CN112268891B - LIBS-Raman immersion type salt lake brine element detector - Google Patents

LIBS-Raman immersion type salt lake brine element detector Download PDF

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CN112268891B
CN112268891B CN202011096825.XA CN202011096825A CN112268891B CN 112268891 B CN112268891 B CN 112268891B CN 202011096825 A CN202011096825 A CN 202011096825A CN 112268891 B CN112268891 B CN 112268891B
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spectrum
spectrometer
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CN112268891A (en
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武中臣
凌宗成
吴得福
张江
辛艳青
张鹏彦
蔡雷
王永淇
隋宗斌
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Shandong University
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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
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A90/00—Technologies having an indirect contribution to adaptation to climate change
    • Y02A90/30—Assessment of water resources

Abstract

The invention discloses a LIBS-Raman immersed brine element detector. Pulse laser output by the pulse laser is input to the laser beam expander through the excitation optical fiber to be expanded, the converging lens focuses the laser after being expanded, the transmission direction of the laser is changed through the reflector, so that the focal point is positioned in the liquid excitation cavity, the excitation probe collects the spectrum emitted by the excited sample, and the spectrum is input to the Raman probe or the LIBS spectrometer through the signal collection branched optical fiber; the Raman probe is used for filtering the acquired spectrum signal and sending the filtered spectrum to the Raman spectrometer; and the computer stores and analyzes the spectral information sent by the Raman spectrometer and/or the LIBS spectrometer and determines the types of the cations and/or the anions in the sample. The invention analyzes and detects ions in the solution sample by the LIBS and Raman combined technology, improves the detection speed, realizes the real-time on-line analysis, and plays an important role in scientific research and pollution prevention and control.

Description

LIBS-Raman immersion salt lake brine element detector
Technical Field
The invention relates to the field of salt lake brine element detection, in particular to a LIBS-Raman immersed salt lake brine element detector.
Background
The salt lake is a common salt water lake on the earth, is mostly seen in arid regions, is rich in various salt minerals such as Li, K, Na, Mg, Br and other elements, for example, the B content in the small chai dan salt lake is as high as 4000Mg/L, and the LiCl content in some salt lakes in Tibet can reach more than 10000Mg/L, and is a naturally-occurring resource treasury. The salt lake has great development potential, and the reasonable development can provide rich raw materials for chemical industry, agriculture, metallurgy and other industries in China. At present, the analysis and detection means for salt lake brine mainly comprise atomic absorption spectrophotometry, flame atomic absorption photometry, electric coupling plasma spectrometry and some traditional chemical methods (such as neutralization method, various titration methods and the like). Although the above methods have very high detection accuracy, they all require sampling and tedious, complex, time-consuming pretreatment of the sample to allow detection. If a traditional method is adopted for sampling and submitting for inspection in an unknown water area, a large amount of time and manpower are wasted, the research progress is slowed down, strict requirements are also imposed on the collection, transportation and storage processes of samples, and the final result is influenced when careless mistakes occur in any one link. For the detection of salt lake brine, an instant and effective detection method is required.
Disclosure of Invention
Based on the above, the invention aims to provide the LIBS-Raman immersed salt lake brine element detector, which utilizes LIBS to detect the type and concentration of cations and utilizes Raman to detect acid radical ions so as to achieve comprehensive analysis of salt lake brine.
In order to achieve the purpose, the invention provides the following scheme:
a LIBS-Raman immersion salt lake brine element detector comprises: a chassis portion and an immersion probe;
the case part comprises a computer, a Raman probe, a Raman spectrometer, an LIBS spectrometer and a pulse laser;
the immersion probe comprises an immersion probe shell, and a laser beam expander, a convergent lens, a reflector, a liquid excitation cavity and a fiber probe which are arranged in the immersion probe shell and connected in sequence;
pulse laser output by the pulse laser is input to the laser beam expander through an excitation optical fiber to be expanded, the converging lens focuses the laser after being expanded, the transmission direction of the laser is changed through the reflector, so that the focal point is positioned in the liquid excitation cavity, the excitation probe collects a spectrum emitted by an excited sample and inputs the spectrum to a Raman probe or a LIBS spectrometer through a signal collection branched optical fiber; the Raman probe is used for filtering the acquired spectrum signals and sending the filtered spectrum to the Raman spectrometer; and the computer stores and analyzes the spectral information sent by the Raman spectrometer and/or the LIBS spectrometer and determines the types of the cations and/or the anions in the sample.
