CN209911230U - Laser Raman analysis device - Google Patents
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- CN209911230U CN209911230U CN201822068047.8U CN201822068047U CN209911230U CN 209911230 U CN209911230 U CN 209911230U CN 201822068047 U CN201822068047 U CN 201822068047U CN 209911230 U CN209911230 U CN 209911230U
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Abstract
The utility model discloses a laser Raman analysis device. The device comprises a laser emitting device, a spectrum collecting device, an optical device and a sample cell, wherein the optical device is arranged in the sample cell, a laser output end of the laser emitting device is arranged opposite to the optical device in the sample cell, and the spectrum collecting device is arranged on the sample cell; the laser emission device is used for emitting laser signals into the sample cell, and the sample cell comprises a gas sample to be detected; the optical device is used for reflecting the laser signal back and forth for multiple times in the sample cell, wherein the laser signal and the gas sample to be detected generate Raman scattering during transmission in the sample cell to obtain a spectrum signal; the spectrum acquisition device is used for acquiring the spectrum signals in the sample pool. The application can improve the detection sensitivity.
Description
Technical Field
The utility model relates to a gas analysis technical field, in particular to laser raman analysis device.
Background
When a hydrocarbon substance is irradiated with laser light, the substance generates scattered light, in which, in addition to rayleigh light having the same frequency as that of the incident light, a series of lights having other frequencies are present on both sides of the rayleigh light, and the intensity thereof is generally only minus six to minus nine of ten times of the rayleigh light, and this scattered light is named raman light.
Although the frequency of the raman line varies with the frequency of incident light, the difference between the frequency of raman light and the frequency of rayleigh scattered light does not vary with the frequency of incident light, but is related to the vibrational rotation energy level of the sample molecules. The intensity of the raman line is in direct proportion to the intensity of the incident light and the concentration of the sample molecules, and quantitative analysis can be performed by using the raman line.
In the aspect of gas analysis, a raman analyzer is generally required for analysis, and in the existing raman analyzer, due to the fact that the density of gas molecules is small and the raman scattering is weak, the signal intensity of the raman scattering is weak, the detection sensitivity is low, and particularly, accurate determination cannot be performed on trace gas contained in a sample gas to be detected.
SUMMERY OF THE UTILITY MODEL
In order to improve the detection sensitivity, the application provides a laser Raman analysis device, and the technical scheme is as follows.
The application provides a laser raman analysis device, includes:
the device comprises a laser emitting device, a spectrum collecting device, an optical device and a sample cell, wherein the optical device is arranged in the sample cell, a laser output end of the laser emitting device is arranged opposite to the optical device in the sample cell, and the spectrum collecting device is arranged on the sample cell;
the laser emission device is used for emitting laser signals into the sample cell, and the sample cell comprises a gas sample to be detected;
the optical device is used for reflecting the laser signal back and forth for multiple times in the sample cell, wherein the laser signal and the gas sample to be detected generate Raman scattering during transmission in the sample cell to obtain a spectrum signal;
the spectrum acquisition device is used for acquiring the spectrum signals in the sample pool.
Optionally, the optical device includes a half mirror and a mirror coaxially arranged, the half mirror and the mirror are oppositely disposed in the sample cell, a transmission surface of the half mirror faces a laser output end of the laser emitting device, and a reflection surface of the half mirror faces the mirror;
the laser signal emitted by the laser emitting device penetrates through the transmission surface of the semi-transparent semi-reflective mirror and is emitted to the reflecting mirror, and the laser signal is reflected back and forth for multiple times between the reflection surface of the semi-transparent semi-reflective mirror and the reflecting mirror.
Optionally, the optical device further includes a convex lens, the convex lens is located between the half mirror and the reflector, and the half mirror, the convex lens and the reflector are coaxial;
the convex lens is used for focusing the laser signal from the semi-transparent and semi-reflective mirror and emitting the laser signal to the reflecting mirror, and focusing the laser signal from the reflecting mirror and emitting the laser signal to the semi-transparent and semi-reflective mirror.
