WO2023015605A1 - Laser detection apparatus, organic carbon and elemental carbon analyzer, and laser detection method - Google Patents

Laser detection apparatus, organic carbon and elemental carbon analyzer, and laser detection method Download PDF

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Publication number
WO2023015605A1
WO2023015605A1 PCT/CN2021/114127 CN2021114127W WO2023015605A1 WO 2023015605 A1 WO2023015605 A1 WO 2023015605A1 CN 2021114127 W CN2021114127 W CN 2021114127W WO 2023015605 A1 WO2023015605 A1 WO 2023015605A1
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laser
filter membrane
laser light
reflected
light
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PCT/CN2021/114127
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French (fr)
Chinese (zh)
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刘海东
周旭
彭文姣
郭艳
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力合科技(湖南)股份有限公司
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Publication of WO2023015605A1 publication Critical patent/WO2023015605A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47Scattering, i.e. diffuse reflection
    • G01N21/4738Diffuse reflection, e.g. also for testing fluids, fibrous materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47Scattering, i.e. diffuse reflection
    • G01N21/4738Diffuse reflection, e.g. also for testing fluids, fibrous materials
    • G01N21/474Details of optical heads therefor, e.g. using optical fibres
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47Scattering, i.e. diffuse reflection
    • G01N21/4738Diffuse reflection, e.g. also for testing fluids, fibrous materials
    • G01N2021/4764Special kinds of physical applications

Definitions

  • the invention relates to the technical field of air quality detection, in particular to a laser detection device, an organic carbon carbon analyzer using the laser detection device and a laser detection method.
  • the measurement methods of organic carbon and elemental carbon in air particulate matter include thermal method, optical method and thermo-optical method.
  • the thermal method mainly distinguishes organic carbon and elemental carbon according to their different thermal properties.
  • organic carbon will be partially cracked and carbonized, and a substance with thermal and optical properties similar to elemental carbon will be formed, resulting in high elemental carbon measured.
  • the optical method can only be used to measure elemental carbon.
  • thermo-optical method the most widely used and recognized mature organic carbon and elemental carbon analysis method is the thermo-optical method. Its working principle is to collect particulate matter in the air through filter membrane filtration, and then pass through an oxygen-free carrier gas to make the filter membrane in an oxygen-free environment. At this time, the temperature of the filter membrane is raised step by step, so that the organic carbon on the surface of the filter membrane (and a part of it is carbonized to form cracked carbon) is pyrolyzed and escapes into the oxidation furnace to be oxidized and converted into carbon dioxide, and then the aerobic load is introduced into the desorption furnace.
  • the air makes the filter membrane in an aerobic environment, and continues to raise the temperature of the filter membrane step by step, so that the elemental carbon in the filter membrane is pyrolyzed and escapes into the oxidation furnace to be oxidized and converted into carbon dioxide, so that the carbon dioxide concentration output by the oxidation furnace is detected by a carbon dioxide detector.
  • there is a laser beam hitting the filter membrane, and its transmitted light (or reflected light) will be weakened when the organic carbon is carbonized.
  • the oxygen-free carrier gas is switched to an oxygen carrier gas, and the temperature rises, the elemental carbon will be oxidized and decomposed, and the light intensity of the transmitted light (or reflected light) of the laser beam will gradually increase.
  • Thermo-optic method is an integrated optical method to correct the cracked carbon generated during the analysis of organic carbon at elevated temperature.
  • the invention provides a laser detection device, an organic carbon elemental carbon analyzer and a laser detection method to solve the technical problem that the separation point of organic carbon/elemental carbon cannot be accurately determined.
  • a laser detection device including a laser emitter, a first laser detector and a second laser detector, the laser emitter is used to emit laser light toward the filter membrane, and the first laser detector , the second laser detector is respectively used to receive the transmitted laser light passing through the filter membrane and the reflected laser light reflected by the filter membrane, and the laser emitter includes a first laser emitter arranged on the back side of the filter membrane Part of the laser light emitted by the first laser transmitter toward the filter membrane passes through the filter membrane to form a first transmitted laser light, and part of it is reflected by the filter membrane to form a first reflected laser light.
  • the detector is arranged on the front side of the filter membrane and used to receive the first transmitted laser light
  • the second laser detector is arranged on the back side of the filter membrane and used to receive the first reflected laser light.
  • the laser emitter further includes a second laser emitter disposed on the front side of the filter membrane, and part of the laser light emitted by the second laser emitter towards the filter membrane passes through the filter membrane A second transmitted laser light is formed and received by the second laser detector, and part of it is reflected by the filter film to form a second reflected laser light and received by the first laser detector.
  • a second laser emitter disposed on the front side of the filter membrane, and part of the laser light emitted by the second laser emitter towards the filter membrane passes through the filter membrane A second transmitted laser light is formed and received by the second laser detector, and part of it is reflected by the filter film to form a second reflected laser light and received by the first laser detector.
  • the laser modulation frequencies of the first laser transmitter and the second laser transmitter are different, and both the first laser detector and the second laser detector are equipped with a frequency demodulation module and can pass through the The above-mentioned frequency demodulation module distinguishes and measures lasers with different modulation frequencies.
  • the laser detection device further includes a first beam splitter arranged at the front end of the first laser emitter and a second beam splitter arranged at the front end of the second laser emitter, the first beam splitter and the The second beam splitters are all inclined relative to the surface of the filter membrane; the light emitting direction of one of the laser emitters in the first laser emitter and the second laser emitter is towards the filter membrane, and the emitted At least part of the laser light passes through the beam splitter at its front end and illuminates the filter film; the light output direction of another laser emitter staggers the filter film, and at least part of the laser light emitted is reflected by the beam splitter at its front end and then shines on the filter film.
  • the filter membrane is arranged at the front end of the first laser emitter and a second beam splitter arranged at the front end of the second laser emitter, the first beam splitter and the The second beam splitters are all inclined relative to the surface of the filter membrane; the light emitting direction of one of the laser emitters in the first laser emit
  • the laser detection device also includes a first spectroscopic sheet arranged at the front end of the first laser emitter, the first spectroscopic sheet is inclined relative to the surface of the filter membrane, and the output light of the first laser emitter direction towards the filter film, the light incident direction of the second laser detector is staggered from the filter film, and at least part of the laser light emitted by the first laser emitter passes through the first beam splitter and shines on the filter film. film, the first reflected laser light can enter the second laser detector after being reflected by the first beam splitter and changing its direction.
  • a carbon analyzer for organic carbon comprising an analysis furnace, the analysis furnace includes an analysis furnace tube and a filter membrane arranged in the analysis furnace tube, and is arranged in the analysis furnace
  • the analysis furnace heating device on the tube, the filter membrane is used to collect the particulate matter in the sample gas flowing through the analysis furnace tube
  • the organic carbon element carbon analyzer also includes the above-mentioned laser detection device, and the first laser emits
  • the detector and the second laser detector are arranged at the end of the analysis furnace tube corresponding to the back of the filter membrane, and the first laser detector is arranged at the end of the analysis furnace tube corresponding to the front of the filter membrane.
  • the desorption furnace also includes a sealed cavity arranged around the outer circumference of the desorption furnace tube and enclosed with the desorption furnace tube, and the desorption furnace heating device is arranged in the sealed cavity;
  • the elemental carbon analyzer also includes an intake valve group and a first gas delivery pipeline connected to the intake valve group, the first gas delivery pipeline communicates with the sealed chamber and is used to output the intake valve group A shielding gas is introduced into the sealed cavity.
  • the organic carbon carbon analyzer also includes a power pump and a first exhaust pipeline, the first exhaust pipeline and the first gas transmission pipeline are respectively arranged on opposite sides of the sealed chamber, and the The end of the first exhaust pipe away from the sealed chamber is connected to the power pump, and the power pump is used to discharge the gas in the sealed chamber.
  • a laser detection method is also provided, and the above-mentioned laser detection device is used for detection, and the laser detection method includes the following steps:
  • S100 Use the first laser emitter to emit laser light toward the back of the filter membrane, and make the laser emitted by the first laser emitter partially pass through the filter membrane to form a first transmitted laser light, and part of it is reflected by the filter membrane to form a first laser beam.
  • the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front of the filter membrane, and the intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter membrane;
  • S200 Receive the first transmitted laser light through a first laser detector, and receive the first reflected laser light through a second laser detector;
  • the laser detection method includes the following steps:
  • S100 Use the first laser emitter to emit laser light toward the back of the filter membrane, and make the laser emitted by the first laser emitter partially pass through the filter membrane to form a first transmitted laser light, and part of it is reflected by the filter membrane to form a first laser beam.
  • the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front of the filter membrane, and the intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter membrane;
  • the laser emitter emits laser light toward the front of the filter membrane, and part of the laser light emitted by the second laser emitter passes through the filter membrane to form a second transmitted laser light, and part of it is reflected by the filter membrane to form a second reflected laser light. Both the second transmitted laser light and the second reflected laser light are affected by the intensity of the light source, the optical properties of the filter membrane and the concentration of the sample on the front of the filter membrane;
  • S200 Receive the first transmitted laser light and the second reflected laser light through the first laser detector, and receive the first reflected laser light and the second transmitted laser light through the second laser detector;
  • S300 According to the intensity change data of the first reflected laser light, eliminate the influence of the light source intensity and the change of the optical properties of the filter in the first transmitted laser light, the second transmitted laser light, and the second reflected laser light, and calculate Multiple sets of laser intensity change data that are only affected by the concentration of the sample on the front side of the filter membrane.
  • the first laser emitter since the first laser emitter is arranged on the back side of the filter membrane, part of the emitted laser light passes through the filter membrane to form the first transmitted laser light, and part of it is reflected by the filter membrane to form the first reflected laser light , according to the intensity change of the first reflected laser, the influence caused by the change of the light source intensity and the optical properties of the filter membrane in the first transmitted laser can be effectively eliminated in real time, and the laser intensity change data only affected by the sample concentration on the front of the filter membrane can be calculated. In order to accurately judge the change of the concentration of the sample on the front of the filter membrane.
  • the desorption furnace includes a sealed chamber that is arranged around the periphery of the desorption furnace tube and is isolated from the desorption furnace tube. The air is discharged, so that the sealed chamber is in an oxygen-free or low-oxygen space, and the heating device of the desorption furnace is heated in an oxygen-free or low-oxygen space, thereby preventing the heating device of the desorption furnace from being oxidized at high temperature, thereby improving the service life of the heating device of the desorption furnace .
  • the rapid cooling of the analysis furnace tube can be realized by introducing the protective gas into the sealed chamber, so that the filter membrane can quickly meet the temperature requirements of the next batch of sample detection. Improve heat dissipation efficiency, reduce noise and vibration during equipment operation, ensure operation stability, and effectively protect the heating device of the desorption furnace, which greatly prolongs the life of the heating device of the desorption furnace.
  • Fig. 1 is a schematic structural diagram of a laser detection device provided by an embodiment of the present invention
  • Fig. 2 is a schematic structural diagram of a laser detection device provided by another embodiment of the present invention.
  • Fig. 3 is the structural representation of the organic carbon element carbon analyzer provided by an embodiment of the present invention.
  • Fig. 4 is the structural representation of the organic carbon element carbon analyzer provided by another embodiment of the present invention.
  • FIG. 5 is a step diagram of a laser detection method provided by an embodiment of the present invention.
  • Fig. 6 is a step diagram of a laser detection method provided by another embodiment of the present invention.
  • Detection solenoid valve; 6 power pump; 7, exhaust solenoid valve; 71, first exhaust pipe; 72, second exhaust pipe; 8, laser detection device; 81, laser emitter; 811, first laser emitter; 812, the first Two laser emitters; 82, the first laser detector; 83, the second laser detector; 84, the first beam splitter; 85, the second beam splitter.
  • an embodiment of the present invention provides a laser detection device 8 for setting in an organic carbon elemental carbon analyzer 1000 to realize the segmentation of organic carbon and elemental carbon.
  • the laser detection device 8 includes a laser emitter 81 , a first laser detector 82 and a second laser detector 83, the laser emitter 81 is used to emit laser light toward the filter membrane 23, and part of the emitted laser light passes through the filter membrane 23 to form a transmitted laser light , part of which is reflected by the filter membrane 23 to form reflected laser light.
  • the first laser detector 82 and the second laser detector 83 are respectively arranged on opposite sides of the filter membrane 23 and are used to receive the transmitted laser light and the laser beam respectively. reflected laser light.
  • the laser emitter 81 includes a first laser emitter 811 disposed on the back side of the filter membrane 23, and part of the laser light emitted by the first laser emitter 811 towards the filter membrane 23 passes through
  • the filter film 23 forms the first transmitted laser light, and part of it is reflected by the filter film 23 to form the first reflected laser light.
  • the first laser detector 82 is arranged on the front side of the filter film 23 and is used to receive the first laser light.
  • the second laser detector 83 is arranged on the back side of the filter membrane 23 and used to receive the first reflected laser light.
  • the filter membrane 23 can trap the particulate matter in the air sample on the front of the filter membrane 23, and a small part penetrates into the shallow layer of the filter membrane 23 and In the middle, when the filter membrane 23 reaches a certain thickness, the filter membrane 23 can completely trap the particulate matter on its front side, and does not exist on the back side of the filter membrane 23 .
  • the intensity of the first transmitted laser light that penetrates to the front of the filter membrane 23 from the back side of the filter membrane 23 is affected by the intensity of the light source, the optical properties of the filter membrane and the concentration of cracked carbon/elemental carbon, and from the filter membrane 23
  • the intensity of the first reflected laser directly reflected back from the back is only affected by the intensity of the light source and the optical properties of the filter.
  • the first transmitted laser light is weakened with the increase of the concentration of elemental carbon, and in the process of the oxidation and pyrolysis of elemental carbon by the organic carbon elemental carbon analyzer 1000, with the increase of the elemental carbon concentration, the As the carbon concentration gradually decreases, the first transmitted laser light gradually increases, when the intensity of the first transmitted laser light increases to the intensity before the pyrolysis of the organic carbon (it is considered that the cracked carbon is prior to the oxidation of the elemental carbon that originally existed Decomposition), the node can be judged as the node of the initial elemental carbon concentration, that is, the elemental carbon converted from organic carbon has been completely pyrolyzed at this time, so as to realize the division of organic carbon and elemental carbon.
  • the influence produced by the change of the light source intensity and the optical properties of the filter film in the first transmitted laser light can be eliminated, so that the first transmitted laser light is only affected by cracked carbon and elemental carbon.
  • the back-reflected light is used as the reference light to track and correct the transmitted light intensity in real time, that is, the influence of the light source intensity fluctuation on the transmitted light intensity is corrected, and the influence of the optical property change caused by the temperature change of the filter film on the transmitted light intensity is also corrected. Influence, this optical path can be applied in the measurement of organic carbon and elemental carbon by thermo-optic transmission method, and realize the accurate segmentation of organic carbon and elemental carbon, thereby improving the detection accuracy of organic carbon and elemental carbon.
  • this optical path can realize the accurate determination of elemental carbon, eliminate the influence of other factors on the transmitted light intensity, and improve the accuracy of elemental carbon measurement.
  • the flow paths of gases such as samples and carrier gases are along the front side of the filter membrane 23 and permeate through the back side of the filter membrane 23, that is, the front side of the filter membrane 23 is the side for filtering and collecting particulate matter , the back side of the filter membrane 23 is the side for seeping out gas.
  • the laser detection device 8 also includes a first beam splitter 84 arranged at the front end of the first laser emitter 811, and the first beam splitter 84 is inclined at an angle of 45 degrees relative to the surface of the filter membrane 23 , the light output direction of the first laser emitter 811 is perpendicular to the surface of the filter film 23, the light input direction of the second laser detector 83 is parallel to the surface of the filter film 23, and the first laser emitter 811 At least part of the emitted laser light passes through the first beam splitter 84 and illuminates the filter film 23, and the first reflected laser light can be reflected by the first beam splitter 84 and then enter the second laser for detection The device 83 separates the emitted light and reflected light through the first beam splitter 84 .
  • the The light output direction of the first laser emitter 811 can also be set at other angles relative to the surface of the filter film 23, and it is only necessary to ensure that the light output direction of the first laser emitter 811 faces the filter film 23 to form the The first transmitted laser light and the first reflected laser light are described above. In the same way, it is enough to ensure that the light incident direction of the second laser detector 83 is staggered from the filter film 23, and the angle of inclination of the first beam splitter 84 relative to the surface of the filter film 23 follows the first reflected laser light and the filter film 23. The incident direction of the second laser detector 83 is changed, so that the first reflected laser light can enter the second laser detector 83 after being reflected by the first beam splitter 84 and changing an angle.
  • this embodiment takes the organic carbon element carbon analyzer 1000 as an example to illustrate the structure and operating principle of the laser detection device 8, but it cannot be regarded as a limitation on the scope of use of the laser detection device 8, that is,
  • the laser detection device 8 is not limited to optically correcting the concentration detection of organic carbon and elemental carbon to determine the division point of organic carbon and elemental carbon, and can also be used to detect the concentration of elemental carbon, which can also be set in other Real-time detection of other sample concentrations on the filter membrane in a type of detection device.