Optionally, a miniature camera is further disposed in the immersion probe housing, and is used for shooting an underwater environment.
Optionally, a temperature sensor is further arranged in the immersion probe shell and used for collecting the water body temperature and sending the water body temperature to the computer through a data line for display.
Optionally, the chassis part further includes an image processor for processing the image captured by the micro camera and sending the processing result to the computer.
Optionally, the method further comprises:
and the delayer is respectively connected with the pulse laser, the Raman spectrometer and the LIBS spectrometer, and is used for controlling the LIBS spectrometer to be started after the pulse laser is started and controlling the pulse laser and the Raman spectrometer to be started synchronously.
Optionally, the Raman probe comprises a 532nm sideband filter and a 532nm notch plate.
The invention also provides a detection method using the LIBS-Raman immersed salt lake brine element detector, which comprises the following steps:
selecting a working mode according to the test purpose; the working modes comprise an LIBS mode and a Raman mode;
when the liquid sample is in an LIBS mode, pulse laser is transmitted to a laser beam expander through an excitation optical fiber to expand the beam, a converging lens focuses a light beam after the beam expansion, the transmission direction of the laser is changed through a reflector, so that a focal point is positioned in a liquid excitation cavity, the liquid excitation process is finished in the liquid excitation cavity, an optical fiber probe collects a spectrum emitted by an excited sample, and the spectrum is transmitted into an LIBS spectrometer through a signal collection optical fiber to finish the collection of the spectrum;
when the Raman probe is in a Raman mode, pulse laser is transmitted to the laser beam expander through the excitation optical fiber to expand the beam, the convergent lens focuses the beam after expanding the beam, the transmission direction of the laser is changed through the reflector, so that the focal point is positioned in the liquid excitation cavity, the liquid excitation process is completed in the liquid excitation cavity, the optical fiber probe collects the spectrum emitted by the excited sample, the spectrum is transmitted to the Raman probe through the signal collection optical fiber to be collected and analyzed, the Raman probe is used for filtering out spectral information of bands 532nm and below 532nm, only the components with the wavelength larger than 532nm are reserved and are transmitted to the Raman spectrometer, and the spectrum collection is completed;
the collected spectral information is transmitted to a computer in real time for storage, and the spectrum of the detected target substance is identified and quantitatively analyzed through a pre-built LIBS spectral database, a Raman spectral database, a quantitative analysis model of the heavy metal ions in the salt lake brine based on the LIBS spectrum and a Raman spectral quantitative analysis model, so that the species and abundance values of the cations and the anions of the detected target substance are obtained.
Optionally, when in the LIBS mode, the pulsed laser is a high-energy pulse to excite the sample to be detected into plasma; when in Raman mode, the energy of the pulsed laser reaches the threshold of Raman excitation but is insufficient to excite the sample into a plasma.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention integrates the LIBS system and the Raman system into a set of equipment, the LIBS system and the Raman system share a pulse laser as an excitation light source (532nm laser), the excitation mode is controlled by changing the power of the laser, and the spectral signals collected under the LIBS mode and the Raman mode are respectively sent to different spectrometers for analysis by utilizing the branched optical fibers. The invention analyzes and detects the ions in the solution sample by the LIBS and Raman combined technology, improves the detection speed, realizes the real-time on-line analysis, and plays an important role in scientific research, geological exploration and pollution prevention and control. The LIBS-Raman immersed salt lake brine element detector disclosed by the invention is small in volume and energy consumption, convenient to carry and more beneficial to field detection on site.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a LIBS-Raman immersed salt lake brine element detector according to an embodiment of the invention.