Optionally, the spectrum collecting device includes a fiber spectrometer and a raman probe, the raman probe is mounted at an input end of the fiber spectrometer, and the raman probe extends into the sample cell and is located between the half-mirror and the reflector;
the Raman probe is used for collecting the spectrum signal and sending the spectrum signal to the fiber spectrometer.
Optionally, the raman probe is connected to the input end of the fiber optic spectrometer by a collection fiber.
Optionally, the laser emitting device includes a laser and an excitation fiber, an output end of the laser is connected to one end of the excitation fiber, and the other end of the excitation fiber is opposite to the optical device.
Optionally, one end of the sample cell is provided with an air inlet, and the other end of the sample cell is provided with an air outlet.
Optionally, the sample cell is a sampling tube.
Optionally, the pressure borne by the sample cell is greater than or equal to 6 Mpa.
In the application, because the optical device is arranged in the sample cell, the optical device reflects the laser signal back and forth in the sample cell for multiple times, wherein the laser signal generates Raman scattering with the gas sample to be detected during the transmission of the sample cell to obtain a spectrum signal, and the back and forth reflection of the laser signal causes the optical path to be lengthened, so that the time for the laser signal to generate Raman scattering with the gas sample to be detected is prolonged, and more spectrum signals are obtained, thereby the spectrum signal can be detected more easily, the detection sensitivity is improved, and further the trace gas can be detected accurately. In addition, adopt above-mentioned further scheme's beneficial effect to make half mirror, convex lens, speculum unsettled, can hold sample circulation of air and sweep the sampling pipe by sample gas simultaneously, especially the optical lens of installation in the sampling pipe can prevent the carbon deposit, can also balance the interior pressurized of sampling pipe, protection lens, easily use and wash.
Drawings
Fig. 1 is a schematic structural diagram of a laser raman analysis apparatus provided in the present application;
FIG. 2 is a schematic structural diagram of another laser Raman analysis apparatus provided herein;
fig. 3 is a flow chart of a laser raman analysis provided herein.
Detailed Description
The principles and features of the present invention are described below in conjunction with the following drawings, the examples given are only intended to illustrate the present invention and are not intended to limit the scope of the present invention.
Referring to fig. 1, an embodiment of the present application provides a laser raman analysis apparatus, including:
the device comprises a laser emitting device 1, a spectrum collecting device 2, an optical device 3 and a sample cell 4, wherein the optical device 3 is arranged in the sample cell 4, a laser output end of the laser emitting device 1 is arranged opposite to the optical device 3 in the sample cell 4, and the spectrum collecting device 2 is arranged on the sample cell 4;
the laser emitting device 1 is used for emitting laser signals into the sample cell 4, and the sample cell 4 comprises a gas sample to be detected;
the optical device 3 is used for reflecting the laser signal back and forth for multiple times in the sample cell 4, wherein the laser signal is subjected to Raman scattering with the gas sample to be detected when being transmitted in the sample cell 4 to obtain a spectrum signal;
and the spectrum acquisition device 2 is used for acquiring the spectrum signals in the sample cell 4.
Alternatively, referring to fig. 2, the optical device 3 includes a half mirror 31 and a reflecting mirror 32 coaxially arranged, the half mirror 31 and the reflecting mirror 32 are oppositely disposed in the sample cell 4, a transmission surface of the half mirror 31 faces the laser output end of the laser emitting device 1, and a reflection surface of the half mirror 31 faces the reflecting mirror 32;
the laser signal emitted from the laser emitting device 1 passes through the transmission surface of the half mirror 31 and is emitted to the reflecting mirror 32, and the laser signal is reflected back and forth between the reflection surface of the half mirror 31 and the reflecting mirror 32 for a plurality of times.
Optionally, the optical device further includes a convex lens 33, the convex lens 33 is located between the half mirror 31 and the reflector 32, and the half mirror 31, the convex lens 33 and the reflector 32 are coaxial;
the convex lens 33 focuses the laser light signal from the half mirror 31 and emits the focused laser light signal to the mirror 32, and focuses the laser light signal from the mirror 32 and emits the focused laser light signal to the half mirror 31.
