CN110579466B - Laser-induced breakdown spectroscopy screening method - Google Patents

Laser-induced breakdown spectroscopy screening method Download PDF

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CN110579466B
CN110579466B CN201810596883.5A CN201810596883A CN110579466B CN 110579466 B CN110579466 B CN 110579466B CN 201810596883 A CN201810596883 A CN 201810596883A CN 110579466 B CN110579466 B CN 110579466B
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吕程序
张俊宁
王辉
苑严伟
李亚硕
祁雁楠
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Abstract

A laser-induced breakdown spectrum screening method screens laser-induced breakdown spectra based on Euclidean distance to reject an unstable spectrum of a collected measured object, and screens out a representative spectrum of the measured object, and comprises the following steps: collecting laser-induced breakdown spectra of measured objects, continuously collecting a plurality of spectra of each measured object and recording a spectrum matrix; setting a distance screening threshold value T% to reserve a spectrum with a small Euclidean distance T% in the spectrum matrix; screening spectrums according to the Euclidean distances of the spectrums, deleting two spectrums with the maximum Euclidean distances in the spectrum matrix according to the Euclidean distance matrix of the spectrum matrix, and updating the spectrum matrix; performing circular screening until the number of the spectrums in the updated spectrum matrix reaches the distance screening threshold value; and calculating the average spectrum of the updated spectrum matrix, and taking the average spectrum as the representative spectrum of the measured object. The invention effectively improves the stability of the laser-induced breakdown spectrum of the measured object and the precision of the model.

Description

Laser-induced breakdown spectroscopy screening method
Technical Field
The invention relates to a screening method of a laser-induced breakdown spectrum, in particular to a laser-induced breakdown spectrum screening method based on Euclidean distance.
Background
Laser Induced Breakdown Spectroscopy (LIBS) is an atomic emission spectroscopy technique that uses pulsed Laser to excite the surface of an object to produce a transient plasma, which in turn emits a spectral line with sample element characteristics, and uses a spectrometer to collect wavelength and intensity signals thereof for qualitative and quantitative analysis. The LIBS has the advantages of less sample loss, long-distance in-situ measurement, full-component synchronous analysis, high sensitivity, low detection limit and the like, and is widely used for element measurement research of ores, metals and agricultural products.
Ideally, laser-induced breakdown spectroscopy quantitative detection is based on three scientific assumptions: stoichiometric ablation, local thermodynamic equilibrium and neglecting self-absorption effects, the line intensity can be simply considered to be linear with the concentration of the measured substance element. However, in practical applications, when the characteristics of the measured object are complex and influenced by many factors such as matrix effect, self-absorption, evaporation parameters, excitation temperature, statistical weight, transition probability, excitation potential, etc., the laser-induced breakdown spectrum of the same measured object is still unstable, which may have a certain influence on the accuracy of quantitative analysis. In actual modeling analysis, multiple spectra of the same measured object are collected, averaged and used as a representative spectrum of the sample for analysis, and the method reduces random errors of the spectra and simultaneously keeps noise of each spectrum.
Disclosure of Invention
The invention aims to solve the technical problem of screening a representative laser-induced breakdown spectrum of a measured object in the prior art, and provides a laser-induced breakdown spectrum screening method based on Euclidean distance so as to improve the stability of the laser-induced breakdown spectrum of the measured object and the accuracy of a model.
