CN107121425A - A kind of high sensitivity gas-liquid two-phase Raman spectroscopic detection apparatus and method - Google Patents
A kind of high sensitivity gas-liquid two-phase Raman spectroscopic detection apparatus and method Download PDFInfo
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- CN107121425A CN107121425A CN201710545684.7A CN201710545684A CN107121425A CN 107121425 A CN107121425 A CN 107121425A CN 201710545684 A CN201710545684 A CN 201710545684A CN 107121425 A CN107121425 A CN 107121425A
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- 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
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Abstract
The present invention is a kind of high sensitivity gas-liquid two-phase Raman spectroscopic detection apparatus and method.Including spectra collection and control module 1, Raman liquid detecting module 2, gas-liquid separation module 3 and Raman gas detecting module 4.The present invention using a set of raman spectroscopy measurement device can realize in seawater and seawater it is molten deposit gas while detect, especially for the bicarbonate radical in seawater, currently without a kind of technological means that in situ can directly detect, the present invention realizes the breakthrough of zero；Detection of gas is deposited for molten in water, by means of common spectrometer and detector, only needing increase small part annex to can be achieved, carbon dioxide, oxygen etc. are a variety of molten to be measured while deposit gas, this research for some ocean phenomena, such as research of " hypoxemia " phenomenon, various ingredients are measured simultaneously has special advantage.
Description
Technical field
Patent of the present invention is related to a kind of technology that Marine Chemistry component detection is carried out using laser spectrum means, specifically
It is a kind of Raman spectrum seawater component detection device and method.
Background technology
To the molten detection for depositing carbon dioxide and bicarbonate radical in seawater to the research inorganic carbon exchange of ocean-atmosphere interface and seawater
The research of middle carbon cycle is significant.There are some commercialized sensings for molten carbon dioxide detection in the market of depositing in seawater
Device, these commercialized sensors are based primarily upon infrared absorption principle.But for the live direct detection of bicarbonate radical in seawater,
Have no report at present.
Carbon dioxide and bicarbonate radical all have Raman active, in theory for can be realized to two using Raman spectroscopy
The direct detection of carbonoxide and bicarbonate radical, in the world many units have developed available for underwater in-situ measure Raman light pedigree
System, but sensitivity is limited to, all can not carbon dioxide and bicarbonate radical of the direct measurement into seawater.
The content of the invention
There is provided a kind of titanium dioxide that can simultaneously measure and be dissolved in seawater the need for the present invention is detected according to current Marine Chemistry
The device of carbon and bicarbonate radical, makes up the deficiencies in the prior art.
Multireflection technique can effectively improve Raman spectroscopic detection sensitivity, be used for Raman gas detection, and the present invention will
Multireflection technique be used for liquid direct detection, effectively increase the sensitivity of liquid direct detection so that bicarbonate radical it is straight
Detection is connect to be possibly realized.
High sensitivity gas-liquid two-phase Raman spectroscopic detection device of the present invention is main by spectra collection and control module, Raman liquid
Body detecting module, gas-liquid separation module and the part of Raman gas detecting module four composition.Seawater passes through Raman liquid detecting module
The acid ion signal in the seawater such as bicarbonate radical, sulfate radical can be obtained, it is molten in seawater afterwards after gas-liquid separation module
Gas is deposited into Raman gas detecting module, the gas component signal such as carbon dioxide, oxygen, nitrogen can be obtained, Raman liquid is visited
The raman spectral signal for surveying module and the acquisition of Raman gas detecting module enters spectra collection and control module progress light splitting spy
Survey.
Spectra collection is main by spectrometer 16, spectral detector 17, computer 18, liquid Raman detection mould with control module
Block laser control line 35, gas Raman detecting module laser control line 36, spectrometer control line 37 and vavuum pump control line
38 compositions, it is characterized in that spectrometer 16 and spectral detector 17 are the Raman signal and Raman liquid that Raman gas detecting module is obtained
The Raman signal that body detecting module is obtained is shared.