The output end of the laser emitting device 1 is arranged opposite to the transmission surface of the half mirror 31, and a laser signal emitted by the laser emitting device 1 passes through the transmission surface of the half mirror 31 and is emitted to the convex lens 33; the convex lens 33 focuses the laser signal to form a laser signal, the laser signal is emitted to the reflector 32, the reflector 32 reflects the laser signal to the convex lens 33, the convex lens 33 focuses the laser signal to form a laser signal, the laser signal is emitted to the semi-transmitting and semi-reflecting mirror 31, the semi-transmitting and semi-reflecting mirror 31 reflects the laser signal to the convex lens 33, and therefore the laser signal is reflected back and forth.
When the laser signal is reflected back and forth in the sample cell 4, the laser signal and a gas sample to be detected in the sample cell 4 generate Raman scattering to obtain a spectrum signal, and the spectrum acquisition device is positioned between the semi-transparent semi-reflective mirror 31 and the reflective mirror 32, so that the spectrum signal can be acquired.
Optionally, the sample cell 4 includes three hollow-out mounting frames, the half-mirror 31 is mounted on one hollow-out mounting frame, the mirror 32 is mounted on the other hollow-out mounting frame, and the convex lens 33 is mounted on the remaining hollow-out mounting frame.
Optionally, referring to fig. 1, the spectrum collecting device 2 includes a fiber spectrometer 21 and a raman probe 22, the raman probe 22 is installed at an input end of the fiber spectrometer 21, and the raman probe 22 extends into the sample cell 4 and is located between the half mirror 31 and the reflecting mirror 32;
and a raman probe 22 for collecting the spectral signal and transmitting the spectral signal to the fiber spectrometer 21.
Optionally, the raman probe 22 is connected to the input end of the fiber optic spectrometer 21 by a collection fiber 23.
Optionally, referring to fig. 1, the laser emitting device 1 includes a laser 11 and an excitation fiber 12, an output end of the laser 11 is connected to one end of the excitation fiber 12, and the other end of the excitation fiber 12 is disposed opposite to the optical device 3.
Alternatively, the other end of the excitation fiber 12 is disposed opposite to the transmission surface of the half mirror 31. The laser 11 generates a laser signal, and transmits the laser signal to the half mirror 31 through the excitation fiber 12.
Optionally, one end of the sample cell 4 is provided with an air inlet 41, and the other end is provided with an air outlet 42.
Optionally, the sample cell 4 is a sampling tube.
Optionally, the sample cell 4 is subjected to a pressure greater than or equal to 6 Mpa.
Optionally, the sample cell 4 may be a high-pressure sample cell, and can normally work under a pressure of 6.0Mpa, so that a gas sample to be detected can be pressurized to 6.0Mpa, and the high pressure of the gas sample makes raman scattering optical signals stronger, and improves detection sensitivity; the laser emitting device adopts a high-power laser with the power of more than three watts.
The laser raman analysis device is described in detail above in connection with fig. 1 and 2, and the method of using the device is described in detail below, with reference to fig. 3, including the following steps;
step 201: and introducing a gas sample to be detected into the sample cell 4.
Step 202: the laser emitting device 1 emits a laser signal into the sample cell 4.
Step 203: the optical device 3 which is mounted in the sample cell 4 in a suspended manner reflects the laser signal in the sample cell 4 back and forth for multiple times, and the laser signal is reflected for multiple times and simultaneously generates Raman scattering with the gas sample to be detected to obtain a spectrum signal.
The optical device 3 includes a half mirror 31, a convex lens 33, and a reflecting mirror 32; the step may specifically be:
s31, the half mirror 31 is used to receive the laser signal emitted by the laser emitting device 1, and the received laser signal is transmitted to the convex lens 33.
S32, the convex lens 33 is used to focus the received laser signal.
S33, the focused laser signal is reflected by the mirror 32.
S34, the laser signal in the sample cell is reflected by the half mirror 31.
Step 204: the spectrum signal in the sample cell 4 is collected using the spectrum collecting device 2.