  • this embodiment also provides a laser detection method using the above-mentioned laser detection device 8 for detection, and the laser detection method includes the following steps:
  • Step S100 emit laser light toward the back of the filter membrane 23 through the first laser emitter 811, and make the laser emitted by the first laser emitter 811 partly pass through the front of the filter membrane 23 to form a first transmitted laser light, Part of it is reflected back by the back of the filter membrane 23 to form the first reflected laser light.
  • the intensity of the light source may fluctuate and drift during the use of the laser emitter, and the optical properties of the filter film 23 will change with the temperature of the analytical furnace 2, resulting in the first transmitted laser and the The intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter, resulting in that the intensity change data of the first transmitted laser light cannot accurately reflect the concentration conversion process of organic carbon and elemental carbon, so that organic carbon, elemental carbon
  • the segmentation point of the sample changes, and accurate segmentation cannot be performed, which affects the accurate measurement of the concentration of organic carbon and elemental carbon.
  • the first laser emitter 811 is arranged on the back side of the filter membrane 23, and the filter membrane 23 retains the particles at the front position, and the particles containing organic carbon and elemental carbon do not exist in the filter membrane 23.
  • the back of the filter membrane 23 Therefore, when the back side of the filter membrane 23 is irradiated by the first laser emitter 811, the intensity of the first transmitted laser light will be affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front side of the filter membrane, and from the The first reflected laser light reflected from the back of the filter membrane 23 is only affected by the intensity of the light source and the optical properties of the filter membrane.
  • Step S200 receiving the first transmitted laser light through the first laser detector 82 and receiving the first reflected laser light through the second laser detector 83 .
  • the light incident direction of the first laser detector 82 faces the filter film 23, the first transmitted laser light directly enters the first laser detector 82 and is detected by it, and the incident laser light of the second laser detector 83 The light direction deviates from the filter film 23 , and the first reflected laser light is reflected by the first beam splitter 84 and changes direction, then enters the second laser detector 83 and is detected by it.
  • Step S300 According to the intensity change data of the first reflected laser, eliminate the influence of the light source intensity and the change of the optical properties of the filter in the first transmitted laser, and calculate the value that is only affected by the concentration of the sample on the front side of the filter. Laser intensity variation data.
  • the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane, and the sample concentration on the front of the filter membrane, while the first reflected laser light is only affected by the intensity of the light source and the optical properties of the filter membrane, it can be determined according to the The intensity change data of the first reflected laser light is processed one-to-one with the intensity change data of the first transmitted laser light, and the influence caused by the light source intensity and the change of the optical property of the filter film in the first transmitted laser light is eliminated, so that the The first transmitted laser light is only affected by the sample concentration on the front of the filter membrane, and the change process of the sample concentration on the front of the filter membrane 23 is accurately fed back through the laser intensity change data of the first transmitted laser.
  • the concentration change process of organic carbon and elemental carbon can be accurately reflected, and then the organic carbon and elemental carbon on the filter membrane 23 can be accurately measured. Segmentation improves the detection accuracy of organic carbon and elemental carbon concentrations. That is to say, the first reflected laser (back reflected laser) received by the second laser detector is used as a reference light to track and correct the intensity of the first transmitted laser in real time, that is, the influence of the fluctuation of the light source intensity on the intensity of the first transmitted laser is corrected, and also The influence of the change of optical properties caused by the temperature change of the filter film on the intensity of the first transmitted laser is corrected.
  • This optical path can be applied to the measurement of organic carbon and elemental carbon by thermo-optic transmission method, and realize the accurate division of organic carbon and elemental carbon, thereby improving The detection accuracy of organic carbon and elemental carbon is improved.
  • the laser emitter 81 also includes a second laser emitter 812 disposed on the front side of the filter membrane 23, and the second laser emitter 812 faces the Among the laser light emitted by the filter membrane 23, part passes through the back side of the filter membrane 23 to form the second transmitted laser light and is received by the second laser detector 83, and part is directly reflected back by the front side of the filter membrane 23 to form the second transmitted laser light.
  • the laser light is reflected and received by the first laser detector 82 .
  • first laser transmitter 811 and the second laser transmitter 812 have different laser modulation frequencies
  • first laser detector 82 and the second laser detector 83 are both provided with frequency demodulation
  • the module can also distinguish and measure the lasers with different modulation frequencies through the frequency demodulation module, so that when receiving the lasers emitted by the first laser transmitter 811 and the second laser transmitter 812 at the same time, the The lasers emitted by the first laser emitter 811 and the second laser emitter 812 are distinguished, and the intensity change data of the two lasers are respectively detected.
  • the light output direction of the second laser emitter 812 is parallel to the surface of the filter film 23, and the laser detection device 8 further includes a second beam splitter 85 arranged at the front end of the second laser emitter 812, The second beam splitter 85 is also inclined at an angle of 45 degrees relative to the surface of the filter membrane 23 .
  • the laser light emitted by the second laser emitter 812 can be reflected by the second beam splitter 85 to change its direction and then illuminate the front side of the filter film 23 in a direction perpendicular to the surface of the filter film 23, and pass through the The second reflected laser light reflected by the filter membrane 23 can enter the first laser detector 82 after passing through the second beam splitter 85 .
  • the second laser emitter 812 when the second laser emitter 812 cannot emit laser light in a direction parallel to the surface of the filter membrane 23 due to the structure and position of itself or other components, the second laser emitter 812
  • the light emitting direction of 812 can also be set obliquely relative to the surface of the filter membrane 23 .
  • the angle at which the second beam splitter 84 is inclined relative to the surface of the filter membrane 23 needs to follow the direction of the second laser emitter. 811 to change the direction of light output, so that the laser light emitted by the second laser emitter 811 can be directed to the filter membrane 23 after being adjusted by the second beam splitter 84 .
  • the laser detection method specifically includes the following steps:
  • Step S100 emit laser light toward the back of the filter membrane 23 through the first laser emitter 811, and let the laser light emitted by the first laser emitter 811 partly pass through the filter membrane 23 to form a first transmitted laser light, and part of the laser light is transmitted by the filter membrane 23.
  • Film 23 reflects to form the first reflected laser light, the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front side of the filter membrane, and the intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter membrane Impact.
  • the second laser emitter 812 While the first laser emitter 811 emits laser light, the second laser emitter 812 emits laser light toward the front of the filter membrane 23, and the laser light emitted by the second laser emitter 812 partially passes through the filter membrane 23
  • the second transmitted laser light is formed, and part of it is reflected by the filter membrane to form the second reflected laser light. Both the second transmitted laser light and the second reflected laser light are affected by the intensity of the light source, the optical properties of the filter membrane, and the sample concentration on the front side of the filter membrane.
  • Step S200 receiving the first transmitted laser light and the second reflected laser light through the first laser detector 82, and receiving the first reflected laser light and the second transmitted laser light through the second laser detector 83 laser.
  • Step S300 According to the intensity change data of the first reflected laser, eliminate the influence caused by the change of the light source intensity and the optical properties of the filter in the first transmitted laser, the second transmitted laser, and the second reflected laser in real time, and calculate Multiple sets of laser intensity change data that are only affected by the concentration of the sample on the front side of the filter membrane are obtained.
  • the second transmitted laser light and the second reflected laser light formed by the second laser emitter 812 can be corrected in real time to eliminate the changes caused by the initial light source intensity and the optical properties of the filter.
  • the impact produced can realize the accurate segmentation of organic carbon and elemental carbon content of the two methods of thermo-optic transmission method and thermo-optic reflection method, and improve the detection accuracy.
  • the segmentation point of organic carbon and elemental carbon determined by the intensity change of the laser and/or the second reflected laser realizes mutual verification between multiple segmentation points, and further improves the accuracy of organic carbon and elemental carbon content segmentation through multiple verifications and data corrections This greatly reduces the error in the segmentation of organic carbon and elemental carbon concentrations.
  • the embodiment of the present invention also provides an organic carbon elemental carbon analyzer, which is used to detect the content of organic carbon and elemental carbon in the air. There is no low-temperature area between the furnaces, which effectively avoids the adsorption loss of the desorbed gas and can provide accurate air quality data.
  • the organic carbon element carbon analyzer 1000 includes an analysis furnace 2, and the analysis furnace 2 includes an analysis furnace tube 21 and an analysis furnace heating device arranged on the analysis furnace tube 21, and is fixed on the analysis furnace tube 21.
  • the filter membrane 23 in the analysis furnace tube 21 is described, and the filter membrane 23 is used to collect the particulate matter in the sample gas flowing through the analysis furnace tube 21, and the analysis furnace heating device can specifically be wound around the analysis furnace tube
  • the analysis furnace heating wire 22 on the 21 is used to heat the internal space of the analysis furnace tube 21 so that the filter membrane 23 is in a high-temperature environment, so that the organic carbon or the organic carbon in the particulate matter on the surface of the filter membrane 23 Elemental carbon is pyrolyzed out.
  • the organic carbon element carbon analyzer 1000 also includes the above-mentioned laser detection device 8, the first laser emitter 811 and the second laser detector 83 are arranged on the analysis furnace tube 21 corresponding to the filter membrane 23, the first laser detector 82 is set at the end of the analysis furnace tube 21 corresponding to the front of the filter membrane 23.
  • the intensity change data of the transmitted laser light passing through the filter membrane 23 can feed back the change process of the sample concentration on the surface of the filter membrane 23 in real time.
  • the first transmitted laser light and the first reflected laser light formed by the first laser emitter 811 are respectively received by the first laser detector 82 and the second laser detector 83, and the first reflected laser light can be passed through the
  • the intensity change data of the first transmitted laser light is used as reference data, and the influence caused by the change of the light source intensity and the optical properties of the filter film in the intensity change data of the first transmitted laser light is eliminated, so that the front side of the filter film 23 can be accurately fed back through the first transmitted laser light. Data on changes in sample concentration.
  • the second laser emitter 812 is located at one end of the analysis furnace tube 21 corresponding to the front of the filter membrane 23 and is used for Laser light is emitted toward the front of the filter membrane 23 to form the second transmitted laser light that penetrates to the back side of the filter membrane 23 and the second reflected laser light that is reflected back by the front of the filter membrane 23.
  • the intensity change is affected by the concentration of the sample on the surface of the filter membrane 23 .
  • the intensity change of the first reflected laser light the influence caused by the change of the light source intensity and the optical property of the filter film in the first transmitted laser light, the second transmitted laser light, and the second reflected laser light can be eliminated, and the calculated Multiple sets of laser intensity change data that are only affected by the concentration of the sample on the front side of the filter membrane can more accurately feed back the change data of the sample concentration on the surface of the filter membrane 23 by comparing multiple sets of data.
  • the desorption furnace 2 further includes a sealed cavity 24, the sealed cavity 24 surrounds the outer circumference of the desorption furnace tube 21 and forms a joint enclosure with the desorption furnace tube 21, that is An independent sealed space is formed on the outer periphery of the desorption furnace tube 21 , and the desorption furnace heating wire 22 is arranged in the sealed cavity 24 .
  • the organic carbon carbon analyzer 1000 also includes an inlet valve group 1 and a first gas delivery pipeline 11 connected to the inlet valve group 1, and the first gas delivery pipeline 11 is connected to the sealed chamber 24 communicates and is used to introduce the protective gas output by the intake valve group 1 into the sealed cavity 24 .
  • the organic carbon carbon analyzer 1000 also includes a power pump 6 and a first exhaust pipeline 71, one end of the first exhaust pipeline 71 is connected to the sealed chamber 24, and the other end is connected to the power pump 6, the power pump 6 is used to discharge the gas in the sealed cavity 24 along the first exhaust pipe 71.
  • the air inlet valve group 1 can enter the sealing chamber 24 along the first gas pipeline 11 at this time.
  • a protective gas which can be an oxygen-free or low-oxygen gas, so that the air in the sealed cavity 24 is discharged along the first exhaust pipe 71, so that the sealed cavity 24 is in an oxygen-free or hypoxic state.
  • Hypoxic space so that the desorption furnace heating wire 22 is heated in an oxygen-free or hypoxic space, thereby preventing the desorption furnace heating wire 22 from being oxidized at high temperature and improving the service life of the desorption furnace heating wire 22.
  • the sealed cavity 24 seals and wraps the heating wire 22 of the desorption furnace in a sealed space, which can play a role in gathering heat, which is beneficial to reduce the heat loss of the heating wire 22 of the desorption furnace, and improve heating efficiency and heat preservation. Effect.
  • the temperature of the analysis furnace tube 21 needs to be rapidly lowered before the next sample detection, so as to avoid that In the sampling stage, the residual high temperature in the analysis furnace tube 21 directly pyrolyzes the organic carbon or elemental carbon in the sample, which affects the subsequent detection results.
  • the existing organic carbon elemental carbon analyzer usually uses a cooling fan with a large air volume Blowing to cool down the temperature, the cooling effect is not good and there is a lot of noise and vibration, which cannot guarantee the stable operation of the equipment, resulting in poor user experience and a large volume of the instrument.
  • the desorption furnace 2 includes a sealed cavity 24 surrounding the outer periphery of the desorption furnace tube 21, and a protective gas (such as nitrogen) is introduced into the sealed cavity 24
  • a protective gas such as nitrogen
  • the rapid cooling of the desorption furnace tube 21 and the desorption furnace heating wire 22 can be realized inside, the temperature of the desorption furnace tube 21 can be quickly dropped from 850°C to about 400°C, and the desorption furnace tube can be 21
  • the temperature drops below 400°C air is input to the sealed chamber 24 through the air intake valve group 1 switching air path, and at the same time, the input air is quickly discharged by the power pump 6 through the first exhaust pipe 71
  • the sealed cavity 24, the power pump 6 preferably adopts a large flow air pump, and the flow rate can reach 80L/min without resistance, so that rapid ventilation can be realized in the sealed cavity 24, and the rapid circulation of air facilitates It can achieve the effect of rapid cooling.
  • oxygen-free protective gas is used for rapid cooling, which can avoid the oxidation of the heating wire 22 of the analysis furnace, and switch to the air extraction heat dissipation mode in the semi-high temperature stage to ensure that the heating wire 22 of the analysis furnace service life, while reducing the gas consumption of nitrogen and other protective gases, reducing cooling costs.
  • the volume of the organic carbon carbon analyzer 1000 is further reduced, and the noise and vibration during operation can be reduced.
  • the first exhaust pipeline 71 and the first gas delivery pipeline 11 are respectively arranged on opposite sides of the sealed chamber 24, so that the protective gas output by the first gas delivery pipeline 11 first passes through the
  • the analysis furnace heating wire 22 is discharged from the first exhaust pipe 71, that is, a gas circulation channel is naturally formed around the analysis furnace heating wire 22, so that the protective gas can surround the analysis furnace tube 21 and the analysis furnace.
  • the heating wire 22 circulates to improve the cooling effect on the desorption furnace tube 21 when the gas circulates.
  • described organic carbon element carbon analyzer 1000 also comprises the analysis pipe 3 that is connected with described analysis furnace tube 21 successively, oxidation furnace 4 and detector 5, through described analysis furnace 2 heat
  • the decomposed organic carbon and elemental carbon can enter the oxidation furnace 4 along the analysis pipeline 3 for oxidation, and finally detect the carbon dioxide concentration output by the oxidation furnace 4 through the detector 5 to calculate the organic carbon and elemental carbon specific content.
  • the analysis pipeline 3 and the analysis furnace tube 21 are coaxially arranged and communicated with each other, that is, the analysis pipeline 3 and the analysis furnace tube 21 are linear structures and are butted back and forth along the same line to form a straight line. gas flow channels.
  • the desorption pipeline 3 may also be formed by directly extending from the desorption furnace tube 21 .
  • the oxidation furnace 4 includes an oxidation furnace tube 41 sleeved on the analysis pipeline 3 and an oxidation furnace heating device arranged on the oxidation furnace tube 41.
  • the oxidation furnace heating device is specifically wound around the oxidation furnace
  • the oxidation furnace heating wire 42 on the outer periphery of the tube 41, the analysis furnace tube 41 includes a cavity with a certain thickness, so as to form a storage space on the outer circumference of the analysis pipeline 3, and the storage space is built with an oxidant (not shown in the figure, the same below). ).
  • An air inlet and an air outlet are respectively provided at the two opposite ends of the oxidation furnace tube 41, and the air inlet is provided with a communication pipe 43 communicated with the analysis pipe 3, and the air outlet is connected to the detector.
  • the oxidation furnace tube 41 has a cylindrical structure and forms an annular oxidation channel with the analysis pipe 3 .
  • the oxidation furnace tube 41 is not limited to a cylindrical structure, and the oxidation channel is not limited to a ring shape.
