CN110749588B - Visualization method of process Raman signal - Google Patents
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- CN110749588B CN110749588B CN201911163299.1A CN201911163299A CN110749588B CN 110749588 B CN110749588 B CN 110749588B CN 201911163299 A CN201911163299 A CN 201911163299A CN 110749588 B CN110749588 B CN 110749588B
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- 238000001069 Raman spectroscopy Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000008569 process Effects 0.000 title claims abstract description 17
- 238000007794 visualization technique Methods 0.000 title abstract description 9
- 239000013598 vector Substances 0.000 claims abstract description 28
- 230000000007 visual effect Effects 0.000 claims abstract description 23
- 238000012800 visualization Methods 0.000 claims abstract description 10
- 238000013079 data visualisation Methods 0.000 claims abstract description 3
- 238000001228 spectrum Methods 0.000 claims description 17
- 238000010586 diagram Methods 0.000 claims description 5
- 239000013604 expression vector Substances 0.000 claims description 5
- 101150054439 TRHR gene Proteins 0.000 claims description 2
- 238000001237 Raman spectrum Methods 0.000 abstract description 9
- 238000012544 monitoring process Methods 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 5
- 230000003595 spectral effect Effects 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 20
- 230000008859 change Effects 0.000 description 11
- 230000004044 response Effects 0.000 description 11
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 8
- 239000002989 correction material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 3
- 206010034701 Peroneal nerve palsy Diseases 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N21/65—Raman scattering
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
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Abstract
The invention relates to the technical field of spectral measurement, in particular to a visualization method of process Raman signals. The invention relates to a visualization method of a process Raman signal, which comprises the following steps: 1) Establishing a data visualization coordinate; 2) Defining a scale mark and solving a visual vector parameter; 3) And drawing a tracked component visualization vector. The invention provides a visualization method for the signal intensity of a component to be focused, which solves the problem of interference of environment and background on the component measurement result and helps Raman spectrum to realize accurate, visual and convenient process monitoring application.
Description
Technical Field
The invention relates to the technical field of spectral measurement, in particular to a visualization method of process Raman signals.
Background
The raman spectrum has the advantages of fast response, non-contact, strong characteristics and the like, and can directly reflect the change condition of the concerned components in the process by directly recording the change condition of characteristic peaks, thereby being more and more concerned by the process on-line monitoring application. However, the raman spectrum collects scattered light, which is easily affected by other factors such as ambient light, particle scattered light, and fluorescence, and if only the raman spectrum is modified from physical conditions such as apparatus and environment, not only hardware cost is increased, but also application scenarios are limited.
The characteristic peaks of the Raman spectrum have better independence, which is the basis for the process tracking monitoring; the direct observed fluctuations are due to baseline elevation, and since the background baseline is usually sloped, the slope will also change most of the time, complicating the problem.
Disclosure of Invention
In order to solve the problems in the prior art, the present invention aims to provide a method for visualizing a raman signal in a process, the method comprising the following steps:
1) Establishing a data visualization coordinate;
2) Defining a scale mark and solving a visual vector parameter;
3) And drawing a tracked component visualization vector.
Preferably, step 1) is divided into the following steps:
a. selecting a characteristic peak of a tracked component, determining the initial position of the characteristic peak, and reading a sequence spectrum intensity value [ X ] in an interval as an X axis;
b. selecting a sequence spectrum intensity value [ Y ] corresponding to the characteristic peak from the actually measured Raman signal as a Y axis;
and c, forming a data point [ X, Y ] by using [ X ] and [ Y ], and drawing a rectangular coordinate graph which is a visual coordinate XY graph.
Preferably, step 2) is divided into the following steps:
a. drawing a series of data points [ X, Y0] formed by the [ X ] and a background signal [ Y0] without the tracked component on an XY diagram to obtain a characteristic peak P;
if the absolute intensity of the tracked component does not need to be reflected, only the relative intensity change needs to be observed, and the state with the lowest content of the tracked component can also be selected as the background, namely, the starting point moment of the chemical reaction is often used as the reference background [ Y0] during the process monitoring, and the component change condition at the subsequent moment is observed.
b. Drawing a graduation line Tx parallel to the x-axis at the transverse vertex T of P;
c. determining a point on an x axis at the peak waist of P, drawing scale lines Ty and Ty parallel to the y axis through the point, and intersecting the upper edge and the lower edge of Tx and P with C, A, B respectively;
d. measuring the lengths of AC and CB, and calculating the ratio of | AC |/| CB | to obtain a parameter value R of the visual vector;
e. and extending the TC cross-y axis to H, translating TH downwards to the origin, wherein the translated vector T' O is the visual expression vector with the tracked component content of 0.