In order to achieve the above object, the present invention provides a method for screening a laser-induced breakdown spectrum, wherein the method for screening a laser-induced breakdown spectrum based on euclidean distance to reject an unstable spectrum of an acquired measured object and screen out a representative spectrum of the measured object comprises the following steps:
s100, collecting laser-induced breakdown spectra of measured objects, continuously collecting a plurality of spectra of each measured object and recording a spectrum matrix, wherein the spectrum matrix is marked as M (W)m，Sn) Where M is the spectral matrix, WmFor m wavelength variables, SnThe spectrum matrix comprises m wavelengths and n spectra which are acquired for n times;
s200, setting a distance screening threshold value T% to reserve a spectrum with T% of small European distance in the spectrum matrix, wherein the reserved spectrum number T is n multiplied by T%;
s300, screening spectrums according to the Euclidean distances of the spectrums, deleting two spectrums with the maximum Euclidean distances in the spectrum matrix according to the Euclidean distance matrix D of the spectrum matrix, and updating the spectrum matrix;
s400, circularly screening to meet the requirement of a threshold value, and repeating the step S300 until the number of the spectrums in the updated spectrum matrix reaches the distance screening threshold value; and
s500, averaging the spectrum, and calculating the updated spectrum matrix M (W)m，St) Average spectrum of
Figure BDA0001691932230000021
And averaging the spectra
Figure BDA0001691932230000022
As a representative spectrum of the measured object, wherein StFor the updated t spectra of the spectral matrix, W is the average wavelength of the t spectra.
The screening method of laser-induced breakdown spectroscopy described above, wherein the step S300 further includes:
calculating a Euclidean distance matrix D of the spectrum matrix;
finding the maximum value D in the Euclidean distance matrix DmaxSaid maximum value dmaxIs a spectrum m (W, S)x) And m (W, S)y) The Euclidean distance of (c);
from the spectral matrix M (W)m，Sn) In deleting the spectrum m (W, S)x) And m (W, S)y) (ii) a And
updating the spectral matrix to M (W)m，Sn 2)。
In the method for screening laser-induced breakdown spectroscopy, calculating the euclidean distance matrix D of the spectral matrix includes:
calculating the Euclidean distance between every two spectrums to obtain a matrix element D in the Euclidean distance matrix DijWherein d isijIs the Euclidean distance d between the ith spectrum and the jth spectrumijAnd calculated using the formula:
Figure BDA0001691932230000023
wherein M is a spectral matrix, WkIs K wavelength variables, K being 1-m, Si,SjThe spectra collected at the i and j times, respectively.
The screening method of laser-induced breakdown spectroscopy is characterized in that the average spectrum
Figure BDA0001691932230000031
Calculated using the following formula:
Figure BDA0001691932230000032
the method for screening laser-induced breakdown spectroscopy further includes, in step S400:
s401, judging whether the screened spectrum meets the threshold requirement, if so, executing the step S500 to obtain an average spectrum; if not, the step S300 is repeated to continue to screen the spectrum according to the euclidean distance of the spectrum.
The invention has the technical effects that:
aiming at the problem that the spectrum of the same measured object is unstable under different acquisition times in the process of acquiring the laser-induced breakdown spectrum of the measured object with a complex matrix, the invention adopts a laser-induced breakdown spectrum screening method based on Euclidean distance to reject the acquired unstable spectrum of the measured object and screen out the representative spectrum of the measured object. Setting a distance screening threshold value for a plurality of collected laser-induced breakdown spectra of the same measured object, sequentially rejecting spectra with large Euclidean distances according to Euclidean distances among different spectra until the number of the remaining spectra meets the requirement of the distance screening threshold value, and averaging the remaining spectra to be used as a representative spectrum of the measured object. The stability of the laser-induced breakdown spectrum of the measured object and the precision of the model are effectively improved.
The invention is described in detail below with reference to the drawings and specific examples, but the invention is not limited thereto.
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FIG. 1 is a flow chart of a method according to an embodiment of the present invention;
FIG. 2 is an unscreened spectrogram of an embodiment of the present invention;
FIG. 3 is a graph of a filtered spectrum according to one embodiment of the present invention;
FIG. 4 is a spectral standard deviation of an embodiment of the present invention;
FIG. 5A is a graph of the results of a filtered spectrum modeling in accordance with one embodiment of the present invention;
FIG. 5B is a graph of unscreened spectral modeling results, in accordance with an embodiment of the present invention.