  • the organic carbon carbon analyzer 1000 also includes a second gas pipeline 12, an exhaust solenoid valve 7 and a second exhaust pipeline 72, one end of the second gas pipeline 12 is connected to the inlet valve Group 1 is connected, and the other end communicates with the analysis furnace tube 21 and is used to switchably introduce gases such as atmospheric samples, anaerobic carrier gas, aerobic carrier gas, and calibration gas output by the intake valve group 1 into the analysis Inside the furnace tube 21.
  • the exhaust solenoid valve 7 includes two input ends and an output end, and the two input ends are respectively connected to the first exhaust pipe 71 and the second exhaust pipe 72 in one-to-one correspondence, and the output end is connected to the second exhaust pipe 72 in a one-to-one manner.
  • the power pump 6 is connected and switchably connected to one of the two input ends. So that the power pump 6 can communicate with the first exhaust pipe 71 or communicate with the second exhaust pipe 72 under the control of the exhaust solenoid valve 7, so that one power pump 6 can
  • the gas in the sealed cavity 24 or the gas in the desorption furnace 2, desorption pipeline 3 and oxidation furnace 4 can be flexibly switched to simplify the structure and reduce the cost, and realize the function of exhausting and controlling the gas flow.
  • the specific detection process of the organic carbon element carbon analyzer 1000 includes: inputting an atmospheric sample containing particulate matter into the desorption furnace tube 21 through the inlet valve group 1 along the second gas pipeline 12, so that the sample gas The particulate matter is filtered and collected by the filter membrane 23 in the desorption furnace tube 21, and the particulate matter is attached to the surface of the filter membrane 23 at this time. Then, through the inlet valve group 1 and along the second gas pipeline 12, an oxygen-free carrier gas is input into the desorption furnace tube 21. Specifically, helium can be used as the oxygen-free carrier gas, so that the desorption furnace The gas in the tube 21 is completely replaced to form an oxygen-free environment, so that the filter membrane 23 is in an oxygen-free environment.
  • the temperature of the analysis furnace 21 is gradually raised by the heating wire 22 of the analysis furnace, so that the filter membrane 23 is in an oxygen-free environment.
  • Most of the organic carbon on the surface of the membrane 23 is released by pyrolysis (a small part of the organic carbon is converted into elemental carbon and continues to adhere to the surface of the filter membrane 23), and the resolved organic carbon gas enters the oxidation gas through the analysis pipeline 3.
  • the organic carbon gas is oxidized by the oxidation furnace 4 and converted into carbon dioxide, which can be detected by the detector 5 , to judge the organic carbon content in the sample.
  • the aerobic carrier gas is input to the analysis furnace tube 21 along the second gas pipeline 12 through the inlet valve group 1, and the aerobic carrier gas can be specifically used Helium-oxygen mixed gas to completely replace the gas in the analysis furnace tube 21 to form an aerobic environment, so that the filter membrane 23 is in an aerobic environment, and now continue to pass through the analysis furnace heating wire 22 to the described
  • the analysis furnace 21 heats up step by step, so that the elemental carbon on the surface of the filter membrane 23 is pyrolyzed and escaped, and the analyzed elemental carbon gas enters the oxidation furnace tube 41 through the analysis pipeline 3, and passes through the oxidation furnace heating wire Under the continuous heating at 42 and the chemical reaction of the oxidant, the elemental carbon gas is oxidized by the oxidation furnace 4 and converted into carbon dioxide, which can be detected by the detector 5 to determine the elemental carbon content in the sample.
  • the transmitted light (or reflected light) formed by the filter membrane 23 will be weakened when the organic carbon is carbonized.
  • the oxygen-free carrier gas is switched to an oxygen carrier gas, and the temperature rises, the elemental carbon will be oxidized and decomposed, and the light intensity of the transmitted light (or reflected light) of the laser beam will gradually increase.
  • this moment is considered as the separation point of organic carbon and elemental carbon, that is, all carbon detected before this moment is considered as organic carbon, and all carbon detected after this time is considered as elemental carbon.
  • the integrated optics method corrects for the cracked carbon (thought to have the same light absorption coefficient as the native elemental carbon) generated during the elevated temperature analysis of the organic carbon.
  • the calibration gas can also be input into the desorption furnace tube 21 through the inlet valve group 1 along the second gas pipeline 12, the The calibration gas can specifically be methane gas, which can directly pass through the filter membrane 23 into the oxidation furnace tube 41, and be detected by the detector 5 after being oxidized by the oxidation furnace 41. According to the detector 5 Compare the detection result of the calibration gas with the standard carbon content in the calibration gas, calculate the detection error of the organic carbon elemental carbon analyzer 1000, and then compare the organic carbon and elemental carbon by the detection error The test results are calibrated to obtain more accurate test data.
  • the organic carbon carbon analyzer 1000 also includes a detection solenoid valve 51 arranged between the detector 5 and the oxidation furnace tube 41, and the detection solenoid valve 51 is opened and closed to control the detection The detection time of device 5 is used to ensure the accuracy of the detection results.
  • the oxidation furnace 4 since the oxidation furnace 4 is arranged around the periphery of the analysis pipeline 3, the temperature of the oxidation furnace 4 itself realizes the heating and heat preservation effect on the analysis pipeline 3, so that the analysis furnace 2 and The overall gas path between the oxidation furnaces 4 is in a high-temperature state, avoiding the existence of low-temperature regions in the analysis pipeline 3, greatly weakening the adsorption capacity of the analysis pipeline 3 to the analysis gas, thereby reducing the loss of the sample during the transfer process. Loss, improve the accuracy of the test results.
  • this structure can also effectively reduce the distance between the oxidation furnace 4 and the analysis furnace 2, so that the overall structure of the organic carbon element carbon analyzer 1000 is more compact, which is convenient for realizing miniaturization design, and has a higher Strong, not easy to damage.
  • the air inlet is located at the end of the oxidation furnace tube 41 away from the desorption furnace 2, that is, the oxidation furnace tube 41 is connected to the end of the desorption pipeline 3 away from the desorption furnace 2, so as to avoid
  • the gas in the end of the analysis pipeline 3 far away from the analysis furnace 2 has retained samples to avoid excessive dead volume, so that the pyrolysis gas in the analysis pipeline 3 can basically be transferred to the oxidation furnace tube 41 , to ensure the accuracy of the test sample.
  • the organic carbon element carbon analyzer 1000 also includes a heat insulation layer (not shown in the figure, the same below) arranged between the analysis furnace 2 and the oxidation furnace 4, and the heat insulation layer can be made of thermal insulation cotton Made of heat insulating materials, so as to avoid the high temperature of the oxidation furnace 4 itself from affecting the temperature of the desorption furnace 2, and ensure the temperature control effect of the desorption furnace 2.
  • a heat insulation layer (not shown in the figure, the same below) arranged between the analysis furnace 2 and the oxidation furnace 4, and the heat insulation layer can be made of thermal insulation cotton Made of heat insulating materials, so as to avoid the high temperature of the oxidation furnace 4 itself from affecting the temperature of the desorption furnace 2, and ensure the temperature control effect of the desorption furnace 2.
  • the organic carbon elemental carbon analyzer 1000 provided by the embodiment of the present invention has strong stability, reliability, long service life, can realize miniaturization design, can accurately find the segmentation point of organic carbon and elemental carbon, and the detection results Accurate and reliable.

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Abstract

A laser detection apparatus (8), an organic carbon and elemental carbon analyzer (1000), and a laser detection method. The laser detection apparatus (8) comprises a first laser emitter (811), a first laser detector (82) and a second laser detector (83), wherein the first laser emitter (811) is arranged on the side of the back face of a filter membrane (23), and is used for emitting a laser towards the filter membrane (23), and part of the emitted laser passes through the filter membrane (23) to form a first transmitted laser, and the other part of the emitted laser is reflected by the filter membrane (23) to form a first reflected laser; the first laser detector (82) is used for receiving the first transmitted laser; and the second laser detector (83) is used for receiving the first reflected laser. Since the first laser emitter (811) is arranged on the side of the back face of the filter membrane (23), the effect of the first transmitted laser that is generated by the intensity of a light source and the optical properties of the filter membrane (23) can be eliminated according to the first reflected laser, and laser intensity change data which is affected by only a sample concentration on the front face of the filter membrane (23) is calculated. When the laser detection method is applied to the organic carbon and elemental carbon analyzer (1000), accurate separation of organic carbon and elemental carbon can be realized.

Description

激光检测装置、有机碳元素碳分析仪及激光检测方法Laser detection device, organic carbon carbon analyzer and laser detection method 技术领域technical field
本发明涉及空气质量检测技术领域,特别地,涉及一种激光检测装置、采用所述激光检测装置的有机碳元素碳分析仪及激光检测方法。The invention relates to the technical field of air quality detection, in particular to a laser detection device, an organic carbon carbon analyzer using the laser detection device and a laser detection method.
背景技术Background technique
近年来,随着全球社会经济的不断发展,城市规模的不断扩大,空气质量问题日益严峻,对空气颗粒物中的有机碳、元素碳含量进行检测对研究大气化学反应和污染物的源解析具有重要意义,成为当今环境监测领域的热点。In recent years, with the continuous development of the global social economy and the continuous expansion of the city scale, the air quality problem has become increasingly severe. The detection of organic carbon and elemental carbon content in air particulate matter is of great importance for the study of atmospheric chemical reactions and source apportionment of pollutants. Significance has become a hot spot in the field of environmental monitoring today.
空气颗粒物中有机碳、元素碳的测量方法包括热学法、光学法、热光法。热学法主要根据有机碳和元素碳不同的热学特性对它们进行区分,但是在升温过程中有机碳会部分裂解炭化,生成热学和光学特性类似于元素碳的物质,造成测量得到的元素碳偏高。光学法由于其原理的限制,只能用于测量元素碳。The measurement methods of organic carbon and elemental carbon in air particulate matter include thermal method, optical method and thermo-optical method. The thermal method mainly distinguishes organic carbon and elemental carbon according to their different thermal properties. However, during the heating process, organic carbon will be partially cracked and carbonized, and a substance with thermal and optical properties similar to elemental carbon will be formed, resulting in high elemental carbon measured. . Due to the limitation of its principle, the optical method can only be used to measure elemental carbon.
目前,使用最多的、公认较成熟的有机碳、元素碳分析方法是热光法,其工作原理为通过滤膜过滤采集空气中的颗粒物,然后通入无氧载气使滤膜处于无氧环境中,此时对滤膜进行逐级升温,使滤膜表面的有机碳(还有一部分被炭化形成裂解碳)热解并逸出进入氧化炉内氧化转换为二氧化碳,再向解析炉通入有氧载气使滤膜处于有氧环境中,继续对滤膜进行逐级升温,使滤膜中的元素碳热解并逸出进入氧化炉内氧化转换为二氧化碳,从而通过二氧化碳检测器检测氧化炉输出的二氧化碳浓度计算出有机碳和元素碳的含量。整个过程中,都有一束激光打在滤膜上,其透射光(或反射光)在有机碳炭化时会减弱。随着无氧载气切换成有氧载气,同时温度升高,元素碳会被氧化分解,激光束的透射光(或反射光)的光强就会逐渐增强,当恢复到最初的透射(或反射)光强时,这一时刻就认为是有机碳、元素碳的分割点,即:此时刻之前检出的碳都认为是有机碳(OC),之后检出的碳都认为是元素碳(EC)。热光法是综合光学方法对有机碳在升温分析过程中产生的裂解碳进行修正。然而,由于透射光(反射光)的光强除了受裂解碳和元素碳浓度的影响外,还会受光源强度、滤膜光学性质的影响,现有技术中,只考虑了对光源波动的影响进行修正,未考虑滤膜性状变化等其他因素对透射光(反射光)光强的影响,导致有机碳/元素碳的分割点无法精准确定。At present, the most widely used and recognized mature organic carbon and elemental carbon analysis method is the thermo-optical method. Its working principle is to collect particulate matter in the air through filter membrane filtration, and then pass through an oxygen-free carrier gas to make the filter membrane in an oxygen-free environment. At this time, the temperature of the filter membrane is raised step by step, so that the organic carbon on the surface of the filter membrane (and a part of it is carbonized to form cracked carbon) is pyrolyzed and escapes into the oxidation furnace to be oxidized and converted into carbon dioxide, and then the aerobic load is introduced into the desorption furnace. The air makes the filter membrane in an aerobic environment, and continues to raise the temperature of the filter membrane step by step, so that the elemental carbon in the filter membrane is pyrolyzed and escapes into the oxidation furnace to be oxidized and converted into carbon dioxide, so that the carbon dioxide concentration output by the oxidation furnace is detected by a carbon dioxide detector. Calculate the content of organic carbon and elemental carbon. During the whole process, there is a laser beam hitting the filter membrane, and its transmitted light (or reflected light) will be weakened when the organic carbon is carbonized. As the oxygen-free carrier gas is switched to an oxygen carrier gas, and the temperature rises, the elemental carbon will be oxidized and decomposed, and the light intensity of the transmitted light (or reflected light) of the laser beam will gradually increase. When it returns to the original transmission ( or reflected) light intensity, this moment is considered as the separation point of organic carbon and elemental carbon, that is, all carbon detected before this moment is considered as organic carbon (OC), and all carbon detected after this time is considered as elemental carbon (EC). Thermo-optic method is an integrated optical method to correct the cracked carbon generated during the analysis of organic carbon at elevated temperature. However, since the intensity of transmitted light (reflected light) is not only affected by the concentration of cracked carbon and elemental carbon, but also by the intensity of the light source and the optical properties of the filter membrane, in the prior art, only the influence on the fluctuation of the light source is considered The correction was made without considering the influence of other factors such as the change of the properties of the filter membrane on the intensity of the transmitted light (reflected light), which resulted in the inability to accurately determine the split point of organic carbon/elemental carbon.
发明内容Contents of the invention
本发明提供了一种激光检测装置、有机碳元素碳分析仪及激光检测方法,以解决有机碳/元素碳的分割点无法精准确定的技术问题。The invention provides a laser detection device, an organic carbon elemental carbon analyzer and a laser detection method to solve the technical problem that the separation point of organic carbon/elemental carbon cannot be accurately determined.
根据本发明的一个方面,提供一种激光检测装置,包括激光发射器、第一激光探测器和 第二激光探测器,所述激光发射器用于朝向滤膜发射激光,所述第一激光探测器、第二激光探测器分别用于接收穿过所述滤膜的透射激光和被所述滤膜反射的反射激光,所述激光发射器包括设于所述滤膜背面一侧的第一激光发射器,所述第一激光发射器朝向所述滤膜发射的激光中,部分穿过所述滤膜形成第一透射激光,部分被所述滤膜反射形成第一反射激光,所述第一激光探测器设于所述滤膜正面一侧并用于接收所述第一透射激光,所述第二激光探测器设于所述滤膜背面一侧并用于接收所述第一反射激光。According to one aspect of the present invention, a laser detection device is provided, including a laser emitter, a first laser detector and a second laser detector, the laser emitter is used to emit laser light toward the filter membrane, and the first laser detector , the second laser detector is respectively used to receive the transmitted laser light passing through the filter membrane and the reflected laser light reflected by the filter membrane, and the laser emitter includes a first laser emitter arranged on the back side of the filter membrane Part of the laser light emitted by the first laser transmitter toward the filter membrane passes through the filter membrane to form a first transmitted laser light, and part of it is reflected by the filter membrane to form a first reflected laser light. The detector is arranged on the front side of the filter membrane and used to receive the first transmitted laser light, and the second laser detector is arranged on the back side of the filter membrane and used to receive the first reflected laser light.
优选地,所述激光发射器还包括设于所述滤膜正面一侧的第二激光发射器,所述第二激光发射器朝向所述滤膜发射的激光中,部分穿过所述滤膜形成第二透射激光并被所述第二激光探测器接收,部分被所述滤膜反射形成第二反射激光并被所述第一激光探测器接收。Preferably, the laser emitter further includes a second laser emitter disposed on the front side of the filter membrane, and part of the laser light emitted by the second laser emitter towards the filter membrane passes through the filter membrane A second transmitted laser light is formed and received by the second laser detector, and part of it is reflected by the filter film to form a second reflected laser light and received by the first laser detector.
进一步地,所述第一激光发射器和所述第二激光发射器的激光调制频率不同,所述第一激光探测器和所述第二激光探测器均设有频率解调模块并可通过所述频率解调模块对不同调制频率的激光进行区分测量。Further, the laser modulation frequencies of the first laser transmitter and the second laser transmitter are different, and both the first laser detector and the second laser detector are equipped with a frequency demodulation module and can pass through the The above-mentioned frequency demodulation module distinguishes and measures lasers with different modulation frequencies.