Preferably, step 3) is divided into the following steps:
a. drawing a data point [ X, yr ] formed by the [ X ] and an actually measured spectrum signal [ Yr ] on an XY diagram to obtain an actually measured transverse peak Pr;
and b, crossing Pr and Ty at two points of Ar and Br, marking Cr according to the R value, connecting the vertex Tr with the marked Cr, prolonging TrCr, and crossing Y axis with Hr.
c. And (3) translating the TrHr up and down, coinciding the Hr 'with the original point O, wherein the translated vector Tr' O is the visual expression vector Vr of the Raman intensity of the tracked component.
The invention restrains the observation signal in the pure spectrum profile of the tracked component, because the spectrum profile can not be changed, the spectrum response contained in the profile is further induced to the base vector of the foot drop from the peak point to the base line, the vector avoids the influence of the base line slope, and the foot drop point is orthogonal projected and does not contain the response of the tracked component, namely, the lifting and the reduction of the vector are independent of the tracked component, therefore, the change of the component spectrum intensity can be reflected by the change of the vector slope degree.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a visualization method for the signal intensity of a component of interest, which solves the problem of interference of environment and background on a component measurement result and helps Raman spectrum to realize accurate, intuitive and convenient process monitoring application.
2. The invention provides an accurate, visual and convenient visualization process tracking expression method, which does not need hardware change or measurement condition limitation, does not need complex operations such as modeling and calculation such as reverse estimation of the content of a tracked component, and the visualization result can be directly used as an instrument setting parameter for monitoring a process system.
Drawings
FIG. 1 shows the pure Raman signals of each of the three components methanol, ethanol and propanol.
FIG. 2 shows Raman signals S1-S4 of mixed samples at different mixing ratios of methanol, ethanol and propanol.
FIG. 3 shows that S1-S4 have a wavenumber range of 2778cm -1 -2878cm -1 Raman signal of (a).
Fig. 4 is a schematic diagram of the visualization vector parameter R.
Fig. 5 shows the visualized vector calculation of methanol in state S1.
FIG. 6 shows the transformation and expression of the four states S1-S4.
FIG. 7 is a comparison of the direct raw spectra with the effect of the present invention on tracking methanol.
FIG. 8 is a comparison of the direct raw spectra with the ethanol effect of the present invention.
FIG. 9 is a comparison of the direct raw spectra with the ethanol effect of the present invention.
FIG. 10 shows Raman spectra of 11 correction fluid samples A1 to A11 and analytically pure carbon tetrachloride.
Fig. 11 shows the results of conventional raman viewing and the visualization effect of the present invention.
Detailed Description
The technical scheme of the invention is further described in detail by combining the drawings and the detailed implementation mode:
example one
As shown in FIGS. 1 and 2, if the system is kept pure and free of bubble and particle scattering interference, a flat spectrum can be detected, as in states S1-S3, but in the presence of scattering interference, scattering interference inevitably occurs, resulting in an elevated baseline, as in state S4.
2830cm of methanol -1 The peaks have relatively prominent features and the components used in this example track the peak locations. Although the characteristic peak of methanol is remarkable, the characteristic peak is still interfered by signals of other adjacent components.
In the four states of S1, S2, S3, S4, S1, S2 and S4 have the same methanol content of 10% and S3 has a methanol content of 15%. Under the conditions of system mixing and background interference, the actual content of the tracked methanol is difficult to judge intuitively and accurately only by direct observation of characteristic peaks.
As can be seen from fig. 3, the methanol content of S1 is the lowest, the methanol content of S2 is greater than that of S1, and S4 is affected by baseline drift, and if it is determined from the peak height only, the methanol content is equivalent to S3, and the error from the actual content is about 50%, the actual content of methanol in the four states cannot be intuitively determined.
The invention is implemented as follows:
1. and establishing visual coordinates.
1) Selecting characteristic peak of methanol, wave number range is 2778cm -1 -2878cm -1 In the range of the migration wavenumber, the Raman intensity value [ X ] of pure methanol]As the x-axis;
2) Selecting a sequence spectrum intensity value [ Y ] corresponding to the characteristic peak from the actually measured Raman signal as a Y axis;
3) X and Y form data points X, Y, and a rectangular coordinate graph is drawn, which is a visual coordinate XY.