In this step, a spectrum signal between the convex lens 33 and the reflecting mirror 32 in the sample cell 4 is collected using the spectrum collection device 2.
As can be seen from the above method, in this apparatus, the components that play an important role are the sample cell 4 and the optics 3 within the sample cell 4. Hereinafter, it will be described in detail.
In step S31, the laser beam is incident into the sample cell 4 by the transmission action of the half mirror 31, the optional half mirror 31 transmits and reflects half of the incident light, and half of the laser beam emitted from the laser emitting device 1 can enter the sample cell 4.
In step S32, the convex lens 33 receives the incoming laser signal, and focuses all the laser signals contacting the convex lens 33 at the same point and perpendicularly toward the mirror 32, ensuring that the laser signals are concentrated.
In step S33, since the laser beam is incident vertically, the reflecting mirror 32 reflects the laser beam focused by the convex lens 33 along the original path due to the reflection characteristic of the reflecting mirror 32, and the reflected laser beam is concentrated to minimize the loss, and then is reflected back again to the half mirror 31 through the convex lens 33.
In step S34, the half mirror 31 reflects the reflected laser signal, one half of which is transmitted to the outside and leaves the cuvette 4, and the other half is reflected again into the cuvette 4. Thus, although the laser signal is weakened by half, the remaining half can be repeated again in steps S32, S33, and S34, and by the time step S34 is reached for the second time, the portion of the laser signal that can be reflected into the sample cell 4 is half of the first time. Similarly, although the laser signal is attenuated, the steps S32, S33 and S34 … … can be repeated continuously and repeatedly, theoretically, infinite back-and-forth reflections can be achieved, the optical path of the laser signal is increased infinitely, and the sensitivity of laser raman measurement is improved. In practice, there is a depletion of the laser signal in the back and forth reflections, eventually stopping after a finite number of reflections. Here, the degree of improvement in sensitivity and the effect thereof in gas component analysis will be described below, taking coal bed gas as an example.
When the gas sample to be detected is coal bed gas, the components mainly comprise 98% of methane, 1.4% of nitrogen, 0.49% of ethane and 0.01% of propane. The content of propane is very little, only 0.01%, the measuring result of the common laser Raman analysis system for propane fluctuates between (0-0.05), the reliability of the measuring result is poor, the sensitivity is improved by at least five times after the optical path is increased, and the accurate measurement of propane can be completely achieved. Thus, this problem can be solved by the present method, allowing accurate determination of all components.
Next, the degree of sensitivity improvement and the effect thereof in gas component analysis will be described by taking natural gas as an example.
When the gas sample to be detected is natural gas, the components mainly comprise 95% of methane, 0.9% of nitrogen, 3.05% of ethane, 1.02% of propane, 0.02% of n-butane, 0.01% of isobutane and 15ppm of hydrogen sulfide. It can be seen that the composition generally contains trace amounts of n-butane, isobutane and hydrogen sulfide, but due to the very small content, the presence of the compounds cannot be detected or accurately measured by a raman analysis device of a common institution. The method can detect normal butane, isobutane and hydrogen sulfide and ensure certain accuracy.
Optionally, in the above apparatus, the optical device 3 is mounted in the sample cell 4 in a suspended manner; the laser emitting end of the laser emitting device 1 is disposed opposite to one surface of the half mirror 31, and the other surface of the half mirror 31 is opposite to the first convex surface of the convex lens 33. The half mirror 31 allows light to be divided into two parts, one part of which directly transmits through the half mirror 31 and the other part of which reflects when in contact with the half mirror 31, so that the light passing therethrough can be reflected and transmitted simultaneously.
The other convex surface of the convex lens 33 is arranged opposite to the mirror 32;
specifically, the centers of the half mirror 31, the convex lens 33 and the reflecting mirror 32 are collinear, and it is ensured that all the laser light reflected or transmitted by the half mirror 31 into the sampling tube 4 can be emitted to the convex lens 33, and meanwhile, the laser signal focused by the convex lens 33 can be emitted to the reflecting mirror 32 exactly vertically, so that the reflecting mirror 32 can reflect the laser signal focused by the convex lens 33 back to the convex lens 33 along the original path. Therefore, laser signals can be reflected back and forth for an infinite number of times in the sample cell 4, the optical path of the laser is infinitely increased, and the sensitivity of laser Raman measurement is improved.
