CN112763436A - Spectrum measuring system - Google Patents
Spectrum measuring system Download PDFInfo
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- CN112763436A CN112763436A CN202011553314.6A CN202011553314A CN112763436A CN 112763436 A CN112763436 A CN 112763436A CN 202011553314 A CN202011553314 A CN 202011553314A CN 112763436 A CN112763436 A CN 112763436A
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
- G01N21/274—Calibration, base line adjustment, drift correction
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Abstract
The invention belongs to the technical field of spectral measurement, and particularly relates to a spectral measurement system. The device comprises a light source (1) and a spectrometer (3) which are connected to a multiplexer (2), and also comprises a plurality of measuring optical fiber probes (5) which are connected with the multiplexer (2), wherein the measuring optical fiber probes (5) can be arranged in solutions of different measuring points (8); the multiplexer (2) can select one of the measuring optical fiber probes (5), the detection light emitted by the light source (1) is coupled to the selected measuring optical fiber probe (5), the reflected light obtained by the selected measuring optical fiber probe (5) is coupled to the spectrometer (3), the spectrometer (3) is used for obtaining a spectrum signal of the reflected light, and the spectrum signal is used for obtaining the solution concentration. The online spectrum measurement of a plurality of measurement optical fiber probes (5) is realized, and the background signal drift is corrected online on the premise that the measurement optical fiber probes (5) are not pulled out and the online measurement of the measurement optical fiber probes (5) is not influenced.
Description
Technical Field
The invention belongs to the technical field of spectral measurement, and particularly relates to a spectral measurement system.
Background
In some chemical product production or chemical experiments, the concentration of some intermediate reaction liquid or final product liquid needs to be measured by multipoint online spectrum. Of these measurements, many employ fiber optic probe technology for on-line monitoring, but these monitoring suffer from two major drawbacks: firstly, one light source and one spectrometer are needed for monitoring one process point, and a plurality of light sources and a plurality of spectrometers are needed for a plurality of process points. Secondly, the online correction can not be realized under the condition of not pulling out the online measuring probe.
Disclosure of Invention
The invention aims to provide spectral measurement equipment which can monitor a plurality of process points on line and can correct background signal drift on line on the premise of not pulling out a measurement probe.
In order to achieve the above purpose, the technical scheme adopted by the invention is a spectral measurement system, which is used for measuring the concentration of a solution, and comprises a light source and a spectrometer which are connected to a multiplexer, and also comprises a plurality of measurement optical fiber probes connected with the multiplexer, wherein the measurement optical fiber probes can be arranged in the solution at different measurement points; the multiplexer can select one of the measurement fiber probes, couple the detection light emitted by the light source to the selected measurement fiber probe, and couple the reflected light acquired by the selected measurement fiber probe to the spectrometer, wherein the spectrometer is used for acquiring a spectrum signal of the reflected light, and the spectrum signal is used for acquiring the solution concentration of a measurement point where the selected measurement fiber probe is located.
The system further comprises a computer connected with the spectrometer, wherein the computer is used for processing the spectral signal generated by the spectrometer to obtain the concentration of the solution.
Furthermore, the light source is connected with the multiplexer through one path of optical fiber, and the spectrometer is connected with the multiplexer through the other path of optical fiber.
Furthermore, each measuring fiber probe is connected with the multiplexer through one optical fiber.
The optical fiber correction device further comprises a correction optical fiber probe arranged in the external air environment, wherein the correction optical fiber probe is used for obtaining a first correction signal and a second correction signal, the first correction signal refers to an optical signal obtained by the correction optical fiber probe before the spectrograph and the light source drift, and the second correction signal refers to an optical signal obtained by the correction optical fiber probe after the spectrograph and the light source drift.
Further, the computer is further configured to calculate the first correction signal and the second correction signal to obtain a proportional relationship, and correct the spectral signal according to the proportional relationship and then process the spectral signal to obtain the solution concentration.