Description of the symbols: 1-a computer, 2-an image processor, 3-a Raman probe, 4-a Raman spectrometer, 5-a LIBS spectrometer, 6-a pulse laser, 7-a delayer, 8-a data line, 9-an excitation optical fiber, 10-a signal collection branched optical fiber and 11-an immersion probe; 12-a miniature camera, 13-a laser beam expander, 14-a fiber probe, 15-a convergent lens, 16-a liquid excitation cavity, 17-a reflector and 18-a temperature sensor.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention aims to provide a LIBS-Raman immersed salt lake brine element detector, which utilizes LIBS to detect the type and concentration of cations and utilizes Raman to detect acid radical ions so as to achieve the comprehensive analysis of salt lake brine.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1, the LIBS-Raman submerged salt lake brine element detector includes: a chassis portion and an immersion probe;
the cabinet part comprises a computer 1, a Raman probe 3, a Raman spectrometer 4, a LIBS spectrometer 5 and a pulse laser 6. The Raman probe comprises a 532nm wave-trap plate and a 532nm sideband filter plate. The Raman spectrometer can be replaced by a photomultiplier tube fitted with a specific color filter.
The immersion probe comprises an immersion probe shell 11, and a laser beam expander 13, a convergent lens 15, a reflecting mirror 17, a liquid excitation cavity 16 and a fiber probe 14 which are arranged in the immersion probe shell 11 and are sequentially connected.
The pulse laser output by the pulse laser 1 is input to the laser beam expander 13 through the excitation optical fiber 9 for beam expansion, the converging lens 15 focuses the laser after beam expansion, the transmission direction of the laser is changed through the reflecting mirror 17, so that the focal point is positioned in the liquid excitation cavity 16, the excitation probe 14 collects the spectrum emitted by the excited sample, and the spectrum is input to the Raman probe 3 or the LIBS spectrometer 5 through the signal collection branched optical fiber; the Raman probe 3 is used for filtering the acquired spectrum signals and sending the filtered spectrum to the Raman spectrometer 4; the computer 1 stores and analyzes the spectral information sent by the Raman spectrometer 4 and/or the LIBS spectrometer 5, and determines the types of the cations and/or the anions in the sample.
In an alternative embodiment, a miniature camera 12 is further disposed in the immersion probe housing 11, and the chassis portion further includes an image processor 2. The underwater working environment is detected by the micro camera 12 (with a lighting source), and whether the surrounding situation of the detection place is suitable for spectrum detection (the detection object is a water body immersed around the probe) is mainly observed by continuously taking underwater pictures. The image processor 2 functions to process the picture transmitted from the micro-camera 12, display it and simultaneously display the temperature and depth information at the time of taking the picture.
As an optional embodiment, a temperature sensor 18 is further arranged in the immersion probe shell 11, and temperature information of the water body at the depth is recorded and transmitted back in real time by using the temperature sensor 18 and is dynamically displayed on the computer 1.
As an optional implementation manner, the laser system further comprises a delayer 7, the delayer 7 plays a role of controlling a switch on the LIBS spectroscopy system and the Raman spectroscopy system, in the LIBS mode, a suitable delay parameter can be set, and after the pulse laser 1 works for a certain time, the LIBS spectrometer 5 is started in a delay manner, so that the influence of bremsstrahlung and composite radiation excited at the initial stage of plasma cooling is reduced, and the signal-to-noise ratio is improved; in the Raman mode, the delayer controls the Raman spectrometer 4 to be synchronously opened with the pulse laser 1, and the shutter is closed after the acquisition for a certain time, so that the influence of a fluorescence spectrum generated in the later period is reduced, and the signal-to-noise ratio is improved.
