CN106442431B - A kind of modification method improving LIBS technology measurement sample repeatability - Google Patents
A kind of modification method improving LIBS technology measurement sample repeatability Download PDFInfo
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- CN106442431B CN106442431B CN201610798296.5A CN201610798296A CN106442431B CN 106442431 B CN106442431 B CN 106442431B CN 201610798296 A CN201610798296 A CN 201610798296A CN 106442431 B CN106442431 B CN 106442431B
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention discloses a kind of modification methods of raising LIBS technology measurement sample repeatability.Principle is that the recurrence correlation returned using air plasma spectroscopic data correlation corrects sample plasma spectroscopic data.Because experimental situation is stablized, so being stored in database profession using air plasma spectrum as standard spectrum.When the repetition sexual abnormality of LIBS measurement sample, re-measure the air plasma spectrum at the moment, and the normal air plasma spectrometry stored in this spectrum and database progress correlation is returned to obtain and returns correlation, sample plasma spectrum is corrected using this correlation, obtains final sample plasma spectrum.The present invention effectively increases the repeatability of LIBS technology measurement sample, and method is simple and reliable.
Description
Technical field
The present invention relates to the modification methods for improving LIBS technology measurement sample repeatability, in particular to a kind of to utilize airlight
The method that spectrum correlation returns amendment sample spectra.
Background technique
Laser induced breakdown spectroscopy (Laser-Induced Breakdown Spectroscopy, LIBS) technology uses arteries and veins
Induction tool of the impulse light as emission spectrographic analysis, by being not necessarily to or simple sample pretreatment, damage micro- to sample and polynary
The plain simultaneously and rapidly advantages such as detection, have gradually developed into a kind of potential industrial process online measuring technique, have been attempted application
In the quality control of various industrial process or condition diagnosing.But due to technology own characteristic, when carrying out duplicate measurements, sample
Spectroscopic data it is unstable, it is less reproducible, directly affect LIBS technology to the accuracy and reliability of sample duplicate measurements,
So it is particularly important to improve LIBS technology repeatability.
Summary of the invention
The purpose of the present invention is to provide a kind of modification methods of raising LIBS technology measurement sample repeatability.Utilize air
Spectroscopic data (repeating to test new survey air spectrum and database Plays air spectroscopic data) carries out correlation recurrence, by
That arrives returns amendment of the correlation realization to sample spectra.
The technical scheme is that
1. a kind of modification method for improving LIBS technology measurement sample repeatability, it is characterised in that include the following steps:
1) sample plasma spectrum and air plasma spectrum are measured when repeating to test and record its data;
2) by the air plasma spectroscopic data newly measured and database Plays air plasma spectroscopic data into
Row correlation returns, and obtains returning correlation;
3) it brings new sample plasma spectrometry into 2) resulting recurrence correlation and obtains revised sample plasma
Body spectrum;
2. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, feature
Be 1), 2) spectroscopic data described in step be transverse and longitudinal coordinate be respectively wavelength and peak intensity several points data group.
3. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, feature
Be the 2) database described in step include standard air plasma spectrum.
4. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, feature
Being the, 2) correlation described in step returns is returned to what the spectral intensity of the air plasma in same spectral range carried out
Return.
5. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, feature
Be the 2) correlation recurrence described in step be least square regression, and think that normal air spectrum is independent variable, newly survey air
Spectroscopic data is dependent variable.
6. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, feature
Be 2) recurrence correlation described in step be linear or nonlinear equation.The present invention has the advantage that
The present invention is by conjunction with laser induced breakdown spectroscopy, providing one kind and proposing regression analysis in mathematical statistics
The modification method of high LIBS technology measurement sample repeatability, utilizes air plasma middle-low alloy steels sample plasma spectrum
It is simple and reliable, convenient and efficient the spectroscopic data for repeating experiment can be modified, effectively improve the repeatability of LIBS technology, reproduce
Property, make data normalization.
Detailed description of the invention
Fig. 1 is the flow chart of modification method of the present invention;
The linear equation that Fig. 2 air plasma spectroscopic data correlation returns;
It is right after first time experiment, second of experiment, amendment that Mg, Ca characteristic spectral line in case is embodied in Fig. 3-Fig. 7
Than.
Specific embodiment
Flow diagram as shown in connection with fig. 1, it is proposed by the present invention a kind of to improve LIBS technology measurement sample repeatability
Modification method includes following steps:
1) measure powder sample (particles used stream sample is different meshes powdered mineral quality sample in the present embodiment)
Spectroscopic data acquires 200 data to 80,100,150,200,325,400 mesh powder samples respectively, is then averaging to it,
It is stored in database.Measure air spectroscopic data at that time, it is believed that normal air spectrum acquires 100 averagings, is stored in data
Library.