Detailed Description
The invention will be described in detail with reference to the following drawings, which are provided for illustration purposes and the like:
referring to fig. 1, fig. 1 is a flow chart of a method according to an embodiment of the invention. The invention aims at the problem that the spectrum of the same measured object is unstable under different acquisition times in the process of acquiring the laser-induced breakdown spectrum of the measured object with a complex matrix. The laser-induced breakdown spectrum screening method screens the laser-induced breakdown spectrum based on the Euclidean distance to remove the unstable spectrum of the collected measured object and screen out the representative spectrum of the measured object. The method comprises the following steps:
s100, collecting laser-induced breakdown spectra of measured objects, continuously collecting a plurality of spectra of each measured object and recording a spectrum matrix, wherein the spectrum matrix is marked as M (W)m，Sn) Where M is the spectral matrix, WmFor m wavelength variables, SnThe spectrum matrix comprises m wavelengths and n spectra which are acquired for n times;
step S200, setting a distance screening threshold value T%, eliminating the spectrum with the European distance being 1-T% larger in the spectrum matrix, and reserving the spectrum with the European distance being smaller in the spectrum matrix, namely reserving the spectrum with the quantity T being T-n multiplied by T%;
s300, screening spectrums according to the Euclidean distances of the spectrums, deleting two spectrums with the maximum Euclidean distances in the spectrum matrix according to the Euclidean distance matrix D of the spectrum matrix, and updating the spectrum matrix;
wherein, step S300 further comprises:
step S301, calculating a Euclidean distance matrix D of the spectrum matrix, including:
calculating the Euclidean distance between every two spectrums to obtain a matrix element D in the Euclidean distance matrix DijWherein d isijIs the Euclidean distance d between the ith spectrum and the jth spectrumijAnd calculated using the formula:
Figure BDA0001691932230000041
wherein M is a spectral matrix, WkIs K wavelength variables, K being 1-m, Si,SjThe spectra collected for the ith and jth times respectively;
step S302, searching the maximum value D in the Euclidean distance matrix DmaxSaid maximum value dmaxIs a spectrum m (W, S)x) And m (W, S)y) The Euclidean distance of (c);
step S303, from the spectrum matrix M (W)m，Sn) In deleting the spectrum m (W, S)x) And m (W, S)y) (ii) a And
step S304, updating the spectrum matrix to be M (W)m，Sn-2)；
Step S400, circularly screening to meet the threshold requirement, and repeating the step S300 until the number of the spectrums in the updated spectrum matrix reaches the distance screening threshold, namely the updated spectrum matrix is M (W)m，St) Wherein, in step S400, the method may further include:
s401, judging whether the screened spectrum meets the threshold requirement, if so, executing the step S500 to obtain an average spectrum; if not, repeating the step S300 to continue to screen the spectrum according to the Euclidean distance of the spectrum; and
step S500, averaging the spectrum, and calculating the updated spectrum matrix M (W)m，St) Average spectrum of
Figure BDA0001691932230000051
And averaging the spectra
Figure BDA0001691932230000052
As a representative spectrum of the measured object, wherein StFor the updated t spectra of the spectral matrix, W is the average wavelength of the t spectra.
Wherein the average spectrum
Figure BDA0001691932230000053
Calculated using the following formula:
Figure BDA0001691932230000054
in this embodiment, the method may further include:
and S600, effect analysis, namely comparing and analyzing the screening effect of the laser-induced breakdown spectroscopy based on the Euclidean distance in the steps S100-S500. May include comparing the unscreened spectral matrix to the screened spectral matrix; comparing the position standard deviation of the unseen spectrum matrix and the screened spectrum matrix at the characteristic peak; and establishing a multiple linear regression model, and comparing the average spectrum of the unseen spectrum matrix with the average spectrum of the screened spectrum matrix by using the cross validation decision coefficient and the cross validation mean square error respectively.