Further, the number of the measuring fiber probes is 6.
The invention has the beneficial effects that:
1. one light source 1 and one spectrometer 3 realize online spectrum measurement of a plurality of measurement fiber probes 5.
2. The background signal drift is corrected on line on the premise of not pulling out the measuring optical fiber probe 5 and not influencing the on-line measurement of the measuring optical fiber probe 5.
Drawings
FIG. 1 is a schematic diagram of a spectroscopic measurement system according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the linear relationship of uranium tetraoxide in an embodiment of the present invention;
FIG. 3 is a diagram of a 2g/L uranium tetravalent spectrum normally measured in an example of the present invention;
FIG. 4 is a spectrum of 2g/L uranium before correction in example of the present invention;
FIG. 5 is a spectrogram of 2g/L corrected uranium in the example of the present invention;
in the figure: 1-light source, 2-multiplexer, 3-spectrometer, 4-computer, 5-measuring optical fiber probe, 6-correcting optical fiber probe, 7-optical fiber and 8-measuring point.
Detailed Description
The invention is further described below with reference to the figures and examples.
As shown in fig. 1, the spectrum measuring system provided by the present invention is used for measuring solution concentration, and includes a light source 1 and a spectrometer 3 connected to a multiplexer 2, and also includes a plurality of measuring fiber probes 5 (total 6) connected to the multiplexer 2, the measuring fiber probes 5 can be disposed in solutions at different measuring points 8 (the measuring points 8 are in a reaction solution in which an element to be measured is located); the multiplexer 2 can select one of the measurement fiber probes 5, couple the probe light emitted by the light source 1 to the selected measurement fiber probe 5, and couple the reflected light obtained by the selected measurement fiber probe 5 to the spectrometer 3 (the reflected light is a light signal which is reflected back to the measurement fiber probe 5 through a mirror after the probe light is absorbed by an element to be measured in a reaction solution), the spectrometer 3 is used for obtaining a spectrum signal of the reflected light, and the spectrum signal is used for obtaining a solution concentration of a measurement point 8 where the selected measurement fiber probe 5 is located (the light absorbed by the element to be measured is in a proportional relationship with the concentration of the element to be measured, and the concentration of the element to be measured is calculated and measured by the data processing. If the concentration of the element to be measured at another measuring point 8 is measured, the optical path switching part of the multiplexer 2 is rotated to switch the optical path to the corresponding measuring optical fiber probe 5, and the spectrum signal measured by the measuring optical fiber probe 5 is in proportional relation with the concentration of the element to be measured. And obtaining the concentration of the element to be detected through corresponding data processing. Other measurement point measurements and so on.
The device further comprises a computer 4 connected with the spectrometer 3, wherein the computer 4 is used for processing the spectrum signal generated by the spectrometer 3 to obtain the solution concentration.
The light source 1 is connected with the multiplexer 2 through one path of optical fiber 7, and the spectrometer 3 is connected with the multiplexer 2 through the other path of optical fiber 7.
Each measuring fiber probe 5 is connected to the multiplexer 2 via a respective optical fiber 7.
The optical fiber correction device further comprises a correction optical fiber probe 6 (placed in a place where the light intensity in the air is stable) arranged in the external air environment, wherein the correction optical fiber probe 6 is used for obtaining a first correction signal and a second correction signal, the first correction signal refers to an optical signal obtained by the correction optical fiber probe 6 before the spectrometer 3 and the light source 1 drift, and the second correction signal refers to an optical signal obtained by the correction optical fiber probe 6 after the spectrometer 3 and the light source 1 drift.
The computer 4 is further configured to calculate the first correction signal and the second correction signal to obtain a proportional relationship, and process the spectrum signal after the proportional relationship is corrected to obtain the solution concentration.