进一步地,所述激光检测装置还包括设于所述第一激光发射器前端的第一分光片和设于所述第二激光发射器前端的第二分光片,所述第一分光片和所述第二分光片均相对所述滤膜表面倾斜设置;所述第一激光发射器和所述第二激光发射器中的其中一个激光发射器的出光方向朝向所述滤膜,并且发射出的至少部分激光穿过其前端的分光片照向所述滤膜;另一个激光发射器的出光方向错开所述滤膜,并且发射出的至少部分激光通过其前端的分光片反射改变方向后照向所述滤膜。Further, the laser detection device further includes a first beam splitter arranged at the front end of the first laser emitter and a second beam splitter arranged at the front end of the second laser emitter, the first beam splitter and the The second beam splitters are all inclined relative to the surface of the filter membrane; the light emitting direction of one of the laser emitters in the first laser emitter and the second laser emitter is towards the filter membrane, and the emitted At least part of the laser light passes through the beam splitter at its front end and illuminates the filter film; the light output direction of another laser emitter staggers the filter film, and at least part of the laser light emitted is reflected by the beam splitter at its front end and then shines on the filter film. The filter membrane.
进一步地,所述激光检测装置还包括设于所述第一激光发射器前端的第一分光片,所述第一分光片相对所述滤膜表面倾斜设置,所述第一激光发射器的出光方向朝向所述滤膜,所述第二激光探测器的入光方向错开所述滤膜,所述第一激光发射器发射出的至少部分激光穿过所述第一分光片照向所述滤膜,所述第一反射激光可通过所述第一分光片反射改变方向后进入所述第二激光探测器。Further, the laser detection device also includes a first spectroscopic sheet arranged at the front end of the first laser emitter, the first spectroscopic sheet is inclined relative to the surface of the filter membrane, and the output light of the first laser emitter direction towards the filter film, the light incident direction of the second laser detector is staggered from the filter film, and at least part of the laser light emitted by the first laser emitter passes through the first beam splitter and shines on the filter film. film, the first reflected laser light can enter the second laser detector after being reflected by the first beam splitter and changing its direction.
根据本发明的第二方面,还提供一种有机碳元素碳分析仪,包括解析炉,所述解析炉包括解析炉管和设于所述解析炉管内的滤膜,以及布设于所述解析炉管上的解析炉加热装置,所述滤膜用于收集流经所述解析炉管的样品气体中的颗粒物,所述有机碳元素碳分析仪还包括上述激光检测装置,所述第一激光发射器和所述第二激光探测器设于所述解析炉管对应所述滤膜背面的一端,所述第一激光探测器设于所述解析炉管对应所述滤膜正面的一端。According to the second aspect of the present invention, there is also provided a carbon analyzer for organic carbon, comprising an analysis furnace, the analysis furnace includes an analysis furnace tube and a filter membrane arranged in the analysis furnace tube, and is arranged in the analysis furnace The analysis furnace heating device on the tube, the filter membrane is used to collect the particulate matter in the sample gas flowing through the analysis furnace tube, the organic carbon element carbon analyzer also includes the above-mentioned laser detection device, and the first laser emits The detector and the second laser detector are arranged at the end of the analysis furnace tube corresponding to the back of the filter membrane, and the first laser detector is arranged at the end of the analysis furnace tube corresponding to the front of the filter membrane.
优选地,所述解析炉还包括环绕所述解析炉管的外周设置并与所述解析炉管围合形成的密封腔,所述解析炉加热装置设于所述密封腔内;所述有机碳元素碳分析仪还包括进气阀组以及与所述进气阀组连接的第一输气管道,所述第一输气管道与所述密封腔连通并用于将所述进气阀组输出的保护气体导入所述密封腔内。Preferably, the desorption furnace also includes a sealed cavity arranged around the outer circumference of the desorption furnace tube and enclosed with the desorption furnace tube, and the desorption furnace heating device is arranged in the sealed cavity; the organic carbon The elemental carbon analyzer also includes an intake valve group and a first gas delivery pipeline connected to the intake valve group, the first gas delivery pipeline communicates with the sealed chamber and is used to output the intake valve group A shielding gas is introduced into the sealed cavity.
进一步地,所述有机碳元素碳分析仪还包括动力泵和第一排气管道,所述第一排气管道和所述第一输气管道分设于所述密封腔相对的两侧,所述第一排气管道远离所述密封腔的一端与所述动力泵连接,所述动力泵用于将所述密封腔内的气体排出。Further, the organic carbon carbon analyzer also includes a power pump and a first exhaust pipeline, the first exhaust pipeline and the first gas transmission pipeline are respectively arranged on opposite sides of the sealed chamber, and the The end of the first exhaust pipe away from the sealed chamber is connected to the power pump, and the power pump is used to discharge the gas in the sealed chamber.
根据本发明的第三方面,还提供一种激光检测方法,采用上述激光检测装置进行检测, 所述激光检测方法包括以下步骤:According to a third aspect of the present invention, a laser detection method is also provided, and the above-mentioned laser detection device is used for detection, and the laser detection method includes the following steps:
S100:通过第一激光发射器朝向滤膜背面发射激光,并使所述第一激光发射器发射的激光部分穿过所述滤膜形成第一透射激光,部分被所述滤膜反射形成第一反射激光,所述第一透射激光的强度受光源强度、滤膜光学性质和滤膜正面样品浓度的影响,所述第一反射激光的强度受光源强度和滤膜光学性质的影响;S100: Use the first laser emitter to emit laser light toward the back of the filter membrane, and make the laser emitted by the first laser emitter partially pass through the filter membrane to form a first transmitted laser light, and part of it is reflected by the filter membrane to form a first laser beam. Reflecting laser light, the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front of the filter membrane, and the intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter membrane;
S200:通过第一激光探测器接收所述第一透射激光,并通过第二激光探测器接收所述第一反射激光;S200: Receive the first transmitted laser light through a first laser detector, and receive the first reflected laser light through a second laser detector;
S300:根据所述第一反射激光的强度变化数据,将所述第一透射激光中由光源强度和滤膜光学性质的变化产生的影响消除,计算得出仅受滤膜正面样品浓度影响的激光强度变化数据。S300: According to the intensity change data of the first reflected laser light, eliminate the influence of the light source intensity and the change of the optical properties of the filter film in the first transmitted laser light, and calculate the laser light only affected by the concentration of the sample on the front side of the filter film Intensity change data.
进一步地,当所述激光检测装置还包括第二激光发射器时,所述激光检测方法包括以下步骤:Further, when the laser detection device further includes a second laser emitter, the laser detection method includes the following steps:
S100:通过第一激光发射器朝向滤膜背面发射激光,并使所述第一激光发射器发射的激光部分穿过所述滤膜形成第一透射激光,部分被所述滤膜反射形成第一反射激光,所述第一透射激光的强度受光源强度、滤膜光学性质和滤膜正面样品浓度的影响,所述第一反射激光的强度受光源强度和滤膜光学性质的影响;通过第二激光发射器朝向滤膜正面发射激光,并使所述第二激光发射器发射的激光部分穿过所述滤膜形成第二透射激光,部分被所述滤膜反射形成第二反射激光,所述第二透射激光、第二反射激光均受光源强度、滤膜光学性质和滤膜正面样品浓度的影响;S100: Use the first laser emitter to emit laser light toward the back of the filter membrane, and make the laser emitted by the first laser emitter partially pass through the filter membrane to form a first transmitted laser light, and part of it is reflected by the filter membrane to form a first laser beam. Reflecting laser light, the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front of the filter membrane, and the intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter membrane; through the second The laser emitter emits laser light toward the front of the filter membrane, and part of the laser light emitted by the second laser emitter passes through the filter membrane to form a second transmitted laser light, and part of it is reflected by the filter membrane to form a second reflected laser light. Both the second transmitted laser light and the second reflected laser light are affected by the intensity of the light source, the optical properties of the filter membrane and the concentration of the sample on the front of the filter membrane;
S200:通过所述第一激光探测器接收所述第一透射激光和所述第二反射激光,并通过所述第二激光探测器接收所述第一反射激光和所述第二透射激光;S200: Receive the first transmitted laser light and the second reflected laser light through the first laser detector, and receive the first reflected laser light and the second transmitted laser light through the second laser detector;
S300:根据所述第一反射激光的强度变化数据,将所述第一透射激光、第二透射激光、第二反射激光中由光源强度和滤膜光学性质的变化产生的影响消除,计算得出多组均仅受滤膜正面样品浓度影响的激光强度变化数据。S300: According to the intensity change data of the first reflected laser light, eliminate the influence of the light source intensity and the change of the optical properties of the filter in the first transmitted laser light, the second transmitted laser light, and the second reflected laser light, and calculate Multiple sets of laser intensity change data that are only affected by the concentration of the sample on the front side of the filter membrane.
本发明具有以下有益效果:The present invention has the following beneficial effects:
1.本发明实施例提供的激光检测装置中,由于第一激光发射器设于滤膜的背面,其发射的激光部分穿过滤膜形成第一透射激光,部分被滤膜反射形成第一反射激光,根据第一反射激光的强度变化,可实时将第一透射激光中由光源强度和滤膜光学性质的变化产生的影响有效消除,计算出仅受滤膜正面样品浓度影响的激光强度变化数据,从而精准判断滤膜正面样品浓度的变化情况。1. In the laser detection device provided by the embodiment of the present invention, since the first laser emitter is arranged on the back side of the filter membrane, part of the emitted laser light passes through the filter membrane to form the first transmitted laser light, and part of it is reflected by the filter membrane to form the first reflected laser light , according to the intensity change of the first reflected laser, the influence caused by the change of the light source intensity and the optical properties of the filter membrane in the first transmitted laser can be effectively eliminated in real time, and the laser intensity change data only affected by the sample concentration on the front of the filter membrane can be calculated. In order to accurately judge the change of the concentration of the sample on the front of the filter membrane.
2.本发明实施例提供的有机碳元素碳分析仪中,解析炉包括环绕解析炉管的外周设置并相对解析炉管隔绝的密封腔,通过向密封腔通入保护气体,并将密封腔内的空气排出,使得密封腔处于无氧或低氧空间,解析炉加热装置处于无氧或低氧空间内加热,从而避免解析炉加热装置在高温下被氧化,进而提高解析炉加热装置的使用寿命。在降温阶段,通过将保护气体导入密封腔内可实现对解析炉管的快速降温,从而使滤膜能够快速满足下批次样本检测的 温度需求,相比通过散热风机进行降温的方式,有效提高散热效率,并减少设备运行时的噪音和振动,保证运行稳定性的同时,对解析炉加热装置进行有效保护,极大地延长了解析炉加热装置的寿命。2. In the organic carbon element carbon analyzer provided by the embodiment of the present invention, the desorption furnace includes a sealed chamber that is arranged around the periphery of the desorption furnace tube and is isolated from the desorption furnace tube. The air is discharged, so that the sealed chamber is in an oxygen-free or low-oxygen space, and the heating device of the desorption furnace is heated in an oxygen-free or low-oxygen space, thereby preventing the heating device of the desorption furnace from being oxidized at high temperature, thereby improving the service life of the heating device of the desorption furnace . In the cooling stage, the rapid cooling of the analysis furnace tube can be realized by introducing the protective gas into the sealed chamber, so that the filter membrane can quickly meet the temperature requirements of the next batch of sample detection. Improve heat dissipation efficiency, reduce noise and vibration during equipment operation, ensure operation stability, and effectively protect the heating device of the desorption furnace, which greatly prolongs the life of the heating device of the desorption furnace.
除了上面所描述的目的、特征和优点之外,本发明还有其它的目的、特征和优点。下面将参照图,对本发明作进一步详细的说明。In addition to the objects, features and advantages described above, the present invention has other objects, features and advantages. Hereinafter, the present invention will be described in further detail with reference to the drawings.
附图说明Description of drawings
构成本申请的一部分的附图用来提供对本发明的进一步理解,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。在附图中:The accompanying drawings constituting a part of this application are used to provide further understanding of the present invention, and the schematic embodiments and descriptions of the present invention are used to explain the present invention, and do not constitute an improper limitation of the present invention. In the attached picture:
图1为本发明一种实施例提供的激光检测装置的结构示意图;Fig. 1 is a schematic structural diagram of a laser detection device provided by an embodiment of the present invention;
图2为本发明另一实施例提供的激光检测装置的结构示意图;Fig. 2 is a schematic structural diagram of a laser detection device provided by another embodiment of the present invention;
图3为本发明一种实施例提供的有机碳元素碳分析仪的结构示意图;Fig. 3 is the structural representation of the organic carbon element carbon analyzer provided by an embodiment of the present invention;
图4为本发明另一实施例提供的有机碳元素碳分析仪的结构示意图;Fig. 4 is the structural representation of the organic carbon element carbon analyzer provided by another embodiment of the present invention;
图5为本发明一种实施例提供的激光检测方法的步骤图;5 is a step diagram of a laser detection method provided by an embodiment of the present invention;
图6为本发明另一实施例提供的激光检测方法的步骤图。Fig. 6 is a step diagram of a laser detection method provided by another embodiment of the present invention.
图例说明:illustration:
1000、有机碳元素碳分析仪;1、进气阀组;11、第一输气管道;12、第二输气管道;2、解析炉;21、解析炉管;22、解析炉加热丝;23、滤膜;24、密封腔;3、解析管道;4、氧化炉;41、氧化炉管;42、氧化炉加热丝;43、连通管道;5、检测器;51、检测电磁阀;6、动力泵;7、排气电磁阀;71、第一排气管道;72、第二排气管道;8、激光检测装置;81、激光发射器;811、第一激光发射器;812、第二激光发射器;82、第一激光探测器;83、第二激光探测器;84、第一分光片;85、第二分光片。1000. Organic carbon carbon analyzer; 1. Intake valve group; 11. First gas pipeline; 12. Second gas pipeline; 2. Desorption furnace; 21. Desorption furnace tube; 22. Desorption furnace heating wire; 23. Filter membrane; 24. Sealed cavity; 3. Analysis pipeline; 4. Oxidation furnace; 41. Oxidation furnace tube; 42. Oxidation furnace heating wire; 43. Connecting pipeline; 5. Detector; 51. Detection solenoid valve; 6 , power pump; 7, exhaust solenoid valve; 71, first exhaust pipe; 72, second exhaust pipe; 8, laser detection device; 81, laser emitter; 811, first laser emitter; 812, the first Two laser emitters; 82, the first laser detector; 83, the second laser detector; 84, the first beam splitter; 85, the second beam splitter.
具体实施方式Detailed ways
以下结合附图对本发明的实施例进行详细说明,但是本发明可以由下述所限定和覆盖的多种不同方式实施。The embodiments of the present invention will be described in detail below with reference to the accompanying drawings, but the present invention can be implemented in various ways defined and covered below.
如图1所示,本发明实施例提供一种激光检测装置8,用于设置在有机碳元素碳分析仪1000内实现有机碳、元素碳的分割,所述激光检测装置8包括激光发射器81、第一激光探测器82和第二激光探测器83,所述激光发射器81用于朝向所述滤膜23发射激光,并使其发射出的激光部分穿过所述滤膜23形成透射激光,部分被所述滤膜23反射形成反射激光,所述第一激光探测器82、第二激光探测器83分设于所述滤膜23相对的两侧并分别用于接收所述透射激光和所述反射激光。As shown in FIG. 1 , an embodiment of the present invention provides a laser detection device 8 for setting in an organic carbon elemental carbon analyzer 1000 to realize the segmentation of organic carbon and elemental carbon. The laser detection device 8 includes a laser emitter 81 , a first laser detector 82 and a second laser detector 83, the laser emitter 81 is used to emit laser light toward the filter membrane 23, and part of the emitted laser light passes through the filter membrane 23 to form a transmitted laser light , part of which is reflected by the filter membrane 23 to form reflected laser light. The first laser detector 82 and the second laser detector 83 are respectively arranged on opposite sides of the filter membrane 23 and are used to receive the transmitted laser light and the laser beam respectively. reflected laser light.
优选地,所述激光发射器81包括设于所述滤膜23背面一侧的第一激光发射器811,所述 第一激光发射器811朝向所述滤膜23发射的激光中,部分穿过所述滤膜23形成第一透射激光,部分被所述滤膜23反射形成第一反射激光,所述第一激光探测器82设于所述滤膜23正面一侧并用于接收所述第一透射激光,所述第二激光探测器83设于所述滤膜23背面一侧并用于接收所述第一反射激光。由于含有颗粒物的大气样品在穿过所述滤膜23时,所述滤膜23可将大气样品中的颗粒物截留在所述滤膜23的正面,小部分渗入所述滤膜23的浅层及中间,当所述滤膜23达到一定厚度时,所述滤膜23便能完全将颗粒物截留在其正面的位置,而不存在于所述滤膜23的背面。因此,从所述滤膜23的背面穿透至所述滤膜23正面的第一透射激光的强度受光源强度、滤膜光学性质和裂解碳/元素碳浓度的影响,而从所述滤膜23背面直接反射回来的第一反射激光的强度仅受光源强度和滤膜光学性质的影响。Preferably, the laser emitter 81 includes a first laser emitter 811 disposed on the back side of the filter membrane 23, and part of the laser light emitted by the first laser emitter 811 towards the filter membrane 23 passes through The filter film 23 forms the first transmitted laser light, and part of it is reflected by the filter film 23 to form the first reflected laser light. The first laser detector 82 is arranged on the front side of the filter film 23 and is used to receive the first laser light. To transmit laser light, the second laser detector 83 is arranged on the back side of the filter membrane 23 and used to receive the first reflected laser light. Because the air sample containing particulate matter passes through the filter membrane 23, the filter membrane 23 can trap the particulate matter in the air sample on the front of the filter membrane 23, and a small part penetrates into the shallow layer of the filter membrane 23 and In the middle, when the filter membrane 23 reaches a certain thickness, the filter membrane 23 can completely trap the particulate matter on its front side, and does not exist on the back side of the filter membrane 23 . Therefore, the intensity of the first transmitted laser light that penetrates to the front of the filter membrane 23 from the back side of the filter membrane 23 is affected by the intensity of the light source, the optical properties of the filter membrane and the concentration of cracked carbon/elemental carbon, and from the filter membrane 23 The intensity of the first reflected laser directly reflected back from the back is only affected by the intensity of the light source and the optical properties of the filter.