The working process of the laser-induced breakdown spectroscopy screening method based on the Euclidean distance is further described by a specific embodiment as follows:
s100, collecting the laser-induced breakdown spectrum of the measured object
In this example, the test substance was a mixed sample of silica, methylcellulose, and potassium sulfate. The silicon dioxide model is used for simulating a soil substrate, methylcellulose is used as a binder, and potassium sulfate is used as a target object of a target element to be detected, namely potassium. The content of methyl cellulose in the concrete sample is 30%; the content of potassium sulfate is 7.4 percent, and the content of potassium element is 3.3 percent; the silica content was 62.6%. After the samples were mixed well, the samples were pressed into an aluminum box 30mm in diameter and 5mm in height using a tablet press under a pressure of 20 Mpa.
The laser-induced breakdown spectroscopy acquisition apparatus adopted in this embodiment is preferably: quantel CFR laser, Andor SROPT24-15 fiber, Andor AR500i spectrometer, Andor Istar DH334T detector. The spectral acquisition parameters are preferably: the time delay of the flash lamp and the Q switch is 320 mu s, the spectrum range is 723.6-808.2 nm, the resolution is 0.08nm, the number of collected data points is 1024, the time delay is 1 mu s, the door width is 2 mu s, and 100 spectrums are collected by a measured object. The collected laser induced breakdown spectrum of the measured object is shown in fig. 2.
Here, the spectrum matrix shown in FIG. 2 is denoted as M (W)1024，S100) Where M represents the spectral matrix, W1024Represents a wavelength variable, S100Representing spectra, the matrix contains 1024 wavelengths and 100 spectra.
Step S200, setting a distance screening threshold value T%
The distance filtering threshold T is set to 70, and in fig. 2, for example, spectra of 1 to 70% with a large euclidean distance are rejected, and spectra of 70% with a small euclidean distance (T is 70) are retained.
Step S300, single screening, namely screening spectrums according to the Euclidean distances of the spectrums, deleting two spectrums with the maximum Euclidean distances in the spectrum matrix according to the Euclidean distance matrix D of the spectrum matrix, and updating the spectrum matrix;
taking the spectrum shown in fig. 2 as an example, a euclidean distance matrix D of 100 spectra is calculated. In particular, element dijCalculated by the following equation
Figure BDA0001691932230000061
FindingMaximum D in distance matrix DmaxWhich is the spectrum m (W, S)2) And m (W, S)79) The euclidean distance of (c).
From the spectral matrix M (W)1024，S100) Deletion of m (W, S)2) And m (W, S)79) 2 spectra of (a), the updated spectrum matrix is M (W)1024，S70)
Step S400, circularly screening to the threshold value requirement
Repeating the step S300 until the number of the spectrums in the updated spectrum matrix reaches the distance screening threshold requirement, namely the updated spectrum matrix is M (W)1024，S70). As shown in fig. 3.
Step S500, averaging the spectrum
Get the update matrix M (W)1024，S70) The average spectrum of (a) is a representative spectrum of the collected spectrum, and subsequent analysis calculation is carried out.
Figure BDA0001691932230000062
S600, effect analysis, namely screening effect analysis of laser-induced breakdown spectroscopy based on Euclidean distance
The unscreened spectrum matrix and the screened spectrum matrix are respectively shown in fig. 2 and 3, and as can be seen from the figure, the screened spectrum is more concentrated in visual distribution. The standard deviation is shown in fig. 4, and it can be seen that the standard deviation of the screened spectrum is small at the position of the characteristic peak and is more stable.
17 mixed samples of silica, methylcellulose, potassium sulfate were prepared. Wherein the methylcellulose content is 30%; potassium sulfate content of 0.2-7.4%, concentration gradient of 0.45%, content converted into potassium element of 0.1-3.3%, concentration gradient of 0.2%; the content of silicon dioxide is 62.6-69.8%. Sample mixing, tabletting and spectrum collection like the previous steps, spectra are collected at 3 positions on each sample selection plane, and 51 groups of sample spectrum matrixes are collected. Calculating the unsereened average spectrum and the screened average spectrum of 51 groups of spectrum matrixes respectively, and establishing a multiple linear regression model by combining the concentration of potassium elementAs shown in fig. 5A and 5B. The model adopts full interactive verification, and the interactive verification determines the coefficient (R)2 CV) 0.845 and 0.886, respectively, and cross-validation mean square error (RMSECV) 0.388 and 0.331, respectively. As can be seen from fig. 5A and 5B, the accuracy of the quantitative model can be effectively improved by using the laser-induced breakdown spectroscopy screening method based on the euclidean distance.
