CN108414475A - The LIBS analysis methods rebuild based on optical chromatography Simultaneous Iteration - Google Patents
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Abstract
The invention discloses a kind of LIBS analysis methods rebuild based on optical chromatography Simultaneous Iteration, polynary LIBS quantitative solvings problem is equivalent to high-precision optical chromatography Problems of Reconstruction, the solution of incidence matrix F is equivalent to the distribution of the reconstruction three dimensional physical amount in optical chromatography.It is decomposed using high-precision SIRT iterative algorithms associate(d) matrix column vector, each column vector of incidence matrix F is iteratively solved by column, to obtain incidence matrix F.Then it realizes that the high-precision of each element in unknown sample solves according to the operation of the actual measurement normalization light spectral intensity vector of unknown sample and incidence matrix to analyze.The invention has the advantages that using class optical chromatography model and being solved in multi-variables analysis calibration, to solve the influence of different element competition transmittings in chemical matrix effect；It is solved using SIRT chromatography iterative algorithms, effectively inhibits the noise in measurement data, and obtain the incidence matrix of lowest mean square root error, to improve LIBS accuracy of quantitative analysis.
Description
Technical field
The present invention relates to a kind of laser spectrum detection methods, more particularly to a kind of quantitative laser induced breakdown spectroscopy analysis side
Method, quantitative solving is analyzed while being suitable for detection target multielement, belongs to photodetection field.
Background technology
Laser induced breakdown spectroscopy (Laser-induced breakdown spectroscopy, abbreviation LIBS) is a kind of
Analytical atomic spectroscopy skill wood.It uses nanosecond short-pulse laser focus objects surface, TRANSIENT HIGH TEMPERATURE that target is made to degrade generation etc.
Gas ions, atom and ion fall after rise to lower state from upper state and launch the spectral line containing element information in cooling procedure, can use
It is detected in material composition element.LIBS technologies can preferably realize object element qualitative analysis, but quantitative analysis meeting
It is influenced by chemical matrix effect, i.e., a certain element of same content, which is placed on its spectral line of emission under different matrix, to have any different.
To solve influence of the chemical matrix effect to LIBS quantitative analyses, Multivariate can be used, i.e., by a variety of members
The a plurality of spectral line of element establishes relevant equation with the relationship of its content, by solving multivariate mathematical matrix equation, is waited for
Survey the content of the multiple element of target.The advantages of this method is can to eliminate chemical matrix effect to a certain extent to quantitative analysis
The influence of precision, the disadvantage is that derivation algorithm precision depends on the multielement calibration mathematical model of early period and the design of derivation algorithm.
The Solve problems of LIBS multivariate quantitative analysis rebuild Solve problems with the optical chromatography under few projecting direction number to be had
Similitude, and optical chromatography rebuilds the precision higher for LIBS quantitative analyses.Simultaneous Iteration reconstruction technique
In (Simultaneous Iterative Reconstruction Technique, abbreviation SIRT) be reconstructed each pixel be
Corresponding to what is be modified again after all projection values calculating of each ray, it can effectively inhibit the noise in measurement data.For
This, high-precision optical chromatography reconstruction model is used for polynary LIBS quantitative solvings problem by this patent.Using high in optical chromatography
The SIRT iterative algorithm associate(d) matrix column vectors of precision are decomposed, and are iteratively solved by column, get standard samples normalization light spectral intensity
Incidence matrix between matrix and each constituent content.Then according to the actual measurement normalization light spectral intensity vector of unknown sample and pass
The operation for joining matrix realizes that the high-precision of each element in unknown sample solves analysis, solves the solving precision of LIBS multivariate analyses
Problem.
Invention content
The purpose of the present invention is to provide a kind of polynary LIBS matrixes multielement analysis method for solving, this method is initially set up
LIBS multivariate analyses rebuild similar matrix mathematical model with optical chromatography, and the SIRT iteration being then based in optical chromatography is calculated
Method associate(d) matrix column vector decomposes the solution for being associated vector, incidence matrix is obtained, according to the normalization spectrum of object to be measured
The operation of intensity and incidence matrix obtains the atomic fraction of the multiple elements of object to be measured, to realize that high-precision fixed quantization LIBS is examined
It surveys.