The working process is as follows:
when the instrument is used, the probe is required to be completely immersed below the liquid level, the instrument is powered on, the computer is started, and the system enters a working state. At the moment, the underwater working environment can be detected through the micro camera (with the illumination light source), the surrounding situation of a detection place is mainly observed through continuously shooting underwater pictures, and whether the spectrum detection is suitable or not is further judged manually (a detection object is immersed in a water body around the probe). The image processor is used for processing the picture transmitted by the camera, displaying the picture and simultaneously displaying the temperature and depth information when the picture is taken. And recording and transmitting temperature information of the water body at the depth in real time by using the temperature sensor, and dynamically displaying the temperature information on a computer. And then according to the purpose of the test, selecting to independently perform LIBS (mainly detect the cation information of the target substance) or independently perform Raman (mainly detect the anion group information of the target substance) or sequentially perform LIBS and Raman detection, and starting the spectral excitation and collection work. In LIBS mode, a 532nm pulsed laser outputs high energy pulses with energy above the LIBS excitation threshold. Laser is transmitted to the probe part through the excitation optical fiber, beam expansion is carried out by the laser beam expander, the converging lens focuses the light beam after beam expansion, and the transmission direction of the laser is changed through the reflector, so that the focus is positioned in the excitation cavity. The excitation cavity is internally separated by glass and externally communicated with the outside for liquid to enter, and the excitation process of the liquid is finished in the cavity. The optical fiber probe is positioned above the cavity and is responsible for collecting the spectrum emitted by the excited sample and then transmitting the spectrum into the cavity through the signal collecting optical fiberAnd (5) completing the collection of the spectrum by using the LIBS spectrometer. When the Raman mode is selected, the laser output power is reduced and the pulse energy reaches the threshold for Raman excitation but is insufficient to excite the sample into a plasma. Laser is likewise through expanding the beam and focusing back with liquid excitation in arousing the cavity, gathers by the fiber probe, and the difference is, and the branching optic fibre can be with light information transmission to Raman probe collection analysis this moment. A532 nm trap wave plate and a 532nm sideband filter plate are arranged in front of the Raman probe and are used for filtering out spectral information of 532nm and other wave bands lower than 532nm, only components with the wavelength larger than 532nm are reserved and are sent to a 4-Raman spectrometer. In the system operation process, the delayer plays a role of controlling a switch on the LIBS (laser induced breakdown spectroscopy) spectrum system and the Raman spectrum system, a proper delay parameter can be set in the LIBS mode, and after a pulse laser outputs a laser pulse (microsecond level), the LIBS spectrometer is started in a delayed mode, so that the influence of bremsstrahlung and composite radiation excited at the plasma cooling initial stage is reduced, and the signal-to-noise ratio is improved; in the Raman mode, the delayer controls the Raman spectrometer and the laser to be synchronously opened, and the shutter is closed after the acquisition for a certain time, so that the influence of a fluorescence spectrum generated in the later period is reduced, and the signal-to-noise ratio is improved. The whole instrument analyzes and detects metal ions in the solution through a LIBS system, and analyzes and detects anions such as (SO) in the solution through a Raman system4 2-、CO3 2-) And detecting, wherein the acquired spectral information is transmitted to a computer in real time for storage, and the spectrum of the detected target substance is identified and quantitatively analyzed through a pre-built LIBS spectral database, a Raman spectral database, a quantitative analysis model of the heavy metal ions in the salt lake brine based on the LIBS spectrum and a Raman spectral quantitative analysis model, so that the types and abundance values of the cations and anions of the detected target substance are obtained.
The invention integrates the LIBS system and the Raman system into a set of equipment, the LIBS system and the Raman system share a pulse laser as a laser source, the excitation mode is controlled by changing the power of laser, and the spectral signals collected under the LIBS mode and the Raman mode are respectively sent to different spectrometers to be analyzed by utilizing the branched optical fibers.
The invention has simple structure, and consists of a water machine case part and an underwater probe part, wherein the probe and the machine case are connected through a data line and an optical fiber. By selecting different working modes, LIBS excitation and Raman excitation are respectively carried out on a sample (underwater liquid analyte), and collected spectral information is transmitted back to a computer for subsequent analysis and processing. And respectively setting the optimal sampling delay time and the optimal spectrum accumulation time in different modes, and improving the signal-to-noise ratio of the acquired spectrum. LIBS is used for detecting the type and concentration of cations, and Raman is used for detecting acid radical ions so as to achieve comprehensive analysis of a detected sample.
In the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.