其次,由于在有机碳元素碳分析仪1000对有机碳无氧热解的过程中,部分有机碳会被转换成裂解碳(被认为与原本就存在的元素碳具有相同的光吸收系数)附着于所述滤膜23的表面,此时所述第一透射激光随着元素碳浓度的增加而减弱,而在所述有机碳元素碳分析仪1000对元素碳氧化热解的过程中,随着元素碳浓度的逐步降低,所述第一透射激光逐步增强,当所述第一透射激光的强度增加至所述有机碳热解之前的强度时(被认为裂解碳先于原本就存在的元素碳氧化分解),便可将该节点判断为初始元素碳浓度的节点,即此时由有机碳被转换成的元素碳已被全部热解出,从而实现对有机碳和元素碳进行分割。Secondly, during the anaerobic pyrolysis of organic carbon by the organic carbon elemental carbon analyzer 1000, part of the organic carbon will be converted into cracked carbon (which is considered to have the same light absorption coefficient as the original elemental carbon) attached to the The surface of the filter membrane 23, at this time, the first transmitted laser light is weakened with the increase of the concentration of elemental carbon, and in the process of the oxidation and pyrolysis of elemental carbon by the organic carbon elemental carbon analyzer 1000, with the increase of the elemental carbon concentration, the As the carbon concentration gradually decreases, the first transmitted laser light gradually increases, when the intensity of the first transmitted laser light increases to the intensity before the pyrolysis of the organic carbon (it is considered that the cracked carbon is prior to the oxidation of the elemental carbon that originally existed Decomposition), the node can be judged as the node of the initial elemental carbon concentration, that is, the elemental carbon converted from organic carbon has been completely pyrolyzed at this time, so as to realize the division of organic carbon and elemental carbon.
因此,根据所述第一反射激光的强度变化,便可将所述第一透射激光中由光源强度和滤膜光学性质的变化产生的影响消除,使得第一透射激光只受裂解碳和元素碳浓度的影响,以对有机碳、元素碳进行精准分割,从而实现有机碳、元素碳含量的准确测量。换言之,采用背向反射光作为参考光实时跟踪修正透射光强度,即修正了光源强度波动对透射光光强的影响,也修正了滤膜温度变化导致的光学性质的变化对透射光光强的影响,该光路可应用于热光透射法测有机碳、元素碳中,实现有机碳、元素碳的准确分割,从而提高了有机碳、元素碳的检测精度。Therefore, according to the intensity change of the first reflected laser light, the influence produced by the change of the light source intensity and the optical properties of the filter film in the first transmitted laser light can be eliminated, so that the first transmitted laser light is only affected by cracked carbon and elemental carbon. In order to accurately divide the organic carbon and elemental carbon, so as to realize the accurate measurement of organic carbon and elemental carbon content. In other words, the back-reflected light is used as the reference light to track and correct the transmitted light intensity in real time, that is, the influence of the light source intensity fluctuation on the transmitted light intensity is corrected, and the influence of the optical property change caused by the temperature change of the filter film on the transmitted light intensity is also corrected. Influence, this optical path can be applied in the measurement of organic carbon and elemental carbon by thermo-optic transmission method, and realize the accurate segmentation of organic carbon and elemental carbon, thereby improving the detection accuracy of organic carbon and elemental carbon.
另外,当使用光学法测元素碳的含量时,该光路可实现元素碳的准确测定,消除了其他因素对透射光强的影响,提高了元素碳测量的准确性。In addition, when using the optical method to measure the content of elemental carbon, this optical path can realize the accurate determination of elemental carbon, eliminate the influence of other factors on the transmitted light intensity, and improve the accuracy of elemental carbon measurement.
应当理解的是,样品、载气等气体的流通路径为沿所述滤膜23的正面渗过所述滤膜23的背面,即所述滤膜23的正面为用于过滤并收集颗粒物的一面,所述滤膜23的背面为用于渗出气体的一面。It should be understood that the flow paths of gases such as samples and carrier gases are along the front side of the filter membrane 23 and permeate through the back side of the filter membrane 23, that is, the front side of the filter membrane 23 is the side for filtering and collecting particulate matter , the back side of the filter membrane 23 is the side for seeping out gas.
进一步地,所述激光检测装置8还包括设于所述第一激光发射器811前端的第一分光片84,所述第一分光片84相对所述滤膜23表面呈45度夹角倾斜设置,所述第一激光发射器811的出光方向与所述滤膜23表面垂直,所述第二激光探测器83的入光方向与所述滤膜23表面平行,所述第一激光发射器811发射出的至少部分激光穿过所述第一分光片84照向所述滤膜23,并且所述第一反射激光可通过所述第一分光片84反射改变方向后进入所述第二激光探测器83,通过所述第一分光片84将出射光和反射光进行分离。Further, the laser detection device 8 also includes a first beam splitter 84 arranged at the front end of the first laser emitter 811, and the first beam splitter 84 is inclined at an angle of 45 degrees relative to the surface of the filter membrane 23 , the light output direction of the first laser emitter 811 is perpendicular to the surface of the filter film 23, the light input direction of the second laser detector 83 is parallel to the surface of the filter film 23, and the first laser emitter 811 At least part of the emitted laser light passes through the first beam splitter 84 and illuminates the filter film 23, and the first reflected laser light can be reflected by the first beam splitter 84 and then enter the second laser for detection The device 83 separates the emitted light and reflected light through the first beam splitter 84 .
在其他实施方式中,当受自身或其他部件的结构、位置的限制导致所述第一激光发射器811无法沿垂直于所述滤膜23表面的方向朝所述滤膜23发射激光时,所述第一激光发射器811的出光方向也可相对所述滤膜23的表面呈其他角度设置,仅需保证所述第一激光发射器 811的出光方向朝向所述滤膜23,便可形成所述第一透射激光和第一反射激光。同理,保证所述第二激光探测器83的入光方向错开所述滤膜23即可,所述第一分光片84相对所述滤膜23表面倾斜的角度跟随所述第一反射激光和所述第二激光探测器83的入光方向而变换,以使所述第一反射激光能够通过所述第一分光片84的反射改变角度后进入所述第二激光探测器83。In other embodiments, when the first laser emitter 811 cannot emit laser light toward the filter membrane 23 in a direction perpendicular to the surface of the filter membrane 23 due to the structure and position constraints of itself or other components, the The light output direction of the first laser emitter 811 can also be set at other angles relative to the surface of the filter film 23, and it is only necessary to ensure that the light output direction of the first laser emitter 811 faces the filter film 23 to form the The first transmitted laser light and the first reflected laser light are described above. In the same way, it is enough to ensure that the light incident direction of the second laser detector 83 is staggered from the filter film 23, and the angle of inclination of the first beam splitter 84 relative to the surface of the filter film 23 follows the first reflected laser light and the filter film 23. The incident direction of the second laser detector 83 is changed, so that the first reflected laser light can enter the second laser detector 83 after being reflected by the first beam splitter 84 and changing an angle.
应当理解的是,本实施例以所述有机碳元素碳分析仪1000为例说明所述激光检测装置8的结构和使用原理,但不能视为对所述激光检测装置8使用范围的限定,即所述激光检测装置8并不局限于用来对有机碳和元素碳浓度检测进行光学修正,以判断有机碳、元素碳的分割点,还可以用于检测元素碳浓度,其还可设置在其他类型的检测设备中对滤膜上的其他样品浓度进行实时检测。It should be understood that this embodiment takes the organic carbon element carbon analyzer 1000 as an example to illustrate the structure and operating principle of the laser detection device 8, but it cannot be regarded as a limitation on the scope of use of the laser detection device 8, that is, The laser detection device 8 is not limited to optically correcting the concentration detection of organic carbon and elemental carbon to determine the division point of organic carbon and elemental carbon, and can also be used to detect the concentration of elemental carbon, which can also be set in other Real-time detection of other sample concentrations on the filter membrane in a type of detection device.
请结合图5,本实施例还提供一种采用上述激光检测装置8进行检测的激光检测方法,所述激光检测方法包括以下步骤:Please refer to FIG. 5, this embodiment also provides a laser detection method using the above-mentioned laser detection device 8 for detection, and the laser detection method includes the following steps:
步骤S100:通过第一激光发射器811朝向所述滤膜23的背面发射激光,并使所述第一激光发射器811发射的激光部分穿过所述滤膜23的正面形成第一透射激光,部分被所述滤膜23的背面反射回来形成第一反射激光。Step S100: emit laser light toward the back of the filter membrane 23 through the first laser emitter 811, and make the laser emitted by the first laser emitter 811 partly pass through the front of the filter membrane 23 to form a first transmitted laser light, Part of it is reflected back by the back of the filter membrane 23 to form the first reflected laser light.
由于激光发射器在使用过程中光源强度可能发生波动、漂移,并且所述滤膜23的光学性质会随着所述解析炉2的温度变化而发生变化,导致所述第一透射激光和所述第一反射激光的强度均受光源强度和滤膜光学性质的影响,导致所述第一透射激光的强度变化数据无法精确体现出有机碳、元素碳的浓度变换过程,从而使得有机碳、元素碳的分割点发生变化,无法进行准确分割,进而影响对有机碳和元素碳浓度的准确测量。Since the intensity of the light source may fluctuate and drift during the use of the laser emitter, and the optical properties of the filter film 23 will change with the temperature of the analytical furnace 2, resulting in the first transmitted laser and the The intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter, resulting in that the intensity change data of the first transmitted laser light cannot accurately reflect the concentration conversion process of organic carbon and elemental carbon, so that organic carbon, elemental carbon The segmentation point of the sample changes, and accurate segmentation cannot be performed, which affects the accurate measurement of the concentration of organic carbon and elemental carbon.
此时将所述第一激光发射器811设于所述滤膜23背面一侧,而所述滤膜23将颗粒物截留在其正面的位置,含有机碳、元素碳的颗粒物并不存在于所述滤膜23背面。因此,通过所述第一激光发射器811朝所述滤膜23的背面照射时,其第一透射激光的强度会受光源强度、滤膜光学性质和滤膜正面样品浓度的影响,而从所述滤膜23背面反射的第一反射激光只受光源强度和滤膜光学性质的影响。At this time, the first laser emitter 811 is arranged on the back side of the filter membrane 23, and the filter membrane 23 retains the particles at the front position, and the particles containing organic carbon and elemental carbon do not exist in the filter membrane 23. The back of the filter membrane 23. Therefore, when the back side of the filter membrane 23 is irradiated by the first laser emitter 811, the intensity of the first transmitted laser light will be affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front side of the filter membrane, and from the The first reflected laser light reflected from the back of the filter membrane 23 is only affected by the intensity of the light source and the optical properties of the filter membrane.
步骤S200:通过第一激光探测器82接收所述第一透射激光,并通过第二激光探测器83接收所述第一反射激光。Step S200 : receiving the first transmitted laser light through the first laser detector 82 and receiving the first reflected laser light through the second laser detector 83 .
所述第一激光探测器82的入光方向朝向所述滤膜23,所述第一透射激光直接进入所述第一激光探测器82并被其探测,所述第二激光探测器83的入光方向错开所述滤膜23,所述第一反射激光通过所述第一分光片84反射改变方向后进入所述第二激光探测器83并被其探测。The light incident direction of the first laser detector 82 faces the filter film 23, the first transmitted laser light directly enters the first laser detector 82 and is detected by it, and the incident laser light of the second laser detector 83 The light direction deviates from the filter film 23 , and the first reflected laser light is reflected by the first beam splitter 84 and changes direction, then enters the second laser detector 83 and is detected by it.
步骤S300:根据所述第一反射激光的强度变化数据,将所述第一透射激光中由光源强度和滤膜光学性质的变化产生的影响消除,计算得出仅受滤膜正面样品浓度影响的激光强度变化数据。Step S300: According to the intensity change data of the first reflected laser, eliminate the influence of the light source intensity and the change of the optical properties of the filter in the first transmitted laser, and calculate the value that is only affected by the concentration of the sample on the front side of the filter. Laser intensity variation data.
由于所述第一透射激光的强度会受光源强度、滤膜光学性质和滤膜正面样品浓度的影响,而所述第一反射激光只受光源强度和滤膜光学性质的影响,可根据所述第一反射激光的强度 变化数据与所述第一透射激光的强度变化数据进行一对一处理,将所述第一透射激光中由光源强度和滤膜光学性质的变化产生的影响消除,使所述第一透射激光仅受滤膜正面样品浓度的影响,通过所述第一透射激光的激光强度变化数据精准反馈出所述滤膜23正面样品浓度的变化过程。因此,在所述激光检测方法应用于有机碳元素碳分析仪1000中时,能够精准体现出有机碳、元素碳的浓度变化过程,进而对所述滤膜23上的有机碳、元素碳进行精确分割,提升有机碳和元素碳浓度的检测精度。也就是说,通过第二激光探测器接收的第一反射激光(背向反射激光)作为参考光实时跟踪修正第一透射激光强度,即修正了光源强度波动对第一透射激光强度的影响,也修正了滤膜温度变化导致的光学性质的变化对第一透射激光强度的影响,该光路可应用于热光透射法测有机碳、元素碳中,实现有机碳、元素碳的准确分割,从而提高了有机碳、元素碳的检测精度。Since the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane, and the sample concentration on the front of the filter membrane, while the first reflected laser light is only affected by the intensity of the light source and the optical properties of the filter membrane, it can be determined according to the The intensity change data of the first reflected laser light is processed one-to-one with the intensity change data of the first transmitted laser light, and the influence caused by the light source intensity and the change of the optical property of the filter film in the first transmitted laser light is eliminated, so that the The first transmitted laser light is only affected by the sample concentration on the front of the filter membrane, and the change process of the sample concentration on the front of the filter membrane 23 is accurately fed back through the laser intensity change data of the first transmitted laser. Therefore, when the laser detection method is applied to the organic carbon elemental carbon analyzer 1000, the concentration change process of organic carbon and elemental carbon can be accurately reflected, and then the organic carbon and elemental carbon on the filter membrane 23 can be accurately measured. Segmentation improves the detection accuracy of organic carbon and elemental carbon concentrations. That is to say, the first reflected laser (back reflected laser) received by the second laser detector is used as a reference light to track and correct the intensity of the first transmitted laser in real time, that is, the influence of the fluctuation of the light source intensity on the intensity of the first transmitted laser is corrected, and also The influence of the change of optical properties caused by the temperature change of the filter film on the intensity of the first transmitted laser is corrected. This optical path can be applied to the measurement of organic carbon and elemental carbon by thermo-optic transmission method, and realize the accurate division of organic carbon and elemental carbon, thereby improving The detection accuracy of organic carbon and elemental carbon is improved.
如图2所示,在另一实施例中,所述激光发射器81还包括设于所述滤膜23正面一侧的第二激光发射器812,所述第二激光发射器812朝向所述滤膜23发射的激光中,部分穿过所述滤膜23的背面形成第二透射激光并被所述第二激光探测器83接收,部分被所述滤膜23的正面直接反射回来形成第二反射激光并被所述第一激光探测器82接收。As shown in FIG. 2 , in another embodiment, the laser emitter 81 also includes a second laser emitter 812 disposed on the front side of the filter membrane 23, and the second laser emitter 812 faces the Among the laser light emitted by the filter membrane 23, part passes through the back side of the filter membrane 23 to form the second transmitted laser light and is received by the second laser detector 83, and part is directly reflected back by the front side of the filter membrane 23 to form the second transmitted laser light. The laser light is reflected and received by the first laser detector 82 .
进一步地,所述第一激光发射器811和所述第二激光发射器812具有不同的激光调制频率,所述第一激光探测器82和所述第二激光探测器83均设有频率解调模块并可通过所述频率解调模块对不同调制频率的激光进行区分测量,以在同时接收到所述第一激光发射器811和所述第二激光发射器812发射出的激光时,能够将所述第一激光发射器811和所述第二激光发射器812发射出的激光区分开,分别探测两种激光的强度变化数据。Further, the first laser transmitter 811 and the second laser transmitter 812 have different laser modulation frequencies, and the first laser detector 82 and the second laser detector 83 are both provided with frequency demodulation The module can also distinguish and measure the lasers with different modulation frequencies through the frequency demodulation module, so that when receiving the lasers emitted by the first laser transmitter 811 and the second laser transmitter 812 at the same time, the The lasers emitted by the first laser emitter 811 and the second laser emitter 812 are distinguished, and the intensity change data of the two lasers are respectively detected.