Raman liquid detecting module is by laser 5, half-wave plate 6, beam compressor 7, plane mirror 8, spherical reflector
9-1, spherical reflector 9-2 assisted collections spherical mirror 10, cemented doublet 11, high-pass filtering piece 12, cemented doublet 13, liquid
Sample cell 14 and optical fiber 15-1 compositions.It is characterized in that the sample in liquid sample pool 14 is usually seawater, liquid sample pool 14 is put
In the middle of the multiple reflections chamber being made up of spherical reflector 9-1 and spherical reflector 9-2, laser is by multiple reflections chamber in liquid
Sample cell center is focused on more than 10 times.
Above-mentioned liquid sample pool 14 be four-way quartz glass samples pond, upper and lower surface is stainless steel material, below feed liquor,
Liquid is discharged above.
Above-mentioned beam compressor 7 is respectively 100mm convex lens -50mm concavees lens group by diameter 25.4mm, focal length
Into.
Gas-liquid separation module is by peristaltic pump 29, Liquid valve 30, gas-liquid separation component 31, liquid emission valve door 32, gas
Pressure gauge 33 and vavuum pump 34 are constituted, it is characterized in that when flow velocity is 500mL/min, the gas of abjection can make 20ml cavity 10
Minute reaches balance.
Raman gas detecting module is anti-by laser 19, half-wave plate 20, beam compressor 21, plane mirror 22, sphere
Penetrate mirror 23-1, spherical reflector 23-2, assisted collection spherical mirror 24, cemented doublet 25, high-pass filtering piece 26, cemented doublet
27th, gas sample cell 28 and optical fiber 15-2 compositions.It is characterized in that during the sample in gas sample cell 28 is usually the seawater of abjection
The gas of dissolving, is nearly concentric cavity by spherical reflector 23-1 and spherical reflector 23-2 the multiple reflections chamber constituted, sphere is anti-
Mirror focal length is penetrated for 25mm, a diameter of 25.4mm, two minute surfaces are relative to be put, and spacing is that the angle between 101mm, two optical axises is
0.5°。
Above-mentioned gas sample cell 28 is four-way quartz glass samples pond, and quartz glass surfaces externally and internally is coated with 400~700nm
Wavelength anti-reflection film.
It is an advantage of the invention that can be realized using a set of raman spectroscopy measurement device gas is deposited to molten in seawater and seawater
Detected while body, especially for the bicarbonate radical in seawater, currently without a kind of technology hand that in situ can directly detect
Section, the present invention realizes the breakthrough of zero, detection of gas is deposited for molten in water, by means of common spectrometer and detector, it is only necessary to
Increase small part annex can be achieved carbon dioxide, oxygen etc. it is a variety of it is molten measure while deposit gas, this is for one
The research of the research, such as " hypoxemia " phenomenon of a little oceans phenomenon, various ingredients are measured simultaneously has special advantage.
Brief description of the drawings
Fig. 1 is high sensitivity gas-liquid two-phase Raman spectroscopic detection system global structure block diagram.
Fig. 2 is high sensitivity gas-liquid two-phase Raman spectroscopic detection system structure diagram.
In Fig. 1,1 is spectra collection and control module, and 2 be Raman liquid detecting module, and 3 be gas-liquid separation module, and 4 be drawing
Graceful detection of gas module.
In Fig. 2,5 be laser, and 6 be half-wave plate, and 7 be beam compressor, and 8 be plane mirror, and 9-1 and 9-2 are sphere
Speculum, 10 be assisted collection spherical mirror, and 11 is collect cemented doublet, and 12 be high-pass filtering piece, and 13 is double glued saturating for coupling
Mirror, 14 be liquid sample pool, and 15 be that Y types collect optical fiber, and 15-1 is liquid Raman collection optical fiber, and 15-2 is that gas Raman collects light
Fibre, 16 be spectrometer, and 17 be spectral detector, and 18 be computer, and 19 be laser, and 20 be half-wave plate, and 21 be beam compressor,
22 be plane mirror, and 23-1 and 23-2 are spherical reflector, 24 is assisted collection spherical mirror, 25 is cemented doublet, 26 is
High-pass filtering piece, 27 be cemented doublet, and 28 be gas sample cell, and 29 be peristaltic pump, and 30 be Liquid valve, and 31 be gas-liquid separation
Component, 32 be liquid emission valve door, and 33 be gas gauge, and 34 be vavuum pump, and 35 be liquid Raman detection module laser control
Line processed, 36 be gas Raman detecting module laser control line, and 37 be spectrometer control line, and 38 be vavuum pump control line.