Claims (8)

1. The LIBS-Raman immersed salt lake brine element detector is characterized by comprising: a chassis portion and an immersion probe;
the case part comprises a computer, a Raman probe, a Raman spectrometer, an LIBS spectrometer and a pulse laser;
the immersion probe comprises an immersion probe shell, and a laser beam expander, a convergent lens, a reflector, a liquid excitation cavity and a fiber probe which are arranged in the immersion probe shell and connected in sequence;
pulse laser output by the pulse laser is input to the laser beam expander through an excitation optical fiber to be expanded, the converging lens focuses the laser after being expanded, the transmission direction of the laser is changed through the reflector, so that the focal point is positioned in the liquid excitation cavity, the excitation probe collects a spectrum emitted by an excited sample and inputs the spectrum to a Raman probe or a LIBS spectrometer through a signal collection branched optical fiber; the Raman probe is used for filtering the acquired spectrum signals and sending the filtered spectrum to the Raman spectrometer; and the computer stores and analyzes the spectral information sent by the Raman spectrometer and/or the LIBS spectrometer and determines the types of the cations and/or the anions in the sample.
2. The LIBS-Raman immersion salt lake brine element detector of claim 1, wherein a micro-camera is further disposed within the immersion probe housing for capturing images of the underwater environment.
3. The LIBS-Raman immersion salt lake brine element detector of claim 1, wherein a temperature sensor is further disposed within the immersion probe housing for acquiring the temperature of the water body and transmitting the temperature of the water body to the computer for display via a data line.
4. The LIBS-Raman immersion salt lake brine element detector of claim 2, wherein the cabinet portion further comprises an image processor for processing the image captured by the micro-camera and sending the result to the computer.
5. The LIBS-Raman submerged salt lake brine element detector of claim 1, further comprising:
and the delayer is respectively connected with the pulse laser, the Raman spectrometer and the LIBS spectrometer, and is used for controlling the LIBS spectrometer to be started after the pulse laser is started and controlling the pulse laser and the Raman spectrometer to be started synchronously.
6. The LIBS-Raman immersion salt lake brine element detector of claim 1, wherein the Raman probe comprises a 532nm trap plate and a 532nm sideband filter plate.
7. A detection method using the LIBS-Raman immersed salt lake brine element detector as claimed in any one of claims 1 to 6, comprising:
selecting a working mode according to the test purpose; the working modes comprise an LIBS mode and a Raman mode;
when the sample plasma is in an LIBS mode, pulse laser is transmitted to a laser beam expander through an excitation optical fiber to expand the beam, a converging lens focuses the beam after expanding the beam, the transmission direction of the laser is changed through a reflector, so that the focal point is positioned in a liquid excitation cavity, the liquid excitation process is finished in the liquid excitation cavity, an optical fiber probe collects the emission spectrum of the excited sample plasma, and the emission spectrum is transmitted to an LIBS spectrometer through a signal collection optical fiber to finish the spectrum collection;
when the Raman probe is in a Raman mode, pulse laser is transmitted to the laser beam expander through the excitation optical fiber to expand the beam, the convergent lens focuses the beam after expanding the beam, the transmission direction of the laser is changed through the reflector, so that the focal point is positioned in the liquid excitation cavity, the liquid excitation process is completed in the liquid excitation cavity, the optical fiber probe collects the spectrum emitted by the excited sample, the spectrum is transmitted to the Raman probe through the signal collection optical fiber to be collected and analyzed, the Raman probe is used for filtering out spectral information of bands 532nm and below 532nm, only the components with the wavelength larger than 532nm are reserved and are transmitted to the Raman spectrometer, and the spectrum collection is completed;
the collected spectral information is transmitted to a computer in real time for storage, and the spectrum of the detected target substance is identified and quantitatively analyzed through a pre-built LIBS spectral database, a Raman spectral database, a quantitative analysis model of the heavy metal ions in the salt lake brine based on the LIBS spectrum and a Raman spectral quantitative analysis model, so that the species and abundance values of the cations and the anions of the detected target substance are obtained.
8. The detection method according to claim 7, wherein the pulsed laser is a high energy pulse to excite the sample to be detected into plasma when in the LIBS mode; when in Raman mode, the energy of the pulsed laser reaches the threshold of Raman excitation but is insufficient to excite the sample into a plasma.
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