The sample cell 4 is provided with an air inlet 41 and an air outlet 12, the air inlet 41 is arranged at one end of the sample cell 4 close to the reflector 32, and the air outlet 42 is arranged at one end of the sample cell 4 close to the half-mirror 31;
the sample cell 4 is a sampling tube capable of resisting pressure of 6 Mpa. Specifically, the sampling tube which can withstand pressure and is larger than or equal to 6Mpa is adopted in the sample pool 4, so that high-pressure sample gas can be borne, and the detection sensitivity can be improved through the high pressure of the sample gas.
The sampling tube is internally and fixedly provided with three hollowed-out installation frames, the three installation frames are respectively provided with a clamping groove, and the outer edges of the semi-transparent and semi-reflective mirror 31, the convex lens 33 and the reflector 32 are respectively arranged in one clamping groove.
Specifically, the mounting frame is used to fix the half mirror 31, the convex lens 33 and the reflecting mirror 31, and suspend the optical devices 3 in the sample cell 3 to ensure that the light can freely propagate between the optical devices.
Specifically, the installation frame is hollow out construction, makes the sample gas can flow to gas outlet 42 from air inlet 41, and the sample gas circulation is covered in order to guarantee that laser and sample gas contact in sample cell 3, takes place raman scattering to detect raman signal through raman probe 22. The pressure balance in the sample cell 3 is ensured, and the safety degree can be ensured even if the sample cell works under high pressure, so that the purging is convenient.
Therefore, the optical device is arranged in the high-pressure sample tank in a hollow mode, the pressure of the high-pressure sample on two sides of the optical mirror surface is balanced, high-pressure purging is achieved to prevent carbon deposition, normal work under high pressure is guaranteed, high-pressure and high-power lasers act simultaneously, Raman gas analysis signals are enhanced, the high-intensity lasers can be reflected back and forth for a plurality of times after entering the high-pressure sample tank through the arrangement of the optical device, the optical path is increased, Raman detection sensitivity is further improved, and accurate determination of trace components in gas can be achieved.
When the Raman signal detection device works, a gas sample to be detected is introduced into the sample cell 3 from the gas inlet 41, the whole sample cell 3 is filled through the hollow part on the mounting frame, and finally flows out of the gas outlet 42, the air pressure in the sample cell 3 is kept balanced, meanwhile, laser emitted by the high-power laser 11 is emitted into the sample cell 3 through the semi-transmitting and semi-reflecting mirror 31, is focused through the convex lens 33 and then vertically emitted into the reflecting mirror 32, the reflecting mirror 32 reflects the laser along the original light path, the laser returns to the semi-transmitting and semi-reflecting mirror 31 through the convex lens 33 again, at the moment, the semi-transmitting and semi-reflecting mirror 31 reflects the laser again, the laser is condensed by the convex lens 33 and then vertically reflected by the reflecting mirror 32, the reflecting mirror 32 reflects the laser along the original light path again, … …, the operations are repeated, theoretically, the laser can be reflected for countless times, the light path is expanded by times, so that the Raman, can accurately measure trace components in the gas, and the result of an analysis experiment is more accurate.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included within the protection scope of the present invention.
Claims (9)
1. A laser Raman analysis apparatus, comprising:
the device comprises a laser emitting device, a spectrum collecting device, an optical device and a sample cell, wherein the optical device is arranged in the sample cell, a laser output end of the laser emitting device is arranged opposite to the optical device in the sample cell, and the spectrum collecting device is arranged on the sample cell;
the laser emission device is used for emitting laser signals into the sample cell, and the sample cell comprises a gas sample to be detected;
the optical device is used for reflecting the laser signal back and forth for multiple times in the sample cell, wherein the laser signal and the gas sample to be detected generate Raman scattering during transmission in the sample cell to obtain a spectrum signal;
the spectrum acquisition device is used for acquiring the spectrum signals in the sample pool.