The light source 1 and the spectrometer 3 can generate the drift change of the background light signal after long-term use. Other components such as the multiplexer 2, the optical fiber connector, the measuring optical fiber probe 5 and the like are fixed as long as physical geometric changes and connector tightness do not change, and once the optical path is connected, the influence factors are fixed and cannot change along with time, and the influence factors are eliminated by blank buckling. Even if the geometry of the light source 1 and the spectrometer 3 is fixed, the light emitting efficiency of the light source 1 and the detection efficiency of the spectrometer 3 will change. Because the signal drift mainly comes from the light source 1 and the spectrometer 3, the measuring light path of other 6 measuring optical fiber probes 5 and the correcting light path of the correcting optical fiber probe 6 share one light source 1 and one spectrometer 3, the light path can be switched to the correcting light path, the correcting light path can capture the drift signal change, and the correcting light path calculates the proportional relation through the light signal change before and after the measuring drift. When the optical path is switched to 6 measuring optical paths, the optical signal measured by each measuring optical fiber probe 5 is corrected by the proportional relation generated by the correction optical path, and then concentration calculation is performed. The operation of pulling out the probe and the like on the measuring light path is not needed, and the online spectrum correction is realized.
Examples
In a certain continuous extraction experiment, the content of the tetravalent uranium in each stage of solution needs to be measured in real time so as to reflect the extraction state.
If the concentration of the uranium in a certain level of feed liquid is measured, the optical signal is switched to a corresponding measuring optical fiber probe 5 through the multiplexer 2. The absorbance measured by the measuring optical fiber probe 5 is in proportional relation with the concentration of the uranium, the concentration of the uranium is obtained through calculation of a mathematical model, and 6 independent measuring optical fiber probes 5 are connected with the multiplexer 2, so that the measurement of the uranium in 6 extraction tanks is completed.
Analytical range of uranic: different concentrations of organic phase (30% TBP kerosene) tetravalent uranium were prepared and the absorbance of different standards was measured at 1076.25nm in the absence of 30% TBP kerosene (see Table 1). The change in the concentration of tetravalent uranium is plotted on the abscissa and the absorbance on the ordinate (see FIG. 2).
TABLE 1 results of formulating concentration of tetravalent uranium and measuring absorbance
Concentration of tetravalent uranium (g/L) | A(1076.25nm) |
0.0978 | 0.00038 |
0.1956 | 0.01521 |
0.3912 | 0.04307 |
0.489 | 0.06613 |
1.0106 | 0.12065 |
1.9886 | 0.24829 |
2.9992 | 0.3808 |
4.0098 | 0.50166 |
5.9984 | 0.75136 |
The experimental results show that: the linear relation of the concentration of the uranium in the range of 0.1-6.0g/L is good, and the R of the working curve of the probe 1-620.9995, 0.9996, 0.9995, 0.9988 and 0.9995, respectively.
Tetravalent uranium measurement accuracy (see table 2): and (3) measuring the absorbance of the same uranium sample by using a No. 1-6 probe, respectively introducing the absorbance into respective mathematical models, calculating the concentration of the tetravalent uranium, and inspecting the precision. Samples of uranium of different concentrations were investigated.
TABLE 2 uranium measurement accuracy
The experimental results show that: the precision of the uranium with different concentrations is better than 10%.
The linear relation of the concentration of the uranium in the range of 0.1-6.0g/L is good, and the R of the working curve of the probe 1-620.9995, 0.9996, 0.9995, 0.9988 and 0.9995, respectively. The measurement precision of the uranium quadrivalent with different concentrations is better than 10 percent.
On-line correction is considered, fig. 3 is an absorption spectrogram of a 2g/L tetravalent uranium sample during on-line measurement, a fiber connector of a light source 1 and a connector of a spectrometer 3 are loosened slightly artificially, signal change and drift are simulated and manufactured, as shown in fig. 4, a light path is switched to a correction light path of a correction fiber probe 6 for correction, and then the light path is switched back to a measurement fiber probe 5, and as signals at the moment can be corrected, the absorbance value is restored to an original value, as shown in fig. 5.