Embodiment
The present invention for it is a kind of based on Raman spectroscopy to the molten Raman signal combined detection for depositing gas in liquid and liquid
System.The system includes spectra collection and control module 1, Raman liquid detecting module 2, gas-liquid separation module 3 and Raman gas
Detecting module 4, the present invention is first detected to the Raman spectrum of liquid, then carries out gas-liquid separation to the molten gas of depositing in liquid,
Then the gas of abjection is detected.Specific embodiment is as follows：
Raman liquid detecting module laser 5 is 532nm continuous wave lasers, and power 300mW, the laser of outgoing passes through half-wave plate 6
Laser is changed into s polarizations, laser beam spot sizes are compressed to less than 1mm by laser compressor reducer 7, beam compressor is by focal length
The concavees lens composition for being -50mm for 100mm convex lens and focal length, reflexes to multiple reflections chamber by speculum 8 by light beam afterwards
Interior, it by two panels focal length is 25mm that multiple reflections chamber 9, which is, and a diameter of 25.4mm speculum 9-1 and 9-2 are constituted, between two hysteroscopes
Be spaced about 99mm, angle is about 0.5 °.Liquid sample pool 14 is placed on chamber center, and laser is in intracavitary multiple reflections, in
Heart multi-focusing strengthens liquid Raman signal intensity, and the scattered signal of generation is collected by cemented doublet 11, high by 532nm
Pass filter piece 12 filters Rayleigh scattering signal, and Raman signal is coupled into optical fiber 15-1 by cemented doublet 13, imported into light
Spectrometer 16 is detected by spectral detector 17 again, and finally carrying out processing to spectrum on computer 18 shows.Raman gas is detected
Module is similar with Raman liquid detecting device structure, and careful parameter is slightly different, and such as gas sample cell window is coated with visible ray
Anti-reflection film, multiple reflections chamber spacing is also different, and gas multiple reflections chamber spacing is 101mm.
Liquid is pumped into fluid sample chamber 14 by the peristaltic pump 29 in gas-liquid separation module, by controlling Liquid valve 30
Aperture, carry out coutroi velocity size.The liquid flowed out by sample room is entered in gas-liquid separation component 31, and the gas of abjection enters
Into gas sample cell 28, remaining liquid is flowed out by liquid emission valve door 32.In probe gas concentration, pressure gauge 33
The pressure in gas sample cell 28 is detected, vavuum pump 34 is used for being vacuumized in sample cell.
Spectra collection mainly controls laser 5 and laser 19 including computer with control device by data wire 35 and 36
Switch；Signal detection and the collection of spectral detector 17 are controlled by data wire 37；Vacuum is controlled by data wire 38
The switch of pump 34 and its valve.
Gas-liquid two-phase Raman spectroscopic detection method of the present invention is as follows：
(1) peristaltic pump 29 and liquid line valve are opened, liquid is extracted；Open laser 5 and laser 19, spectrometer 16, light
Compose detector 17 and carry out Raman detection；
(2) gas sample chamber is evacuated to less than 5kPa with vavuum pump 34, closes vavuum pump 34, opening is connected with gas-liquid separation module
Gas piping；
(3) Raman liquid detecting module starts to detect fluid sample (being usually seawater sample), and the 30s times of integration obtain
One spectrum, continuous probe；
(4) after gas-liquid separation device works 5 minutes, Raman gas detecting module starts to detect the molten gas of depositing of abjection,
The 30s times of integration obtain a spectrum, close gas sample cell 28 and gas-liquid separation device connecting line, open vavuum pump 34,
Repeat step (2), circulation measurement；
(5) spectrographic detection data are read, into computer 18, raman spectral signal pretreatment are carried out, including baseline is removed, put down
Sliding, removal abnormity point etc.；
(6) liquid Raman signal is handled, chooses 850~1200cm-1Scope raman spectral signal, to sulfate radical Raman
Signal carries out peak-seeking, and Voigt fittings are carried out to sulfate radical signal, after the signal for subtracting sulfate radical fitting, then bicarbonate radical is entered
Row Gaussian is fitted, and obtains the concentration of bicarbonate radical；
(7) gas Raman signal is handled, peak-seeking is carried out to carbon dioxide, oxygen, nitrogen signal, Gauss plan is carried out afterwards
Close, concentration is obtained according to areal intensity.