2) it carries out repeating experiment (consistent with first time experiment condition).200 sample spectras are equally measured and recorded respectively
Data are averaged, and 100 air spectroscopic datas are averaged.
3) the first time quasi- air spectroscopic data of institute's mark is set as independent variable X, second of surveyed air spectroscopic data is set as
Dependent variable Y, (this example application linear regression) obtains equation of linear regression Y=-48.34736+1.12128X after correlation returns.
4) it brings the sample spectral data Y ' that second is surveyed into Y=-48.34736+1.12128X and obtains corresponding X '
It is then revised sample spectral data, by first time institute's sample spectrum, sample light after second sample spectrum, amendment
Spectrum drawing (Fig. 3-Fig. 7) is compared.Second sample spectrum after amendment with first time institute's sample spectrum by that can keep
Extraordinary consistency illustrates the repeatability that LIBS measurement can be effectively improved by the amendment of air plasma spectrum.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (5)
1. a kind of modification method for improving LIBS technology measurement sample repeatability, it is characterised in that include the following steps:
1) sample plasma spectrum and air plasma spectrum are measured when repeating to test and record its data;
2) the air plasma spectroscopic data newly measured and database Plays air plasma spectroscopic data are subjected to phase
Closing property returns, and obtains returning correlation;
3) it brings new sample plasma spectrometry into 2) resulting recurrence correlation and obtains revised sample plasma light
Spectrum.
2. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, it is characterised in that
1), 2) spectroscopic data described in step be transverse and longitudinal coordinate be respectively wavelength and peak intensity several points data group.
3. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, it is characterised in that
The 2) correlation described in step returns is the recurrence carried out to the spectral intensity of the air plasma in same spectral range.
4. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, it is characterised in that
The 2) correlation recurrence described in step be least square regression, and think that normal air spectrum is independent variable, it is new to survey air spectrum
Data are dependent variable.
5. a kind of modification method for improving LIBS technology measurement sample repeatability according to claim 1, it is characterised in that
2) recurrence correlation described in step be linear or nonlinear equation.
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CN101509872A (en) * | 2009-03-20 | 2009-08-19 | 清华大学 | Coal quality on-line detecting analytical method based on regression analysis |
CN101949852A (en) * | 2010-07-30 | 2011-01-19 | 清华大学 | Spectral standardization-based coal quality on-line detection method |
CN102507512A (en) * | 2011-11-07 | 2012-06-20 | 大连理工大学 | On-line in situ detecting method for infrared-ultraviolet double pulse laser induced breakdown spectroscopy |
CN102830096A (en) * | 2012-08-29 | 2012-12-19 | 国电燃料有限公司 | Method for measuring element concentration and correcting error based on artificial neural network |
CN103234944A (en) * | 2013-04-17 | 2013-08-07 | 清华大学 | Coal quality characteristic analysis method based on combination of dominant factors and partial least square method |
CN104697966A (en) * | 2015-03-10 | 2015-06-10 | 西北大学 | Method for quantitatively analyzing chromium and manganese in steel based on least square support vector machine algorithm combined with laser-induced breakdown spectroscopy |
CN105044050A (en) * | 2015-07-07 | 2015-11-11 | 中国农业大学 | Rapid quantitative analysis method for metallic elements in crop straw |
-
2016
- 2016-08-31 CN CN201610798296.5A patent/CN106442431B/en not_active Expired - Fee Related
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101509872A (en) * | 2009-03-20 | 2009-08-19 | 清华大学 | Coal quality on-line detecting analytical method based on regression analysis |
CN101949852A (en) * | 2010-07-30 | 2011-01-19 | 清华大学 | Spectral standardization-based coal quality on-line detection method |
CN102507512A (en) * | 2011-11-07 | 2012-06-20 | 大连理工大学 | On-line in situ detecting method for infrared-ultraviolet double pulse laser induced breakdown spectroscopy |
CN102830096A (en) * | 2012-08-29 | 2012-12-19 | 国电燃料有限公司 | Method for measuring element concentration and correcting error based on artificial neural network |
CN103234944A (en) * | 2013-04-17 | 2013-08-07 | 清华大学 | Coal quality characteristic analysis method based on combination of dominant factors and partial least square method |
CN104697966A (en) * | 2015-03-10 | 2015-06-10 | 西北大学 | Method for quantitatively analyzing chromium and manganese in steel based on least square support vector machine algorithm combined with laser-induced breakdown spectroscopy |
CN105044050A (en) * | 2015-07-07 | 2015-11-11 | 中国农业大学 | Rapid quantitative analysis method for metallic elements in crop straw |
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