2. Defining scale lines Ty and finding visual vector parameter R
1) Selecting the other component sequence spectrum intensity value [ Y0] without methanol, and drawing a series of responses by using a series of data points [ X, Y0] formed by [ X ] and [ Y0], wherein the series of data points is a transverse peak P in the graph 4.
If the absolute intensity of the methanol does not need to be reflected, only the relative intensity change needs to be observed, and the state with the lowest methanol content can also be selected as the background, namely, the component change condition at the subsequent moment is observed by taking the starting moment of the chemical reaction as the reference background [ Y0] during process monitoring.
2) A graduation line Tx parallel to the x-axis is drawn through the transverse vertex T of P, x =25000 is selected at the peak waist of P, and graduation lines Ty parallel to the y-axis are drawn, wherein Ty intersects C, A, B with the upper and lower edges of Tx and P, respectively.
3) The value of R = | AC |/| CB | is calculated to be equal to 1.738.
4) At the same time, the line segment TH is translated downward to the x-axis, and T' O indicates that its corresponding methanol response is equal to 0.
3. Drawing a tracked component visualization vector corresponding to the actual state
1) Collecting the S1 spectrum signal value [ Y1], drawing a data point [ X, Y1] formed by the pure methanol Raman intensity value [ X ] and [ Y1] on an XY coordinate to obtain P1.
2) P1 and the scale mark Ty are respectively crossed at two points A1 and B1; the position of C1 is determined by R, connecting vertex T1 with labeled C1, extending T1C1, intersecting the y-axis at H1.
3) Translating T1H1 up and down to make H1 coincide with the origin O, wherein the translated vector T1' O is a visual expression vector V1 of the Raman intensity of the tracked component, as shown in FIG. 5.
As shown in FIG. 6, the four states S1-S4 correspond to four visual vectors V1-V4 respectively, wherein V1, V2 and V4 are coincident, i.e. the Raman response intensities of the methanol are consistent, the ordinate value corresponding to the end point is 6560, i.e. 1/10 of the pure substance signal, the end point value of V3 is 9865, and the intensity ratio of V3 corresponding to V4 is 1.504, which accurately reflects the actual methanol intensity response tracked in S1-S4.
As can be seen from fig. 7, the visualized vectors fulfill the purpose of clear and accurate expression.
In the four states of S5-S8, the ethanol content of S5 is 60%, the ethanol content of S6 is 45%, and the ethanol content of S7 and S8 is 50%.
The selection was 398cm according to the procedure of the invention -1 -481cm -1 And analyzing the spectrogram in the wave number range to obtain four visual vectors respectively corresponding to V5-V8 in the component ethanol in the four states S5-S8. From fig. 8, it is seen that the ordinate value corresponding to the V5 endpoint is 2480, which is 59.76% of the pure material signal; v7 and V8 are almost overlapped, which shows that the ethanol Raman response intensity of S7 is consistent with that of S8, and the visualization vector can be adopted to clearly express the tracked actual ethanol intensity response in S5-S8.
In the four states of S9-S12, the propanol content of S9 is 30%, the propanol content of S11 and S12 is 40%, and the propanol content of S10 is 45%.
Selecting 380cm according to the implementation procedure of the invention -1 -520cm -1 And analyzing the spectrogram in the wave number range to obtain four visual vectors, wherein the propanol component in the four states S9-S12 respectively corresponds to V9-V12. From fig. 9, it is seen that the ordinate value corresponding to the V9 endpoint is 3600, which is 30% of the pure substance signal; v11 and V12 are overlapped, namely the propanol Raman response intensities of S11 and S12 are consistent, and the visualization vector can be used for clearly and accurately expressing the tracked actual propanol intensity response in S9-S12.
The visualization method provided by the invention can accurately track and express the Raman intensity of the tracked component, and visually reflect the component change condition in the process of background fluctuation.
Example two
Preliminary screening judgment of correction fluid solvent
Carbon tetrachloride is a forbidden component of the correction fluid, and the Raman spectrum is adopted in the embodiment to screen the existence condition of the carbon tetrachloride consisting of the raw materials of the correction fluid. It is known that A5 contains carbon tetrachloride by an off-line chemical method. Raman spectra of 11 correction fluid samples A1-A11 and analytically pure carbon tetrachloride are shown in FIG. 10.
According to the implementation steps of the invention, the range of 286cm of the characteristic peak wave number of carbon tetrachloride is selected -1 -348cm -1 Taking x =2900, R =0.4784 is obtained, and visualized vectors VA1-VA11 of carbon tetrachloride in A1-a11 are obtained, as shown in fig. 11.