The present invention can detect the molten Raman signal for depositing gas in liquid and liquid simultaneously, be provided for Marine Chemistry detection
A kind of detection means for obtaining more comprehensive information.
Claims (10)
1. a kind of high sensitivity gas-liquid two-phase Raman spectroscopic detection device, including spectra collection are visited with control module 1, Raman liquid
Survey module 2, gas-liquid separation module 3 and Raman gas detecting module 4.
2. it is characterized in that lead between Raman liquid detecting module 2 and Raman gas detecting module 4 and spectra collection and control module 1
Cross optical fiber and control line connection；Connected between Raman liquid detecting module 2 and gas-liquid separation module 3 by liquid line, gas-liquid
Connected between separation module 3 and Raman gas detecting module 4 by gas piping.
3. spectra collection according to claim 1 is with control module 1 by spectrometer 16, spectral detector 17 and computer 18
Composition, it is characterized in that spectrometer 16 and spectral detector 17 are the Raman signal and Raman gas that Raman liquid detecting module 2 is obtained
The Raman signal that body detecting module 4 is obtained is shared.
4. Raman liquid detecting module 2 according to claim 1 is by laser 5, half-wave plate 6, beam compressor 7, plane
Speculum 8, spherical reflector 9-1, spherical reflector 9-2 assisted collections spherical mirror 10, cemented doublet 11, high-pass filtering piece
12nd, cemented doublet 13, liquid sample pool 14 and optical fiber 15-1 compositions.
5. it is characterized in that sample in liquid sample pool 14 is liquid, usually seawater, liquid sample pool 14 is the quartzy glass of four-way
Glass sample cell, upper and lower surface is stainless steel material, below feed liquor, liquid is discharged above, is placed in by spherical reflector 9-1 and sphere
In the middle of the multiple reflections chamber of speculum 9-2 compositions, the laser that laser 5 is sent is by multiple reflections chamber at liquid sample pool center
Place is focused on more than 10 times.
6. gas-liquid separation module 3 according to claim 1 by peristaltic pump 29, Liquid valve 30, gas-liquid separation component 31, go out
Liquid mouthful 32, gas gauge 33 and vavuum pump 34 are constituted, it is characterized in that when the flow velocity of peristaltic pump 29 is 500mL/min, gas-liquid point
The gas deviate from from component can make 20ml cavity reach balance less than 10 minutes.
7. Raman gas detecting module according to claim 1 is by laser 19, half-wave plate 20, beam compressor 21, flat
Face speculum 22, spherical reflector 23-1, spherical reflector 23-2 assisted collections spherical mirror 24, cemented doublet 25, high pass filter
Wave plate 26, cemented doublet 27, gas sample cell 28 and optical fiber 15-2 compositions.
8. it is characterized in that the sample in gas sample cell 28 is usually the gas dissolved in the seawater of abjection, gas sample cell 28 is
Four-way quartz glass samples pond, quartz glass surfaces externally and internally is coated with 400~700nm wavelength anti-reflection films.
9. being nearly concentric cavity by spherical reflector 23-1 and spherical reflector 23-2 the multiple reflections chamber constituted, spherical reflector is burnt
Puts away from for 25mm, a diameter of 25.4mm, two minute surfaces are relative, spacing is that the angle between 101mm, two optical axises is 0.5 °.