Aiming at the problem that the spectrum of the same measured object is unstable under different acquisition times in the process of acquiring the laser-induced breakdown spectrum of the measured object with a complex matrix, the invention adopts a laser-induced breakdown spectrum screening method based on Euclidean distance to reject the acquired unstable spectrum of the measured object and screen out the representative spectrum of the measured object. Setting a distance screening threshold value for a plurality of collected laser-induced breakdown spectra of the same measured object, sequentially rejecting spectra with large Euclidean distances according to Euclidean distances among different spectra until the number of the remaining spectra meets the requirement of the distance screening threshold value, and averaging the remaining spectra to be used as a representative spectrum of the measured object. The stability of the laser-induced breakdown spectrum of the measured object and the precision of the model are effectively improved.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (3)

1. A laser-induced breakdown spectrum screening method is characterized in that laser-induced breakdown spectra are screened based on Euclidean distance to reject unstable spectra of a collected measured object, and representative spectra of the measured object are screened, and the method comprises the following steps:
s100, collecting laser-induced breakdown spectra of measured objects, continuously collecting a plurality of spectra of each measured object and recording a spectrum matrix, wherein the spectrum matrix is marked as M (W)m，Sn) Where M is the spectral matrix, WmFor m wavelength variables, SnThe spectrum matrix comprises m wavelengths and n spectra which are acquired for n times;
s200, setting a distance screening threshold value T% to reserve a spectrum with T% of small European distance in the spectrum matrix, wherein the reserved spectrum number T is n multiplied by T%;
s300, screening spectrums according to the Euclidean distances of the spectrums, deleting two spectrums with the maximum Euclidean distances in the spectrum matrix according to the Euclidean distance matrix D of the spectrum matrix, and updating the spectrum matrix;
s400, circularly screening to meet the requirement of a threshold value, and repeating the step S300 until the number of the spectrums in the updated spectrum matrix reaches the distance screening threshold value; and
s500, averaging the spectrum, and calculating the updated spectrum matrix M (W)m，St) Average spectrum of
Figure FDA0002575950890000011
And averaging the spectra
Figure FDA0002575950890000012
As a representative spectrum of the measured object, wherein StFor the updated t spectra of the spectrum matrix, W is the average wavelength of the t spectra;
wherein the step S300 further includes:
calculating a Euclidean distance matrix D of the spectrum matrix;
finding the maximum value D in the Euclidean distance matrix DmaxSaid maximum value dmaxIs a spectrum m (W, S)x) And m (W, S)y) The Euclidean distance of (c);
from the spectral matrix M (W)m，Sn) In deleting the spectrum m (W, S)x) And m (W, S)y) (ii) a And
updating the spectral matrix to M (W)m，Sn-2)；
Wherein calculating the Euclidean distance matrix D of the spectrum matrix comprises:
calculating the Euclidean distance between every two spectrums to obtain a matrix element D in the Euclidean distance matrix DijWherein d isijIs the ith spectrum andeuclidean distance d of j-th spectrumijAnd calculated using the formula:
Figure FDA0002575950890000021
wherein M is a spectral matrix, WkIs K wavelength variables, K being 1-m, Si,SjThe spectra collected at the i and j times, respectively.
2. The method for laser induced breakdown spectroscopy screening of claim 1, wherein the average spectrum
Figure FDA0002575950890000022
Calculated using the following formula:
Figure FDA0002575950890000023
。
3. the method for screening laser induced breakdown spectroscopy of claim 2, further comprising, in step S400:
s401, judging whether the screened spectrum meets the threshold requirement, if so, executing the step S500 to obtain an average spectrum; if not, the step S300 is repeated to continue to screen the spectrum according to the euclidean distance of the spectrum.
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