The present invention is achieved like this,
1. it is M to assume to need the element number (i.e. element dimension) of quantitative analysis, and sequences sequence.Prepare N number of standard sample
To be demarcated (i.e. sample dimension is N).This N number of sample is solid-state, and size dimension is impartial, the above-mentioned M containing different proportion
Kind element, the atomic fraction (i.e. atomicity percentage) of each element is it is known that the uniform ingredients in each sample are distributed；
2. with reference to projection matrix in optics tomographic reconstruction, flow field physical quantity image array, calculation matrix three relationship, structure
Polynary LIBS quantitative analyses matrix equation is built, i.e.,
WF=P
In formula, W is standard sample normalization light spectral intensity matrix, the projection matrix being equivalent to during optical chromatography is rebuild；F is
Incidence matrix, the flow field physical quantity image array being equivalent to during optical chromatography is rebuild, P are standard sample atomic fraction matrix, phase
When in calculation matrix；
3. standard sample normalization light spectral intensity matrix W is built as follows：
To this N number of standard sample with identical test condition and test parameter, LIBS detection is carried out, obtains and corresponds to this N
This N number of LIBS spectrogram is normalized in N number of LIBS spectrograms of a calibration sample, obtains N number of normalization LIBS light
Spectrogram.Take k characteristic spectral line (it is required that sample dimension N each element respectively>Spectral Dimensions kM), then it builds following N rows and multiplies
The standard sample normalization light spectral intensity matrix W of kM row：
KM value in the first row in normalization light spectral intensity matrix represents M element kM root generation of first standard sample
The normalization spectral intensity values of table spectral line；KM value in second row represents M element kM root of second standard sample and represents spectrum
The normalization spectral intensity values of line；And so on ...；KM value in Nth row represents M element kM of n-th standard sample and represents
The normalization spectral intensity values of spectral line；
4. the following N rows of structure multiply the standard sample atomic fraction matrix P of M row：
M value in the first row in atomic fraction matrix represents the atomic fraction of M element of first standard sample；The
M value in two rows represents the atomic fraction of M element of second standard sample；And so on ...；M value generation in Nth row
The atomic fraction of table n-th M element of standard sample；
5. the incidence matrix F connected each other between reflection W and P is represented by：
Incidence matrix F is the matrix that kM rows multiply M row, demand solution kM2A cell value can just obtain F matrix.By incidence matrix
F is decomposed into M interconnection vector F into ranks1、F2、F3、...、FM；Standard sample atomic fraction matrix P is decomposed into M into ranks
Atomic fraction vector P1、P2、P3、...、PM；
6. converting the solution of incidence matrix F to M interconnection vector F1、F2、F3、...、FMSolution, solving model is such as
Under：
Pi=WFi+Ei
In formula, i=1,2,3 ..., M, EiFor error vector, in N>In the case of kM, for FiBe solved to overdetermined equation
Solution, it is necessary to make error minimum to get to the best fit approximation solution under the Optimality Criteria based on certain Optimality Criteria, use
SIRT iterative algorithms based on criterion of least squares are to interconnection vector FiIt is solved：
In above formula, subscript 0 represents initial value；Subscript T represents transposition；Subscript q represents the q times iterative value；Subscript q+1 represents
Q+1 iterative value；λ is relaxation factor, and value size represents iterative constrained tightness；
The suspension condition of iteration is：
ε is the number of a very little, and 0.001 is taken in the present embodiment；After iteration termination, FiLast time iterative value is Fi's
Solving result；
7. by M all interconnection vector FiIt solves after completing, obtains incidence matrix F；To object to be measured with N number of mark
The identical test condition of quasi- sample, carries out LIBS detection, obtains a LIBS spectrogram, and normalizing is carried out to this LIBS spectrogram
Change is handled, and obtains the normalization LIBS spectrograms of sample to be tested.It therefrom obtains M element kM item of object to be measured and represents returning for spectral line
One changes spectral intensity vector：
D=[d1,d2,d3,...,dkM]
The atomic fraction of M element of object to be measured is calculated as follows：
The invention has the advantages that using class optical chromatography model and being solved in multi-variables analysis calibration, to solve
The influence of different element competition transmittings in chemical matrix effect；It is solved using SIRT chromatography iterative algorithms, effectively inhibits to measure number
Noise in, and the incidence matrix of lowest mean square root error is obtained, to improve LIBS accuracy of quantitative analysis.
Description of the drawings
Fig. 1 is the schematic diagram of the method for the present invention.
Specific implementation mode
The purpose of the present invention is to provide a kind of polynary LIBS quantitative analyses method for solving, by high-precision optical chromatography weight
Established model is modeled for polynary LIBS quantitative solvings problem, it is established that standard sample normalization light spectral intensity matrix W, incidence matrix
F, the relationship between standard sample atomic fraction matrix P three；It is combined using high-precision SIRT iterative algorithms in optical chromatography
Matrix column vector is decomposed, and iteratively solves each column vector of incidence matrix F by column, to obtain being connected each other between reflection W and P
Incidence matrix F.Then it is realized according to the operation of the actual measurement normalization light spectral intensity vector of unknown sample and incidence matrix unknown
The high-precision of each element solves analysis in sample, solves the problems, such as the solving precision of LIBS multivariate analyses.
