5) carry out scene to full spectrum direct-reading spectrometer to prepare, described scene prepares to comprise:
5.1) carry out installation to described full spectrum direct-reading spectrometer to power on;
5.2) detected state data;
6) use full spectrum direct-reading spectrometer to analyze sample, described sample analysis to be comprised:
6.1) analytic curve is called, excited sample;
6.2) gather spectrum;
6.3) carry out data prediction, described data prediction comprises one or more processing modes in substrate deduction, filtering, interpolation and the correction of spectral singularity point;
6.4) by the calibration position of peak-seeking method computing reference spectral line and the side-play amount of spectral line peak value and using described side-play amount as the side-play amount of analysis spectral line;
6.5) according to the side-play amount of analysis spectral line, offset correction is carried out to analysis spectral line;
6.6) calculate line strength, bring analytic curve into, calculate the content of element.
Wherein, before carrying out scale operation to full spectrum direct-reading spectrometer, also need to carry out reliability testing to full spectrum direct-reading spectrometer.After full spectrum direct-reading spectrometer completes test, spectral line proving operation can be carried out.
In the analysis sample of above-mentioned step 6), usually there is several stage, each phase analysis is several element wherein, and the process that each element calculates content is similar.Complete after sample excitation collects spectrum when analysis software controls spectrometer, can data processing be carried out.
For step 6.4), first check the shape of corresponding reference spectral line and neighbouring spectrum thereof.Due to when carrying out spectrometer calibration, it is local that the calibration position with reference to spectral line is all set in spectral line peak value.When normal use spectrometer carries out the test of sample chemical constituent content, if do not drop on timing signal spectral line peak with reference to spectral line, can judge that spectral position there occurs skew.According to during test in the value at peak place of timing signal with reference to spectral line, with reference to the peak of spectral line and the side-play amount of the peak of timing signal reference spectral line when calculating test by peak-seeking method.And using described side-play amount as the side-play amount of analysis spectral line, offset correction is carried out to analysis spectral line.After completing the position correction of analysis spectral line, then calculate spectral line light intensity, then bring into and analyze opisometer calculation constituent content.
As shown in Figure 2, for element silicon analysis, the sample analysis that above-mentioned full spectrum direct-reading spectrometer measures the step 6) in the method for chemical element is described.The analysis spectral line wavelength that element silicon is selected is 288.159nm, the reference spectral line of setting is 266.039nm, the analysis phase at element silicon place is the first stage, after spectrometer excited sample completes, gathers spectrum, carry out pre-service, then calculate position skew according to reference to spectral line 266.039nm, as the side-play amount of 288.159nm spectral line, then calculate the light intensity of 288.159nm spectral line, bring analytic curve polynomial expression into, calculate the content of element silicon.In Fig. 2, curve 1 is the instrumental calibration moment curve of spectrum, curve 2 is the curve of spectrum test moment analyzing the sample moment, relative to the calibration moment, there is skew to the right in spectral line, analysis spectral line has identical side-play amount with reference to spectral line, analysis spectral line peak shape is better than with reference to spectral line peak shape, by reference to spectral line place peak-seeking algorithm, can calculate and offset by about 1 pixel with reference to spectral line, as the side-play amount of analysis spectral line, the advanced line displacement correction of analysis spectral line, then calculates line strength, then effectively can eliminate offset error.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can 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 right.
Claims (2)
1. full spectrum direct-reading spectrometer measures a method for chemical element, comprises the steps:
1) scale operation is carried out to full spectrum direct-reading spectrometer;
2) carry out data customization to full spectrum direct-reading spectrometer according to demand, described data customization comprises:
2.1) the scope selection analysis spectral line of the chemical element kind analyzed as required and Water demand,
2.2) arrange with reference to spectral line according to every bar analysis spectral line;
3) select complete standard substance, set up analytic curve according to the different analysis phases, preserve data;
4) analytical standard material, the repeatability of inspection full spectrum direct-reading spectrometer;
5) carry out scene to full spectrum direct-reading spectrometer to prepare, described scene prepares to comprise:
5.1) carry out installation to described full spectrum direct-reading spectrometer to power on;
5.2) detected state data;
6) full spectrum direct-reading spectrometer is used to analyze sample,
It is characterized in that: described step 6) comprises:
6.1) analytic curve is called, excited sample;
6.2) spectrum is gathered;
6.3) data prediction is carried out;
6.4) by the calibration position of peak-seeking method computing reference spectral line and the side-play amount of spectral line peak value and using described side-play amount as the side-play amount of analysis spectral line;
6.5) according to the side-play amount of analysis spectral line, offset correction is carried out to analysis spectral line;
6.6) calculate line strength, bring analytic curve into, calculate the content of element.
2. full spectrum direct-reading spectrometer according to claim 1 measures the method for chemical element, it is characterized in that: described step 6.3) described in data prediction comprise one or more processing modes in substrate deduction, filtering, interpolation and the correction of spectral singularity point.
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| CN106500840A (en) * | 2016-10-20 | 2017-03-15 | 无锡创想分析仪器有限公司 | A kind of exceptional spectrum elimination method of full spectrum formula direct-reading spectrometer |
| CN106596499A (en) * | 2016-11-01 | 2017-04-26 | 北京华泰诺安技术有限公司 | Real-time Raman spectrum calibration method |
| CN107037012A (en) * | 2017-04-05 | 2017-08-11 | 华中科技大学 | The echelle spectrometer dynamic correcting method gathered for LIBS |
| 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 |
| CN107941714A (en) * | 2017-11-22 | 2018-04-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Use the method for direct-reading spectrometer measure titanium alloy component |
| CN109187497A (en) * | 2018-10-26 | 2019-01-11 | 成都以太航空保障工程技术有限责任公司 | A kind of initial method of Element detection spectrometer |
| 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 |
| CN117213631A (en) * | 2023-09-26 | 2023-12-12 | 无锡创想分析仪器有限公司 | Spectrometer operation monitoring method and system |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107941714A (en) * | 2017-11-22 | 2018-04-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Use the method for direct-reading spectrometer measure titanium alloy component |
| CN109187497A (en) * | 2018-10-26 | 2019-01-11 | 成都以太航空保障工程技术有限责任公司 | A kind of initial method of Element detection spectrometer |
| CN109187497B (en) * | 2018-10-26 | 2019-10-18 | 成都以太航空保障工程技术有限责任公司 | A kind of initial method of Element detection spectrometer |
| 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 |
| CN117213631A (en) * | 2023-09-26 | 2023-12-12 | 无锡创想分析仪器有限公司 | Spectrometer operation monitoring method and system |
| CN117213631B (en) * | 2023-09-26 | 2024-08-20 | 无锡创想分析仪器有限公司 | Spectrometer operation monitoring method and system |
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Application publication date: 20151104 |