10. a kind of gas-liquid two-phase Raman spectroscopic detection method, it is characterised in that it comprises the following steps：
Peristaltic pump 29 and liquid line valve are opened, liquid is extracted；Open laser 5 and laser 19, spectrometer 16, spectrum are visited
Survey device 17 and carry out Raman detection；Gas sample chamber is evacuated to less than 5kPa with vavuum pump 34, vavuum pump 34 is closed, opened and gas-liquid
Separation module connects gas piping；Raman liquid detecting module starts to detect fluid sample (being usually seawater sample),
The 30s times of integration obtain a spectrum, continuous probe；After gas-liquid separation device works 5 minutes, Raman gas detecting module starts
The molten gas of depositing of abjection is detected, the 30s times of integration obtain a spectrum, close gas sample cell 28 and filled with gas-liquid separation
Connecting line is put, vavuum pump 34 is opened, step (2), circulation measurement is repeated；Spectrographic detection data are read, into computer 18,
Carry out raman spectral signal pretreatment, including baseline removal, smooth, removal abnormity point etc.；Liquid Raman signal is handled,
Choose 850~1200cm-1Scope raman spectral signal, peak-seeking is carried out to sulfate radical Raman signal, and sulfate radical signal is carried out
Voigt is fitted, after the signal for subtracting sulfate radical fitting, then carries out Gaussian fittings to bicarbonate radical, obtains bicarbonate radical
Concentration；Gas Raman signal is handled, peak-seeking is carried out to carbon dioxide, oxygen, nitrogen signal, Gauss plan is carried out afterwards
Close, concentration is obtained according to areal intensity.
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| CN113218930A (en) * | 2021-03-31 | 2021-08-06 | 中国船舶重工集团公司第七一八研究所 | Raman spectrum enhancement device and gas analysis system |
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| CN107843581A (en) * | 2017-10-20 | 2018-03-27 | 国家电网公司 | Raman spectrum based on Voigt peak type fitting algorithms quantitatively detects SF6Feature decomposition gas SO2The method of content |
| CN107831159A (en) * | 2017-12-13 | 2018-03-23 | 中国科学院上海应用物理研究所 | The detection means of metallic element in a kind of aerosol |
| CN108507974A (en) * | 2018-03-22 | 2018-09-07 | 中国科学院合肥物质科学研究院 | Extra large gas dissolved water laser spectrum on-line measuring device |
| CN109030366A (en) * | 2018-08-23 | 2018-12-18 | 中国科学院海洋研究所 | A kind of raman response cabin |
| CN109655445A (en) * | 2019-01-22 | 2019-04-19 | 重庆大学 | A kind of multistage circle multi-pass gas chamber improving gas Raman detection sensitivity |
| CN109655445B (en) * | 2019-01-22 | 2021-08-24 | 重庆大学 | Multi-section circular multi-pass air chamber for improving gas Raman detection sensitivity |
| CN109799204B (en) * | 2019-01-26 | 2020-08-21 | 上海交通大学 | Low concentration COD measuring device based on spectrum method |
| CN109799204A (en) * | 2019-01-26 | 2019-05-24 | 上海交通大学 | A kind of low strength COD measuring device based on spectroscopic methodology |
| CN110530848A (en) * | 2019-09-27 | 2019-12-03 | 国网重庆市电力公司电力科学研究院 | A kind of detection device and detection method |
| CN110987900A (en) * | 2019-12-12 | 2020-04-10 | 蒋霖坤 | High-sensitivity Raman spectrometer based on photomultiplier |
| WO2022212344A1 (en) * | 2021-03-29 | 2022-10-06 | Schlumberger Technology Corporation | Processes and systems for monitoring one or more gases dissolved in a liquid |
| CN113218930A (en) * | 2021-03-31 | 2021-08-06 | 中国船舶重工集团公司第七一八研究所 | Raman spectrum enhancement device and gas analysis system |
| CN113295669A (en) * | 2021-05-14 | 2021-08-24 | 重庆大学 | Folded multi-cavity for enhancing gas Raman signal |
| CN113295669B (en) * | 2021-05-14 | 2023-10-24 | 重庆大学 | Folding type multi-reflecting cavity for enhancing gas Raman signal |
| WO2023027774A1 (en) * | 2021-08-24 | 2023-03-02 | Horiba Instruments Incorporated | A system and method for detecting contaminants in a sample fluid |
| CN114264642A (en) * | 2021-11-23 | 2022-04-01 | 中国船舶重工集团公司第七一八研究所 | Gas Raman signal enhancement device and method in multiple reflection and pressurization mode |
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