Illustrate this LIBS quantitative analysis methods with following specific embodiments：
1. assume need quantitative analysis element number be 12 (taking element dimension M=12), including sodium, magnesium, calcium, iron,
Manganese, copper, silicon, carbon, oxygen, sulphur, nitrogen and hydrogen sort by said sequence from 1 to 12.Prepare 100 standard samples to be demarcated
(taking sample dimension N=100).This 100 samples are solid-state, and size dimension is impartial, above-mentioned 12 kinds containing different proportion
Element, the atomic fraction (i.e. atomicity percentage) of each element is it is known that the uniform ingredients in each sample are distributed；
2. with reference to projection matrix in optics tomographic reconstruction, flow field physical quantity image array, calculation matrix three relationship, structure
Polynary LIBS quantitative analyses matrix equation as shown in Figure 1 is built, i.e.,
WF=P
In formula, W is standard sample normalization light spectral intensity matrix, the projection matrix being equivalent to during optical chromatography is rebuild；F is
Incidence matrix, the flow field physical quantity image array being equivalent to during optical chromatography is rebuild, P are standard sample atomic fraction matrix, phase
When in calculation matrix；
3. standard sample normalization light spectral intensity matrix W is built as follows：
To this 100 standard samples with identical test condition and test parameter, LIBS detection is carried out, obtains and corresponds to this
100 LIBS spectrograms of 100 calibration samples are normalized this 100 LIBS spectrograms, obtain 100 and return
One changes LIBS spectrograms.3 characteristic spectral lines are taken (to take k=3, it is desirable that sample dimension N each element respectively>Spectral Dimensions kM,
This embodiment sample dimension N=100 is more than spectral Dimensions kM=36), then it builds following N rows and multiplies kM row (the present embodiment is
100 rows multiply 36 row) standard sample normalization light spectral intensity matrix W：
KM value in the first row in normalization light spectral intensity matrix represents M element kM root generation of first standard sample
The normalization spectral intensity values of table spectral line；KM value in second row represents M element kM root of second standard sample and represents spectrum
The normalization spectral intensity values of line；And so on ...；KM value in Nth row represents M element kM of n-th standard sample and represents
The normalization spectral intensity values of spectral line；
4. the following N rows of structure multiply the standard sample atomic fraction matrix P of M row：
In implementation, M=12, N=100.M value in the first row in atomic fraction matrix represents first standard sample
The atomic fraction of M element；M value in second row represents the atomic fraction of M element of second standard sample；With such
It pushes away ...；M value in Nth row represents the atomic fraction of M element of n-th standard sample；
5. the incidence matrix F connected each other between reflection W and P is represented by：
Incidence matrix F is the matrix that kM rows multiply M row, is that 36 rows multiply 12 matrixes in specific embodiment.Demand solution kM2=432
A cell value can just obtain F matrix.As shown in Figure 1, incidence matrix F is decomposed into M interconnection vector F into ranks1、F2、
F3、...、FM；Standard sample atomic fraction matrix P is decomposed into M atomic fraction vector P into ranks1、P2、P3、...、PM；
6. converting the solution of incidence matrix F to M interconnection vector F1、F2、F3、...、FMSolution, solving model is such as
Under：
Pi=WFi+Ei
In formula, i=1,2,3 ..., M, EiFor error vector, in N>In the case of kM, for FiBe solved to overdetermined equation
Solution, it is necessary to make error minimum to get to the best fit approximation solution under the Optimality Criteria based on certain Optimality Criteria, use
SIRT iterative algorithms based on criterion of least squares are to interconnection vector FiIt is solved：
In above formula, subscript 0 represents initial value；Subscript T represents transposition；Subscript q represents the q times iterative value；Subscript q+1 represents
Q+1 iterative value；λ is relaxation factor, and for value between 0 to 2, value size represents iterative constrained tightness, this implementation
Example takes 0.5；
The suspension condition of iteration is：
ε is the number of a very little, and 0.001 is taken in the present embodiment；After iteration termination, FiLast time iterative value is Fi's
Solving result；
7. by M all interconnection vector FiIt solves after completing, obtains incidence matrix F；To object to be measured with N number of mark
The identical test condition of quasi- sample, carries out LIBS detection, obtains a LIBS spectrogram, and normalizing is carried out to this LIBS spectrogram
Change is handled, and obtains the normalization LIBS spectrograms of sample to be tested.It therefrom obtains M element kM item of object to be measured and represents returning for spectral line
One changes spectral intensity vector：
D=[d1,d2,d3,...,dkM]
The atomic fraction of M element of object to be measured is calculated as follows：
In formula, M=12.