The data shows that the online correction function is realized by switching the correction light path on the premise of not pulling out the measurement optical fiber probe 5.
The device according to the present invention is not limited to the embodiments described in the specific embodiments, and those skilled in the art can derive other embodiments according to the technical solutions of the present invention, and also belong to the technical innovation scope of the present invention.
Claims (7)
1. A spectral measurement system for measuring the concentration of a solution, characterized in that: the device comprises a light source (1) and a spectrometer (3) which are connected to a multiplexer (2), and also comprises a plurality of measuring optical fiber probes (5) which are connected with the multiplexer (2), wherein the measuring optical fiber probes (5) can be arranged in solutions of different measuring points (8); the multiplexer (2) can select one of the measuring fiber probes (5), couple the detection light emitted by the light source (1) to the selected measuring fiber probe (5), and couple the reflected light acquired by the selected measuring fiber probe (5) to the spectrometer (3), wherein the spectrometer (3) is used for acquiring a spectral signal of the reflected light, and the spectral signal is used for acquiring the solution concentration of a measuring point (8) where the selected measuring fiber probe (5) is located.
2. A spectroscopic measurement system as set forth in claim 1 wherein: the device is characterized by further comprising a computer (4) connected with the spectrometer (3), wherein the computer (4) is used for processing the spectrum signal generated by the spectrometer (3) to obtain the solution concentration.
3. A spectroscopic measurement system as set forth in claim 2 wherein: the light source (1) is connected with the multiplexer (2) through one path of optical fiber (7), and the spectrometer (3) is connected with the multiplexer (2) through the other path of optical fiber (7).
4. A spectroscopic measurement system as set forth in claim 3 wherein: each measuring fiber probe (5) is connected with the multiplexer (2) through one optical fiber (7).
5. A spectroscopic measurement system as set forth in claim 4 wherein: the optical fiber correction device further comprises a correction optical fiber probe (6) arranged in the external air environment, wherein the correction optical fiber probe (6) is used for obtaining a first correction signal and a second correction signal, the first correction signal refers to an optical signal obtained by the correction optical fiber probe (6) before the spectrometer (3) and the optical source (1) drift, and the second correction signal refers to an optical signal obtained by the correction optical fiber probe (6) after the spectrometer (3) and the optical source (1) drift.
6. A spectroscopic measurement system as set forth in claim 5 wherein: the computer (4) is further used for calculating the first correction signal and the second correction signal to obtain a proportional relation, and processing the spectrum signal after the proportional relation is corrected to obtain the solution concentration.
7. A spectroscopic measurement system as set forth in claim 6 wherein: the number of the measuring optical fiber probes (5) is 6.
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CN108375546A (en) * | 2018-01-31 | 2018-08-07 | 中国科学院合肥物质科学研究院 | The online multipoint detection device of chemical fertilizer based on Vis/NIR technology and its detection method |
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Patent Citations (10)
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US20080190557A1 (en) * | 2001-09-25 | 2008-08-14 | Eci Technology, Inc. | Apparatus for real-time dynamic chemical analysis |
CN101135640A (en) * | 2007-07-06 | 2008-03-05 | 华南师范大学 | Quasi-distributed optical fiber concentration sensor |
CN101329271A (en) * | 2008-07-15 | 2008-12-24 | 浙江大学 | Industry on-line near-infrared spectrum detection device |
US20130100439A1 (en) * | 2009-12-04 | 2013-04-25 | Duke University | Smart fiber optic sensors systems and methods for quantitative optical spectroscopy |
CN102818776A (en) * | 2012-08-08 | 2012-12-12 | 赵晓明 | Dye liquor concentration in-situ on-line monitoring system |
CN103398966A (en) * | 2013-08-20 | 2013-11-20 | 杭州北斗星膜制品有限公司 | Method for detecting TMC concentration in organic solution by using spectrometer |
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