更进一步地,所述第二激光发射器812的出光方向与所述滤膜23表面平行,所述激光检测装置8还包括设于所述第二激光发射器812前端的第二分光片85,所述第二分光片85同样相对所述滤膜23表面呈45度夹角倾斜设置。所述第二激光发射器812发射出的激光可通过所述第二分光片85的反射改变方向后沿垂直于所述滤膜23表面的方向照向所述滤膜23的正面,并且经所述滤膜23反射回来的第二反射激光可在穿过所述第二分光片85之后进入所述第一激光探测器82。Further, the light output direction of the second laser emitter 812 is parallel to the surface of the filter film 23, and the laser detection device 8 further includes a second beam splitter 85 arranged at the front end of the second laser emitter 812, The second beam splitter 85 is also inclined at an angle of 45 degrees relative to the surface of the filter membrane 23 . The laser light emitted by the second laser emitter 812 can be reflected by the second beam splitter 85 to change its direction and then illuminate the front side of the filter film 23 in a direction perpendicular to the surface of the filter film 23, and pass through the The second reflected laser light reflected by the filter membrane 23 can enter the first laser detector 82 after passing through the second beam splitter 85 .
在其他实施方式中,当受自身或其他部件的结构、位置的限制导致所述第二激光发射器812无法沿平行于所述滤膜23表面的方向发射激光时,所述第二激光发射器812的出光方向也可相对所述滤膜23的表面倾斜设置。对应地,在所述第二激光发射器811的出光方向错开所述滤膜23时,需将所述第二分光片84相对所述滤膜23表面倾斜的角度跟随所述第二激光发射器811的出光方向而变换,以使所述第二激光发射器811发射出的激光能够被所述第二分光片84调整方向之后照向所述滤膜23。In other embodiments, when the second laser emitter 812 cannot emit laser light in a direction parallel to the surface of the filter membrane 23 due to the structure and position of itself or other components, the second laser emitter 812 The light emitting direction of 812 can also be set obliquely relative to the surface of the filter membrane 23 . Correspondingly, when the light emitting direction of the second laser emitter 811 is staggered from the filter membrane 23, the angle at which the second beam splitter 84 is inclined relative to the surface of the filter membrane 23 needs to follow the direction of the second laser emitter. 811 to change the direction of light output, so that the laser light emitted by the second laser emitter 811 can be directed to the filter membrane 23 after being adjusted by the second beam splitter 84 .
请结合图6,当所述激光检测装置8还包括第二激光发射器812时,所述激光检测方法具体包括以下步骤:Please refer to FIG. 6, when the laser detection device 8 further includes a second laser emitter 812, the laser detection method specifically includes the following steps:
步骤S100:通过第一激光发射器811朝向滤膜23背面发射激光,并使所述第一激光发射器811发射的激光部分穿过所述滤膜23形成第一透射激光,部分被所述滤膜23反射形成第一反射激光,所述第一透射激光的强度受光源强度、滤膜光学性质和滤膜正面样品浓度的影响,所述第一反射激光的强度受光源强度和滤膜光学性质的影响。Step S100: emit laser light toward the back of the filter membrane 23 through the first laser emitter 811, and let the laser light emitted by the first laser emitter 811 partly pass through the filter membrane 23 to form a first transmitted laser light, and part of the laser light is transmitted by the filter membrane 23. Film 23 reflects to form the first reflected laser light, the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front side of the filter membrane, and the intensity of the first reflected laser light is affected by the intensity of the light source and the optical properties of the filter membrane Impact.
在所述第一激光发射器811发射激光的同时,通过第二激光发射器812朝向滤膜23正面发射激光,并使所述第二激光发射器812发射的激光部分穿过所述滤膜23形成第二透射激光,部分被所述滤膜反射形成第二反射激光,所述第二透射激光、第二反射激光均受光源强度、滤膜光学性质和滤膜正面样品浓度的影响。While the first laser emitter 811 emits laser light, the second laser emitter 812 emits laser light toward the front of the filter membrane 23, and the laser light emitted by the second laser emitter 812 partially passes through the filter membrane 23 The second transmitted laser light is formed, and part of it is reflected by the filter membrane to form the second reflected laser light. Both the second transmitted laser light and the second reflected laser light are affected by the intensity of the light source, the optical properties of the filter membrane, and the sample concentration on the front side of the filter membrane.
步骤S200:通过所述第一激光探测器82接收所述第一透射激光和所述第二反射激光,并通过所述第二激光探测器83接收所述第一反射激光和所述第二透射激光。Step S200: receiving the first transmitted laser light and the second reflected laser light through the first laser detector 82, and receiving the first reflected laser light and the second transmitted laser light through the second laser detector 83 laser.
步骤S300:根据所述第一反射激光的强度变化数据,实时将所述第一透射激光、第二透射激光、第二反射激光中由光源强度和滤膜光学性质的变化产生的影响消除,计算得出多组均仅受滤膜正面样品浓度影响的激光强度变化数据。Step S300: According to the intensity change data of the first reflected laser, eliminate the influence caused by the change of the light source intensity and the optical properties of the filter in the first transmitted laser, the second transmitted laser, and the second reflected laser in real time, and calculate Multiple sets of laser intensity change data that are only affected by the concentration of the sample on the front side of the filter membrane are obtained.
首先,根据所述第一反射激光的强度变化,可对所述第二激光发射器812形成的第二透射激光和第二反射激光进行实时修正,消除由初始光源强度和滤膜光学性质的变化产生的影响,实现热光透射法和热光反射法两种方法的有机碳和元素碳含量的准确分割,提高检测精度。其次,也能根据所述第一激光发射器811穿过滤膜后形成的第一透射激光强度变化所确定的有机碳、元素碳的分割点结合所述第二激光发射器812形成的第二透射激光和/或第二反射激光强度变化所确定的有机碳、元素碳的分割点,实现多个分割点之间相互佐证,通过多重验证及修正数据,进一步提高有机碳、元素碳含量分割的准确性,极大地降低了有机碳和元素碳浓度分割的误差。Firstly, according to the change in the intensity of the first reflected laser light, the second transmitted laser light and the second reflected laser light formed by the second laser emitter 812 can be corrected in real time to eliminate the changes caused by the initial light source intensity and the optical properties of the filter. The impact produced can realize the accurate segmentation of organic carbon and elemental carbon content of the two methods of thermo-optic transmission method and thermo-optic reflection method, and improve the detection accuracy. Secondly, the separation point of organic carbon and elemental carbon determined according to the intensity change of the first transmitted laser formed after the first laser emitter 811 passes through the filter membrane combined with the second transmitted laser formed by the second laser emitter 812 The segmentation point of organic carbon and elemental carbon determined by the intensity change of the laser and/or the second reflected laser realizes mutual verification between multiple segmentation points, and further improves the accuracy of organic carbon and elemental carbon content segmentation through multiple verifications and data corrections This greatly reduces the error in the segmentation of organic carbon and elemental carbon concentrations.
在图3和图4中示出,本发明实施例还提供一种有机碳元素碳分析仪,其用于检测空气中的有机碳及元素碳的含量,由于结构小巧紧凑且在解析炉与氧化炉之间不存在低温区域,有效避免解析气体产生吸附损耗,能够提供准确的空气质量数据。As shown in Figures 3 and 4, the embodiment of the present invention also provides an organic carbon elemental carbon analyzer, which is used to detect the content of organic carbon and elemental carbon in the air. There is no low-temperature area between the furnaces, which effectively avoids the adsorption loss of the desorbed gas and can provide accurate air quality data.
如图3所示,所述有机碳元素碳分析仪1000包括解析炉2,所述解析炉2包括解析炉管21和设于所述解析炉管21上的解析炉加热装置,以及固定于所述解析炉管21内的滤膜23,所述滤膜23用于收集流经所述解析炉管21的样品气体中的颗粒物,所述解析炉加热装置具体可为缠绕于所述解析炉管21上的解析炉加热丝22,其用于对所述解析炉管21的内部空间加热以使所述滤膜23处于高温环境中,从而将所述滤膜23表面的颗粒物中的有机碳或者元素碳热解出来。As shown in Figure 3, the organic carbon element carbon analyzer 1000 includes an analysis furnace 2, and the analysis furnace 2 includes an analysis furnace tube 21 and an analysis furnace heating device arranged on the analysis furnace tube 21, and is fixed on the analysis furnace tube 21. The filter membrane 23 in the analysis furnace tube 21 is described, and the filter membrane 23 is used to collect the particulate matter in the sample gas flowing through the analysis furnace tube 21, and the analysis furnace heating device can specifically be wound around the analysis furnace tube The analysis furnace heating wire 22 on the 21 is used to heat the internal space of the analysis furnace tube 21 so that the filter membrane 23 is in a high-temperature environment, so that the organic carbon or the organic carbon in the particulate matter on the surface of the filter membrane 23 Elemental carbon is pyrolyzed out.
优选地,所述有机碳元素碳分析仪1000还包括上述激光检测装置8,所述第一激光发射器811和所述第二激光探测器83设于所述解析炉管21对应所述滤膜23背面的一端,所述第一激光探测器82设于所述解析炉管21对应所述滤膜23正面的一端。Preferably, the organic carbon element carbon analyzer 1000 also includes the above-mentioned laser detection device 8, the first laser emitter 811 and the second laser detector 83 are arranged on the analysis furnace tube 21 corresponding to the filter membrane 23, the first laser detector 82 is set at the end of the analysis furnace tube 21 corresponding to the front of the filter membrane 23.
由于所述解析炉2在对所述滤膜23表面颗粒物进行热解的过程中,穿过所述滤膜23的透射激光强度变化数据可实时反馈出所述滤膜23表面样品浓度的变化过程,此时通过所述第一激光探测器82和第二激光探测器83分别接收所述第一激光发射器811形成的第一透射激光和第一反射激光,便可通过所述第一反射激光的强度变化数据作为参考数据,将所述第一透射激光的强度变化数据中由光源强度和滤膜光学性质的变化产生的影响消除,以通过所述第一透射激光精准反馈出滤膜23正面样品浓度的变化数据。Since the analysis furnace 2 is in the process of pyrolyzing the particles on the surface of the filter membrane 23, the intensity change data of the transmitted laser light passing through the filter membrane 23 can feed back the change process of the sample concentration on the surface of the filter membrane 23 in real time. At this time, the first transmitted laser light and the first reflected laser light formed by the first laser emitter 811 are respectively received by the first laser detector 82 and the second laser detector 83, and the first reflected laser light can be passed through the The intensity change data of the first transmitted laser light is used as reference data, and the influence caused by the change of the light source intensity and the optical properties of the filter film in the intensity change data of the first transmitted laser light is eliminated, so that the front side of the filter film 23 can be accurately fed back through the first transmitted laser light. Data on changes in sample concentration.
如图4所示,当所述激光检测装置8还包括第二激光发射器812时,所述第二激光发射 器812设于所述解析炉管21对应所述滤膜23正面的一端并用于朝向所述滤膜23的正面发射激光,以形成穿透至所述滤膜23背面一侧的第二透射激光和被所述滤膜23正面反射回来的第二反射激光,此时由于所述第二透射激光和所述第二反射激光均直接照射于所述滤膜23表面的样品上,强度变化均受所述滤膜23表面样品浓度的影响。As shown in Figure 4, when the laser detection device 8 also includes a second laser emitter 812, the second laser emitter 812 is located at one end of the analysis furnace tube 21 corresponding to the front of the filter membrane 23 and is used for Laser light is emitted toward the front of the filter membrane 23 to form the second transmitted laser light that penetrates to the back side of the filter membrane 23 and the second reflected laser light that is reflected back by the front of the filter membrane 23. At this time, due to the Both the second transmitted laser light and the second reflected laser light are directly irradiated on the sample on the surface of the filter membrane 23 , and the intensity change is affected by the concentration of the sample on the surface of the filter membrane 23 .
因此,可根据所述第一反射激光的强度变化,将所述第一透射激光、第二透射激光、第二反射激光中由光源强度和滤膜光学性质的变化产生的影响消除,计算得出多组均仅受滤膜正面样品浓度影响的激光强度变化数据,通过多组数据对照,能够更加精确反馈出所述滤膜23表面样品浓度的变化数据。Therefore, according to the intensity change of the first reflected laser light, the influence caused by the change of the light source intensity and the optical property of the filter film in the first transmitted laser light, the second transmitted laser light, and the second reflected laser light can be eliminated, and the calculated Multiple sets of laser intensity change data that are only affected by the concentration of the sample on the front side of the filter membrane can more accurately feed back the change data of the sample concentration on the surface of the filter membrane 23 by comparing multiple sets of data.
请结合图3和图4,优选地,所述解析炉2还包括密封腔24,所述密封腔24环绕所述解析炉管21的外周并与所述解析炉管21共同围合形成,即在所述解析炉管21的外周构成一个独立的密封空间,所述解析炉加热丝22设于所述密封腔24内。Please refer to FIG. 3 and FIG. 4 , preferably, the desorption furnace 2 further includes a sealed cavity 24, the sealed cavity 24 surrounds the outer circumference of the desorption furnace tube 21 and forms a joint enclosure with the desorption furnace tube 21, that is An independent sealed space is formed on the outer periphery of the desorption furnace tube 21 , and the desorption furnace heating wire 22 is arranged in the sealed cavity 24 .
进一步地,所述有机碳元素碳分析仪1000还包括进气阀组1以及与所述进气阀组1连接的第一输气管道11,所述第一输气管道11与所述密封腔24连通并用于将所述进气阀组1输出的保护气体导入所述密封腔24内。Further, the organic carbon carbon analyzer 1000 also includes an inlet valve group 1 and a first gas delivery pipeline 11 connected to the inlet valve group 1, and the first gas delivery pipeline 11 is connected to the sealed chamber 24 communicates and is used to introduce the protective gas output by the intake valve group 1 into the sealed cavity 24 .
进一步地,所述有机碳元素碳分析仪1000还包括动力泵6和第一排气管道71,所述第一排气管道71的一端与所述密封腔24连接,另一端与所述动力泵6连接,所述动力泵6用于沿所述第一排气管道71将所述密封腔24内的气体排出。Further, the organic carbon carbon analyzer 1000 also includes a power pump 6 and a first exhaust pipeline 71, one end of the first exhaust pipeline 71 is connected to the sealed chamber 24, and the other end is connected to the power pump 6, the power pump 6 is used to discharge the gas in the sealed cavity 24 along the first exhaust pipe 71.
由于在所述解析炉管21外设置密封包裹所述解析炉加热丝22的密封腔24,此时可由所述进气阀组1沿所述第一输气管道11向所述密封腔24内充入保护气体,所述保护气体具体可为无氧或低氧气体,以将所述密封腔24内的空气沿所述第一排气管道71排出,使得所述密封腔24处于无氧或低氧空间,使所述解析炉加热丝22处于无氧或低氧空间内升温加热,从而避免所述解析炉加热丝22在高温下被氧化,提高所述解析炉加热丝22的使用寿命。此外,所述密封腔24将所述解析炉加热丝22密封包裹于一个密封空间内,能起到聚集热量的作用,有利于降低所述解析炉加热丝22的热量损耗,提高加热效率和保温效果。Since the sealing chamber 24 that seals and wraps the heating wire 22 of the desorption furnace is set outside the desorption furnace tube 21, the air inlet valve group 1 can enter the sealing chamber 24 along the first gas pipeline 11 at this time. Inflate a protective gas, which can be an oxygen-free or low-oxygen gas, so that the air in the sealed cavity 24 is discharged along the first exhaust pipe 71, so that the sealed cavity 24 is in an oxygen-free or hypoxic state. Hypoxic space, so that the desorption furnace heating wire 22 is heated in an oxygen-free or hypoxic space, thereby preventing the desorption furnace heating wire 22 from being oxidized at high temperature and improving the service life of the desorption furnace heating wire 22. In addition, the sealed cavity 24 seals and wraps the heating wire 22 of the desorption furnace in a sealed space, which can play a role in gathering heat, which is beneficial to reduce the heat loss of the heating wire 22 of the desorption furnace, and improve heating efficiency and heat preservation. Effect.
另外,由于在检测过程中,所述解析炉2在解析时的最高温度可达到850℃,因此在进行下次样品检测之前需先对所述解析炉管21进行快速降温,以避免在下次检测的采样阶段所述解析炉管21内残留的高温直接将样品中的有机碳或元素碳热解,影响后续的检测结果,对此,现有有机碳元素碳分析仪通常采用大风量的散热风机进行吹风降温,其降温效果不佳并且具备较大的噪音和振动,无法保证设备稳定运行,导致用户体验不佳,且仪器体积较大。In addition, since the maximum temperature of the analysis furnace 2 during analysis can reach 850° C. during the detection process, the temperature of the analysis furnace tube 21 needs to be rapidly lowered before the next sample detection, so as to avoid that In the sampling stage, the residual high temperature in the analysis furnace tube 21 directly pyrolyzes the organic carbon or elemental carbon in the sample, which affects the subsequent detection results. For this, the existing organic carbon elemental carbon analyzer usually uses a cooling fan with a large air volume Blowing to cool down the temperature, the cooling effect is not good and there is a lot of noise and vibration, which cannot guarantee the stable operation of the equipment, resulting in poor user experience and a large volume of the instrument.