Claims (1)
1. a kind of LIBS analysis methods rebuild based on optical chromatography Simultaneous Iteration, it is characterised in that comprise the steps of：
1) assume to need the element number of quantitative analysis, i.e., element dimension is M, and sequences sequence, prepare N number of standard sample into
Rower is fixed, i.e., sample dimension is N, this N number of sample is solid-state, and size dimension is impartial, the above-mentioned M kinds element containing different proportion,
The atomic fraction of each element, i.e. atomicity percentage are it is known that the uniform ingredients in each sample are distributed；
2) with reference to projection matrix in optics tomographic reconstruction, flow field physical quantity image array, calculation matrix three relationship, structure is more
First LIBS quantitative analyses matrix equation, i.e.,
WF=P
In formula, W is standard sample normalization light spectral intensity matrix, the projection matrix being equivalent to during optical chromatography is rebuild；F is association
Matrix, flow field physical quantity image array, the P being equivalent to during optical chromatography is rebuild are standard sample atomic fraction matrix, are equivalent to
Calculation matrix；
3) standard sample normalization light spectral intensity matrix W is built as follows：
To this N number of standard sample with identical test condition and test parameter, LIBS detection is carried out, obtains and corresponds to this N number of sample
This N number of LIBS spectrogram is normalized in N number of LIBS spectrograms of quasi- sample, obtains N number of normalization LIBS spectrum
Figure.Take k characteristic spectral line (it is required that sample dimension N each element respectively>Spectral Dimensions kM), then it builds following N rows and multiplies kM
The standard sample normalization light spectral intensity matrix W of row：
KM value in the first row in normalization light spectral intensity matrix represents M element kM root of first standard sample and represents spectrum
The normalization spectral intensity values of line；KM value in second row represents M element kM root of second standard sample and represents spectral line
Normalize spectral intensity values；And so on ...；KM value in Nth row represents M element kM of n-th standard sample and represents spectral line
Normalization spectral intensity values；
4) the standard sample atomic fraction matrix P that following N rows multiply M row is built：
M value in the first row in atomic fraction matrix represents the atomic fraction of M element of first standard sample；Second row
In M value represent the atomic fraction of M element of second standard sample；And so on ...；M value in Nth row represents N
The atomic fraction of M element of a standard sample；
5) reflect that the incidence matrix F connected each other between W and P is represented by：
Incidence matrix F is the matrix that kM rows multiply M row, demand solution kM2A cell value can just obtain F matrix.Incidence matrix F is carried out
Row are decomposed into M interconnection vector F1、F2、F3、...、FM；Standard sample atomic fraction matrix P is decomposed into M atom into ranks
Scores vector P1、P2、P3、...、PM；
6) solution of incidence matrix F is converted to M interconnection vector F1、F2、F3、...、FMSolution, solving model is as follows：
Pi=WFi+Ei
In formula, i=1,2,3 ..., M, EiFor error vector, in N>In the case of kM, for FiBe solved to asking for overdetermined equation
Solution, it is necessary to make error minimum to get to the best fit approximation solution under the Optimality Criteria based on certain Optimality Criteria, using based on
The SIRT iterative algorithms of criterion of least squares are to interconnection vector FiIt is solved：
Fi 0=WTPi
In above formula, subscript 0 represents initial value；Subscript T represents transposition；Subscript q represents the q times iterative value；Subscript q+1 represents q+1
Secondary iterative value；λ is relaxation factor, and value size represents iterative constrained tightness；
The suspension condition of iteration is：
ε is the number of a very little, value 0.001；After iteration termination, FiLast time iterative value is FiSolving result；
7) by M all interconnection vector FiIt solves after completing, obtains incidence matrix F；To object to be measured with N number of standard sample
The identical test condition of product carries out LIBS detection, obtains a LIBS spectrogram, place is normalized to this LIBS spectrogram
Reason, obtains the normalization LIBS spectrograms of sample to be tested.Therefrom obtain the normalization that M element kM item of object to be measured represents spectral line
Spectral intensity vector：
D=[d1,d2,d3,...,dkM]
The atomic fraction of M element of object to be measured is calculated as follows：
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| CN111445964A (en) * | 2020-03-27 | 2020-07-24 | 合肥金星机电科技发展有限公司 | Method for visualizing component analysis results |
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