The left side of fig. 11 shows the results of conventional raman spectroscopy, and the judgment effect is very insignificant due to the small content, the background scattering and the like. The right side of fig. 11 shows the visual effect of the present invention, and it can be seen that, except VA5, the ordinate values corresponding to the other VA1-VA11 tend to be 0, and it is easy to determine that the 10 samples do not use carbon tetrachloride as the solvent. Wherein VA5 is the visual effect of sample A5, the signal intensity of carbon tetrachloride for verification is 7140, the visual display of the invention VA5 corresponds to the ordinate value of 690, i.e. the A5 sample contains about 9.7% of the pure amount of carbon tetrachloride.
By adopting the visualization method provided by the invention, the halogenated hydrocarbon or benzene series in the correction fluid can be screened and judged visually, and the field analysis is realized.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (1)
1. A method for visualizing a process raman signal, comprising the steps of:
1) Establishing a data visualization coordinate;
2) Defining a scale mark and solving a visual vector parameter;
3) Drawing a tracked component visualization vector;
the step 1) is divided into the following steps:
a. selecting a characteristic peak of a tracked component, determining the initial position of the characteristic peak, and reading a sequence spectrum intensity value [ X ] in an interval as an X axis;
b. selecting a sequence spectrum intensity value [ Y ] corresponding to the characteristic peak from the actually measured Raman signal as a Y axis;
forming data points [ X, Y ] by [ X ] and [ Y ], and drawing a rectangular coordinate graph which is a visual coordinate XY graph; the step 2) is divided into the following steps:
a. will [ X ]]With background signal [ Y ] without tracked component 0 ]Formed series of data points [ X, Y0]]Drawing on an XY diagram to obtain a characteristic peak P;
b. drawing a graduation line Tx parallel to the x axis at the transverse vertex T of the P;
c. determining a point on the x axis at the peak waist of P, drawing a scale line Ty parallel to the y axis through the point, and intersecting the Ty with the upper and lower edges of Tx and P at C, A, B respectively;
d. measuring the lengths of AC and CB, and calculating the ratio of | AC |/| CB | to obtain a parameter value R of the visual vector;
e. extending the TC cross-y axis to H, translating TH downwards to the original point, wherein the translated vector T' O is a visual expression vector with the tracked component content of 0;
the step 3) is divided into the following steps:
a. drawing a data point [ X, yr ] formed by the [ X ] and an actually measured spectrum signal [ Yr ] on an XY diagram to obtain an actually measured transverse peak Pr;
b, crossing Pr and Ty at two points of Ar and Br, marking Cr according to the R value, connecting the vertex Tr and the marked Cr, prolonging TrCr, and crossing Y axis at Hr;
c. and translating the TrHr up and down, coinciding the Hr with the original point O, wherein the translated vector Tr' O is the visual expression vector Vr of the Raman intensity of the tracked component.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102998294A (en) * | 2012-12-20 | 2013-03-27 | 中国环境科学研究院 | Three-dimensional spectroscopic data correction method |
| CN105241866A (en) * | 2015-11-16 | 2016-01-13 | 广西科技大学 | Method for eliminating base line interference in Raman spectrum by utilizing fluorescent bleaching effect |
| CN108510519A (en) * | 2017-02-28 | 2018-09-07 | 哈尔滨工业大学 | The characteristic spectrum extracting method of dynamic object during a kind of tracking |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102998294A (en) * | 2012-12-20 | 2013-03-27 | 中国环境科学研究院 | Three-dimensional spectroscopic data correction method |
| CN105241866A (en) * | 2015-11-16 | 2016-01-13 | 广西科技大学 | Method for eliminating base line interference in Raman spectrum by utilizing fluorescent bleaching effect |
| CN108510519A (en) * | 2017-02-28 | 2018-09-07 | 哈尔滨工业大学 | The characteristic spectrum extracting method of dynamic object during a kind of tracking |
Non-Patent Citations (3)
| Title |
|---|
| Baseline correction for Raman spectra using penalized spline smoothing based on vector transformation;Yaoyi Cai et al.;《Analytical Method》;20181231;第10卷(第28期);第3525-3533页 * |
| 基于三次样条曲线拟合的激光拉曼光谱基线校正研究;聂磊 等;《湖北工业大学学报》;20170228;第32卷(第1期);第63-67页 * |
| 通过向量角转换校正拉曼光谱中乘性干扰;姚志湘 等;《光谱学与光谱分析》;20160229;第36卷(第2期);第419-423页 * |
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