而在本实施例提供的有机碳元素碳分析仪1000中,所述解析炉2包括环绕所述解析炉管21的外周的密封腔24,通过将保护气体(例如氮气)导入所述密封腔24内可实现对所述解析炉管21和所述解析炉加热丝22的快速降温,可将所述解析炉管21的温度从850℃快速降到400℃左右,并可在所述解析炉管21温度降到400℃以下时,通过所述进气阀组1切换气路对所述密封腔24输入空气,同时,输入的空气由所述动力泵6通过第一排气管道71快速排出所述密封腔24,所述动力泵6优选采用大流量气泵,在无阻力的情况下,流量可达80L/min,从而能够在所述密封腔24内实现快速换气,通过空气的快速流通便可达到快速降 温的效果。由此,在高温阶段采用无氧的保护气体进行快速降温,可避免所述解析炉加热丝22发生氧化,而在半高温阶段切换为抽取空气式的散热模式,保证所述解析炉加热丝22的使用寿命,同时减少了氮气等保护气体的耗气量,减少降温成本。并且,由于没有散热风机的存在,进一步缩小了所述有机碳元素碳分析仪1000的体积,并可降低运行时的噪音和振动。In the organic carbon elemental carbon analyzer 1000 provided in this embodiment, the desorption furnace 2 includes a sealed cavity 24 surrounding the outer periphery of the desorption furnace tube 21, and a protective gas (such as nitrogen) is introduced into the sealed cavity 24 The rapid cooling of the desorption furnace tube 21 and the desorption furnace heating wire 22 can be realized inside, the temperature of the desorption furnace tube 21 can be quickly dropped from 850°C to about 400°C, and the desorption furnace tube can be 21 When the temperature drops below 400°C, air is input to the sealed chamber 24 through the air intake valve group 1 switching air path, and at the same time, the input air is quickly discharged by the power pump 6 through the first exhaust pipe 71 The sealed cavity 24, the power pump 6 preferably adopts a large flow air pump, and the flow rate can reach 80L/min without resistance, so that rapid ventilation can be realized in the sealed cavity 24, and the rapid circulation of air facilitates It can achieve the effect of rapid cooling. Thus, in the high temperature stage, oxygen-free protective gas is used for rapid cooling, which can avoid the oxidation of the heating wire 22 of the analysis furnace, and switch to the air extraction heat dissipation mode in the semi-high temperature stage to ensure that the heating wire 22 of the analysis furnace service life, while reducing the gas consumption of nitrogen and other protective gases, reducing cooling costs. Moreover, since there is no cooling fan, the volume of the organic carbon carbon analyzer 1000 is further reduced, and the noise and vibration during operation can be reduced.
优选地,所述第一排气管道71和所述第一输气管道11分设于所述密封腔24相对的两侧,以使所述第一输气管道11输出的保护气体先经过所述解析炉加热丝22再由所述第一排气管道71排出,即在所述解析炉加热丝22的周边自然形成气体流通通道,使保护气体能够环绕所述解析炉管21及所述解析炉加热丝22流通,提升气体流通时对所述解析炉管21的降温效果。Preferably, the first exhaust pipeline 71 and the first gas delivery pipeline 11 are respectively arranged on opposite sides of the sealed chamber 24, so that the protective gas output by the first gas delivery pipeline 11 first passes through the The analysis furnace heating wire 22 is discharged from the first exhaust pipe 71, that is, a gas circulation channel is naturally formed around the analysis furnace heating wire 22, so that the protective gas can surround the analysis furnace tube 21 and the analysis furnace. The heating wire 22 circulates to improve the cooling effect on the desorption furnace tube 21 when the gas circulates.
在图3和图4中示出,所述有机碳元素碳分析仪1000还包括与所述解析炉管21依次连接的解析管道3、氧化炉4和检测器5,经所述解析炉2热解出的有机碳和元素碳可沿所述解析管道3进入所述氧化炉4内进行氧化,最后通过所述检测器5检测所述氧化炉4输出的二氧化碳浓度以计算出有机碳和元素碳的具体含量。Shown in Fig. 3 and Fig. 4, described organic carbon element carbon analyzer 1000 also comprises the analysis pipe 3 that is connected with described analysis furnace tube 21 successively, oxidation furnace 4 and detector 5, through described analysis furnace 2 heat The decomposed organic carbon and elemental carbon can enter the oxidation furnace 4 along the analysis pipeline 3 for oxidation, and finally detect the carbon dioxide concentration output by the oxidation furnace 4 through the detector 5 to calculate the organic carbon and elemental carbon specific content.
具体地,所述解析管道3与所述解析炉管21同轴设置并相互连通,即所述解析管道3和所述解析炉管21均为直线结构并沿同一直线前后对接,以形成一条直线的气体流通通道。在其他实施方式中,所述解析管道3也可由所述解析炉管21直接延伸形成。Specifically, the analysis pipeline 3 and the analysis furnace tube 21 are coaxially arranged and communicated with each other, that is, the analysis pipeline 3 and the analysis furnace tube 21 are linear structures and are butted back and forth along the same line to form a straight line. gas flow channels. In other embodiments, the desorption pipeline 3 may also be formed by directly extending from the desorption furnace tube 21 .
所述氧化炉4包括套设于所述解析管道3上的氧化炉管41和布设于所述氧化炉管41上的氧化炉加热装置,所述氧化炉加热装置具体为缠绕于所述氧化炉管41外周的氧化炉加热丝42,所述解析炉管41包括具有一定厚度的空腔,以在所述解析管道3的外周形成收容空间,该收容空间内置有氧化剂(图未示,下同)。在所述氧化炉管41相对的两端分别设有进气口和出气口,并且所述进气口上设有与所述解析管道3连通的连通管道43,所述出气口与所述检测器5连通。具体的,氧化炉管41呈筒状结构并与所述解析管道3形成环形氧化通道,当然,所述氧化炉管41不局限于筒状结构,所述氧化通道也不局限于环形。The oxidation furnace 4 includes an oxidation furnace tube 41 sleeved on the analysis pipeline 3 and an oxidation furnace heating device arranged on the oxidation furnace tube 41. The oxidation furnace heating device is specifically wound around the oxidation furnace The oxidation furnace heating wire 42 on the outer periphery of the tube 41, the analysis furnace tube 41 includes a cavity with a certain thickness, so as to form a storage space on the outer circumference of the analysis pipeline 3, and the storage space is built with an oxidant (not shown in the figure, the same below). ). An air inlet and an air outlet are respectively provided at the two opposite ends of the oxidation furnace tube 41, and the air inlet is provided with a communication pipe 43 communicated with the analysis pipe 3, and the air outlet is connected to the detector. 5 connected. Specifically, the oxidation furnace tube 41 has a cylindrical structure and forms an annular oxidation channel with the analysis pipe 3 . Of course, the oxidation furnace tube 41 is not limited to a cylindrical structure, and the oxidation channel is not limited to a ring shape.
进一步地,所述有机碳元素碳分析仪1000还包括第二输气管道12、排气电磁阀7和第二排气管道72,所述第二输气管道12的一端与所述进气阀组1连接,另一端与所述解析炉管21连通并用于将所述进气阀组1输出的大气样品、无氧载气、有氧载气、校准气体等气体可切换地导入所述解析炉管21内。所述排气电磁阀7包括两个输入端和一个输出端,两个所述输入端分别与所述第一排气管道71、第二排气管道72一一对应连接,所述输出端与所述动力泵6连接并可切换地与两个所述输入端中的其中一个输入端导通。以使所述动力泵6可在所述排气电磁阀7的控制下与所述第一排气管道71连通或者与所述第二排气管道72连通,从而通过一个动力泵6便能够可灵活切换地排出所述密封腔24内的气体或者排出所述解析炉2、解析管道3及氧化炉4内的气体,简化结构并降低成本,实现排气及控制气体流量的作用。Further, the organic carbon carbon analyzer 1000 also includes a second gas pipeline 12, an exhaust solenoid valve 7 and a second exhaust pipeline 72, one end of the second gas pipeline 12 is connected to the inlet valve Group 1 is connected, and the other end communicates with the analysis furnace tube 21 and is used to switchably introduce gases such as atmospheric samples, anaerobic carrier gas, aerobic carrier gas, and calibration gas output by the intake valve group 1 into the analysis Inside the furnace tube 21. The exhaust solenoid valve 7 includes two input ends and an output end, and the two input ends are respectively connected to the first exhaust pipe 71 and the second exhaust pipe 72 in one-to-one correspondence, and the output end is connected to the second exhaust pipe 72 in a one-to-one manner. The power pump 6 is connected and switchably connected to one of the two input ends. So that the power pump 6 can communicate with the first exhaust pipe 71 or communicate with the second exhaust pipe 72 under the control of the exhaust solenoid valve 7, so that one power pump 6 can The gas in the sealed cavity 24 or the gas in the desorption furnace 2, desorption pipeline 3 and oxidation furnace 4 can be flexibly switched to simplify the structure and reduce the cost, and realize the function of exhausting and controlling the gas flow.
所述有机碳元素碳分析仪1000的具体检测过程包括:通过所述进气阀组1沿所述第二输气管道12向所述解析炉管21输入含有颗粒物的大气样品,使样品气体中的颗粒物被所述解析炉管21中的滤膜23过滤并收集起来,此时颗粒物附着于所述滤膜23的表面。然后再通过所述进气阀组1沿所述第二输气管道12向所述解析炉管21内输入无氧载气,该无氧载气具体可采用氦气,以将所述解析炉管21中的气体全部置换干净形成无氧环境,使所述滤膜23 处于无氧环境中,此时通过所述解析炉加热丝22对所述解析炉21进行逐级升温,使所述滤膜23表面的大部分有机碳被热解逸出(少部分有机碳被转换成元素碳之后继续附着于所述滤膜23的表面),解析出的有机碳气体通过解析管道3进入所述氧化炉管41内,通过所述氧化炉加热丝42的持续加热并所述氧化剂的化学反应下,使有机碳气体被所述氧化炉4氧化转换为二氧化碳,从而可被所述检测器5检测出来,判断样品中的有机碳含量。当样品中的有机碳全部解析完成之后,再通过所述进气阀组1沿所述第二输气管道12向所述解析炉管21输入有氧载气,该有氧载气具体可采用氦氧混合气体,以将所述解析炉管21中的气体全部置换干净形成有氧环境,使所述滤膜23处于有氧环境中,此时继续通过所述解析炉加热丝22对所述解析炉21进行逐级升温,使所述滤膜23表面的元素碳被热解逸出,解析出的元素碳气体通过解析管道3进入所述氧化炉管41内,通过所述氧化炉加热丝42的持续加热并所述氧化剂的化学反应下,使元素碳气体被所述氧化炉4氧化转换为二氧化碳,进而可被所述检测器5检测出来,判断样品中的元素碳含量。整个过程中,都有至少一束激光打在所述滤膜23上,经所述滤膜23形成的透射光(或反射光)在有机碳炭化时会减弱。随着无氧载气切换成有氧载气,同时温度升高,元素碳会被氧化分解,激光束的透射光(或反射光)的光强就会逐渐增强,当恢复到最初的透射(或反射)光强时,这一时刻就认为是有机碳、元素碳的分割点,即:此时刻之前检出的碳都认为是有机碳,之后检出的碳都认为是元素碳。综合光学方法对有机碳在升温分析过程中产生的裂解碳(被认为与原本就存在的元素碳具有相同的光吸收系数)进行修正。The specific detection process of the organic carbon element carbon analyzer 1000 includes: inputting an atmospheric sample containing particulate matter into the desorption furnace tube 21 through the inlet valve group 1 along the second gas pipeline 12, so that the sample gas The particulate matter is filtered and collected by the filter membrane 23 in the desorption furnace tube 21, and the particulate matter is attached to the surface of the filter membrane 23 at this time. Then, through the inlet valve group 1 and along the second gas pipeline 12, an oxygen-free carrier gas is input into the desorption furnace tube 21. Specifically, helium can be used as the oxygen-free carrier gas, so that the desorption furnace The gas in the tube 21 is completely replaced to form an oxygen-free environment, so that the filter membrane 23 is in an oxygen-free environment. At this time, the temperature of the analysis furnace 21 is gradually raised by the heating wire 22 of the analysis furnace, so that the filter membrane 23 is in an oxygen-free environment. Most of the organic carbon on the surface of the membrane 23 is released by pyrolysis (a small part of the organic carbon is converted into elemental carbon and continues to adhere to the surface of the filter membrane 23), and the resolved organic carbon gas enters the oxidation gas through the analysis pipeline 3. In the furnace tube 41, through the continuous heating of the oxidation furnace heating wire 42 and the chemical reaction of the oxidant, the organic carbon gas is oxidized by the oxidation furnace 4 and converted into carbon dioxide, which can be detected by the detector 5 , to judge the organic carbon content in the sample. After all the analysis of the organic carbon in the sample is completed, the aerobic carrier gas is input to the analysis furnace tube 21 along the second gas pipeline 12 through the inlet valve group 1, and the aerobic carrier gas can be specifically used Helium-oxygen mixed gas to completely replace the gas in the analysis furnace tube 21 to form an aerobic environment, so that the filter membrane 23 is in an aerobic environment, and now continue to pass through the analysis furnace heating wire 22 to the described The analysis furnace 21 heats up step by step, so that the elemental carbon on the surface of the filter membrane 23 is pyrolyzed and escaped, and the analyzed elemental carbon gas enters the oxidation furnace tube 41 through the analysis pipeline 3, and passes through the oxidation furnace heating wire Under the continuous heating at 42 and the chemical reaction of the oxidant, the elemental carbon gas is oxidized by the oxidation furnace 4 and converted into carbon dioxide, which can be detected by the detector 5 to determine the elemental carbon content in the sample. During the whole process, there is at least one laser beam hitting the filter membrane 23, and the transmitted light (or reflected light) formed by the filter membrane 23 will be weakened when the organic carbon is carbonized. As the oxygen-free carrier gas is switched to an oxygen carrier gas, and the temperature rises, the elemental carbon will be oxidized and decomposed, and the light intensity of the transmitted light (or reflected light) of the laser beam will gradually increase. When it returns to the original transmission ( or reflected) light intensity, this moment is considered as the separation point of organic carbon and elemental carbon, that is, all carbon detected before this moment is considered as organic carbon, and all carbon detected after this time is considered as elemental carbon. The integrated optics method corrects for the cracked carbon (thought to have the same light absorption coefficient as the native elemental carbon) generated during the elevated temperature analysis of the organic carbon.
进一步地,为确保检测结果的准确性,在检测完成元素碳含量之后,还可通过所述进气阀组1沿所述第二输气管道12向所述解析炉管21输入校准气体,该校准气体具体可采用甲烷气体,其可直接穿过所述滤膜23进入所述氧化炉管41内,并经过所述氧化炉41氧化之后被所述检测器5检测出来,根据所述检测器5对校准气体的检测结果与所述校准气体中的标准碳含量进行比对,计算出所述有机碳元素碳分析仪1000的检测误差,再通过所述检测误差对所述有机碳和元素碳的检测结果进行校准,以得到更加精准的检测数据。Further, in order to ensure the accuracy of the detection results, after the detection of the elemental carbon content is completed, the calibration gas can also be input into the desorption furnace tube 21 through the inlet valve group 1 along the second gas pipeline 12, the The calibration gas can specifically be methane gas, which can directly pass through the filter membrane 23 into the oxidation furnace tube 41, and be detected by the detector 5 after being oxidized by the oxidation furnace 41. According to the detector 5 Compare the detection result of the calibration gas with the standard carbon content in the calibration gas, calculate the detection error of the organic carbon elemental carbon analyzer 1000, and then compare the organic carbon and elemental carbon by the detection error The test results are calibrated to obtain more accurate test data.
进一步地,所述有机碳元素碳分析仪1000还包括设于所述检测器5与所述氧化炉管41之间的检测电磁阀51,通过所述检测电磁阀51的开合控制所述检测器5的检测时间,以确保检测结果的准确性。Further, the organic carbon carbon analyzer 1000 also includes a detection solenoid valve 51 arranged between the detector 5 and the oxidation furnace tube 41, and the detection solenoid valve 51 is opened and closed to control the detection The detection time of device 5 is used to ensure the accuracy of the detection results.