2. The device according to claim 1, wherein the optical device comprises a semi-transparent and semi-reflective mirror and a reflective mirror which are coaxially arranged, the semi-transparent and semi-reflective mirror and the reflective mirror are oppositely arranged in the sample cell, the transmission surface of the semi-transparent and semi-reflective mirror faces to the laser output end of the laser emission device, and the reflective surface of the semi-transparent and semi-reflective mirror faces to the reflective mirror;
the laser signal emitted by the laser emitting device penetrates through the transmission surface of the semi-transparent semi-reflective mirror and is emitted to the reflecting mirror, and the laser signal is reflected back and forth for multiple times between the reflection surface of the semi-transparent semi-reflective mirror and the reflecting mirror.
3. The apparatus of claim 2, wherein the optical device further comprises a convex lens, the convex lens is located between the half mirror and the reflector, and the half mirror, the convex lens and the reflector are coaxial;
the convex lens is used for focusing the laser signal from the semi-transparent and semi-reflective mirror and emitting the laser signal to the reflecting mirror, and focusing the laser signal from the reflecting mirror and emitting the laser signal to the semi-transparent and semi-reflective mirror.
4. The device as claimed in claim 2 or 3, wherein the spectrum collecting device comprises a fiber optic spectrometer and a Raman probe, the Raman probe is mounted at the input end of the fiber optic spectrometer, and the Raman probe extends into the sample cell and is positioned between the half-mirror and the reflecting mirror;
the Raman probe is used for collecting the spectrum signal and sending the spectrum signal to the fiber spectrometer.
5. The apparatus of claim 4, wherein the Raman probe is coupled to the input of the fiber optic spectrometer by a collection fiber.
6. The device according to any one of claims 1 to 3, wherein the laser emitting device comprises a laser and an excitation fiber, an output end of the laser is connected with one end of the excitation fiber, and the other end of the excitation fiber is arranged opposite to the optical device.
7. The device according to any one of claims 1 to 3, wherein the sample cell is provided with an air inlet at one end and an air outlet at the other end.
8. The device of claim 7, wherein the sample cell is a sampling tube.
9. The apparatus of claim 7, wherein the sample cell is subjected to a pressure greater than or equal to 6 Mpa.
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| CN201822068047.8U CN209911230U (en) | 2018-12-10 | 2018-12-10 | Laser Raman analysis device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111426677A (en) * | 2020-04-29 | 2020-07-17 | 中国工程物理研究院核物理与化学研究所 | Raman spectrum multi-site excitation structure and gas analysis method |
| CN111504963A (en) * | 2020-04-10 | 2020-08-07 | 上海蓝长自动化科技有限公司 | Data space-time fusion method applied to chlorophyll and blue-green algae fluorescence detection |
| 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 |
| CN117288740A (en) * | 2023-11-27 | 2023-12-26 | 四方光电股份有限公司 | Raman probe-based battery charge-discharge gas production in-situ test device and test method |
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2018
- 2018-12-10 CN CN201822068047.8U patent/CN209911230U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111504963A (en) * | 2020-04-10 | 2020-08-07 | 上海蓝长自动化科技有限公司 | Data space-time fusion method applied to chlorophyll and blue-green algae fluorescence detection |
| CN111426677A (en) * | 2020-04-29 | 2020-07-17 | 中国工程物理研究院核物理与化学研究所 | Raman spectrum multi-site excitation structure and gas analysis method |
| CN111426677B (en) * | 2020-04-29 | 2023-09-19 | 中国工程物理研究院核物理与化学研究所 | Raman spectrum multi-site excitation structure and gas analysis method |
| 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 |
| CN117288740A (en) * | 2023-11-27 | 2023-12-26 | 四方光电股份有限公司 | Raman probe-based battery charge-discharge gas production in-situ test device and test method |
| CN117288740B (en) * | 2023-11-27 | 2024-03-19 | 四方光电股份有限公司 | Raman probe-based battery charge-discharge gas production in-situ test device and test method |
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