值得注意的是,由于所述氧化炉4环绕所述解析管道3的外周设置,通过所述氧化炉4自身的温度实现对所述解析管道3的加温保温作用,使所述解析炉2与所述氧化炉4之间的整体气路都处于高温状态,避免所述解析管道3中存在低温区域,极大地削弱所述解析管道3对解析气体的吸附能力,从而减少样品在转移过程中的损耗,提高检测结果的准确性。其次,该结构还可有效缩减所述氧化炉4与所述解析炉2之间的间距,使所述有机碳元素碳分析仪1000的整体结构更加紧凑,便于实现小型化设计,并具备较高强度,不易损坏。It is worth noting that since the oxidation furnace 4 is arranged around the periphery of the analysis pipeline 3, the temperature of the oxidation furnace 4 itself realizes the heating and heat preservation effect on the analysis pipeline 3, so that the analysis furnace 2 and The overall gas path between the oxidation furnaces 4 is in a high-temperature state, avoiding the existence of low-temperature regions in the analysis pipeline 3, greatly weakening the adsorption capacity of the analysis pipeline 3 to the analysis gas, thereby reducing the loss of the sample during the transfer process. Loss, improve the accuracy of the test results. Secondly, this structure can also effectively reduce the distance between the oxidation furnace 4 and the analysis furnace 2, so that the overall structure of the organic carbon element carbon analyzer 1000 is more compact, which is convenient for realizing miniaturization design, and has a higher Strong, not easy to damage.
优选地,所述进气口设于所述氧化炉管41远离所述解析炉2的一端,即所述氧化炉管41与所述解析管道3远离所述解析炉2的一端连接,以避免所述解析管道3远离所述解析炉2的一端内的气体出现滞留样本,避免死体积过大,使所述解析管道3内的热解气体基本都能被转移至所述氧化炉管41内,确保检测样本的精准。Preferably, the air inlet is located at the end of the oxidation furnace tube 41 away from the desorption furnace 2, that is, the oxidation furnace tube 41 is connected to the end of the desorption pipeline 3 away from the desorption furnace 2, so as to avoid The gas in the end of the analysis pipeline 3 far away from the analysis furnace 2 has retained samples to avoid excessive dead volume, so that the pyrolysis gas in the analysis pipeline 3 can basically be transferred to the oxidation furnace tube 41 , to ensure the accuracy of the test sample.
进一步地,所述有机碳元素碳分析仪1000还包括设于所述解析炉2与所述氧化炉4之间的隔热层(图未示,下同),所述隔热层可由保温棉等隔热材料制成,以避免所述氧化炉4自身的高温对所述解析炉2的温度产生影响,保证所述解析炉2的控温效果。Further, the organic carbon element carbon analyzer 1000 also includes a heat insulation layer (not shown in the figure, the same below) arranged between the analysis furnace 2 and the oxidation furnace 4, and the heat insulation layer can be made of thermal insulation cotton Made of heat insulating materials, so as to avoid the high temperature of the oxidation furnace 4 itself from affecting the temperature of the desorption furnace 2, and ensure the temperature control effect of the desorption furnace 2.
综上,本发明实施例提供的有机碳元素碳分析仪1000具备较强的稳定性、可靠性,使用寿命长,可实现小型化设计,能够准确找到有机碳和元素碳的分割点,检测结果精准可靠。To sum up, the organic carbon elemental carbon analyzer 1000 provided by the embodiment of the present invention has strong stability, reliability, long service life, can realize miniaturization design, can accurately find the segmentation point of organic carbon and elemental carbon, and the detection results Accurate and reliable.
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.

Claims (10)

  1. 一种激光检测装置,包括激光发射器(81)、第一激光探测器(82)和第二激光探测器(83),所述激光发射器(81)用于朝向滤膜(23)发射激光,所述第一激光探测器(82)、第二激光探测器(83)分别用于接收穿过所述滤膜(23)的透射激光和被所述滤膜(23)反射的反射激光,其特征在于,所述激光发射器(81)包括设于所述滤膜(23)背面一侧的第一激光发射器(811),所述第一激光发射器(811)朝向所述滤膜(23)发射的激光中,部分穿过所述滤膜(23)形成第一透射激光,部分被所述滤膜(23)反射形成第一反射激光,所述第一激光探测器(82)设于所述滤膜(23)正面一侧并用于接收所述第一透射激光,所述第二激光探测器(83)设于所述滤膜(23)背面一侧并用于接收所述第一反射激光。A laser detection device, comprising a laser emitter (81), a first laser detector (82) and a second laser detector (83), the laser emitter (81) is used to emit laser light towards the filter membrane (23) , the first laser detector (82) and the second laser detector (83) are respectively used to receive the transmitted laser light passing through the filter membrane (23) and the reflected laser light reflected by the filter membrane (23), It is characterized in that the laser emitter (81) includes a first laser emitter (811) arranged on the back side of the filter membrane (23), and the first laser emitter (811) faces the filter membrane (23) Among the emitted laser light, part passes through the filter film (23) to form the first transmitted laser light, and part is reflected by the filter film (23) to form the first reflected laser light, and the first laser detector (82) It is arranged on the front side of the filter membrane (23) and is used to receive the first transmitted laser light, and the second laser detector (83) is arranged on the back side of the filter membrane (23) and is used to receive the first A reflected laser.
  2. 根据权利要求1所述的激光检测装置,其特征在于,所述激光发射器(81)还包括设于所述滤膜(23)正面一侧的第二激光发射器(812),所述第二激光发射器(812)朝向所述滤膜(23)发射的激光中,部分穿过所述滤膜(23)形成第二透射激光并被所述第二激光探测器(83)接收,部分被所述滤膜(23)反射形成第二反射激光并被所述第一激光探测器(82)接收。The laser detection device according to claim 1, characterized in that, the laser emitter (81) also includes a second laser emitter (812) arranged on the front side of the filter membrane (23), the first laser emitter (812) Among the laser light emitted by the two laser emitters (812) toward the filter membrane (23), part passes through the filter membrane (23) to form a second transmitted laser light and is received by the second laser detector (83), and part The second reflected laser light is formed by being reflected by the filter membrane (23) and received by the first laser detector (82).
  3. 根据权利要求2所述的激光检测装置,其特征在于,所述第一激光发射器(811)和所述第二激光发射器(812)的激光调制频率不同,所述第一激光探测器(82)和所述第二激光探测器(83)均设有频率解调模块并可通过所述频率解调模块对不同调制频率的激光进行区分测量。The laser detection device according to claim 2, characterized in that, the laser modulation frequencies of the first laser emitter (811) and the second laser emitter (812) are different, and the first laser detector ( 82) and the second laser detector (83) are both equipped with a frequency demodulation module, and the laser light with different modulation frequencies can be differentiated and measured through the frequency demodulation module.
  4. 根据权利要求2所述的激光检测装置,其特征在于,所述激光检测装置还包括设于所述第一激光发射器(811)前端的第一分光片(84)和设于所述第二激光发射器(812)前端的第二分光片(85),所述第一分光片(84)和所述第二分光片(85)均相对所述滤膜(23)表面倾斜设置;The laser detection device according to claim 2, characterized in that, the laser detection device further comprises a first beam splitter (84) arranged at the front end of the first laser emitter (811) and a first beam splitter (84) arranged at the second The second light splitter (85) at the front end of the laser emitter (812), the first light splitter (84) and the second light splitter (85) are all inclined relative to the surface of the filter (23);
    所述第一激光发射器(811)和所述第二激光发射器(812)中的其中一个激光发射器的出光方向朝向所述滤膜(23),并且发射出的至少部分激光穿过其前端的分光片照向所述滤膜(23);另一个激光发射器的出光方向错开所述滤膜(23),并且发射出的至少部分激光通过其前端的分光片反射改变方向后照向所述滤膜(23)。The light emitting direction of one of the first laser emitter (811) and the second laser emitter (812) is towards the filter membrane (23), and at least part of the emitted laser light passes through it The beam splitter at the front end illuminates the filter membrane (23); the light exit direction of the other laser transmitter staggers the filter membrane (23), and at least part of the laser emitted is reflected by the beam splitter at the front end and shines on the filter membrane (23). The filter membrane (23).
  5. 根据权利要求1所述的激光检测装置,其特征在于,所述激光检测装置还包括设于所述第一激光发射器(811)前端的第一分光片(84),所述第一分光片(84)相对所述滤膜(23)表面倾斜设置,所述第一激光发射器(811)的出光方向朝向所述滤膜(23),所述第二激光探测器(83)的入光方向错开所述滤膜(23),所述第一激光发射器(811)发射出的至少部分激光穿过所述第一分光片(84)照向所述滤膜(23),并且所述第一反射激光可通过所述第一分光片(84)反射改变方向后进入所述第二激光探测器(83)。The laser detection device according to claim 1, characterized in that, the laser detection device further comprises a first beam splitter (84) arranged at the front end of the first laser emitter (811), the first beam splitter (84) inclined relative to the surface of the filter (23), the light output direction of the first laser emitter (811) faces the filter (23), and the incident light of the second laser detector (83) The direction staggers the filter membrane (23), at least part of the laser light emitted by the first laser emitter (811) passes through the first beam splitter (84) and illuminates the filter membrane (23), and the The first reflected laser light can enter the second laser detector (83) after being reflected by the first beam splitter (84) and changing its direction.
  6. 一种有机碳元素碳分析仪,包括解析炉(2),所述解析炉(2)包括解析炉管(21)和设于所述解析炉管(21)内的滤膜(23),以及布设于所述解析炉管(21)上的解析炉加热装置,所述滤膜(23)用于收集流经所述解析炉管(21)的样品气体中的颗粒物,其特征在于,所述有机碳元素碳分析仪还包括如权利要求1所述的激光检测装置,所述第一激光发射器 (811)和所述第二激光探测器(83)设于所述解析炉管(21)对应所述滤膜(23)背面的一端,所述第一激光探测器(82)设于所述解析炉管(21)对应所述滤膜(23)正面的一端。A kind of organic carbon element carbon analyzer, comprises analysis furnace (2), and described analysis furnace (2) comprises analysis furnace tube (21) and is located at the filter membrane (23) in described analysis furnace tube (21), and The desorption furnace heating device arranged on the desorption furnace tube (21), the filter membrane (23) is used to collect the particulate matter in the sample gas flowing through the desorption furnace tube (21), it is characterized in that the The organic carbon element carbon analyzer also includes the laser detection device as claimed in claim 1, and the first laser emitter (811) and the second laser detector (83) are arranged on the analysis furnace tube (21) Corresponding to one end of the back of the filter membrane (23), the first laser detector (82) is arranged at one end of the analysis furnace tube (21) corresponding to the front of the filter membrane (23).
  7. 根据权利要求6所述的有机碳元素碳分析仪,其特征在于,所述解析炉(2)还包括环绕所述解析炉管(21)的外周设置并与所述解析炉管(21)围合形成的密封腔(24),所述解析炉加热装置设于所述密封腔(24)内;The organic carbon element carbon analyzer according to claim 6, characterized in that, the desorption furnace (2) also includes a set around the outer circumference of the desorption furnace tube (21) and surrounds the desorption furnace tube (21) The sealing cavity (24) that forms together, described analytical furnace heating device is arranged in the described sealing cavity (24);
    所述有机碳元素碳分析仪还包括进气阀组(1)以及与所述进气阀组(1)连接的第一输气管道(11),所述第一输气管道(11)与所述密封腔(24)连通并用于将所述进气阀组(1)输出的保护气体导入所述密封腔(24)内。The organic carbon carbon analyzer also includes an intake valve group (1) and a first gas pipeline (11) connected to the gas inlet valve group (1), and the first gas pipeline (11) is connected with the gas inlet valve group (1). The sealing cavity (24) communicates and is used for introducing the protective gas output by the intake valve group (1) into the sealing cavity (24).
  8. 根据权利要求7所述的有机碳元素碳分析仪,其特征在于,所述有机碳元素碳分析仪还包括动力泵(6)和第一排气管道(71),所述第一排气管道(71)和所述第一输气管道(11)分设于所述密封腔(24)相对的两侧,所述第一排气管道(71)远离所述密封腔(24)的一端与所述动力泵(6)连接,所述动力泵(6)用于将所述密封腔(24)内的气体排出。The organic carbon carbon analyzer according to claim 7, characterized in that, the organic carbon carbon analyzer also includes a power pump (6) and a first exhaust pipe (71), and the first exhaust pipe (71) and the first gas delivery pipeline (11) are separately located on opposite sides of the sealed cavity (24), and the end of the first exhaust pipeline (71) away from the sealed cavity (24) is connected to the sealed cavity (24). The power pump (6) is connected, and the power pump (6) is used to discharge the gas in the sealed cavity (24).
  9. 一种激光检测方法,其特征在于,采用如权利要求1所述的激光检测装置进行检测,所述激光检测方法包括以下步骤:A laser detection method, characterized in that, the laser detection device as claimed in claim 1 is used for detection, and the laser detection method comprises the following steps:
    S100:通过第一激光发射器(811)朝向滤膜(23)背面发射激光,并使所述第一激光发射器(811)发射的激光部分穿过所述滤膜(23)形成第一透射激光,部分被所述滤膜(23)反射形成第一反射激光,所述第一透射激光的强度受光源强度、滤膜光学性质和滤膜正面样品浓度的影响,所述第一反射激光的强度受光源强度和滤膜光学性质的影响;S100: Use the first laser emitter (811) to emit laser light toward the back of the filter membrane (23), and make the laser light emitted by the first laser emitter (811) partly pass through the filter membrane (23) to form a first transmission Laser light is partially reflected by the filter membrane (23) to form the first reflected laser light, the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front side of the filter membrane, the first reflected laser light The intensity is affected by the intensity of the light source and the optical properties of the filter;
    S200:通过第一激光探测器(82)接收所述第一透射激光,并通过第二激光探测器(83)接收所述第一反射激光;S200: Receive the first transmitted laser light through a first laser detector (82), and receive the first reflected laser light through a second laser detector (83);
    S300:根据所述第一反射激光的强度变化数据,将所述第一透射激光中由光源强度和滤膜光学性质的变化产生的影响消除,计算得出仅受滤膜正面样品浓度影响的激光强度变化数据。S300: According to the intensity change data of the first reflected laser light, eliminate the influence of the light source intensity and the change of the optical properties of the filter film in the first transmitted laser light, and calculate the laser light only affected by the concentration of the sample on the front side of the filter film Intensity change data.
  10. 根据权利要求9所述的激光检测方法,其特征在于,当所述激光检测装置还包括第二激光发射器时,所述激光检测方法包括以下步骤:The laser detection method according to claim 9, wherein when the laser detection device further includes a second laser emitter, the laser detection method comprises the following steps:
    S100:通过第一激光发射器(811)朝向滤膜(23)背面发射激光,并使所述第一激光发射器(811)发射的激光部分穿过所述滤膜(23)形成第一透射激光,部分被所述滤膜(23)反射形成第一反射激光,所述第一透射激光的强度受光源强度、滤膜光学性质和滤膜正面样品浓度的影响,所述第一反射激光的强度受光源强度和滤膜光学性质的影响;S100: Use the first laser emitter (811) to emit laser light toward the back of the filter membrane (23), and make the laser light emitted by the first laser emitter (811) partly pass through the filter membrane (23) to form a first transmission Laser light is partially reflected by the filter membrane (23) to form the first reflected laser light, the intensity of the first transmitted laser light is affected by the intensity of the light source, the optical properties of the filter membrane and the sample concentration on the front side of the filter membrane, the first reflected laser light The intensity is affected by the intensity of the light source and the optical properties of the filter;
    通过第二激光发射器(812)朝向滤膜(23)正面发射激光,并使所述第二激光发射器(812)发射的激光部分穿过所述滤膜(23)形成第二透射激光,部分被所述滤膜(23)反射形成第二反射激光,所述第二透射激光、第二反射激光均受光源强度、滤膜光学性质和滤膜正面样品浓度的影响;emit laser light towards the front of the filter membrane (23) through the second laser emitter (812), and make the laser light emitted by the second laser emitter (812) partly pass through the filter membrane (23) to form a second transmitted laser light, Part of it is reflected by the filter membrane (23) to form a second reflected laser, and both the second transmitted laser and the second reflected laser are affected by the intensity of the light source, the optical properties of the filter and the concentration of the sample on the front side of the filter;
    S200:通过所述第一激光探测器(82)接收所述第一透射激光和所述第二反射激光,并 通过所述第二激光探测器(83)接收所述第一反射激光和所述第二透射激光;S200: Receive the first transmitted laser light and the second reflected laser light through the first laser detector (82), and receive the first reflected laser light and the second reflected laser light through the second laser detector (83) second transmitted laser light;
    S300:根据所述第一反射激光的强度变化数据,将所述第一透射激光、第二透射激光、第二反射激光中由光源强度和滤膜光学性质的变化产生的影响消除,计算得出多组均仅受滤膜正面样品浓度影响的激光强度变化数据。S300: According to the intensity change data of the first reflected laser light, eliminate the influence of the light source intensity and the change of the optical properties of the filter in the first transmitted laser light, the second transmitted laser light, and the second reflected laser light, and calculate Multiple sets of laser intensity change data that are only affected by the concentration of the sample on the front side of the filter membrane.
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